INTERNATIONAL SERIES ON THE

STRENGTH AND FRACTURE OF MATERIALS AND STRUCTURES

Selected Titles in the Series

CARLSSON & OHLSON
Mechanical Behaviour of Materials (ICM4) (2 volumes)
KETTUNEN et al.
Strength of Metals and Alloys (ICSMA8) (3 volumes)
MILLER & SMITH
Mechanical Behaviour of Materials (ICM3) (3 volumes)
SALAMA et al.
Advances in Fracture Research (ICF7) (6 volumes)
YAN et al.
Mechanical Behaviour of Materials (ICM5) (2 volumes)

Related Titles of Interest

ASHBY & JONES
Engineering Materials 1 and 2
KELLY
Concise Encyclopedia of Composite Materials
KHAN & TOKUDA
Advances in Plasticity
TAYA & ARSENAULT
Metal Matrix Composites
THOMASON
Ductile Fracture of Metals

Pergamon Related Journals

(free sample copy gladly sent on request)
Acta Mechanica Solida Sinica
Acta Metallurgica et Materialia
Canadian Metallurgical Quarterly
Computers and Structures
Corrosion Science
Engineering Fracture Mechanics
Fatigue and Fracture of Engineering Materials and Structures
International Journal of Impact Engineering
International Journal of Plasticity
International Journal of Solids and Structures
Journal of the Mechanics and Physics of Solids
Materials Research Bulletin
Scripta Metallurgica et Materialia
Welding in the World
Mechanical Behaviour
of Materials—VI
Proceedings of the Sixth International Conference,
Kyoto, Japan, 29 July-2 August 1991

Edited by

MASAHIRO JONO TATSUO INOUE

Osaka University, Japan Kyoto University, Japan

Organized by

The Society of Materials Science, Japan

and
The Foundation for Advancement of International Science

Supported by
THE SCIENCE COUNCIL OF JAPAN

Volume 1

PERGAMON PRESS
OXFORD NEW YORK SEOUL TOKYO
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Copyright © 1992 Pergamon Press pic

All Rights Reserved. No part of this publication may be
reproduced, stored in a retrieval system or transmitted in any
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tape, mechanical, photocopying, recording or otherwise,
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First edition 1992
Library of Congress Cataloging-in-Publication Data
Mechanical behaviour of materials—VI: proceedings of the
sixth international conference, Kyoto, Japan, 29 July-
2 August 1991/edited by Masahiro Jono, Tatsuo Inoue;
organized by the Society of Materials Science, Japan, and
the Foundation for Advancement of International Science.
p. cm.—(International series on the strength and fracture of
materials and structures)
1. Materials—Mechanical properties—Congresses. I. Jono,
Masahiro, 1940- . II. Inoue, Tatsuo, 1939- . III.
International Conference on Behavior of Materials (6th: 1991:
Kyoto, Japan) IV. Nihon Zairyo Gakkai. V. Kokusai Kagaku
Shinko Zaidan (Japan) VI. Title: Mechanical behaviour of
materials—6. VII. Series.
TA405.M478 1991 620.V1—<Jc20 91—16271
British Library Cataloguing in Publication Data
Mechanical Behaviour of Materials {Conference: 6th: 1991:
Kyoto)
Mechanical Behaviour of Materials VI.
I. Title II. Jono, Masahiro III. Inoue, Tatsuo, 1939—
620.112
ISBN 0 08 037890 0

In order to make this volume available as economically

and as rapidly as possible the authors' typescripts have
been reproduced in their original form. This method has its
typographical limitations but it is hoped that they in no way
distract the reader.

Printed in Great Britain by B.P.C.C. Wheatons Ltd, Exeter

 PREFACE
The International Conference on Mechanical Behaviour of Materials, ICM, the first of
which was held in Kyoto, 1971, at the time of the twentieth anniversary of the Soc-
iety of Materials Science, Japan, was held again in Kyoto after successful Conf-
ferences in Boston, Cambridge, Stockholm and Beijing. The Sixth Conference, ICN-6,
was held as one of the activities commemorating the fortieth anniversary of the
Society of Materials Science, Japan, being coorganized by the Foundation for Adv-
ancement of International Science, and was also supported by the Science Council of
Japan.

Progress in science and technology in the field of mechanical behaviour of materials

has been significant in recent years. Technological innovation has advanced parti-
cularly in the area of advanced materials with high performance such as engineering
ceramics, composite materials, intermetallic compounds and functional materials,
advanced techniques for evaluation methods of the material properties and refined
analytical techniques achieved through research and development. The purpose of the
Conference was to provide scientists and engineers throughout the world an oppo-
tunity to review recent progress in analytical and experimental works of interest
as well as to discuss and propose solutions to future problems.

Approximately 850 delegates including 100 accompanying persons from 34 countries and
regions attended the Conference, showing a wide and even representation of research
activities in this fields from and around the world. Two distinguished scientists,
Dr. J.W. Edington, Canada, and Prof. N. Shiraishi, Japan, delivered plenary lectures
highlighting the development of light materials and frontiers of bridge const-
ruction.

The following twelve workshops were propounded by the organizers in each respective
field:
WS.l Computational Plasticity - Challenge to Hierarchical Microstructure
(H.Kitagawa and S.Shima)
WS.2 Dynamic Plasticity and Fracture (S.Tanimura and H. Homma)
WS.3 Reliability Analysis and Reliability-based Design (H. Ishikawa and A.Tsurui)
WS.4 Statistical Properties of Advanced Materials (Z.Maekawa and N.Okabe)
WS.5 Computer Assisted Fatigue Technology (M.Jono and T.Tanaka)
WS.6 Advanced Techniques in Structural Integrity Assesment (N.Kitagawa and
K.Kuwabara)
WS.7 Fatigue of Advanced and Functional Materials (Y.Murakami and H.Kishimoto)
WS.8 Localized Corrosion - Mechanisms and Advanced Evaluation Techniques
(K.Yamakawa and K.Komai)
WS.9 Interface and Processing of Fibre-reinforced Composites(T.Hirai and T.Fukuda)
WS.10 Strength and Fracture of Metal Matrix Composites (H.Fukunaga and A.Okura)
WS.ll Mechanical Properties of Intermetallic Compounds (M.Yamaguchi, M.Tokizane and
P.H.Shingu)
WS.12 Polymer Alloys - Structure and Properties (T.Masuda and T.Inoue)
v
In addition, the technical sessions for the basic probleis and applications in
progress were also organized by the Technical Subcommittee. They addressed Mecha-
nical Behaviour of Advanced Materials, Constitutive Relations and Damage Mechanics,
Fracture and Fracture Mechanics, Fatigue and Fatigue Mechanists, Creep and High
Temperature Strength and New Technology in Testing and Evaluation.

The workshops and technical sessions with 36 invited papers, 20 keynote lectures and
469 contributed papers were divided into ten parallel sessions during five day conf-
erence. About 90 papers were presented in the poster sessions which were held in
the afternoon on the second and fourth days. The participants could spend these days
with full of enthusiastic presentations and active discussions. We have experienced
a number of new findings as well as exchange of scientific information of mutual in-
terest and friendships, which are, the editors are sure, very helpful to promote the
cooperation on an international level in the field of mechanical behaviour of mate-
materials.

More than 830 abstracts were submitted for the Conference from all over the world,
which forced the Organizing and Exextive Committees to each registered participant
restrict to only one oral presentation. Papers presented in the oral sessions are
included in the Proceedings while the extended abstracts of papers presented in the
poster sessions were distributed at the Conference.

The editors would like to express their sincere gratitude to the members of the
international and domestic committees, workshop organizations and all participants as
well as staffs of JSMS for their advice, cooperation, and support to the successful
Conference, ICM-6.

September, 1991

Editors
Masahiro Jono
Tatsuo Inoue

VI
 CONFERENCE ORGANIZATION

ICM EXECUTIVE COMMITTEE AND GOVERNORS AT LARGE (1987-

1991)
President M.G. Yan (China)
Vice President J. Carlsson (Sweden), K.J. Miller (UK),
H. Miyamoto (Japan)
Member A. Argon* (USA), D. Francois* (France),
J. Hult* (Sweden), T. Inoue (Japan),
L. Maslov (USSR), W. Nix (USA),
S. Sedmak (Yugoslav]ia),> D. Taplin (Ireland),
R.O. Ritchie* (USA),
H. Jinno (Chairman of ICM-6)
Secretary X.R. Wu (China)
( * : Governors at Large)

ICM BOARD OF GOVERNORS (1987-1991)

J.C. Balthazar (Brasil), C. Bathias(France), S. Bhattacharyya(India),
H. Blumenauer (Germany), B. Boardman (USA), B. Cina (Israel),
K. Heckel (Germany), B.R. Irimescu(Rumania), P. Kettunen (Finland),
J.R. Klepaczko (France), J. Lankford (USA), V. Lupine (Italy),
A. Marques (France), L.I. Maslov (USSR), K.W. Neal (Canada),
A. Neimitz (Poland), K.J. Pascoe (UK), C. de Pater (Netherland)
W.J. Plumbridge(Australia), A. Plumtree (Canada), P.Rama Rao (India),
R.B. Scarlin (Switzerland) ,M.O. Speidel (Switzerland), R. Stickler (Austria),
S.W. Nam (Korea), S.K. Teh (Malaysia), J. Zdarek (Czechoslovakia)

INTERNATIONAL ADVISORY COMMITTEE, ICM-6

Chairman H. Miyamoto (Japan),
Member J. Altenbach (Germany), A. Bakker (Netherlands),
S.R. Bodner (Israel), K.C. Hwang (China),
J. Hult (Sweden), S.C. Kim (Korea),
A.S. Kobayashi (USA), J. Kratochvil(Czechoslovakia),
Th. Lehmann (Germany), J. Lemaitre (France),
S.S. Manson (USA), Z. Mroz (Poland),
W.J. Plumbridge (Australia), A. Plumtree (Canada),
E.G. Ponyatov sky (USSR), V. Tvergaard (Denmark),
R.B. Waterhouse (UK)

Vll
 ORGANIZING COMMITTEE, ICM-6
Chairman H. Jinno (President of JSNS),
Member T. Abe (Okayama U.), T. Hirai (Doshisha U.),
T. Inoue (Kyoto U.), K. Imamura (FAIS),
M. Jono (Osaka U.), T. Kawamoto (Nagoya U.),
H. Kitagawa (U. Tokyo*), S. Kobayashi (Kyoto U . ) ,
N. Koizumi (Osaka U.*), K. Komai (Kyoto U.),
H. Miyamoto (U. Tokyo*), H. Muguruma (Kyoto U . ) ,
H. Nakazawa (Tokyo Inst. Tech.*), Y. Nishimatsu (U. Tokyo),
H. Nisitani (Kyushu U.), K. Ohji (Osaka U.),
M. Ohnami (Ritsumeikan U.), R. Ohtani (Kyoto U . ) ,
K. Okada (Kyoto U.*), H. Okamura (U. Tokyo),
S. Okuda (Doshisha U.), M. Oyane (Kyoto U.*),
T. Saegusa (Kyoto U.), M. Sakata (Tokyo Inst. Tech.),
T. Shiire (Tokyo Inst. Tech.*), N. Soga (Kyoto U . ) ,
J. Takamura (Kyoto U.*), I. Tamura (Kyoto U.*),
T. Tanaka (Ritsumeikan U.), T. Yokobori (Tohoku U.*)
( * : Professor Emeritus)

EXECUTIVE COMMITTEE, ICM-6

Chairman H. Muguruna (Kyoto U.)

Secratary General T. Inoue (Kyoto U.)
Secretary of Technical Subcommittee N. Jono (Osaka U.)
Secretary of Finance Subcommittee R. Ohtani (Kyoto U.)
Secretary of Social Programs Subcommittee K. Konai (Kyoto U.)
Secretary of Exhibition Subcommittee Y. Miyoshi (Osaka U.)
Member T. Abe (Okayama U.), T. Hasebe* (Kyoto U.)
S. Hashimoto* (Kyoto U.), T. Hoshide* (Kyoto U.)
S. Imatani* (Kyoto Inst. Tech.), T. Kitamira* (Kyoto U.)
S. Kobayashi (Kyoto U . ) , S. Kubo* (Osaka U.)
E. Matsumoto* (Kyoto U . ) , K. Minoshiaa* (Kyoto U.)
N. Miyata* (Kyoto U . ) , M. Mizuno* (Kyoto U.)
Y. Nakai* (Osaka U.), I. Nishikawa* (Osaka U.)
S. Onaka* (Kyoto U.), T. Sakai* (Ritsumeikan U.)
M. Sakane* (Ritsumeikan u.), S. Shiaa (Kyoto U.)
P.H. Shingu (Kyoto U.), N. Soga (Kyoto U.)
A. Sugeta* (Osaka U.), T. Tamura (Kyoto U.)
K. Tanaka (Nagoya U.), T. Tanaka (Ritsumeikan U.)

VUl
 OPENING ADDRESS AT ICM-6

by

Professor Hiroshi Jinno, Chairman of the Organizing Committee

Distinguished Guest, Ladies and Gentlemen.

I regard it a great honor to have an opportunity to deliver the opening

address on behalf of the Organizing Committee of the Sixth International Con-
ference on Mechanical Behaviour of Materials.

The First Conference which was held at this Kyoto International Conference
Hall in 1971, was succeeded by four Conferences; the Second one was held at
Boston in 1976, and it was followed by the Third one in Cambridge organized
by Professor Miller, the Fourth in Stockholm by Professor Carlsson and the
Fifth in Beijing by Professor Yan. You know the First Conference, which was
successfully organized by the late Professor Shuuji Taira, marked the twen-
tieth anniversary of the establishment of The Society of Materials Science,
Japan, with eight hundred participants from eighteen countries. I suppose
some of you participated in that Conference.

This year, our Society has many programs to commemorate the Fortieth Anniver-
sary of its foundation. One of them was the Third International Conference on
Residual Stresses held in Tokushima last week. I think the present Con-
ference is the biggest event of the commemoration of the fortieth anniversary
of our Society. We are happy that our Society has been chosen to host this
Conference at the previous Conference held in Beijing. We are grateful to the
International Executive Committee for their efforts in making this conference
possible. We consider it an honor that our Japanese Society of Materials
Science has been entrusted to make all the preparations for the Conference.
As soon as it was decided, we formed an Organizing Committee and an Executive
Committee, which have worked diligently to make the present Conference a
success.

After severe discussions among scientific committees belonging to the Society

of Materials Science, Japan, topics to be presented were fixed as you see in
the circulars, and twelve Workshops were scheduled corresponding to the Scien-
tific Committees as well as the Technical Sessions.

At the beginning, we expected that the number of participants would be four

hundreds or so. However, over eight hundred absrtacts were sent to us for
screening. In view of the scheduled time allowed for presentation of papers
in the conference, we were forced to limit the number of presentation. Then,
we could not help making regulation that one attendee can orally present one
paper. Finally, six hundred papers were accepted for oral presentation, which
will be included in the Preprints and also in the Proceedings, while other
hundred papers will be presented in the Poster Sessions. Now, we have been
able to welcome a total of eight hundred and sixty registered participants
from thirty six countries including region.

IX
In the last twenty yeaars, we have vast and splendid development in the
science and technology of materials. Many kinds of new and advenced materials
came into practical uses in many fields of engineering, science, medicine, and
so forth. In particular, non-metallic materials such as oxide and non-oxide
ceramics came before the footlights as constructions materials for machinery
or even surgery, for their excellent characteristics against high-temperature
and chemical corrosion. Multiphase materials, as fiber reinforced com-
posites, and metal matrix composites came to be used for construction of
critical parts of aeronautical or astronautical equipments, because of their
light weight and high toughness.

The progress of fracture mechanics in the last two decades is also striking.
Micromechanism of the propagation of cracks in a brittle or a ductile material
came to be able to be described more and more precisely with the fracture
mechanics. The mechanism of toughening with multiphase reinforcement could be
cleared up through cooperative study of mechanical, metallurgical, and chemi-
cal researchers. I suppose that the researchers in the fields of mechanics,
physics, metallurgy, and chemistry will be supplied with many kinds of problem
to be solved from the mechanical behaviour of materials, now and in the fu-
ture.

Depending on the recent developments of computer science, computer-assisted

characterizations of materials are to be common techniques among most re-
searchers. We are able to do analyses as well as simulations of the compli-
cated mechanical behaviour of materials under various conditions with the use
of computers. I really expect you to discuss such interesting problems during
the conference and to find new directions of research in the future. We sin-
cerely hope that all who participate in this conference will report fully of
the results of their continuing research and thus contribute to the advances
in the materials science.

So many people and organizations have contributed to prepare the conference in

both international and domestic sense. I would like to express my hearty
gratitude to all of them. Especially, the members of the I CM Executive Com-
mittee and the International Advisory Committee are acknowledged for their
contribution in the international affairs. Financial support that is worth
about five hundred dollars per participants was provided by over a hundred in-
dustries with the cooperation of the Foundation for Advencement of Interna-
tional Science. Members of the Executive Committee, including young scien-
tists, and Workshop organizers as well as secretaries of the office of the
Society of Materials Science, Japan, devoted themselves in managing the tech-
nical and social programs, accommodation, financial business and all of mis-
cellaneous matters. Finally, my special and sincere gratitude is dedicated to
Profesor Inoue, Secretary General, who has diligently worked and is still
working over twelve hours every day in these years.

Thank you again for your joining us in this Sixth International Conferece on
Mechanical Behaviour of Materials, and I really wish you to have nice days in
Kyoto which is proud of its traditional arts and cultural heritage handed down
over the past twelve centuries.

Thank you very much for your kind attention.

X
 INTRODUCTORY ADDRESS AT ICM-6

by

Professor Ming-gao Yan, President of ICM(1987-1991)

After twenty years of travel around the globe, the International Con-
ference on Mechanical Behaviour of Materials is now revisiting her
birthplace, Kyoto, Japan. Coincidently, the year of 1991 is also the
40th anniversary of the Society of Materials Science, Japan. The two
big celebrations therefore make it most meaningful to hold ICM-6 here in
Kyoto, one of the most beautiful cities in Japan with splendid cultural
heritage and long history.

Since the birth of ICM twenty years ago, there has been tremendous
development in material science and technology: new materials, new test-
ing facilities, new desigh concepts have been keeping emerging at a very
fast pace. The importance of understanding the mechanical behaviour of
materials can not be overestimated because the proper use of any
material relies very heavily on how well its behaviours under actual
working conditions are understood. The central role of ICM is best
manifested by this conference, which has attracted the largest number of
scientists and researchers from all over the world in the ICM-history,
and has greatly widened the scope of ICM as compared to the preceding
five conferences.

I am very pleased, as all the delegates are, to join ICM-6 hosted by

Japan, one of the world's leading industry power where the development
in material technology is faster than in most other nations.

I would like to take this opportunity to thank our Japanese colleagues

who have made great effort in organizing such a large conference. My
special thanks goes to Professor H. Jinno, Chairman of the Organizing
Committee, Professor H. Muguruma, Chairman of the Executive Committee
and Professor T. Inoue, Secretary General and their team for excellent
work. Also I wish to thank the former ICM-Presidents, Professors J.
Carlsson, K. Miller and H. Miyamoto for there constant support of the
ICM course.

I am sure that the objectives of ICM originally set by Professor Shuji

Taira, who organized the first Conference right here in Kyoto twenty
years ago, will be best served by this conference. There is no doubt
that ICM-6 will greatly further the objectives of fostering research on
the mechanical behaviour of materials and promoting international
cooperation.

XI
 Minutes of the Meeting of the Board of Governors of ICM,

in Karasuma-Kyoto Hotel, Kyoto,

from 6:00 to 9:00 p.m., July 31, 1991.

Members Present
1 Australia Grifiths, J.R.
2 Austria Fischer, F.D.
3 Belgium Van Houtte, P.R.
4 Brazil Voorwald, H.J.C.
5 Canada Plumtree, A.; Neal, K.W.
6 China Yan, M.G.; Wu, X.R.
7 Czechoslovakia Polak, J.
8 Denmark Tvergaard, V.
9 Egypt El-Tabi El-Bassyounl
10 France Bathias, C.
11 Germany Heckel, K
12 India Rama Rao, P.
13 Ireland Taplin, D.
14 Israel Bodner, S.R.
15 Italy Lupine, V.
16 Japan Miyamoto, H.; Inoue, T.; Hoshide, T.
17 korea Nam, S,W.
18 Libya Raddad, B.S.
19 Malaysia Sahari, B.B.
20 Norway Gustafson, C.G.
21 Poland Raniecki, B.
22 Rumania Irimescu, B.R.
23 South Africa Vanzyl, F.H.
24 Sweden Carlsson, J
25 Switzerland Schindler, H.J.
26 The Netherlands Bakker, Ad
27 UK Miller, K.J.; Webster, G.A.
28 USA Ritchie, R.O.
29 USSR Pelekh, B.L.; Ponyatosky, E.G.
30 Yugoslavia Sedmak, S.

Professor M.G. Yan, the ICM President, took the chair.

1. Introduction by the President

Professor Yan, the ICM President, opened the meeting and made a brief in-
troduction.

2. Nomination of the Secretary of the Meeting

Dr. X.R. Wu was appointed the Secretary for the meeting.

3. Approval of the Minutes of the Meeting of the Board of Governors Meeting

at ICM-5 held on June 5, 19871 Bei.iing
The Minutes of the Meeting of the Board of Governors at ICM-5 in Beijing,
1987, were approved.

Xlll
4. Approval of the Agenda
The agenda for the meeting (appended to the minutes) was approved with the
addition of an announcement by Dr. Rama Rao concerning ICF-8 in Kiev, 1993.

5. Reports of the Executive Committee Meeting

Dr. X.R. Wu, Secretary of ICM, reported the Meeting of the ICM Executive
Committee held on July 30, 1991, Kyoto International Conference Hall. The
report was then agreed by the full Board of Governors.

6. Report of the Nominating Committee

Professor Mill er, Chairman of the ICM Nominating Committee, presented the
following nominations unanimously agreed by the Executive Committee.

Honorary President H. Miyamoto

President T. Inoue
Vice-President M.G. Yan
J. Carlsson
K.J. Miller
Governors at large A. Argon
D. Francois
K.C. Hwang
M. Jono
P. Rama Rao
Executive Committee K. Heckel
B.R. Irimescu
A. Plumtree
R.O. Ritchie
S. Sedmak
D. Taplin
V. Tvergaard
Chairman of ICM-7

Voting would be necessary to elect five of the seven named persons accord-
ing to the Charter of ICM. The nomination was unanimously approved.

7. Election of ICM Executive Committee

An election of the ICM Executive Committee was conducted by secrete bal-
lot. Among the seven nominated members, the following five were elected:

Heckel, K
Irimescu, B.
Plumtree, A.
Ritchie, R.O.
Tvergaard, V.

All the elected members had received more than half of the votes.

8. Presentations of Bids for ICM-7

Two bids for the ICM-7 were presented, namely Dublin in the Republic of
Ireland and the Hague in the Netherlands; the latter represents the European
Structural Integrity Society (ESIS). Each bid was presented to the Board of
Governors in the absence of the competing bid. After the presentations,

XIV
there were some question put forward to the presenters and discussions.

9. Voting for ICM-7

Voting for ICM-7 location was conducted after the two presentations. Each
country, irrespective of the number of delegates to the Board of Governors,
had one vote. And the two biding countries did not take part in the voting.
The result was 16 votes for the Netherlands representing the ESIS, and 12
for Ireland. It was thus decided that ICM-7 will be held in the Hague, the
Netherlands, in 1995.

10. ICM Affairs Report

Professor Hoshide read a report of the Conference (appended to the
minutes). There was applause. Professor Inoue then appointed Prof. Hoshide
the Secretary of ICM Executive Committee.

11. ICF8
Dr. Rama Rao, made an announcement that ICF-8 is to be held in Kiev, USSR,
June 1-6, 1993.

12. Thanks
Professor Yan expressed his gratitude on behalf of the past Executive Com-
mittee of ICM to the ICM-6 organizers: Prof. Jinno, Prof. Muguruma, Prof.
Inoue, Prof. Jono, and their team for having organized an excellent con-
ference. He also gave his thanks to the ICM Vice-Presidents: Prof. Carls-
son, Prof. Miller and Prof. Miyamoto, to the ICM Secretary, Dr. Wu, and to
all the ICM Governors for the constant support and excellent cooperation
during the past four years.
Professor Carlsson proposed his thanks to Professor M.G. Yan and Dr. X.R.
Wu for their excellent management of ICM affairs.
Professor Inoue paid attribute to his team, especially to the many young
people for their devotion, which had been such an important factor leading
to the success of ICM-6.

13. Closing
Professor M.G. Yan closed the meeting at 21:00.

M.G. Yan X.R. Wu

President Secretary

XV
 ICM-6 Affairs Report

The Sixth International Conference on Mechanical Behaviour of Materials,

ICM-6, was held in Kyoto International Conference Hall, Kyoto, July 28 -
August 2, 1991. The Conference was jointly organized by the Society of
Materials Science, Japan and the Foundation for Advancement of Interna-
tional Science, and sponsored by The Science Council of Japan.

Approximately 850 delegates including 100 accompanying persons from 34

countries and regions attended the Conference, showing a wide and even
representation of the research activities in this field from and around
the world. Two distinguished scientists from Canada and Japan delivered
plenary lectures highlighting the development of light materials and
frontiers of bridge construction. Twelve workshops were organized in
addition to ordinary technical sessions. The 36 invited and 20 keynote
lectures, and the 469 contributed papers were divided into ten parallel
sessions. The poster sessions including 89 presentations and the tech-
nical exhibition were held together in the Event Hall. The main theme
of the exhibition was "supporting technique for development in materials
science toward the twenty-first century".

Pergamon Press is the publisher of the Conference Proceedings. The

Preprints of the Proceedings were distributed to participants at the
registration desk. Formal Proceedings with hard cover including delayed
papers will appear by the begining of 1992.

Half day technical visits of five courses to Hi-Tech industries were or-
ganized during the Conference, and post-conference tours to some repre-
sentative industries and institutes in Nagoya and Tokyo-Tukuba areas
were also prepared.

The delegates have shown satisfaction to the high scientific and techni-
cal level of the Conference and the organizing works including social
program such as welcome reception, banquet and four accompanying
person's programs.

The Board of Governors organized during the Conference accepted the bid
for ICM-7 proposed by Professor A. Bakker, and next International Con-
ference on Mechanical Behaviour of Materials, ICM-7, was decided to be
held in the Hague, the Netherlands, in 1995.

XVI
PL1

MATERIALS DEVELOPMENT FOR LIGHT DESIGN:

A SUPPLIERS VIEW

JEFF W. EDINGTON

Alcan International Limited

1188 Sherbrooke St. West
Montreal, Quebec, Canada H3A 3G2

ABSTRACT

This paper describes two ways in which materials suppliers view materials
technology development for light weighting structures. The first example,
aluminium-lithium alloy development for airframes, describes a classical case where
the alloy development is the key step. The second example, aluminium structured
vehicle technology development for automobile bodies, describes a more complex
situation where the aluminium alloy development is a minor issue. More important
are a broad range of vehicle performance, manufacturing and cost problems which
must be solved jointly between the materials supplier and the automobile
manufacturer. Although the aluminium industry is illustrated here, similar
examples can be found in other structural materials industries, including steel and
plastics.

KEYWORDS

Airframe, Automobile, Aluminium-Lithium Alloys, Adhesive Bonding, Spot

Welding.

3
4

INTRODUCTION

New Materials have been the basis for many new products which have lead to the
development of successful companies and, in some cases, whole new industries.
Consequently, materials development technology has been identified by several
National Governments as an area of strategic significance. However, it is important
to realise that new materials are only an enabling technology. Considerable
additional effort is necessary, both to validate the performance of the new products
they make possible, and to ensure there is a viable low cost production route
consistent with the company's considerable existing investment in both assembly
plant and workforce skills. For these reasons, materials suppliers have recently
moved much closer to their customers, who are usually original equipment
manufacturers, to solve problems jointly. The objective is to produce a fully
integrated material and product manufacturing process that provides value in the
marketplace.

This paper illustrates this change with two examples. The first is the development
of aluminium-lithium alloys for light weighting airframes where specific
combinations of properties were needed in the material itself. The second is the
development of a spot welding and adhesive bonding technology for light weighting
automobile bodies. Here, the properties of the structure of the car were the issue
and a combination of developments were necessary for aluminium, for adhesives, for
lubricant, for spot welding and for automation. Vehicle builds played an important
part in validating the results. Similar examples can be found in other industries
that supply structural materials such as steel or plastics.

LIGHT WEIGHTING OF STRUCTURES

Design of lightweight products that use aluminium alloys efficiently to match

customer needs has become a major driving force in the industry. It arises from
two factors. First, the wish to do more with less, which is driven by the constant
need to provide value to our customers at low cost. Second, legislation aimed at
curbing environmental pollution and increasing recycling which focuses on using
then discarding the product. The aircraft industry and the automobile industry are
good examples of both and have been chosen to illustrate modern materials
development.

THE CIVILIAN AIRFRAME

Approximately 30% of the drag of an airplane flying at cruising speed is induced or

lift dependent drag, which is directly proportional to weight. Consequently, the
most direct way in which environmental pollution can be improved is to make the
airplane lighter without sacrificing reliability and safety. This provides better fuel
consumption which increases either the payload or range, or reduces operating costs
as well as using less material. Figure 1 shows that the density of the material has a
much greater influence on weight saving than strength, stiffness or fracture
toughness (Lageze 1989), and it is here that development by the aluminium industry
 5

has been concentrated. The alloy of choice was aluminium-lithium because it had
the largest practical potential for density reduction.

0 5 10 15 20 25
PROPERTY IMPROVEMENT (%)

Fig. 1. Weight saving achieved from improved material

properties. (Lageze, 1989)

Development of new alloys has in the past concentrated on yield strength, ultimate
tensile strength, reduction in area and fatigue resistance. The latter has been, until
recently, the safety criterion for airframe design. However, there has been a change
in the design criteria for Civil Transport Airplanes which requires structural
integrity assuming certain damage to exist in the structure. This criterion is
generally referred to as "Damage Tolerance". Introduced in the FAR 25 regulation
through amendment 45, this concept includes the crack propagation rate in the
damaged structure together with its residual strength. In effect, damage tolerance
starts at the point where fatigue stops, i.e., at the time when damage is initiated. In
a damage tolerant structure, rigorous inspection schedules ensure that such damage
is detected and repaired while the structure is still completely capable of fulfilling its
function.

It was against this background that the aluminium industry began to work with
airframe manufacturers in the early 1980's. The target was a 10% reduction in
density and a 15% increase in stiffness while providing equivalent mechanical
properties to 2024 and 7150 alloys. The former alloy is the damage tolerant
standard and the latter is the high strength standard. Success would provide the
aircraft designer with improvement in aircraft performance without the need to
change classical design and manufacturing techniques while parts could also be
substituted to improve existing aircraft.

Aluminium-Lithium Alloy Development

The major aluminium alloy characteristics which allow damage tolerance to be

controlled are fatigue resistance, stress corrosion resistance, and fracture toughness.
In addition, the alloy must have appropriate and reproducible static properties for
6

compression, tension or shear loading. All these must be achieved on an industrial

scale.

Physical Metallurgy. To develop alloys with suitable properties, there are five
precipitation processes available.

Al-Li (Silcock 1959, Noble and Thompson 1971, Williams and Edington 1975)

Solid Solution -» £;Al3Li - 6A1-LI (1)

Al-Li-Mg (Thompson and Noble, 1973)

Solid Solution - $'(Al3Li + Mg) - b Al2MgLi (2)

Al-Li-Cu (Silcock 1959, Noble and Thompson 1972, Peel eLaL, 1983)

High Cu:Li Solid Solution -» GP zones -* 9" -* 9'-* 9 CuAl2 (3)

High Li:Cu Solid Solution -» T, AI2CuLi (4)

Al-Li-Cu-Mg (Peel eJLaL, 1983)

Solid Solution -* GP zones - S" - S' - SfAljCuMg) (5)

Increasing the magnesium content in the quaternary favours reaction (5) over
reaction (4). In addition, the grain structure can be controlled through additions of
zirconium, combined with careful thermo-mechanical treatment. However, the
presence of zirconium appears to speed up aging.

In terms of mechanical properties the 6' phase provides considerable strengthening,

but causes slip to be concentrated upon well defined slip planes leading to premature
fracture. Combinations of the Tj phase and 6' and/or 9' can be made to form in
Al-Cu-Li alloys providing dual ageing capability. This makes it possible to achieve
appreciable fracture toughness improvement by independent control of these
precipitation systems and has led to the development of 2020 and 2091 alloys. In
these alloys, two complex phases precipitate at grain boundaries. The most complex
is 2091 which can have five precipitates present simultaneously that confer a high
resistance to recrystallisation but can lead to low short transverse strength, ductility
and toughness because precipitate free zones develop.

To overcome this problem, quaternary alloys 8090 and 8091 in the Al-Li-Cu-Mg
system have been developed in which the S phase Al2CuMg can form, in addition to
b' and Tt. In the short transverse direction, the array of grain boundaries is
weakened to a lesser extent than 2091 because there is no precipitate free zone and
better ductility and toughness are obtained. Grain size control is obtained by
adding zirconium.
 7
200

175

150

125 I-

100
8090 v
A l - Li ALLOYS x
75

50
2091
"X
25

275
0.2% PROOF STRESS MPo

Fig. 2. Plane stress fracture toughness of damage tolerant

sheet. 2091 and 8090 alloys compared with 2024 and
2014 aUoys. (Peel, 1988)

Damage Tolerance. The comparative performance between the two leading Al-Li
alloys 2091 and 8090, and 2024 and 2014 is shown in Fig. 2. The microstructures
and tempers of both alloys have been adjusted to balance strength and fracture
toughness (Peel 1988, Grimes et al.. 1990). It can be seen that at least at present,
whilst the aluminium-lithium alloys compete with 2024 reasonably at the low
strength levels, they fall short of the performance of the 2000 series alloys as the
strength level is increased which limits design loading to lower levels.

§ o.ia

RANG
E IN STRES
S INTENSIT
Y FACTOR
. M P am/

Fig. 3. Fatigue crack growth rates for damage tolerant sheet.

2091 and 8090 alloys compared with 2024 and
laminated 8090. L-T Test Direction R=0.4 (Peel,
1988)

Resistance to the growth of fatigue cracks is also an important contribution to

damage tolerance and here aluminium-lithium alloys offer improvements. They
possess a naturally high resistance to fatigue crack growth (Peel 1988, Grimes et al..
8

1990), (see Fig. 3). This comes in part from their high elastic modulus and the
tortuous fatigue crack paths that are produced in their refined microstructures.

Stress corrosion resistance is also important in promoting damage tolerance. In

general, alloys such as 8090 show superior stress corrosion resistance to 2024 in all
product forms, plate extrusion and sheet. Even underaged 8090 plate which exhibits
the greatest tendency toward stress corrosion cracking (Gray 1987) is superior to
T351 2024.

General Properties. In terms of specific stiffness, specific elastic buckling

resistance, specific tensile design allowable limits and specific compressive design
allowable strengths 8090 and 8091, offer improvements over such alloys as 7010 and
7150 (Peel, 1988), (see Figs. 4 and 5).
■

2.0
•
r i 3
" 1.6 ♦*.*♦* .
[ \ °
[
|
J S
o pi -
l.i. i^VN W .

--
N\\N\ X *X< ♦*.*♦*
0.8
SH Sv^x: *•*♦**

^ S
iiv\>
-
-
0.4
\viiv 0^1

00 ^ ys.*

Fig. 4. Specific stiffness and elastic buckling resistance

for longitudinal testing. (Peel, 1988)

-
,'X\\V

-
u ^ N
^
vk^
§V^ BE
*H« -
M1 :HS S3 yjij
&2 <p?
" :$^j;
x\.xS:
^v^; v.\ li
7150 8091

Fig. 5. Specific tensile and compressive design allowable

strengths. (Longitudinal strengths allowed at limit
load). (Peel, 1988)

Cost Issues. The various items that are used in the structure, such as stringers,
frames, sheets, window forgings, etc, can be evaluated in cost benefit terms. Cost
per weight saving can be estimated for particular buy to fly ratios (Lageze, 1989)
the ratio between the amount of material bought to produce a particular component
in the finished aircraft. The details clearly depend on each individual case.
However, overall, it is clear that at the typical prices of jet fuel over the last five
years, Al-Li has only a limited chance of being used when the waste is high, and the
buy to fly is greater than three, e.g. wing components machined from plate.
 9

Consequently, it is clear that reduction in costs will be necessary to broaden the

applications of these new alloys.

Future Developments

It is increasingly difficult to balance in one new material the whole range of

mechanical properties required for continued light weighting of airplane structures.
Consequently, the future is likely to see increasingly specialized materials, with
combinations of properties designed to enable particular components in the structure
to function. New generic solutions like 2000, 7000 and Al-Li alloys are unlikely.
Thus particulate reinforcement of Al-Li alloys will increase specific stiffness strength
and operating temperature, but achieving good fracture toughness will be difficult,
so damage tolerant applications are unlikely. This may require laminated products
such as Arall, with Al-Li or Al-Li-particulate reinforced skins. High strength 7000
and 8091 will remain dominant for some time.

THE AUTOMOBILE BODY

It is here in the automobile that the greatest single step toward light weighting can
be taken by the substitution with lighter materials. Several automobile
manufactures have shown that, by substituting aluminium for steel, weight savings
of between 40 and 50% can be achieved (see Table). Similar but lower data can be
shown for fibre reinforced plastics. In practice, further secondary savings should be
possible because smaller engines, lighter transmissions, brakes, wheels, etc, can be
used to meet the needs of a lighter body.

In designing structures, the primary criterion is stiffness, not strength, because this
governs road feel, road holding and stability while driving. However, safety in a
crash requires a structure that is strong, yet has the ability to deform in a controlled
manner to absorb energy. Further, since automobile structures are expected to have
a life of many years, the structure must be intrinsically durable. Finally, the body
must be feasible for volume production at an economic cost and have a marketable
appearance. All of this requires good material properties. However, we also
require total material consistency at low cost and very large tonnages. We also need
to develop with our customers, a low cost, easily automated body assembly process
using as much as their existing equipment as possible, and capable of producing, if
necessary, up to 250,000 cars annually. Furthermore, very accurate dimensions and
high paint quality are essential to match innovations in those fields. Finally, we
must ensure that the car passes all standard road tests, including crash tests, and
there will not be product recalls arising from a failure in either material or
technology.
10

Table. Weight savings reported by substituting aluminium for steel in

automobile bodies.
RELATIVE TO STEEL

AUTOMOBILE CONSTRUCTION
WEIGHT IN
STEEL
WEIGHT IN
ALUMINIUM
WEIGHT
SAVING
% %
kg kg % FLEXURAL
STIFFNESS
TORSIONAL
STIFFNESS

SPOT WELDED
PORSCHE 9 2 8 303 161 47 93 70
SHEET

AUDI 1 00 RIVET-BONDED
SHEET
280 149 46.8 113 "
VOLVO LCP 231 115 49.7 " -

-
SPOT WELD
PONTIAC HERO
- B O N D ED SHEET
444 303 32 96

"
LASER WELD
FERRARI 408
- B O N D ED SHEET
99 68 31.3 115

-
SPOT WELD
BRITISH LEYLAND 74
- B O N D ED SHEET
143 48 60
METRO

SPOT WELD
BERTONE X 1/9
- B O N D ED SHEET
192 130 33 82 101

- -
BRITISH LEYLAND SPOT WELD
ECV3 - B O N D ED SHEET
162 83 49

MIG AND
ACURA NSX SPOT WELDED 350 210 40 - "
SHEET

SPOT WELD
TYPICAL
- B O N D ED SHEET
262 138 48 100 106
CURRENT ASV
PROJECT CAR SPOT WELDED
262 158 40 101
ONLY

To illustrate these issues, Alcan's Aluminium Structured Vehicle Technology is

described. It is based on the realization, by British Leyland, that significant
changes in the stiffness in aluminium structure can be obtained when continuous
adhesive bonding of flanges is used instead of conventional spot welding (King,
1983). Structural analysis indicated that, provided a medium strength aluminium
alloy is used, the body will have an adequate load bearing capability at the sheet
gauges needed to meet the overall stiffness target. It is the stiffness requirement,
not the load bearing need that governs the gauge. This is an important result, since
it opens the door to the use of medium strength, low cost aluminium-magnesium
alloys, 5454 series, for all the sheet requirements of full monocoque car structures
except the roof and the rear quarter panels. These alloys have good formability and
excellent corrosion resistance and are cheaper to produce than the stronger heat
treated, dent resistant body sheet alloys such as 6009 and 6111. The latter alloys
are used for hoods and trunk lids and would be used for all other external body
panels including the roof and rear quarter panels of an all aluminium car.

As pointed out earlier, solving the metallurgical and formability problem is only
part of the issue. It was necessary to develop and prove a practical manufacturing
system incorporating adhesive bonding for the structure that meets the demanding
specifications required by the automobile industry (Wheeler et al 1987, Kewley et al
 11

1987). The result is summarized in Fig. 6. Pretreated and prelubricated

aluminium-magnesium alloy material is supplied in coil form in the fully soft
temper, (top sequence, Fig. 6). This would be stored by the car manufacturer in
sheet form and components blanked and press formed exactly as steel is handled
today, the lubricant acting as the press forming lubricant. The adhesive is then
applied to the joining flanges of the components as they are brought together in a
sub-assembly, (centre sequence, Fig. 6). As the sub-assemblies are assembled to
form the complete "body in white", spot welds are applied at appropriate points to
hold the assembly together until the adhesive is cured. In this way, the complete
body in white is assembled and only then is the structure cured in a dedicated cure
oven prior to painting, (bottom sequence, Fig. 6).

It is clear that a wide range of technical problems were overcome to generate this
manufacturing route, some of these are summarized below.

FROM ROLLING MILL O PRETREAT vIENT O PRESS» LUBRICANT O

c
1 £
__Q _d * *
O Q„.0
lit
ADHESIVE APPLICATION <l STORAGE <3 PRESSING

^~^ ;T

SPOT o SUB-ASSEMBLY O BODY BUILD D > THERMAL FINAL

WELDING " CURE ASSEMBLY

.X H
g^i^^D^ «a^
Fig. 6. Aluminium structured vehicle manufacturing system.

Adhesives

The adhesive must be compatible with both pretreatment and press lubricant,
resistant to run-out during assembly and subsequent curing, and highly durable. It
must also be readily applicable by automated equipment. In addition, it must
provide the correct combination of shear, peel and impact strength independent of
12

bondline thickness and have good shelf life. Finally it must retain these properties
in the temperature range - 40°C to + 120°C to cope with climate variations in
service. The solution was a heat cured single part toughened epoxy (Marwick and
Sheasby, 1987).

Lubricant

Clearly the lubricant must confer adequate formability. It must also be compatible
with both pretreatment and adhesive because a separate operation to remove the
lubricant prior to adhesive application would add unacceptable costs as well as
disrupting its flow of parts in a body in white assembly line. In addition, its
residues after curing must be easily removable prior to painting. No commercially
available lubricant would satisfy these demands and a new lubricant was developed
that has been fully proven by extensive laboratory and field testing.

Spot Welding

The number of spot welds required is not large, about one third of that required in
an equivalent steel body. However obtaining large numbers of consistent welds with
aluminium has always been difficult. A complication is the adhesive layer in the
joining flanges but the pretreatment helps by providing a consistent surface
resistance. In addition, the lubricant aids in reducing sticking of the spot welding
electrodes to the aluminium sheet. Thus, a technique has been developed to give an
acceptable number of high quality welds from a single set of electrodes and at
currents significantly lower than those required for bare aluminium.

Pretreatment

Pretreatment of the aluminium alloy surface is the key to ensuring good bond
strength and durability. It must be coil applied for simplicity, low cost and be
unchanged during prolonged storage, both before and after forming. It must not be
significantly affected by forming, but it should be optimized to assist spot welding.
Furthermore, it must act as a pretreatment for painting as necessary. Most
importantly, it must provide for long term durability of the bond. Such a
pretreatment has been fully proven by extensive laboratory and field testing.

Bond Durability

Bond durability is essential to provide long term performance of the vehicle.

Accelerated tests have been conducted using a single shear joint that is
representative of those used in the car (Wheeler et_al, 1987). To further accelerate
potential deterioration, a hole is drilled in the joint. Tests were conducted in a high
humidity high temperature environment both with and without salt sprays and both
stressed and stress free. Performance was compared with material pretreated with
the Boeing 555 phosphoric acid process. This had been the standard for the
 13

aerospace industry for 20 years, but it is unsuitable for this application as it is a

slow, (1 hour), batch process and requires a very clean assembly environment.
Joints produced with the above technology gave comparable performance to the
Boeing standard, (see Fig. 7), even after long storage periods and in the presence of
selected lubricants. Stressed joints have been on tests for nearly seven years without
failure in high temperature, high humidity environments.

[ | ALCAN PRETREATMENT B

HS^l BOEING 555-ESP 105

0 4 12 20

NUMBER OF WEEKS IN NEUTRAL SALT SPRAY AT 43 °C

Fig. 7. Strength retention of adhesively bonded joints during

salt spray accelerated testing. Alcan pretreatment
vs Boeing 555 standard.

Automated Production

To demonstrate the feasibility of applying the adhesive to connecting flanges in the

correct location to ensure good load transfer and clean conditions, Alcan conducted
a project with Volvo and Bertone to build a robot adhesive application cell. Here
adhesive is applied at the linear application rate required to build 1000 cars per day
(250,000 per year). All equipment used is currently available from Norstrom and
ASEA-Brown Boverie. The parts used are standard automobile pressings from
current Volvo model but made in the aluminium alloy developed for the Alcan
technology.

Structural Engineering and Analysis

An important parallel activity has been to develop and quantify the structural
engineering and behaviour characteristics of adhesively bonded aluminium
structures, especially static and dynamic strength, fatigue strength and the ability to
absorb energy under impact conditions. Here, for instance, impact testing of spot
welded and adhesively bonded box beams has shown that they will absorb as much
energy as steel beams twice their weight and this has been confirmed by detailed
finite element modelling of the collapse mechanism (Seeds and Sheasby, 1987).
14

This development program, which has grown and matured over the last eight years,
has shown that the use of weld-bonded aluminium for vehicle structures in volume
production is technically feasible, is suitable for application in volume
manufacturing plants with only minor equipment changes, and that such structures
would give excellent durability and performance.

Vehicle Builds

Replica models in aluminium of the British Leyland Metro, the Bertone Xl/9, the
Pontiac Fiero as well as the prototype British Leyland energy conservation vehicle
ECV3 have all been built with this technology and have been extensively described
elsewhere (Wheeler eLaJ., 1987, Selwood eLaJ., 1987, Warren et al.. 1987, Sheasby
and Wheeler, 1988, Kewley, 1985). These automobiles and the subsequent
experimental prototype Ferrari 408 (Seeds et al.. 1989) showed that the weld bonded
aluminium body in white could provide equivalent stiffness to that of a spot welded
steel structure with significant weight reductions (see Table). Finite element
modelling indicates that a weight saving of almost 50% can be achieved with the
appropriate gauges of material. However, this is not possible with replica vehicles
where the normal steel tooling is used and the choice of gauge is either the original
steel gauge or twice this using doubled parts. Nevertheless, significant weight
savings have been demonstrated (see Table).

Automobiles have been extensively tested under severe road conditions and in very
severe corrosion environments. In all these tests the aluminium structured vehicles
have performed very well, particularly in the corrosion cycle where their
performance was exceptional. Crash test behaviour was also satisfactory.

A different approach has been taken by Alcoa, in collaboration with Audi, who have
built Audi 100 replicas by riveting and bonding a sheet structure (Hasler, 1988).
Here also weight savings are significant.

In an entirely separate development Honda now have in production the NSX all-
aluminium sports car which uses a similar approach to that outlined here. Mazda
will be unveiling this year its own, lower priced all aluminium car. The major
differences between Alcan and Honda are that adhesive is not used and the spot
welded structure is augmented by MIG welding at key points. The weight saving is
still large at 40%, but not the maximum possible (Komatsu et al.. 1991).

Future Developments
In aluminium alloy development, significant improvements in formability are
necessary. Die design developments that allow for springback and ensure accurate
part dimensions are also needed. Finally partial solutions must be developed that
only use adhesive in critical regions, or do not use it at all accepting a smaller
weight saving. Equally important, solutions must be developed to solve weight and
weight distribution problems on particular models involving fabrication of fenders,
hoods, trunk lids and doors.
 15

CONCLUSIONS

The work described here has demonstrated that successful technical solutions to light
weighting design problems may rest on approaches as different as:

♦ Alloy development to meet property specifications developed by a customer,

in the case illustrated an airframe manufacturer.

♦ Innovative use of existing alloys, but focusing with original equipment

manufactures on assuring the performance of the product and its
manufacturability, in the case illustrated an automobile "body in white".

REFERENCES

Gray, A. (1987). Factors Influencing the Environmental Behaviour of Aluminium-

Lithium Alloys, Aluminium-Lithium Alloys IV (G. Champier, Ed.), J. Physique.
48, Chap. 3, pp. 891-904.

Grimes R., Gatenby K. M., Reynolds M. A., Gray A. and Palmer I. G. (1990 in
press). The Evolution of Damage Tolerant Aluminium-Lithium Alloys. Advanced
Aluminium and Magnesium Alloys. ASM, Pittsburg, USA.

Hasler, F. (1988). The Aluminium Body - Advance or Wrong Way. Proc. 3rd.
International Symposium on Aluminium and the Automobile. Aluminium Verlag,
Dusseldorf, F.R.G., pp. 45-49.

Kewley, D. (1985). The B. L. Technology ECV 3 Energy Conservation Vehicle.

SAE Technical Paper 850103, Detroit, USA.

Kewley D., Campbell I. G. and Wheatley J. E. (1987). Manufacturing Feasibility of

Adhesively Bonded Aluminum for Volume Car Production. SAE Technical Paper
870150, Detroit, USA.

King, C. S. (1983). A Car For The Nineties B. L.'s Energy Conservation Vehicle.
Proceedings of the Institution of Mechanical Engineers. 197. n° 64, 1-11.

Komatsu Y., Ban K., Ito T., Muraoka Y., Yahaba T., Yasunaga K. and Shiokawa
M. (1991). Application of All Aluminum Automotive body for Honda NSX. SAE
Technical Paper 910548, Detroit, USA.

Lageze, J. C , (1989). Material Performance Characteristics Required in the

Aerospace Industry. International Symposium on Aluminium in Transportation:
Prospects for the Future. Japan Light Metals Association, Tokyo, Japan, Section
in, 2.

Marwick W. F. and Sheasby P. G. (1987). Evaluation of Adhesives for Aluminum

Structured Vehicles. SAE Technical Paper 870151, Detroit, USA.
16

Noble B., Thompson G. E. (1971). Precipitation Characteristics of An Aluminium-

Lithium Alloy. Met. Sci. J.. 5, 114-120.

Noble B., Thompson G. E. (1972). T, (Al2CuLi) Precipitation in Aluminium

Copper-Lithium Alloys. Met. Sci. J.. 6, 167-174.

Peel C. J. (1988). Current Status of the Application of Conventional Aluminium-

Lithium Alloys and the Potential for Future Development. 67th Meeting of the
Structures and Materials Panel. Hierlo, Netherlands, AGARD Conference
Proceedings 444, pp. 21-1.

Peel C. J., Evans B., Baker C. A., Bennett D. A., Gregson P. J., Flower H. M.
(1983). The Development and Application of Improved Aluminium-Lithium
Alloys. Al-Li Allovs II. Eds. Sanders Jr., T. H. Starke Jr. E. A., AEVIE, pp. 363-
392.

Seeds A., Nardini D. and Cassese F. (1989). The Development of a Center Cell
Structure in Bonded Aluminium for the Ferrari 408 Research Vehicle. SAE
Technical Paper 890717, Detroit, USA.

Seeds A. and Sheasby P. G. (1987). Evaluation of Adhesive Joining Systems in

Aluminum Box Beams. SAE Technical Paper 870152, Detroit, USA.

Selwood P. G., Law F. J., Sheasby P. G. and Wheeler M. J. (1987). The

Evaluation of An Adhesively Bonded Aluminium Structure in an Austin-Rover
Metro Vehicle. SAE Technical Paper 870149, Detroit, USA.

Sheasby P. G. and Wheeler M. J. (1988). Aluminium Structured Vehicle

Technology: A Review. Proc 3rd International Symposium Aluminium and the
Automobile. Aluminium Verlag, Dusseldorf, pp. 49-57.

Silcock J. M., (1959). The Structural Ageing Characteristics of Aluminium-Copper-

Lithium Alloys. J. Inst. Met.. 88, 357-365.

Thompson G. E., Noble B. (1973). Precipitation Characteristics of Aluminium-

Lithium Alloys Containing Magnesium. J. Inst. Met.. 101. 111-115.

Warren A. S., Wheatley J. E., Marwick W. F. and Meadows D. J. (1987). The

Building and Test-Track Evaluation of an Aluminum Structured Bertone Xl/9
Replica Vehicle. SAE Technical Paper 890718, Detroit, USA.

Wheeler M. J., Sheasby P. G. and Kewley D. (1987). Aluminium Structured

Vehicle Technology - A Comprehensive Approach to Vehicle Design and
Manufacturing in Aluminum. SAE Technical Paper 870146, Detroit USA.

Williams D. B., Edington J. W. (1975). The Precipitation of 61 (Al3Li) in Dilute

Aluminium-Lithium Alloys, Met. Sci J.. 9, pp. 529-532.
PL2

FRONTIERS OF HONSHU-SHIKOKU BRIDGE CONSTRUCTIONS

Naruhito Shiraishi

Kyoto University, Kyoto 606, Japan

ABSTRACT

The Honshu-Shikoku Bridge Authority was established in 1970 to construct 3

route of connecting bridges between Honshu (Main Island of Japan) and Shikoku
(Shikoku Island) to cross over the Seto Inland Sea. The central route, called as
the Seto Bridge, was opened for traffic in April, 1988. The two other remaining
routes are now under construction. The east route is particularly high-lightened
by construction of the Akashi Strait Bridge, the longest suspension bridge in the
world of 1990 m long center span. Frontiers of construction technologies,
materials and methods of analysis developed in connection with the Honshu-
Shikoku Bridge Construction Project are briefly described in this paper.

KEYWORDS

Construction Machinery, Prepact Concrete, PWS (Parallel Wire Strand), Aseismic

Design, Wind Resistant Design, TMD (Tunned Mass Damper), Quality Control,
Fatigue Test, Vibration Test

INTRODUCTION
The Honshu-Shikoku Bridge Construction was a dream of more than 100 years.
As well known, there are numerous small islands scattered in the beautiful Seto
Inland Sea to separate Honshu-Island and Shikoku Island. For long time people
could cross this inland sea only by ferry boat. In early morning of May 11, 1955,
a tragedy of ship-collision of "Shi-un Maru" and "Daisan Utaka Maru" occurred
and 168 lives lost. Most of fatalities in this accident were school boys and girls
who were en route for school excursion. A year before this accident, the "Tohya
Maru" of ferry boat for Honshu(Main Island )-Hokkaido (Northern Island of Japan)
sank by typhoon and 1,155 lives lost. These two accidents became a crucial
impact to plan the connecting routes for both Honshu-Hokkaido and Honshu-
Shikoku by either tunnel or bridges. Soon later the Honshu-Hokkaido route was
resolved to plan to construct a tunnel, while the Honshu-Shikoku route was
resolved to plan long span bridges. The Seikan Tunnel between Honshu and
Hokkaido (Tunnel between Aomori of Honshu side and Hakodate of Hokkaido side)
was opened for railway traffic in March, 1988 and the Seto Bridge between Honshu
and Shikoku was opened for traffic in April, 1988 so that all major four islands

17
18
of Japan are now connected with each other by either tunnels or bridges.
In order to clarify engineering problems associate with construction of the
Honshu-Shikoku bridges, the ministry of construction and the national railway
corporation requested an investigation for feasibility and technical possibility of
Honshu-Shikoku Bridge for Japan Society for Civil Engineers in 1963 and the final
report was published in 1967 indicating that the planned Honshu-Shikoku Bridges
for both roadway and railway would be possibly constructed under specially
prepared design and material specifications with the design guide lines for
earthquake and strong winds. And at almost same time the technical survey office
of ministry of constructions was opened in Kobe in 1963 to start to investigate
ground conditions as well as various environmental problems including not only
natural problems but social problems. In 1970 the Honshu-Shikoku Bridge
Authority was established as the public corporation responsible to construct and
operate maintenance of constructed bridges and affiliated facilities.

Major technical problems to be vanquished in connection with the Honshu-Shikoku

Bridge Construction can be illustrated as follows;

(1) To assure aerodynamic stability and safety against action of so strong

winds as typhoon and to assure aseismic safety against earthquake

(2) To assure travelling safety of high speed train on suspended bridges

and fatigue resistant design of welded parts

(3) To develop safe and assured method for construction of foundation in

deep strait under high speed tidal current

(4) To develop safe assured erection method for s u p e r s t r u c t u r e s ,unaffected

under severe meteorological environments

(5) To establish the maintenance and control system to preserve high degree
of safety and invulnerable serviceability of completed Honshu-Shikoku
bridge routes

Development for above mentioned technological problems is illustrated in the

succeeding paragraphs.

FRONTIERS OF STRUCTURAL DESIGN OF HONSHU-SHIKOKU BRIDGES

In connection with the Honshu-Shikoku Bridge Project, fundamental structural

problems are to establish the feasible design specifications for any sort of bridge
s t r u c t u r e s to be employed for this project. Great achievement in this aspect has
been made by number of theoretical and experimental investigations. However the
most important problem among them is the safety evaluation of dynamic behavior
of long span suspended s t r u c t u r e s such as suspension bridge and cable-stayed
bridge. In this paper a particular stress is placed on development of wind and
earthquake resistant design of super-long span suspension bridges.

Wind Resistant Design of Honshu-Shikoku Bridges

It is well known that the Tacoma Narrows Bridge in Washington collapsed in 1940
by wind blowing of wind speed of 19 m/s. The main cause of this failure is
considered due to so-called torsional flutter of stiffening girder of H-lettered
shaped cross section. Since then tremendous efforts have been paid to establish
the feasible wind-resistant design method of suspension bridge. The problem
 19
mainly consists of two parts, namely (1) how to estimate the design wind speed
and (2) how to design aerodynamically stable cross section of stiffening girder.

The large portion of the Seto Inland Sea where the Honshu-Shikoku bridges ought
to be constructed is typhoon prone area, so that a special task committee was
organized to investigate meteorological characteristics of natural strong winds
statistically as well as aerodynamic behaviors of long span suspension bridge.
One of the main difficulties was how to estimate the design basic wind speed for
so complicate topographical typhoon prone area as the Seto Inland Sea, where a
number of the most severe typhoons attacked in past sixty years. The second
problem was how to design the aerodynamically stable cross section of stiffening
girder and pylons of the longest suspension bridge in the world. In order to
achieve this task, a series of theoretical and experimental research works have
been performed in collaboration of researchers from academia, public research
institutes and industrial firms. Stress has been placed on systematic collection
of wind tunnel tests results for various types of bluff cross sections and on
analysis of aerodynamic behaviors of such cross sections by use of the most
advanced and sophisticated experimental techniques. It should be noted that
large scale wind flume was installed to investigate aerodynamic responses of the
one tenth scaled bridge model subjected to natural turbulent winds and also the
large wind tunnel of 41 m x 17.5 m (width x height) has been installed in Tsukuba
in 1991 in order to examine the three dimensional aerodynamic behaviors of the
Akashi Strait Bridge by use of its one tenth model in both uniform and turbulent
flows. The investigation for aerodynamic problems in connection with the Akashi
Strait Bridge, the longest suspension bridge in the world, is now ongoing as the
most important technical subject. Almost 30 year studies on aerodynamic design
of bridge structures including suspension bridge, cable-stayed bridge, truss
bridge and ordinary tubular box girder bridge have clarified number of
fundamental aerodynamic characteristics of bluff bodies; namely,

(1) vortex-induced vibrations can be classified into the following three

categories, (a) the flow-induced vibration associate with perfectly
separated flow (termed as perfectly separation type), (b) the flow-
induced vibration associate with separated bobble at windward edge
(termed as separation at windward edge type or movement excitation
type) and (c) the flow-induced vibration associate with reattached
bobble (termed as reattachment type) Vortex-induced vibrations of
majority of bridge structures are the separation at windward edge type
or the movement excitation type, the onset velocity of which can be so
easily estimated by the recommended onset velocity and slenderness
ratio (the ratio of width to height of the cross section) relation.

(2) The longer the span length of suspension bridge, the higher the tower
of suspension becomes. The height of tower of the Akashi Strait is
approximately 300 m. The natural frequency of free vibrations of the
lowest mode may vary from 0.08 Hz to 0.445 Hz depending on construc-
tion steps. And there is another particular point as for aerodynamic
characteristics of this highly elevated structure, namely aerodynamic
responses of bluff section for large angle of attack to correspond to
action of all wind directions.

(3) In connection with construction of cable-stayed bridges a new type of

aerodynamic problems has become so controversial, namely so called rain
vibrations of inclined cables. It has been clarified that this vibration
is generated and enhanced by both formation of rivulets on both upper
and lower surface of cable and also formation of secondary axial flow at
leeward stagnation region to be considered as galloping type oscillation.
20
(4) For aerodynamic design of various types of so flexible s t r u c t u r e s as
suspension bridges and cable-stayed bridges, new method has been
developed to evaluate fatigue damages due to such wind induced
vibrations as vortex-induced oscillations and buffeting by turbulent
flows.

Earthquake Resistant Design of Honshu-Shikoku Bridges

To design any sort of civil engineering s t r u c t u r e s , earthquake takes an important
role to determine structural system and its safety. A task committee was
organized to investigate fundamental characteristics of expected earthquake in
Seto Inland Sea Area and to make the earthquake resistant design specifications
for the Honshu-Shikoku Bridges. Based on previous earthquake activity records,
rather remote earthquake (namely earthquake to occur at 100 to 150 km remote
from the s t r u c t u r e of concern) is thought to take a dominant role, which
corresponds to earthquake of magnitude or Richter scale 8 at the r e t u r n period
of 100 years.

The response spectrum method is employed for seismic design of the Honshu
Shikoku Bridges, based on the response spectrum obtained from large number of
previous earthquake records and corrected to be feasible enough for design
purpose to be the design acceleration response spectrum. This spectrum is used
to estimate the maximum seismic response of s t r u c t u r e for application of so called
design earthquake force. The structural model for analysis of suspension bridge
includes girder, cables, towers as well as foundations by introducing equivalent
mass and spring. In order to assure feasibility of used model, the time history
analysis was also made by using number of time history records of actual
earthquakes.

Design of Railway Long Span Suspension Bridge

In the central route, namely Kojima-Sakaide route, the Main Island and the
Shikoku Island is now connected by Seto Bridge including three suspension
bridges which are Shimotsui Seto Bridge, North Bisan Seto Bridge and South Bisan
Seto Bridge. The longest is South Bisan Seto Bridge of center span of 1,100 m,
which is the largest in the world as a highway and railroad combined bridge.
Stiffening girders of suspension bridges were so designed to provide the upper
deck for four lane highway and the lower deck for railroad for the conventional
line of double track. A particular attention was paid for the s t r u c t u r e of railroad
so as to be able to add the Shinkansen line of double track in future.

In connection with design of a railway long suspension bridge, two major

problems have been raised at the beginning of investigations, The^ former
problem is travelling safety of high speed trains at ends of girders where
considerably large amount of relative angular displacement and relative
longitudinal displacement are expected, since the ordinary type of suspension
bridge has a stiffening girder simply supported at both ends. And the latter
problem is fatigue damage of local structural part by large number of repetition
of heavy train loadings. In order to have sufficient degree of safety of travelling
train, an attempt was made to reduce the amount of relative angular and
longitudinal displacements structurally by

(1) employing continuous girder over main and side spans,

(2) reducing tfre span ratio of side to main span, namely much shorter side
span than normal length of side span required by ordinary design of
suspension bridge, and
 21
(3) introducing newly developed transition girder expansion joints at both
ends of continuous stiffening g i r d e r s .

As the consequence, the girders were connected to the towers so as to decrease

the eccentricity between the tower and the cable and a protruding bracket was
thus installed for fixing of hanger rope and girder to the outside of stiffening
girder. A series of travelling and durability experiments for the transition girder
expansion joint were performed by using high speed travelling train of 180 km/h
of the Shinkansen Standards to assure its function and travelling safety. The
tests indicated that the transition girder expansion joint was quite effective up
for + 75 cm of relative longitudinal displacement and 10 /QQ of relative angular
displacement at the maximum. More precisely, three kinds of transition girder
railroad expansion joints were developed as
* 1500-type having the contractility capacity of + 750 mm
* special 800-type having the contractility capacity of + 400 mm in regular
condition and + 550 mm in earthquakes
* 600-type having the contractility capacity of + 300 mm
The 1500-type was installed on both bridge ends of each of the three suspension
bridges in Seto Bridges, the special 800-type mounted on both ends of each of
cable-stayed bridge and Ban-no-su viaduct t r u s s , and the 600-type mounted on
both ends of Yo-shima Bridge.

As for railway construction, another problem was raised in connection with the
Bannosu Viaduct, which was located at the most northern part of Shikoku Island.
This viaduct of 2.9 km is directly connected to South Bisan Seto Bridge. Steel box
girders are used for highway and PC box girders continuous over three to five
spans are used for railroad. The problem came from ground condition of soft and
thicker stratum so that the supporting bedrock was only found at the Motoyo
strata or granite of 70 m depth. Since 74 m deep foundation piles were required
and the viaduct itself was highly elevated, train running characteristics were
investigated when an earthquake occurred. Based on the dynamic analysis of
whole viaduct s t r u c t u r e s including ground condition, the span length was so
determined not to exceed the derailment limit of railroad or to differentiate the
natural frequencies of viaduct from natural frequencies of running train.

Fatigue Proof Design of Welded Parts

Main strategy for design of Kojima-Sakaide route of Honshu-Shikoku Bridge was
to alleviate the dead load or own weight of s t r u c t u r e s by employing high strength
steels since the bridge was required to c a r r y both highway load and railway load.
It is well known that heat-treated high strength carbon steels used for Honshu
Shikoku Bridges are mechanically so sensitive for various types of notch,
temperature and also welding that an investigation was carried out to clarify
fatigue limit at various types of welded p a r t s and to lead to the specification for
fatigue proof design of welded members. Because of number of new type of
welded structural p a r t s to be used for this national project, a large scale fatigue
testing machine of maximum loading amplitude of 400 t was used for this purpose.
The theme of this research project were the following;

(1) experimental evaluation of fatigue limit of various welded joints

(2) allowance of initial defects
(3) establishment of effective detective method of initial defects
(4) development of welding method to increase fatigue limit
(5) development of welding materials for high strength carbon steels.

A particular s t r e s s was placed to develop a new non-destructive automatic

detector by use of supersonic waves. It is interesting to note development of
22
supersonic wave detector. In order to a s s u r e detective capability of detectors
for various types of initial defects, it was necessary to produce large number of
different initial defects for welded parts and this lead to clarify various causes
of initial defects at welding. Consequently development of new non-destructive
detector was so useful to develop fatigue proof welding method by eliminating
clarified causes for initial defects.

FRONTIERS OF CONSTRUCTION TECHNOLOGY OF HONSHU-SHIKOKU BRIDGE

For construction of long span suspension bridge and cable-stayed bridge, safe
and feasible construction methods for such s u b s t r u c t u r e s as foundation or piers
for towers and anchorage block takes also as important role for overall safety of
s t r u c t u r e s as those for s u p e r s t r u c t u r e s . In connection with the Honshu-Shikoku
Bridge construction project, a huge mass of undersea concrete constructions
having to be completed in a considerably short limited period, a series of land
experiments were repeatedly performed as well as undersea experiments, placing
a s t r e s s on prepacked concrete construction method which were used in actual
work.

The geological s t r u c t u r e , for example, in the strait for the Seto Bridges comprises
basically granite, particularly weathered granite exposed over a region from Mt.
Washizu of Honshu side to the offshore in the south of Mitsugo Island. A thick
layer of sedimentary layer covers a range in the northern p a r t of Shikoku side.
The sea depth for the route varies from 10 m to 50 m at maximum and tidal
current reaches 5 knots at maximum. And furthermore the site is located at the
major international navigation route with approximately 1000 ships passing per
day and crowed with fishery. Thus the so called rigid foundation was employed
except the pile foundation used in Bannosu area. There are a total of 23
foundations for major 6 bridges in the central route, namely the Seto Bridges,
including 5 foundations on land. Out of 18 undersea foundations, 7 foundations
were constructed by means of the cofferdam method and 11 by means of the
laying-down caisson method.

Excavation for Foundations

As the preliminary works for foundations, surface layer ought to be removed.
And for this purpose the detonating fuse system was used for submerged
blasting. The OD drill, mounted on the self-elevating platform (SEP), was used
to drill holes in which PVC pipes were installed for explosives. The deck of SEP
"Banjaku" is 47 m x 35 m at the center of which there is an opening of 21 m x 10
m, to be used for offshore work up to a depth of 50 m. The OD drilling machine
is a pneumatic rotary impact type machine with dual tubes. The outer tube (drill
tube) normally stops in drill hole in the sedimentary layer at rock base and then
the impact type inner tube (drill rod) is used to drill hole. Also the Wellman
drilling machine, a hydraulically rotary drilling machine, was used for sedimen-
tary and thick weathered rock layer.

Large scale submerged blasting was prohibited at some of construction sites

because of an oil refinery plant located within 400 m to 1 km. However, note that
the foundation was the greatest in scale, a water depth of 50 m, an excavation
dimensions on the bottom of 85 m x 74 m with a volume of about 600,000 m in
undersea excavation. A method for this purpose was developed to the successful
result, namely one second delayed firing method. At a foundation construction
for sedimentary soil and rock deposited on the seabed as thick as about 30 m, the
overburden undersea blasting was used without removal of surface layer.
 23
After underwater blasting, seabed was excavated by grab dredger. The used
grab dredger is one of the Japanese largest and most powerful as the sand
grabbing bucket (13 m wide when opened and weight of 125 t), excavating 25 m .
By introduction of this powerful grab dredger, tremendous amount of seabed soil
was securely excavated even in fast tidal c u r r e n t in shorter period, Besides,
even hard bedrock was found to be possibly excavated by this large powerful
bucket claws, which greatly effected on blasting technology preceding to
excavation. In other words, it was only necessary to create through-cracks in
bedrock to be excavated by large pitches of explosives charged in holes.

Concrete Works
In order to proceed major concrete work of Honshu Shikoku Bridge construction
at sea, a mortar plant barge, 90 m length, 32 m width, 7.5 m depth, 4.5 m draft
and 11,500 t displacement, was built, installed with all machinery and supplies.
The mortar plant consists of 3 lines of the plants of an output of 2,000 lit/min
each, the 2 lines of which are normally used while leaving the other line as
backup. Twenty four mortar pumps are incorporated, among which 20 pumps are
used at 200 lit/min x 20 units = 4,000 lit/min, leaving the other 4 pumps for
backup and cleaning, etc.

The prepacked concrete method was used for the concrete work of undersea
foundations for major concrete works of Honshu-Shikoku Bridge construction for
secure casting of large amount of high quality concrete. In concrete works,
particular attentions were placed on (1) quality of aggregates as well as mortar
, (2) workability or liquidity of mortar so that no spacing between coarse
aggregates should be left, (3) robustness, and (4) thermal s t r e s s control. There
are some trade-offs between above required characteristics so that the optimum
proportion of various mixtures have been sought through experiments.

A fleet of mortar injection barges comprise a main barge of mortar plant together
with material supply barge loaded with cement, sand, water, etc. and work barge
loaded with overflow water treating facilities. And as much as 12,000 tons of
mortar material was used per day, cement and sand were transported using
cement tanker of 2,000 to 3,000 tons and barge of 3,000 m . Since mortar injection
work continued to a maximum of 3 days and nights, for which 150 engineers and
300 workers a day were required. Note that there is no more important than
education and training of personnel for operation of machinery to prevent failure.

Large Block Erection of Superstructures

In a last few decades, large block erection method has been frequently used in
Japan for construction of bridges of various types near sea coast or wherever
floating crane was able to access to the construction site. A majority of bridges
in Honshu-Shikoku Connecting Route being constructed in Seto Inland Sea, the
large block erection method is particularly effective as erection method for
s u p e r s t r u c t u r e s . Advantages to use large erection method are for example the
followings;

(a) alleviation and simplification of construction works at the sites

(b) reduction of period required for construction work at the sites
(c) reduction of the number of fastening or joints at the sites
(d) simplification of construction facilities and machinery at the sites
(e) assurance of safety due to progression of quality and accuracy of
constructed s t r u c t u r e s
24
This large block erection method is so effective if construction plan be made
carefully and all preceding works be made without any delay. For construction
of Seto Bridge, the large block erection method was frequently used for
construction of various types of s t r u c t u r e s including laying-down caissons, p a r t s
of pylons of suspension bridges and cable-stayed bridges, girders of cable-
stayed bridges and t r u s s girders. The maximum weight of one block at
construction of Seto Bridge reached to 6100 tons, carried by two floating crane
boats. However it should be noted that disadvantage of this large block erection
method was to be largely influenced by weather conditions.

The Vibration Attenuator

For a certain period for construction of suspension bridge, tower stands freely
and it is so fexible like a cantlever that it vibrates laterally in longitudinal
direction of bridge axis. As the results of wind tunnel tests, amplitude of vortex
induced vibration in deflectional mode is expected to reach to several meters at
the top of tower and amplitude in torsional mode to reach to more than 5 . For
Seto Bridges, two kinds of attenuators were used, namely (1) a combination of an
oil damper and a weight and (2) a sliding block system. Both the oil damper
system and the sliding block system were used in both South Bisan Bridge and
North Bisan Bridge. For construction of Akashi Strait Bridge, new counter-
measure system for vortex-induced vibrations is now going to be used, namely
tunned mass damper system.

Cables and Cable Erection

There are two different kinds of bridges constructed for Honshu-Shikoku Bridges
of which cables are used as main structural p a r t s , namely suspension bridge and
cable-stayed bridge.

Cable is the most important structural and mechanical p a r t of suspension bridge

to carry both its own weight and all sort of live load to transmit them to
foundations via pylons, The S.B.B. (South Bisan Bridge) cable has the largest
diameter of 1.070 mm among Seto Bridges and receives the effective axial tensile
force of 44,700 tons. The wires of 4 mm in diameter were wrapped around the
circumference of the cable to be painted to be corrosion proof for long period.
Cable bands were installed at the interval of about 13 m to hang the stiffening
girder by hanger ropes with saddles. For both S.B.B. (South Bisan Bridge) and
N.B.B. (North Bisan Bridge), main cables consist of prefabricated parallel wire
strands (termed as the P.S.method), while for S.B. (Shimotsui Seto Bridge) the
aerial spinning method (termed as the A.S. method) was used. In the P.S.
method, 127 wires of 5 mm in diameter were preliminary bundled to form a strand
in the factory and the strand was rolled around a reel to convey to the site. 271
strands for S.B.B. and 234 s t r a n d s for N.B.B, respectively, were bundled to make
a main cable. Thus the number of wires is 127/strand x 271 strands = 34,417 for
S.B.B. And at the site, four wires were drawn out at the same time and 552
wires were bundled as one strand. For S.B., 44 strands were bundled to a main
cable, thus the number of wires per cable is 552/strand x 44 = 24,288. A small
mechanical difference is noticed between the P.S. method and the A.S. method but
significant difference between two methods remains for total number of s t r a n d s
and results in difference for strand fixing area at the anchorage. This was one
 25
of the reasons that the aerial spinning method was employed for the Shimotsui
Seto Bridge, since cable anchoring area was so restricted at the Honshu side.

Cables for the cable-stayed bridges are as well known very different from those
for suspension bridges. For cable-stayed bridge, each cable was manufactured
in the factory according to the design requirement to transport to the c o n s t r u c -
tion site. A cable for cable-stayed bridge consists of the required number of
galvanized steel wires of 7 mm in diameter, sockets (Hi-Am anchor) and P.E. pipes
(polyethylene covering tube). Galvanized steel wires were made of heat treated
extended wires. Each wire was so cut to keep the designed length precisely and
a bundle of predetermined number of wires was formed in approximately parallel
and wrapped with a spacer strand in a spiral form, covered with a polyethylene
pipe. Both ends of wires, heat treated, were fixed together with molding epoxy
resin, zinc powder and steel ball in the sockets. After molding the cable, it was
heated, fiUed with tar-epoxy in the P.E. pipe. The outer surface of the socket
was coated with inorganic zinc rich primer.

For construction of Honshu-Shikoku suspension bridge, a particular attention was

placed on the cable erection method since bridge s t r u c t u r e s were so large and on
the other side the period for construction was so limited. Cables were successful-
ly erected by the P.E. method for the first time in the world for suspension
bridges of more than 1000 m of center span length by means of well organized
quality control system for construction. For cables of cable-stayed bridges, one
should note that variation of induced tensile forces for cables was expected to be
much larger to compare with the variation of induced tensile forces in cables of
suspension bridges and much attention was therefore required on fatigue
resistance of each cable at fixing point of socket. In addition to the above
mentioned problems, the Seto Bridge was required to function as both highway
and railway bridge, so the fatigue problem of cables was of the primary
importance. This was the main reason that Hi-Am anchor socket was extensively
employed for cable^stayed bridges of Honshu-Shikoku Bridges.

TRAFFIC CONTROL & MAINTENANCE SYSTEM

T e s t s for actual b r i d g e s

In design stage, number of mechanical parameters have been assumed to certain

values based on large amount of documented data for constructed bridges in
Japan and also in many foreign countries. For example, wind resistant safety of
Honshu-Shkikoku bridges is largely dependent on damping capacity of both
deflectional and torsional modes of vibrations of suspension bridges and cable
stayed bridges. Thus the vibration test was performed by use of newly
developed vibrators to examine the vibrational characteristics of actual bridges.
The first test was performed for the Ohnaruto bridge and for the Seto Bridges
the tests were made for South Bisan Seto Bridge as suspension bridge and for
Hitsuishi Island Bridge as cable stayed bridge. Displacements, frequencies and
damping capacity were measured by means of number of sensors such as
accelerometers installed at bridges and data were processed on-line. The
displacement of a girder was measured at points L/2 (central point) and L/4
(quarter point) of center span by use of an optical displacement meter.
26

The Seto Bridge was designed and constructed not only as express highway
bridge but also as high-speed railway bridge by introduction of transition girder
expansion joint. In order to examine the function of transition girder expansion
joint and to clarify operational characteristics of train running on railroad on
bridges, the train running tests were undertaken to investigate particularly the
comfort and safety against derailment. Four trains were used and the heaviest
train was 1000 tons. The test trains run on railroad at the maximum speed of 120
km/hour. The results of this test confirmed the safety for train travelling on this
large size bridges.

Traffic Control and Maintenance System

For traffic control and maintenance for Seto Bridges, the following systems were
developed;

Information Collection System

Information Processing and Display System
Information Supply System
Bridge Behavior Observation System
Inspection Vehicle
Security System

The information collection facility consists of (1) a traffic counter to measure

traffic capacity, car speed and exclusive ratio, (2) weather observation system to
measure rain and snowfall, wind direction as well as wind speed, the field of
vision and freezing on the road ,(3) camera to monitor vehicle flows and traffic
accidents and emergency telephones to obtain the information of accidents or
troubles and (4) seismometer. The information from sensors is collected at the
Central Station of information processing and display system, processed and
recorded on the graphic panel, weather monitoring panel or printer to be used
for traffic control. Each kind of highway information that has been collected and
processed, is supplied to drivers on the highway by use of highway information
display and communication system, for example to introduce the car velocity
regulation depending on the weather conditions.

The Seto Bridge consists of three suspension bridges, two cable stayed bridges
and some other types of bridges to span approximately 10 km between Honshu and
Shikoku Island. The bridge behavior observation system was established to
observe mainly dynamic behavior of bridges under action of earthquakes and
typhoons. The quantitative records of various sensors such as seismometers,
acceleration meters, anemometers and displacement meters are collected and
transmitted to the Sakaide Operation Office.

CONCLUDING REMARKS

In this paper the frontiers of Honshu Shikoku Bridges are briefly reviewed and
some fundamental problems investigated in connection with this project are
presented. Stresses were placed on investigations connected with design and
developments of construction methods of long span suspended bridges. During
last few decades there were significant p r o g r e s s in fabrication of structural
steels including cable fabrication and welding technologies. Computer-aided
construction technologies have been also progressed and it is interesting to note
 27
that introduction of new powerful construction machinery has changed the
construction method itself and development of defect detector has revealed
number of causes to produce defects. However note that design and construction
of so highly elevated and so long s t r u c t u r e s as suspended bridges are still
accompanied with unsolved problems. A typical example is wind-induced
vibrations of the Akashi Strait Bridge. A few month ago (in March, 1991) a super
large size of wind tunnel was constructed to examine aerodynamic behavior of this
suspension bridge.

The coming ten years are considered the last stage of construction of Honshu-
Shikoku Connecting Bridge. The Honshu Shikoku Bridge Authority devotes its
major efforts to construction of Akashi Strait Bridge of 3,910 m (960 + 1990 + 960
m), the longest suspension bridge in the world, and construction of bridges of
western route, Imabari route. And by the end of the twentieth century, three
routes will have been connected by a number of newly constructed bridges. It
should be mentioned however that a number of technical problems would be
investigated for clarification even at this moment. And development of various
new technologies in connection with the Honshu-Shikoku Bridge Construction
Project is not only limited advancement for bridge engineering but for other field
of engineering. In the field of bridge engineering, there are a dream of
construction of super long span bridges such as the Messina suspension bridge
in Italy, the Gibraltar suspension bridge at the gate of the Mediterranean Sea, the
Kitan Strait bridge in Japan, etc. It is hard to anticipate when and how these
projects can be possible, but these dream will come out in reality if one could
reveal the encountered problems substantially. And any dream of super long
bridge in future is considered to be successfully constructed only by human
wisdom and cooperation of people from academia, governments, industries,
e t c . t h r o u g h o u t nations.

ACKNOWLEDGEMENT

The author would like to express his sincere thanks for cooperation of the Honshu
Shikoku Bridge Authority for preparation of this paper. Particularly the author
would like to appreciate Mr. Yasuda, the chief of Design Section of Honshu
Shikoku Bridge Authority, for his comments on the manuscript.

REFERENCES
Ishiyama, S. (1988). Technical Development and Construction of Honshu Shikoku
Bridges, Japan Construction Information Center, Vol.3, No.l, 1988, pp 30-36
The Bridge and Foundation Engineering, Special Issue on Honshu Shikoku Bridges
Vol.18, No. 8, 1984,
The Seto Ohashi Bridge (1988), Honshu Shikoku Bridge Authority
The Seto Ohashi Bridge and Foundation (1988), Honshu Shikoku Bridge Authority
 WS1a1

FROM THERMODYNAMCAL STATE COUPLINGS

TO COMPUTATIONAL ANALYSIS
OF PLASTICITY DAMAGE AND MICROSTRUCTURE

Jean. LEMAITRE
Prof. Universite PARIS 6,
L.M.T.
61, Avenue du President Wilson,
94 230CACHAN, FRANCE.

This paper is a review of works listed in references and related to the modeling of phenomena
interacting each other in materials when subjecting to varying loadings and temperature. As
most of details have been published, only the main ideas are developed here.

THE STATE KINETIC COUPLING THEORY CONSISTS IN THE

FOLLOWING STEPS:

- Identify the phenomena to be considered.

- Determination of the main mechanism involved.

- Analysis of micromechanical models to define a state variable Vj for each phenomenon, I.

- Qualitative experiments on specimens to decide which coupling exists between the phenomena
considered at the level of the state variables.

- This alows to write the state potential, the Helmholtz free enregy V for example, to define
the associated variables Ai to the state variables

AI=PMYI)
a A
I (P being the density)

- Qualitative experiments to observe if an associated variable Aj or a state variable Vj

influences the kinetic evolution of a state variable Vi.

31
32

- This allows to write the potential of dissipation P from which derive the kinetic laws of
evolution of the state variables

. = ap(Ai;Vi)

- Analysis of micromechanical models to guide the proper mathematical expression for the
potential P.

- Quantitative experiments to identify, for each material, the coefficients which appaer in the
function 9.

- Last, but not the least! checking the constitutive equations with specific experiments as
different as possible from the experiments of identification.

This procedure has been applied to elasticity, plasticity, or visco-plasticity, damage, aging,
change of microstructure etc...

* The coupling of damage on elasticity is the bassis of damage mechanics which gives rise to
the measurement of damage by means of change of elasticity modulus.

* The coupling of damage on plasticity is a softening process which gives rise to localization
of damage and finaly crack initiation. It is also the basis of measurement of damage by means
of change of microhardness.

* The coupling of aging on plasticity is an hardening process varying with time up to a stady
state.

* The coupling of micro-structure on plasticity allows to model the processes of quenching

and casting of metals.

THE IMPLEMENTATION OF SUCH CONSTITUTIVE EQUATIONS IN FINITE

ELEMENT CODES GIVES RISE TO DIFFICULTIES RELATED TO THE CHOICE OF
THE INCREMENTAL PROCEDURE AND THE CHOICE OF THE MESHE SIZE :

- The constitutive equations are a set of nonlinear differential equations which have to be
integrated step by step in time. The choice of the time or load increment is usually made by
heuristic procedures. The algorithms used to integrate the highly nonlinear constitutive
equations must be "strong" relative to stability.
Implicit integration schemes with a Newton iterative method are prefered.
The local integration of the constitutive equations is performed by using an "elastic predictor"
to calculate the first increment as elastic and a "plastic corrector" to ensure by iterations that the
plasticity criterion and kinetic laws are satisfied up to a certain imposed accuracy.
In order to compute the tangent stiffness matrix of the srtucture at each iteration, a tangent
modulus J consistent with the discretization, calculated as

£<7ij=Jijkl&kl
is used instead of
<Xij=Lijkl£kl

This ensures a much better convergence.

 33

- As to the space discretization is of concern, the convergence regarding the mesh size is of
the same order of difficulty as for classical elasto-plastic calculations up to the crack initiation
that is just before the localization of damage. Afterwards, the problem is no longer elliptic,
its solution involves strain rates discontinuities which cannot be modelled by classical finite
elements. This is the reason why several special concepts have beeen developed such as non
local theories of damage, shearband elements.

- When a periodic loading is considered, as for fatigue, it is not possible to perform the
tremendous amount of increments needed for all of the thousands, or millions of cycles. A
method to save computer time is to use a procedure with "jump in cycles" which avoids
calculating the stress-strain.cycles when the process is a quasi-steady state.

Many applications have been made to model complex processes such as :

- Fatigue of a presurised pipe plastically predeformed and damaged by accident

- Study of a field of aging in a srain hardened structure.

- Crack initiation near a hole in a notched structure submitted to varying thermal stresses at
high temperature.

- Quenching of a super alloy.

- Solidification and residual stresses during a process of casting.

34

BIBLIOGRAPHY

- Abdel-Raouf, H. Plumtree,A. & Topper, T.H. (1974). Temperature and strain rate
dependence of cyclic deformation response and damage accumulations. Met.Trans.,Vol.5,
267.
- Aifantis, E.C. (1985). Mechanics of microstructures. In : Mechanical properties and
behaviour of solids : plastic instabilities. (V.Balakrishnan et al ed). World Scientific.

- Bazant, Z.P. (1989). Stable states and stable paths of propagation of damage zones :
inelastis stability, criteria with applications. In : Strain localization and size effect due to
cracking damage. (J.Mazars and Z.P.Bazant eds). Elsevier.

- Belytschko, T. , Fish, J. &Engelman, A. (1988). A finite element with embeded

localization zones. Comput. Maths Appl. Mech. Engng, 70^ 59-89.

- Benallal, A. & Marquis, D. (1987). Contitutive equations describing nonproportional

loadings. Journal of Engineering Materials and Technology, Vol. 10, 326-336.

- Benallal, A. (1989). Thermoviscoplasticite et endommagement des structures, These

Doctorat es Sciences, Universite Paris 6.

- Benallal, A. ,Florez,J. & Geymonat,G .(1987). Contunuum mechanics and Nash non-
cooperative equilibria : numerical implications. In : Numerical methods in fracture mechanics.
(A.R.Luxmore et al eds). Pineridge Press, 353-367.

- Benallal, A. , Billardon, R. & Lemaitre, J. (1984). Failure analysis of structures by

continuum damage mechanics. ICF 6-Dehli. (S.R.Valluri et al eds)..Pergamon Press, 5,
3669-3676.

- Benallal, A. Billardon, R. & Doghri, I. (1988). An integration algorithm and the

corresponding consistent tangent operator for fully coupled elastoplastic and damage
equations. Com. Appl. Numer. Meths., 4, 731-740.

- Bencheikh, A. (1987). Elastoviscoplasticite a temperature variable. These de Doctorat de

l'Universite Paris 6.

- Billardon, R. (1988). Numerical approach to crack initiation by continuum damage

localization. IUTAM Sympsium on Recent advances m non-linear fracture mechanics,
Pasadena.

- Billardon, R. (1989). Etude de la rupture par la mecanique de rendommagement. These de

Doctorat es Sciences de TUniversite Paris 6.
- Bodner, S.R. Partom, Y. (1975). Constitutive equations for elastic viscoplastic strain
hardening materials, Journal of Applied Mechanics, Vol. 42, 385-389.
- Budiansky, B. & O'Connell, R J . (1976). Elastic moduli of cracked solid. Int. J. Sol.
Struct.,12, 81-97.

- Bui, H.D. & Ehrlacher, A. (1981). Propagation of damage in elastic and plastic solids.
ICF 5 Cannes, 533-551.

- Cailletaud, G. & Chaboche, J.L. Macroscopic descrition of the microstructural changes

induced by varying temperature : example of IN 100 cyclic behaviour. Proceedings ICM3 (ed.
KJ.Miller et R.F.Smith), Vol 2, 23.
 35

- Cailletaud, G. ,Kaczmarek, H. & Pollicella, H. (1984). Some elements on multiaxial

behaviour of 316 stainless steel at room temperature. Mechanics of Materials, Vol. 3.

- Chaboche, J.L. (1978). Description thermodynamique et phenomenologique de la

viscoplasticite cyclique avec endommagement These de Doctorat d'Etat, University Paris 6.

- Chaboche, JX. (1987). A review of computational methods for cyclic plasticity and visco-
plasticity. In : Computational plasticity : models, software and applications. (D.R.J.Owen et
aleds). Pineridge, 379-411.

- Cocks, A.CJ7. & Leckie, (1986). FA. Creep constitutive equations for damage materials,
Theoretical and Applied Mechanics, University of Illinois at Urbana-Champaign, Report 480.

- Dafalias, Y.F. & Popov, E.P. (1975). A model of nonlinearly hardening materials for
complex loadings. Acta Mecanica, Vol. 21,173-192.

- Germain, P. NGuyen, Q.S. & Suquet, P. (1983). Continuum thermodynamics. J. Appl.

Mech. A.S.M.E., 50, 1010-1020.

- Halphen, B. & NGuyen, Q.S. (1975). Sur les materiaux standards generalises. J.
Mecan., 14 39-63;

-Hansen, N. &Leffers, T. (1988). Microstructurtes, textures and mechanical properties

after large strain. Revue Phys. Appl., Vol 23,519.

- Hayhurst, D.R. et al. (1983). Developement of continuum damage in the creep rupture of
notched bars. The role of continuum damage in creep crack growth. Deparmental reports,
Dept. of Engineering, University of Leicester.

- Hermann, G. & Kestin, J. (1989). On thermodynamic foundations of a damage theory in

elastic solids, Cracking and damage. (Ed. J.Mazars et Z.Bazant), Elsevier.

- Hult, J. (1974). Creep in continua and structures, Topics in Applied Continuum Mechanics
(Leman, J.L. , Ziegler, F. Editors), Springer Verlag, 137-155.

- Hutchinson, H. & Tvergaard, V. (1980). Surface instabilities on statically strained plastic

solids. Int. J. Mech.Sci., 22, 339-354.

- Inoue, T. (1988). Inelastic constitutitve relationships and applications to some

thermomecanical processes involving phase transformations. Thermal Stresses, (Ed.
R.B.Helmarski), Elsevier.

- Inoue, T. et al. (1981). Description of transformation kinetics. Ing. Arch., Vol 50, 315.

- Kachanov, L.M. (1958). Time of the rupture process under creep conditions. T.V.Z.
Akad.Nauk. S.S.R. Otd. Tech. Nauk.,8, 26-31.

- Krajcinovic, D. & Sumarac, D. (1989). A meso-mechanical model for brittle deformation

processes. J. Appl. Mech., A.S.M.E., 56, 51-62.

- Krempl et al. (1985). Viscoplasticity theory based on overstresses. Int. J. of Plasticity,

Vol. 1, 259.

-Ladeveze, P. &Lemaitre, J. (1984). Damage effective stress in quasi-unilateral

conditions. IUTAM Conference, Lyngby.
36

- Ladeveze, P. (1983). On an anisotropic damage theory. In : Failure criteria of structural

media, (CNRS ed.).

- Lemaitre, J. & Chaboche, J.L. (1990). Mechanics of solid materials. Cambridge

University Press.

- Lemaitre, J. & Dufailly, J. (1987). Damage measurements. Engng. Fract. Mech.,28

(5/6), 643-661.

- Lemaitre, J. (1987). Micro-mechanics of damage kinetic constitutive equations. In:

Continuum damage mechanics : theory and applications, (D.Krajcinovic & JLLemaitre eds.),
Springer Verlag.

- Lemaitre, J. (to be published in 1991). A course on damage mechanics. Springer Verlag.

- Mac Dowell et al. (1988). Biaxial path dependence of deformation substructure of type
304Stainless Steel. Met. Trans., Vol. 19A, 1277.

- Marigo, J.-J. (1985). Modelling of brittle and fatigue damage for elastic material by growth
of micTOvoids. Engng. Fract. Mech.,21,861-874.

- Marquis. Didier.( 1989). Phenom£nologie et thermodynamique : application aux couplages

entre thermo61asticite\ plasticite, endommagement et vieillissement. TTiese Doctorat es
Sciences, University Paris 6.

-Mazars, J. &Berthaud, Y. (1989). An experimental technique applied to concrete to obtain

distributed damage. C.R. Acad. Sci. Paris, t. 308, Serie II, 579.

- Mazars, J. Saouridis, C. & Billardon, R. (1986). Determination de rendommagement

local en fonction de l'etat au voisinage. Rapport Scientifique du GRECO Rheologie des
geomat&iaux.

-Murakami, S. (1983). Notion of continuum damage mechanics and its application to

anisotropic creep damage theory. Journal of Engineering Materials and Technology, Vol.
105,99-105.

-Murakami, S. , Kawai, M. &Rong, H.. (1988). Finite element analysis of creep crack
growth by a local approach. Int. J. Mech. Sci., 2Q, 69-85.
- Needelman, A. (1988). Material rate dependence and mesh sensivity in localization
problems. Comp. Meths. Phys. Solids, £7, 69-85.

- NGuyen Q.S. & Triantafyllidis. (1989). Plastic bifurcation and post bifurcation analysis
for generalized standard continua.

-Ortiz, M. & Popov, E.P. (1985). Accuracy and stability of integration algorithms for
elastoplastic constitutive equations. Int. J. Numer. Meths. Engng., 21, 1561-1576.

- Owen, D.R.J. & Damjanic, F. (1982). Viscoplastic analysis of solids : Stability

considerations. Recent Advances in Non-Linear Computational Mechanics, Pineridge Press.
- Perzina, P. (1976). On the constitutive equations for work-hardening and rate sensitive
plastic materials. Bulletin de rAcad£mie Polonaise des Sciences, SerieSc. et Tech., Vol. 2,
159-171.
 37

- Pijaudier-Cabot, G. &Bazant, Z.P. (1986). Non-local damage theory. Northwestern

University, Evanston, Report 86-8/428n.

- Ponter, A.R.S. (1976). Constitutive equations for the time-dependent deformation of

metals. Journal of Engineering Materials and Technology.

- Rice, J.R. & Rudnicki, J.W. (1980). A note on some features of the theory of localization
of deformation. IntJ. SolidsStruct. J6, 597-605.

- Rousselier, G. (1981). Finite deformation constitutive relations including ductile fracture

damage. In : Three-dimensional constitutive relations and ductile fracture. North-Holland,
331-355.

- Sjostrom, S. (1985). Interactions and constitutive models for calculating quench stresses in
steel. Materials Science and Technologie, Vol. 1, 823.

-Stolz, C. (1987). Anelasticite et stabilite. These de Doctorat es Sciences, Universite Paris

6.

- Tvergaard, V.., Needleman, A..& LO, K..(1981). Flow localization in the plane strain
tensile test. J. Mech. Phys.Solids, 29, 115-142.
WS1a2

A GENERAL THEORY OF DEFORMATION AND DAMAGE OF SOLIDS

C. C. Hsiao

Department of Aerospace Engineering and Mechanics, University of Minnesota

Minneapolis, MN 55455, U. S. A.

ABSTRACT

Using an energy consideration, the concept of a time-dependent theory of deformation and

damage of solids is put forward. The total critical volumetric energy in any solid system must
be overcome for fracture initiation. In this report, microscopic kinetic behavior of the material
constituents is considered. Volumetric damages by submicroscopic fracturing of the molecular
bonds are evaluated statistically as functions of time. The minimum potential energy state of
the solid represents the stable conformation of the structural system, while the maximum
critical energy governs the non-equilibrium time-dependent damage behavior of the solid.

KEYWORDS:

Deformation, damage, strength, fracture, microstructure

MODEL AND THEORY

A material body is held together as a system of randomly oriented molecular bonds visualized
as microelements in equilibrium when unloaded, possessing a fixed conformational potential
energy. With prescribed stresses the system deforms and the microconstituents engage and
disengage repeatedly according to a kinetic rate process which alters the state of equilibrium.
Under extreme stresses when a certain portion or a fraction of the microconstituents disengage,
damage of the system will result. If f represents the fraction of the engaged constituents, then
the fractional damage will be 1-f. Thus f may be referred to as the fraction of integrity of the
solid system. When f approaches zero, the system fails. If £ 0 *s initially the specific internal
energy of the system, the small amount of specific strain energy of a group of unidirectionally
oriented representative constituents will be given as

f\|/de (1)

39
40

where \|/ is the stress along each individual constituents with de its infinitesimal extension. For
the whole system, the total specific energy can be obtained through integration with respect to
the infinitesimal solid angle do):

£ = J p ( £ o + J fyde)dco

= J P&> + 5c)d<D (2)

where £ c is the specific strain energy of the constituents and p is the distribution function of
constituent orientation which depends on the state of straining rather than the simple extension
only. The damage theory may be stated as: when the total critical specific energy ^ is
overcome, damage initiation will occur.

For a system of constituents under stress and deformation, the total energy density is
expressible as

5 = JcTijdeij (2)

where ay and ey are respectively the stress tensor and the strain tensor. The stress tensor in
the vicinity of a point for such a model system may be written [1-4] with unit vectors Si and SJ:

cry = J p\|/fsiSjdco . (4)

Then from (3), one gets by substitution

£ = J J pyfsiSjdcodeij. (5)

This can be further correlated with the statistical absolute reaction rate theory and dilatational
consideration [1,5].

The variation of the total energy must vanish for the initial equilibrium condition when p=p 0
and ^c=0> then df/dt=0 and the variation of (2) yields: p=po- When £o*0> i-e., the system is
in such a strained or deformational state that

P = r^Vpo (6)

Substituting (6) into (5), the corresponding specific energy state becomes

S = J J 7 % ~ poVfsiSjdco0d£ij (7)

where dco0 is the infinitesimal solid angle in the initial state. Assuming that when the system is
in its deformed state, then this specific energy is representable to a first approximation as some
function O of the specific mean free volume v in place of the nine strain components which
 41

identify the volume change. Here v is the difference of the specific current configuration
volume and the specific initial conformational volume. Analytically, we may write as follows:

S = 3>(v). (8)

Now if O is represented by a series, then the following relationships exist.

oo oo

S(v)= £ anv" or X a n v". (9)

n=-«o n=o

Using rectangular tensor notations with the summation convention, the general damage theory
may be represented in the following series form to take into account the temperature and time-
dependent variation of the dilatation of an anisotropic material system.

£(x, T, t) > £ an ccii9(T) + J JiikKC - *n) a k l ( x , x ) dx (10)

where the various symbols represent quantities as given below:

£ magnitude of the energy per unit volume,

x coordinates in current frame of reference,
T absolute temperature,
t real time,
an expansion coefficients representing different characteristic
parameters
n integers (-00 < n < «>),
an summation of the linear thermal coefficients of expansion,
0(T) thermal function,
_r
Jiikl(C l) anisotropic time-dependent bulk compliances function, with
£=t<|)(T) and T|=T<|>(T) as the shift times defined by the
temperature-time shift function <|)(T) for thermorheologically
simple viscoelastic media,
x time parameter,
tfij> CTki stress tensors, and
Oki time derivative of the stress tensor with respect to x.

The energy density can be reduced to the following forms for homogeneous viscoelastic
material systems:

t
4(T,t)>Ia n 3aoe(T)+Jj2(C-Ti)okk(x)dx (11)
42

where the various additional symbols represent quantities as given below:

n integer (o < n < °o)

oc0 the linear thermal coefficients
J2(C_Tl) time-dependent bulk compliance function, with £=t((t)(T) and
r)=T(|)(T) as the shift times defined by the temperature-time shift
function <|)(T) for thermorheologically simple viscoelastic media,
G\± summation of normal stress components, and
o\± time derivative of the normal stress components with respect to
x.

It may be of interest to explore further the consequences of the formulation arrived at thus far.
Since many strength and damage theories have been intensively investigated and studied for
time-independent elastic material systems at a constant temperature, the above equation may be
further reduced for a reference temperature T 0 . In that case, for thermorheological linear
viscoelastic media (|)(To)=l, 6(T o )=0 and h(£>-T]) reduces to J2(t-x). Thus Equation (11) can
be reduced to

oo

S(To)= X an[aii(T0)/3K]n (12)

n=o
where K is the elastic bulk modulus. Now from the above formulations, the critical energy can
be plotted in general against the specific volume as shown in the upper portion of Fig. 1. This
curve can be correlated with the simple stress-strain behavior as shown in the lower portion in
Fig. 1.

It is seen from the energy-free volume curve that there are several energy quantities
corresponding to different specific mean free volume values. O(v 0 ) represents the lowest
critical energy or the minimum potential energy of the system for which the solid system is in
its stable state without deformation. When stresses are applied, the specific mean free volume
V2 identifies a maximum critical energy state 3>(v2) for which damage due to crazing and
subsequent fracturing will occur. For complex composite systems, the critical energy may
vary according to the arrangement of the composite microstructure and the failure mechanism
of the system. Additional minima and maxima may develop. Reducing to the simple stress-
strain behavior as shown, the initial undeformed state corresponds to the minimum critical
energy state for which there is no volume change and there is no damage of the material
system. However, for damage initiation both yielding or crazing and fracturing may be
identified.
 43

crazing

->■ v
specific mean .free volume

a crazing ^
to 1 k
GO
! ^i- — /
CD
v_
"GO
/^"^ fracturing
0) ^yielding
00
c
a)
CD

E
co

0 ^
simple tensile strain

Fig. 1 Schematic Connection Between Generalized

Damage Theory and Simple Stress-Strain Behavior.
44

SUMMARY

This critical energy-specific mean free volume theory may be stated for stable and damage
states as:

£><*>(v)
For both stable initial state and failure damage state

£-0
dv
from which several values of the specific mean free volume may be obtained. For v=v 0 , ^(vo)
is the minimum; the system is stable and undisturbed. For v=V2, 3>(v2) is a maximum, the
system is unstable under stresses. For v=vi, <I>(vi) represents the inflexion energy point for
which the second derivative of the energy with respect to the specific mean free volume
vanishes. In this case, it can be verified to satisfy the conditions of yielding that the material
system deforms without additional stressing.

REFERENCES

Hsiao, C.C. (1959) Theory of mechanical breakdown and molecular orientation of a model
linear high-polymer solid. J. Appl. Phys. 30, 1492.

Hsiao, C.C. (1960) Time-dependent tensile strength of solids. Nature 186, 535.

Hsiao, C.C. (1966) Fracture. Physics Today 19, 49.

Hsiao, C.C. (1989) Kinetic strength of solids. In: Advances in Fracture Research,
Proceedings of the 7th International Conference on Fracture (ICF7), Houston, Texas,
March 20-24, 1989, 2913.

Graham, P.H., Robinson, C.N. and Henderson, C.B. (1959) Analysis of dilatational failure
of heterogeneous materials by reaction rate theory. Int. J. Fracture Mechanics 5, 57.
 WS1a3

AN INTERNAL VARIABLE APPROACH FOR ELASTIC PLASTIC ANALYSIS

IN THE PRESENCE OF DAMAGE *

A. NAPPI

Istituto di Scienza delle Costruzioni - University of Trieste

P.zza Europa 1 - 34127 Trieste - Italy

ABSTRACT

The paper deals with the finite element quasi-static inelastic analysis of
structural systems made of an elastic-plastic material possibly affected by
damage. An internal variable approach is followed for the relevant stepwise
nonlinear elastic numerical analysis. A solution technique is proposed, which
provides the response to any load increment without modifying (during each
step) the stiffness matrix by means of convenient variables related to
damage. Hence, the material is treated as elastic-plastic and convergence of
properly selected algorithms is guaranteed under convenient hypotheses
concerning the material behaviour, as easily proved on the basis of the
framework developed within the context of the classical theory of plasticity.

KEYWORDS

Backward difference; convex analysis; damage mechanics; finite elements;

internal variables; mathematical programming; plasticity.

INTRODUCTION

Within the context of damage mechanics the process of crack growth can be
described through internal variables (Lemaitre and Chaboche, 1978; Lemaitre,
1985; Mazars, 1984, 1986) related to the material loss of stiffness and/or
strength. According to this approach, defects are assumed as smeared in the
continuum. Hence, their effects are described in an average sense and stress-
strain relationships are also introduced in terms of average quantities.
It is well known that internal variables are currently utilised also in the
framework of elastic-plastic analysis (Kestin and Rice, 1970; Germain, 1973;
Martin, 1975 and 1981; Martin and Nappi, 1990). Indeed, internal variable
formulations of the constitutive equations of plasticity offer potential
advantages when we try to introduce a unified basis for the development of
the mathematical theory of plasticity. Of particular interest, under this

Paper dedicated to Professor Giulio Maier on his sixtieth Anniversary

45
46
point of view, appears to be an approach due to Martin (1975, 1981). It
allows one to describe the material behaviour on the basis of two functions:
the elastic energy (Helmoltz free energy) and the specific dissipation within
an elementary volume of an elastic plastic solid. A characteristic feature of
this approach is represented by the definition of an internal stress vector f
conjugate to the vector of internal variables (say w), such that the scalar
product f w gives the dissipation rate. As pointed out in the paper, the re-
levant implications are quite important. In fact, under convenient hypotheses
concerning the material behaviour some extremal properties can be proved for
the stepwise holonomic (reversible, nonlinear elastic) problem which is to be
solved in order to evaluate the structural response numerically (Martin et
al., 1987; Martin and Reddy, 1988; Nappi, 1991). Indeed, the solution of
certain holonomic elastic-plastic problems also minimises convenient
unconstrained functions and, as a consequence, convergence towards the
correct solution is guaranteed for properly selected algorithms.
The paper is aimed at discussing the inelastic analysis of structural systems
subjected to quasi-static loading conditions in the presence of the combined
effects due to damage and to plastic residual strains. The analysis is
carried out by using the finite element method and by assuming (as usual) a
nonlinear elastic behaviour during each time step (i.e., for each increment
of the applied loads). A convenient elastic domain is considered and, during
each step, inelastic strains are determined by assuming an associated flow
rule. On the other hand, no damage parameter is required as an explicit
variable in order to modify the stiffness matrix during each time-step.
Hence, the structural problem is solved as if the material were
elastic-plastic (which seems to be a non-traditional way of dealing with
materials subjected to damage). The proposed method gives the opportunity of
applying all the algorithms developed within the theory of plasticity. In
addition, under convenient limitations, extremum theorems and convergence
properties found in elastic-plastic analysis can be fully recovered.
Possible applications to concrete structures and to masonry constructions are
discussed. Finally, the close correlation between the numerical results
obtained by using damage mechanics and the actual response of concrete
specimens or masonry panels is pointed out.

THE INCREMENTAL ELASTIC-PLASTIC PROBLEM

Let us follow an internal variable approach due to Martin (1975, 1981) and
generalised by Martin and Nappi (1990) in order to include both kinematic and
isotropic hardening. For a structural system the governing equations read

Ku + Lw = P , L T u + H w + t(w) = - f (la,b)

where u denotes displacements, w internal variables related to inelastic

strains, P external loads and f internal forces conjugate to w. Indeed, along
any structural member or at any strain point where we determine the stress
state, we can conceive an elastic perfectly plastic slip device where energy
may be dissipated. At any time t, the dissipation rate is given by

D1 = {f 1 } 7 w1 > fl = aDVdw 1 for wl * 0 , fl € 5Dl for w1 = 0 (2a,b,c)

with i = 1 n and n = total number of strain points. Clearly, the vector f
in (lb) is made of n subvectors f as defined by Eqs. (2b,c). Eq. (2c) shows
that f is an element of the subdifferential of D at w = 0. In this paper D
will always be a convex positively homogeneous function of degree one in w.
As usual, the (stiffness) matrix K in (la) is symmetric and positive
definite. The matrix L in (lb) transforms the nodal displacements into the
stresses that would occur if the response were fully elastic. The vector t(w)
 47
is related to nonlinear hardening (see below) and the term {H w + t(w)> is
obtained by deriving a convenient function 0(w) = (1/2) w H w + g(w) with
respect to w. Eqs. (1) and (2b,c) are easily understood by considering a
uniaxial model for linear kinematic and isotropic hardening presented by
Martin and Nappi (1990). Referring to the kinematic hardening model of Fig.
la, Eqs. (1) and (2a) become: Ku - Kw = P; - Ku + Kw + K'w = - f ^ D = f w.
The last equation, together with (Ku-Kw = P) and (- Ku + Kw ± 2K'w = -f#), can
be applied to the isotropic hardening model of Fig. lb by setting w =w -w
and w=(w +w )/2 (cf. Fig. lb for #the meaning of w and w ). For nonlinear
hardening, the term K'w or ±2K*w is substituted by a function t(w) or t(w ).
In any case the dissipation rate will be the function D(w) shown in Fig. lc.
Eqs. (1) and (2) can be written again in a form suitable for the numerical
solution of the incremental elastic-plastic problem. To this aim, we refer to
a sequence of time steps At (j = l,...,n and n = total number of time
steps). We also assume that all the relevant quantities be known at the
beginning of the j-th step. Let us denote these quantities as P , f , u and
w . During each time-step we apply a given increment of the external loads AP
and we find increments Au, Aw and Af which satisfy the equations

K Au + L Aw = AP (3a)

L T Au + H Aw + t(w°+Aw) = - {f°+Af> - L T u° - H w° (3b)

In practice the solution is determined by using a predict ion-correct ion

iterative strategy: i) Eq. (3a) is solved and Au is computed for a given
vector Aw; ii) Aw is updated by means of (3b); Hi) Eq. (3a) is solved again
by introducing the new vector Aw until convergence is obtained. If the
backward difference time integration scheme is applied, inelastic strains are
assumed to increase proportionally. In other words, they follow a straight
path in the w-space. Thus, at each slip device, (5D /5w ) = (5D /3Aw ) and the
vector {f +Af> is made of n subvectors f such that
f1 = dDl/5Awl if Aw1 * 0 and f1 € 3D1 if Aw1 = 0 (4a, b)

If {H Aw+t(w°+Aw)} is obtained as the derivative of a positive definite

function 0(Aw) computed with respect to Aw, Eqs. (4) show that Eqs. (3)
represent the optimality conditions for the convex unconstrained problem

min < - Au K Au + Au L Aw + - Aw H Aw + g(Aw) + D(Aw) - AP Au + b Aw

Au,Aw l-
(5)
with b = {L u° + H w°>. Similar theorems can be derived (Martin et al.,
1987; Martin and Reddy, 1988; Romano and Rosati, 1988; Maier and Nappi, 1989;
Nappi, 1991) and, as a consequence, convergence properties of the backward
difference scheme can be proved (Martin and Reddy, 1988; Nappi, 1991).
The above approach based on assemblies of simple components is related to the
theoretical framework due to Maier (1968, 1969, 1970) in the field of
piecewise-1inear elastic plastic models. Indeed, also the nonlinear behaviour
can be recovered by considering a piecewise-1inear model made of m slip
devices associated to m linear springs and by letting m tend to infinite.

NUMERICAL ANALYSIS IN THE PRESENCE OF DAMAGE

*
Let us consider a material susceptible of isotropic damage. If E denotes its
stiffness matrix in the virgin (initial) state, the stress can be expressed
as s = (1-d) E ee, with e e = e - ep. The vectors e e and e p denote elastic
and plastic strains, while d is a parameter related to damage (0 ^ d ^ 1).
In order to carry out a structural analysis, n parameters d are introduced
48
and are usually treated as new, additional variables, so that the element
stiffness matrices become functions of these parameters. Here, it is
suggested to deal with the material as if it were elastic-plastic, so that
the theoretical framework of the previous Section is fully applicable and
damage increments Ad can be computed a posteriori at the end of each step.
To this aim let us consider, the elastic domain of in Fig. 2a, analogous to
the one utilised by Ortiz (1985) in a different context (developement of a
fully consistent associated damage rule). Next we assume that inelastic
strain rates q be normal to the damage locus, $(s ,s ) = a(/i). Here, n
represents the contribution to the compliance c in uniaxial tension or
compression 4 Indeed, account taken of the initial elastic modulus E , we can
set c = 1/E +ii. In view of the normality rule, we also obtain q = A {3$/ds},
with q made of two contributions: e p and e (inelastic strain rate due to
damage). Clearly, the normality hypothesis often represents an approximation
(which, in any case, can be removed), but always provides correct results in
the special case of uniaxial stress states. If we now apply the backward
difference concept, at each time-step we are concerned with the problem of
determining (by an iterative procedure) the increments Aq and As
(i = l n ) . The vectors As shall be in equilibrium with the external loads
AP and each increment Aq^ sha^l be normal to the updated damage locus at the
point {s +As > = {s +(l-d ) E (Ae -Aq )}, where bars denote quantities at
the beginning of the current time-step. The damage locus will be updated by
means of a uniaxial stress-strain relationship, such as the one due to Smith
and Young (1955), shown in Fig. 2b. Indeed, the new damage locus_ will
intersect the positive horizontal semiaxis at a point (s +As ) , where s is
the abscissa of the intersection point at the beginning of the time-step. The
new position of each updated locus is uniquely related to a convenient
increment As and to the current damage (isotropic in this^context). Damage,
in turn, is uniquely related to the compliance c=l/E + ji. Hence, any
increment As implies a certain increment AJI (given by the uniaxial
stress-strain law, since the new damage locus might have been determined as
well by a monotonic uniaxial stress s + As ). Next, we have the equation
Ag = AX {3$ /5s }, where the gradient of $ must be computed at the point
{s + As } according to the backward difference scheme. Thus, at each strain
point, we must satisfy both the normality rule and the relationship between
As and Aji (established through the uniaxial stress-strain law). In addition,
we shall also assume (for a given increment Afi ) a smooth variation of AA as
we move along any updated damage locus. Thus, we get unique increments Aq
and As or Afi . As a consequence, also the updated damage locus and the final
stress {s +As > are uniquely determined. In other words, an evolution law for
the damage locus is implicitly defined and the incremental problem_ can be
solved. Of course, at each a strain point either hardening (As • s >0) or
softening (As • s <0) may occur, as shown in Fig. 2b.
Finally, after convergence damage parameters are updated on the basis of the
uniaxial stress-strain relationship and the relevant elastic stiffness matrix
is computed. At this stage, an elastic analysis is performed by considering
the total loads and by determining the actual response in terms of elastic
components of the displacements. Next, the subsequent time-step is considered
by using the updated stiffness matrix.
It should be noted that we have referred to a particular damage locus. The
same procedure, however, can be applied elsewhere and we may introduce
different damage evolution laws, which can be applied to independent damage
loci: for instance, one defined for 3*^0, the other for 3^0 (with 3 1 =s 1 +s 2 ).

CLOSING REMARKS

An internal variable approach for the numerical solution of elastic plastic

problems has been considered and applied to structural analysis in the
 49
presence of damage. A solution algorithm has been suggested in order to avoid
damage parameters as explicit variables upon which the stiffness matrix
depends during each step. Thus, the nonlinear problem is solved as any
conventional elastic-plastic problem. In addition, convergence properties
proved for convenient time integration schemes are maintained and convergence
can be guaranteed until softening does not occur at any stress point. The
procedure discussed in the paper is suitable for structural systems made of
concrete and rock-like materials. A further application is represented by
masonry structures (Maier et al., 1991), since mortar is a material
susceptible of damage (cf. Fig. 3).

ACKNOWLEDGEMENTS

The financial support of CNR-GNDT is gratefully acknowledged.

REFERENCES

Germain, P. (1973). Cours de M&canique des Mileux Continus. Masson, Paris.

Kestin, J. and Rice, J.R. (1970). Paradoxes on the application of thermodyna-
mics to strained solids. In: A Critical Review of Thermodynamics. (Stuart,
E.B., Gal-or, B. and Brainard, A.J., eds). Mono Book Corpt., 275-298.
Lemaitre, J. (1985). Coupled elasto-plasticity and damage constitutive
equations. Compt. Meth. Appl. Mech. Engng. , 51, 31-49.
Lemaitre, J. and Chaboche, J. (1978). Aspects ph6nomenologiques de la rupture
par endommagement. J. Mec. Appl. , 2, 317-365.
Maier, G. (1968). A quadratic programming approach for certain classes of
nonlinear structural problems. Meccanica, 3, 121-130.
Maier, G. (1969). Teoremi di minimo in termini finiti per continui
elastoplastici con leggi costitutive linearizzate a tratti. Rend. 1st.
Lombardo di Scienze e Lettere, 103, 1066-1080.
Maier, G. (1970). A matrix structural theory of piecewise-linear plasticity
with interacting yield planes, Meccanica, 5, 55-66.
Maier, G. and Nappi, A. (1989). Backward difference, time integration,
nonlinear programming and extremum theorems on elastoplastic analysis. Sol.
Mech. Arch., 14, 1, 37-64.
Maier, G., Nappi A. and Papa, E. (1991). Damage models for masonry: a
numerical and experimental analysis. 3rd Int. Conf. on Constitutive Laws
for Engineering Materials: Theory and Applications, Tucson, Arizona.
Martin, J.B. (1975). Plasticity: Fundamentals and General Results. MIT Press,
Cambridge.
Martin, J.B. (1981). An internal variable approach to finite element problems
in plasticity. In: Physical Nonlinear ities in Structural Analysis. (Hult,
J. and Lemaitre, J. , eds.), Springer Verlag, 165-176.
Martin, J.B., Reddy, B.D., Griffin T.B. and Bird, W.W. (1987). Applications
of mathematical programming concepts to incremental elastic-plastic
analysis. Engng. Struct., 9, 171-176.
Martin, J.B. and Reddy, B.D. (1988). Variational principles and solution
algorithms for internal variable formulations of problems in plasticity.
In: Prof. G. Ceradini Anniversary Volume, Roma, 465-477.
Martin, J.B. and Nappi, A. (1990). An internal variable formulation for
perfectly plastic and linear hardening relations in plasticity. Europ. Eng.
J. Mech., 9, 107-131.
Mazars, J. (1984). Application de la m&canique de 1*endommagement au
comportement non-lin&aire et a la rupture du beton de structure. PhD
Thesis, Universite Paris 6.
Mazars, J. (1986). A model of a unilateral elastic damageable material and
its appliation to concrete. In: Fracture Toughness and Fracture Energy of
50
Concrete. (Wittmann, F.H., ed.), Elsevier Science Publishers, Amsterdam.
Nappi, A. (1991). Application of convex analysis concepts to the numerical
solution of elastic plastic problems by using an internal variable
approach. Engng. Optimization, to appear.
Ortiz, M. (1985). A constitutive theory for the inelastic behaviour of
concrete. Mechanics of materials, 4, 67-93.
Romano, G. and Rosati, L. (1988). Variational principles in convex structural
analysis. In: Prof. G. Ceradini Anniversary Volume, Roma, 591-603.
Smith, G.M. and Young, L.E. (1955). Ultimate theory in flexure by exponential
function. Proc. AC I 52.
w*0 for f=±f°

K'
w >0

K
1
'C
w'sO
Fig. 1 - Simple uniaxial models for kinematic hardening (a) and isotropic
hardening (b), with relevant dissipation rate function (c).

Fig. 2 - Possible elastic domain for plane stress states (a) and stress-
strain curve due to Smith and Young (b): s = s p (e/ep) exp (l-e/ep).
20 i s [MPa] 20 [MPa]

0.12 0.008
Response of a mortar specimen (a) and of a miniaturised masonry
panel (b) made of 25x30x65 mm bricks and 5 mm mortar joints.
 WS1a4

Continuous Daaage Mechanics Model for Interphase

I n t e r f a c e Fracture of Concrete
Weichun Fu and Yigong Yian

Departaent of Engineering Mechanics, J i l i n Engineering I n s t i t u t e , Chang chun 130012 CHINA

ABSTRACT

A continuous daaage theory is eaployed to study Mechanics behavior of concrete aaterial

characterized by strain—softening. The influence of the initiation and growth of
aicrodefects ( daaage) between the interphase interface is studied by analyzing the
condition of interphase.Probleas are considered in teras of elastic—daaage theory for
brittle aaterials. Basic eleaents of continuous daaage Mechanics are given, and the
aaterial aodel of dominant aicrodefect is proposed.In particuler, in order to evaluate
the accuracy of the theory aodel, results obtained through the analytical lsolution are
coapared with the experiaental results and found to be in excellent agreeaent.

KEYWORDS

concrete;continuous daaage;interphase interface;doainant aicrodefect; energy dissipation.

INTRODUCTION

The aicrostructure of concrete is extreaely coaplex.In the concrete, especially upon the
interphase between the different Material, there are coaplex foraations of
aicrodefects. It is widely accepted that concrete aaterials fail because of the
nucleation and growth of a aultitude of aicrodefects.However, it is iapossible to
describe accurately the evolution ofeach aicrodefect distributed randoaly in concrete
particularly on interphase.Hence, continuous daaage Mechanics (C D M)approach is well
adapted to aodel the behavior of aultitude of effects instead of trying to describe the
fine defails of the aicrodefect pattern.

Probleas on the continuous daaage here have been studied by many researchers with a
great deal of valuable results published since Kachanov's work(1958).The CDM approach
was applied to aaterials with Waited plastic deforaitiesC Krajcinovic and
Fonseka, 1981; Krajcinovic, 1983; Krajcinovic and Suaarac, 1986) such as concrete
(Legendrel984; Suaris and Shah, 1984;Siao and Ju, 1987;Ju et al.,1989) .However, aost of
the previous research is related to describing the aacroeffects of aaterial failure but
very little has been researched on the aicroaechanisas of failure.

The purpose of this paper is to study the influence of the initiation and growth of
aicrodefects between the interphase interface. Reaarkable trends in the daaage
accuaulation of the aaterial paraaeters are obtained depending on the various controlled
conditions the interphase.

51
52
INTERPHASE STRUCTURE AND MODEL OF DEFECT

The fact is that both aggregate and mortar are the elastic materials, but concrete is
nonlinear. Hence, it is reasonable that most important reason which result in nonlinear
behavior characterized by strain—softening is the nucleation and growth of defect upon
the interphase interface.As can be seen on figure I, there is formation of an intricate
network of crystals and poorly crystalline compounds upon the interphase interface. The
interphase interface is important because it is characterized by a higher porosity and a
different crystalline network as compared to the metrix, and it is where most of the
microcracks will develop (Ju et al., 1989).This interface is so thin that those multitude
voids can be considered as penny—shaped planar defects. The influence of the
penny-shped microdefact is related to their direction in stress field, and it is the
dominant microdefact which possess with particular direction that developed firstly
during loading.

F<3* Microstructure of jftterphase Fig. 2 Strees-Strain

curves
FORMULATION OF THE THEORY

Basic equation
The nonlinear behavior of engineering materials arises in general as a consequence of a
specific pattern in irreversible changes of microstructure. In thermodynamics of
irreversible processes, the Clausius — Duhem inequality(Coleman et al.,1967; Krajcinovic,
1983)can be written

<Tzj et,-pY-ST-T" l-jradT* 0 en

where als and eij are the stress and strain tensor; p, ij), S, T and q the mass
density, Helmholtz free energy, entropy, temperature, and the heat flux
vector, respectively. In the neighborhood of the equilibrium state, the complementary
constitutive equation (Germain et al.,1983) may be written

Xi -tu y7 (2)
where Y and X are the "fluxes" and "forces" , and have a linear relation between
them; the matrix L is symmetric,non—negatiue and may depend on the thermodynamicial
vriables.Introducing the pseudopotential of dissipation , equation (2) may be written

(3)
H-L„yiy,
To be specific, one will be concerned with materials that admit elastic stresses and
thermodynamic potentials, internal energy and free energy.According to the damage theory
of brittle materials which were given by Krajcinovic et al.(1981;1983) , the internal
variable can be defined as
U)j(X,,t)= U)(X,tt)Nj
(4)
 53

and the Helaholtz free—energy density can be written as

P^=1(A+2/0£KK£IL-/U£KK£U-£/<L£LK,)
-'/I Vi (5)

where the scalar w is the void density in a cross section defined by the noraal Nj( it
should be noted that this fora of the internal varible is very suitable for the aodel of
■aterial defect of the penny); X and \x are the Laae constants;dare the constants of
■aterial.Then the equations of state aay be written

»-/■!£. s-ff > *-'£

where R is daaage energy release rate (Lemaitre, 1986) ; a is internal vareables
a = ( a, a,).

Response Model
It is believed that the nonlinear aspects of the brittle aateriats such as soae concrete
is doainated by aicrocracking.For an isotheraal process, froa equation (5)and (6) > the
stress can be written (Krajcinovic, 1981; 1983) as
(5JJ= KJJKL £KI (7)

Wh6rC
/CyK^AMtt+^Mlt+C^
+ C2 <&>f <A?)VX ( S]* Mi o)i+ in tij u)K) C8)

where 6JJ is kronecker delta;Ci are the aaterial parameters.

In order to arrive at soae nuaerical results about cumulative effect of daaage, it is

necessary to introduce a concept which characterizes irreversible nature of daaage
process.Froa a aicrostructural standpoint, the concept of daaage surface results froa the
initiation and growth of aicrodefects (Fonseka,et al., 1981).Within the fraaework of
this, loading path, loading history and irreversible process of daaage are considered.This
fora of daaage surface can be written as
f = £N«+8JS*"(B;2^+£W/*-8I£W (9)

where f is the state function which is defined by internal variable of daaage;B^B, B, are
aaterial paraaeters;and co.is the largest recorded daaage. In addition to the
state fuction, Krajcinovic et al.(1981)introduced the consistency equation

(1D)
*»*--x&'$„di»'+sLdt^
where K is a paraaeter to define the evolutive direction of daaage.Froa equation ( 9)
and (10). the consistency eguation then takes the fora

Froa(ll) it is not difficult to find the relation ship between the increaents in strain
deij and daaage growth dw,.

For the special case of the uniaxial coapression (space { e u = e » , e „ ) ) , the

increaental fora of the stress —strain relationship can be derived froa (7) (8) in fora
54

d$,-EKld£„+(*?+c 1 »> +i ^-£ I1 )«te (l ] for £(l>£o (13)

and the daaage equation can be derived froi (11) in fora

da)=(5,-b3)"jiEa for i 0;^„d*">0 (14)

where
v „ i-u
) > -■ /c- U + VX/-21/) (15)

Then, considering the initial condition in font

<53j == ^// =r ^2 ==0 , co=ro)0 for £ » £ £ » (16)
equation (12) and (14) can be written as
833 =AIS*I+A2£H
(17)
U)-(A)W—
/
(18)
where «/-Ba
2(2 + d/Ct)
>4i
11
^-f.l+Btto+^eT^, Ct
- (2 6/c, (/- ? )+i>3(*+ c*/cj(S-2(2 * i,) CM ) (19)
/la-" £„-£!+BV.+2B7/C, (20)
(21)

and e,°,, ej,, are the proportionality li«it;Wois initial daaage (void density).

Equation (13)>(17)>(18)constitutes a weel—post boundary—value problei.Substituting the

initial daaage to' and a group strain—value obtained froa experiaent into
(17) ,(18), the systea of equations constitutes a hyperstatic nonlinear equation . It is
not difficult to solve the equation and the aaterial paraaeters (Bi,Ci) are obtained by
numerical method.

EXPERIMETAL VALIDATION

Speciaens Preparation
The three groups of speciaens are used for studying the effect of various
■icrostructures of the interface. All of thea have the saae water/ceaent ratio
(w/c) . Various conditions of interphase interface are produced with the aid of the
doubl—stirring Beans and the conditions are controlled by different stirring tiaes .The
technological process used in this study is shown in Fig.3.

total aggregate total cement U 25-15% total water Speciment

total sand H stir I H Stirn Stir m H H2l>y4 ^

65-75% total 6S-1S s 28 day
15-20 5
H ^ 30-35 s A r
water
Fig.3:Technological process of speciaen prepracion

About 200 SEN (scanning electron aicroscopy) photographs showtl.AU the three groups of
speciaen have similar aicrostructrues of aatrix because they have saae w/c ; 2.It is
the first group (Group I :standard stirring leans ) that has the highest porosity upon
the transition zone aaong the three groups speciaen ; the porosity of the second group
(Group II: double —stirriog leans ) is lower then first group's ; and the porosity of
 55
the third group(Group M i another double —stirriog aeans)is the lowest aaong all of the
specimens.

Results and discussion

A 100T servohydraulic INSTRON testing machine was used to conduct the coapression tests .
A function generator was used to contral the rate of loadiong.

A graphs of stress-strain of three groups speciaen have the shape shown in Fig. 4/ in
which curves
\59 Mf«

o'S -£«
o<i c,3 c.f

Fig .4 Experiaental and calculated date Fig. 5 Poisson's ratio change

are the calculated results and syabols ( A > # / 0 ) a r e the experiaental values. The
poisson's ratio—uniaxial coapression curues, volumetric strain curves and accuaulated
daaage curves are shown in Fig.5>Fig.6^Fig.7 respectively.All of thea show:l.It is the
concrete aaterials which have low porosity on interphase interface that have high
strength! Fig. 4] ; 2. The process aaterial daaage aainly depend on the state of
interphase[ Fig.7];3.It is the state of interphase that is the aain reason resulting in
inelastic behaviour of aaterial;4.The state of interphase interface can be described
perfectly by the aaterial paraaeters of daaage.

Fig. 6 Volumetric strain change Fig. 7 Accuaulated daaage change

It should be pointed out, in addition, that the triaxial behavior can also be described by

the aaterial parameters obtained froa uniaxiaKYigong et al.)

CONCLUSION

Continuous daaage aodel have been presented to predict the behavior of concrate. In
particular, the effects of interphase interface on the initiation and growth of
aicrocracks are demonstrated.The conclutions are suaaarlized as follows:
1. Continuous daaage aodel can describe mechanics behavior of concrete of
aaterial. 2. Material paraaeters of daaage can be obtained by uniaxial coapression
test. 3. States of interphase is the aain reason which results in ultimate inelastic
behaviour of material. 4.States of interphase can be defined by material parameters.
56

REFERENCES

Coleaan, B. D. and Gurtin,M.E.(1967).Thermodynamics with internal state variables.

J.Chea.physics, 47,597-613.
Fonseka, G. I), and Krajcinovic, D. (1981). The continuous daaage theory of brittle
■aterials, Part2 ! Uniaxialandplane Response Nodes.TRANS.ASNE.J.Appl.Nech., 48,816-
824.
Germain, P.and Nguyen, Q.S.and Suguet, P.(1983).Continuua theraodynaaics.Trans.ASNE.J.AppI.
Nech., 50,1010-1020.
Ju, J. VI.and Monteiro,P. J.M.and Rashed, A.I.(1989).Continuua daaage of ceaent paste and
aortar as affected by porosity and sand concentration.J.Engin.Nech., 105-130.
Kachanov, L. M. ( 1958) .Tiae of the Rupture process under creep conditions. IVZ Akad
Nauk,S.S.R.,Otd Tech Nauk, 8, 26-31.
Krajcinovic, D. ( 1983) . Constitutive equtions for daaaging aaterials. ASNE
J.Appl.Nech., 50, 355-360.
Krajcinovic, D. and Fonseka, G. U. (1981). The continuous daaage theory of brittle
aaterials,Port I:General theory.ASNE.J.Appl.Nech., 48,809-815.
Krajcinovic,D. and Suaarac,D.(1986).Nicroaechanically based daaage aodels. Proc. Tenth
U. S. Nat. Congr.ofAppliedNechanics,Univ.ofTexasatAustin,June 16-20,J.P.Laab, ed.,
115- 123.
Legendre, D.and Nazars, J.(1984).Daaage and fracture aechanics for concrete ( A coabined
approach).4th Internatirnal conference of Fracture Mechanics, 2841-2848.
Leaaitre,J. ( 1985) . A continuous daaage aechanics aodel for ductile fracture.
J.Engin.Nater.Tech., 107.83-89.
Siao, J. C. and Ju, J.H.U987 a).Strain and stress based continuua daaage aodels. Part
IxForaulation.Int,J.Solids and Struct., 23,821-840.
Siao,J. C.and Ju, J.W.U987 b).Strain and stress based continuua daaage aodels,Part II
:Computational aspects.Int.J.Solids and Struct., 23 841-869.
Suaris,V). and Shah, S. P.(1984).Rate-sensitive daaage theory for brittle solids.
J.Engin.Nech., 110,985-997.
Yigong, Y.and Weichun.F., Constitutive aodels for concrete structures. 1st International
Conference of Concrete Naterials.
WS1a5

MODELING OF VOID NUCLEATION AND DEVELOPMENT OF

EQUATION OF DAMAGE EVOLUTION DURING PLASTIC DEFORMATION

S. Shima and T. Kikuchi

Dept. of Mech. Eng., Kyoto University

Hon-machi, Yoshida, Sakyo-ku, Kyoto 606, Japan

ABSTRACT

A model for void nucleation due to debonding at the interfaces between the
matrix material and the second phase particles is proposed. Effect of
various parameters on the strain at which void nucleation occurs, €i, is
investigated; they are: the ratio of the strength of the second phase to
that of the matrix material, interfacial strength, volume fraction of the
second phase and environmental pressure. It is thus shown that €i decreases
with increasing volume fraction and with decreasing interfacial strength
and that compressible mean normal stress delays void nucleation. Further,
based on the results obtained, an evolution equation for void nucleation is
proposed.

KEYWORDS

Void Nucleation; Void Growth; Upper Bound Approach; Equation for Damage
Evolution; Constitutive Equation for Compressible Materials

INTRODUCTION

It is well-known that ductile fracture is resulted from growth and coa-

lescence of voids which have been nucleated during plastic deformation.
Void growth has been treated by some researchers (Aravas, 1986; Mathur and
Dawson, 1987) by applying the plasticity theory for compressible materials
(Oyane et al., 1972; Shima and Oyane, 1976; Gurson, 1977). Concerning the
void nucleation, however, not many equations have been proposed (Chu and
Needleman, 1980; Perzyna and Drabik, 1984).

In this study, an attempt is made to develop a simple single-cell model for

void nucleation based on the upper bound theorem; it is assumed that a void
is nucleated at the interface between the ductile matrix and the second
phase particle. Void nucleation is also attributed to fracture of the
second phase particle itself, but in this study this is not considered;
this would be similarly taken into account without any further difficulty.
For simplicity, simple tension in plane strain is dealt with.

57
58
ANALYSIS BY UPPER BOUND METHOD

Preliminary Consideration on Void Nucleation

Avitzur (1968) and Avitzur and Choi (1986) developed velocity fields allow-
ing void opening in extrusion and drawing, and obtained a fracture crite-
rion. However, the criterion was identical for any material, because the
energy dissipation due to void nucleation could not be evaluated. Avitzur
(1973a, b) also made an analysis of strength of a two-phase material em-
ploying a unit cylindrical model, while Tada et al. (1983) developed an
ellipsoidal model and studied yield stress and deformation characteristics.
They analyzed also the case where void nucleation takes place at the
matrix-particle interface. However, its occurrence was independent of the
interfacial properties.

Model for Analysis

Model 1: We shall consider a simple unit-cell model as shown in Fig.l,

where a quarter of the cell is shown because of its symmetry; this is based
on the fact that the arrangement of the particles does not influence sig-
nificantly the macroscopic behaviour of the material (Oyane et al. , 1985).
The cell is divided into four zones 1 to 4, where zone 4 refers to the
particle and others to the matrix material. To simulate void nucleation, we
shall introduce a layer which is of an infinitesimally small thickness of a
compressible material between zone 4 and the matrix. This layer is also a
discontinuity plane in the velocity field; if the velocity discontinuity
normal to this plane exists, this can be regarded as a measure of debonding
or void nucleation. Since the material properties of the layer are varied,
it is possible to investigate their effect on void nucleation.

Model 2: Consider a case when the volume fraction of the second phase is
vp. The interfacial strength naturally varies and distributes in a random
manner so that the void nucleation first occurs at the weakest interface.
If deformation goes on, the voids as such grow and also nucleation will
newly occur at other sites. Based on the mixture rule, the unit-cell model
can be utilized also after the occurrence of void nucleation; once void
nucleation occurs, the matrix, which is strengthened by randomly distribut-
ed particles, is regarded to become compressible and void growth can be
calculated by the plasticity theory for compressible materials.

/k

A B
1 ' 2
1
'
|D E
I

4 3
F C
X.L X.Q X.
Fig.l Unit-cell model
 59
Upper Bound Theorem

The theorem for compressible body with velocity discontinuity has already
been derived elsewhere (Shima et al., 1976; Shima and Nose, 1990), only the
theorem is shown below.

/ FiUidS < /oij€ijdV + /pnc^{(4/9+f2)Aun*2+ Aut* 2 /3F/ 2 dT - / FiUi*dS (1)

where
Fi: surface traction prescribed at surface SF
ui: exact velocity prescribed at surface Su
ui*: admissible velocity, which satisfies velocity boundary conditions
€ij*: strain rate derivable from Ui*
oij*: Cauchy stress related to €ij*
Ui k *: velocity at the plane of discontinuity in zone k (k=l,2)
Fi<k>: traction acting to zone k through plane T (k=l,2) (Fi<1)=-Fi<2>)
T: plane of velocity discontinuity, V: volume of body, S: surface of body.

In (1), Un1* and ut1* (i = l and 2) are the normal and tangential velocities
at the both sides of the zone, with Au n * and Aut* being the velocity dif-
ferences in the normal and tangential directions, respectively. The second
term on the right-hand side of (1) represents the rate of energy dissipa-
tion, WT*, due to the velocity discontinuity. This can be derived similarly
as in the work by Shima and Nose (1990).

In (1) p is originally the density ratio and f is a function of p (Shima

and Oyane, 1976). In this study, p n o and f are considered to be the proper-
ties of the interface (Shima and Nose, 1990).

Velocity Field

We shall assume a velocity field as follows (see Fig.l):

1) Strain rates are uniform in each zone.
2) Velocity is continuous at boundaries between zones 1 and 3 and between
3 and 4 in the x-direction and between 2 and 3 in y-direction. Note tha.t a
velocity discontinuity at DE in the y-direction is allowed to exist.
3) Each zone is always rectangular.
4) Before void nucleation occurs, volume is constant in each zone. But,
once it has occurred, volume change must be allowed; it can be calculated
by the plasticity theory for compressible materials (Shima and Oyane,
1976).
5) Velocity in the y-direction at AB is given.

From the above assumption and the boundary conditions, the number of inde-
pendent variables is two. Let them be vi and V4 at y=yi . Strain rates are
expressed by the two variables and thus the right-hand side of (1) or the
sum of the energy dissipation rate in the zones and that at the interfaces
between the zones can be minimized by changing them.

CALCULATION

Condition for calculation

The stress-strain curve of the matrix was arbitrarily given. It was assumed
that the particle and the interface layer are non-workhardening and that
the strength of the particle is represented by parameter 0 and that of the
60
interface by u.; these are the ratios between the respective strengths and
the initial yield stress of the matrix, TJo .

Calculated Results

First, we shall see some results calculated by Model 1. Figure 2(a) shows
the effect of the bond strength at the interface on the strain at which
void nucleation takes place, *G i, with 0=2 and vp=0.1, where mark x refers
to €i. It is seen that G*i increases with increasing ii. Up to void nuclea-
tion, all the stress-strain curves are the same, while the stress decreases
suddenly when it occurs, although this is not actually the case. This is
due to the fact that the stress is calculated by Model 1. This can be
improved if Model 2 is employed. Figure 2(b) shows the effect of the
volume fraction vP on Gi with 0=2 and u=1.0. Gi increases with decreasing
v P , although the stress is__ obviously higher for larger v P . Figure 2(c)
shows the effect of 0 on Gi with vP=0.1 and u=1.0. It is seen that ~Gi
decreases with increasing 0.

Fracture strain has experimentally been investigated in various ambient

pressures (Oyane, 1972; Osakada et al. , 1977). The results by Osakada et
al. (1977) are shown in Fig. 3. Figure 4 shows calculated relationship be-
tween the strain at which void nucleation occurs, Gi, and pre-strain: the
solid line refers to the case when the pre-strain is given in an atmosperic

U.dU 1 1 1 1
(a) (b) [(c)
0.15 v p =0.1l
r \
«•» 0.10 *=2/1 L\ v . fi-l.O
0.05
^y*^\
^i*.^
0J
0 1 1i — j . = ^ L — 1
f=2 fi-O.fl
1^ 1
~H

0 2 A .6 .8 U0 0 5 10 15 20 0 5 10
Bond strength ratio Volume fraction Strength ratio
Fig.2 Variation of Gi with (a) bond strength, (b) volume
fraction of particles and with (c) 0.

0.015 — 1 — 1 1

cd
/ j
0.010 r— —
C- IS
0.005 ^
4
-P
o L-*H
cd
LL
0 • i

0 0.5 t.O 1.5 0 .005 .010 .015

Pre-strain Pre-strain
Fig.3 Effect of ambient Fig.4 Effect o_f ambient pres-
pressure on fracture sure on Gi.
strain.(Osakada, 1977)
 61
pressure and the subsequent strain in a high pressure; the broken line to
the case where the condition is reverse. The results in Fig.4 agree quali-
tatively with those in Fig.3.

Table 1. Example of distribution of interfacial strength.

(%) (Total volume fraction vP=0.1)

Bond strength
ratio li 0.2 0.3 0.4 0.5 0.6 0.7 0.8

Vol. fraction
of particle (%) 0.24 0.8 3.0 3.0 1.9 0.8 0.26

05

00
CO
£ 200 h
CO

Stra i n
Fig.5 Calculated stress-strain curves at ambient pressure
and at high pressure.

Consider now that the total volume fraction vP=0.1 with an arbitrary dis-
tribution of the bond strength as shown in Table 1; for an easier calcula-
tion, the bond strength is assumed to be in a stepwise distribution. By
employing Model 2 we can calculate the stress-strain curve for various
ambient pressures. Figure 5 shows the stress-strain curves in an atmospher-
ic pressure and at a high pressure. It is obviously seen that there is no
difference between the two curves but that the strains at which void nucle-
ation takes place differs significantly; mark x refers to atmospheric
pressure and f to a high ambient pressure.

Evolution Equation for Void Nucleation

From the calculated results shown in the previous sections, a possible

evolution equation for void nucleation may be expressed in terms of the
above parameters as

C, DUC l =AvP<0o»/iioo>e (2)

where <x>=x when x> and <x>=0 when x<0, because the value of this equation
is meaningless unless it is positive, and A is a proportionality constant.
This equation states that when o» is negative void nucleation does not
occur, but actually it occurs. If this is to be incorporated, we may sub-
stitute on by (o«+C), with C being some positive constant (Oyane et al.,
1972; Shiroa and Nose, 1990). A possible damage evolution equation including
both void nucleation and void growth may be the sum of (2) and the volumet-
62
ric strain rate that is obtained by the constitutive equations already
proposed by Shima and Oyane (1976).

CONCLUSIONS

A model for void nucleation was proposed. Effect of the ratio of the
strength of the second phase to that of the matrix material, the interfa-
cial strength, volume fraction of the second phase and environmental pres-
sure on the strain at which void nucleation occurs was investigated. It was
thus shown that the calculated results were in agreement with the previous-
ly obtained experimental ones. Based on the calculated results, an equa-
tion for damage evolution was developed. The verification of this equation
should be examined further.

REFERENCES

Aravas, N. (1986). The analysis of void growth that leads to central bursts
during extrusion. J. Mech. Phys. Solids, 34, 55-79.
Avitzur, B. (1968). Analysis of central bursting defects in extrusion and
wire drawing, Tr. ASME, J. Eng. Ind. 90, 79-91.
Avitzur, B. (1973a). Tensile strength of composite materials, Part 1: Upper
bound analysis, ibid., 95-3, 827-834.
Avitzur, B. (1973b) Tensile strength of composite materials, Part 2: Inter-
pretation of analysis,ibid., 835-43.
Avitzur,B and J. C. Choi (1986). Analysis of central bursting defects in
plane strain drawing and extrusion, ibid., 108, 317-321.
Chu, C. C. and A. Needleman (1980). Void nucleation effects in biaxially
stretched sheets, Tr. ASME, J. Eng. Mat. & Tech., 102-6, 249-256.
Gurson, A. L. (1977). Continuum theory of ductile rupture by void nuclea-
tion and growth: part 1-yield criteria and flow rules for porous ductile
media. Tr. ASME, J. Eng. Mat. & Tech., 99, 2-15.
Mathur, K. K. and Dawson, P. R. (1987). Damage evolution modeling in bulk
forming processes. In: Computational Methods for predicting Material
processing defects (M. Predeleanu, ed.), pp. 251-262. Elsevier, Amster-
dam.
Osakada, K., A. Watadani, H. Sekiguchi (1977). Ductile fracture of carbon
steel under cold metal forming conditions. Bull. JSME, 20, 1557-1562.
Oyane, M. (1972). Criteria for ductile fracture. Bull. JSME, 13, 265-270.
Oyane, M., S. Shima, H. Akamatsu, and M. Ohmura (1985). Characteristics of
strength and deformation of sintered copper with second phase particles.
Proc. 8th Int. Conf. Powder Me tall., Dresden , 17-31.
Oyane, M., S. Shima and Y. Kono (1972). Theory of plasticity for porous
metals. Bull. JSME, 16, 1254-1262.
Perzyna, P. and A. Drabik (1984). Analysis of the evolution equation
describing the potential behaviour of dissipative solids. Arch. Mech.,
36, 5-6, 733-748.
Shima, S. and M. Oyane (1976). Plasticity theory for porous metals. Int. J.
Mech. Sci., 18, 285-291.
Shima, S. and Y. Nose (1990). Development of upper bound technique for
analysis of fracture in metal forming. Ing. Arch., 60, 311-322.
Shima, S., T. Tabata, M. Oyane, and T. Kawakami (1976). Upper bound theory
for deformation of porous materials. Mem. Vac. Eng., Kyoto Univ., 38-3,
117-137.
Tada, Y., M. Oyane, S. Shima, T. Sato and M. Omura (1983). On upper bound
approach on deformation of two-phase materials in uniaxial tension.
ibid., 105-1, 39-44.
WS1a6

THE COMPUTTER SIMULATION AND ANALYSIS OF VOID

GROWTH IN DIFFERENT STRESS TRIAXIALITY

Z. F. YUE K. S. ZHANG C. Q. ZHENG

Department of Applied Mechanics, Northwestern Polytechnical University
Xian , Shaanxi Province , 710072 , CHINA

ABSTRACT

In the paper, the analysis of the void enlargement during the deformation of axisymmetric tensile specimens made
of alloy steel 40Cr has been carried out by employing an own designed large eslastic—plastic deformation finite el-
ement program . The result obtained shows that the void expands differently in the longitudinal and in the radial
direction , and the stress triaxiality plays an important role on i t . The ratio of void increment in radial direction to
that in longitudinal direction is found to be a linear function of the stress triaxiality . And the extrapolated value of
void growth is reasonably agreeable to the 3-D analysis of void growing in the crack tip field ( McMeeking 1989 ) .
In the paper , it is also indicated that the void enlargement velocity estimated from R - T Model ( Rice et al., 1969 )
is lower than the actual case , while the critical void growth ratio estimated from modified R—T Model is , as
pointed out by Zheng ( 1985 ) , not far away from that of the experiments ( Wang , 1990 ) and calculations of the
same alloy .

KEYWORDS

Computer simulation ; stress triaxiality ; void growth ; critical void growth ratio VQQ

INTRODUCTION

The ductile fracture mechanism of metals can be generally considered as three stages : voids nucleation , growth ,
and finally coalescence . On certain conditions , the void growth may play an important role on the damage of ma-
terials ( Rice et al., 1969 ; Thomson e^al., 1984 ; Zheng et al., 1983 , 1986 ) .

Generally speaking , the void growth is related to the stress triaxiality and strain rate . From theoretical analyses
and micro experiments , it has been known that a void grows much more rapidly in a notched bar with a higher
stress triaxiality than that in a smooth bar with a lower stress triaxiality , and the shape change of a void also de-
pends on the stress triaxiality . Because of the restriction of theoretical hypothesis and the statistical error of micro
examination , the results from different papers could not easy agree with each other ( Zheng et a l . , 1983a ) , espec-
ially there is not a clear expression about the shape change of voids growing . In order to avoid difficulties involved
3-D computation , the paper is only concerned with a isolated spherical void located in the centre of the minimum
cross section of the specimens (including a smooth and 5 different circumferential U-notched bars ) made of Steel
40Cr , which are shown in Fig. 1 . And the chemical composition of the alloy is as follows ( wt % ): C: 0.41 ; Si:
0.31 ; Mn : 0.04 ; P : 0.024 ; S : 0.01 ; Cr : 0.9 ; Cu : 0.09 ; Al : 0.09 and Ni : 0.08 .The curve of true stress vs strain is
shown in Fig.2 .
63
64

£3e^e p
Mpa

f 0.5 H*~
i
1 2
2 4
4 /
6 / |
2 .4 .6 .8
Fig. 1 Geometries of the specimens ( unit: mm ) Fig. 2 True stress vs true strain of 40Cr

CALCULATION MODEL

At first, the original radius of the void is given as R0 =2.5 /im , which is the similar mean size of the inclusions
leading to the first generation voids in this alloy steel. As an example , the mesh for the specimen with a notch ra-
dius p = 2 mm is shown in Fig. 3 . Then , the growth of voids with other two different original radius RQ =1.25
and 5.0 /im has been studied in one specimen , respectively . All the computations stopped as soon as the gauge
displacement reached the failure values of the experiments .

1771
i m (I)
%
111
/

<m (in)

Fig. 3 Initial mesh of the specimen (p = 2mm)

RESULT AND DISCUSSION

Stress Triaxiality

The stress triaxialities in the axial centre of the six group bars in different loading stage have been obtained as
shown in Fig . 4 . From the figure , it can be assured that the stress triaxialities in the axial centre of all six group
specimens maintain approximately contants over the main part during deformation for each one .
Rtr

Fig. 4 The stress triaxialities in the center of the six group specimens
 65

Void Growth

AR
l % A = 7.903(mm) '» l , A = 1.4(mm) U A = 0.494(mm)
2 , A = 6.820(mm) 2 . A = 1.0(mm) AR ^ 2 v A = 0.414(mm)
3 . A = 4.930(mm) 7.5 3 . A = 0.398(mm) 3 , A = 0.22(mm)

AR r "A*r

l % A = 0.684(mm) ^ 1, A = 0.4251 (mm)

2 % A=0.614(mm) f . 2 . A = 0.564(mm)
50 l % A = 0.567(mm)
3 . A = 0.412(mm)
2 , A = 0.460(mm)

-_ARr . A*r
2.5 5 2.5 3.0
P=2 -0.5

A:
Fig. 5 The viod growth in different specimens g a u 8 e displacement

P=co
♦ AR /*ni A R r /im
AR r
ARr AR Z

Fig. 6 The void growth in two directions with plastic strain

66
Fig. 5 shows the void expansion vividly . The figure indicates that a void in different stress triaxiality behaves
differently : in the lower stress triaxial field , such as in a smooth bar , it enlarges in longitudinal direction and con-
tracts in radial direction ; but in the higher stress triaxial field , such as in a notched bar , it enlarges in both direc-
tions . Fig.6 shows the relation of void growth in two directions , i. e. ARr and ARz vs equivalent plastic strain
£p . It is very clear that during the main stage of damage , the stress triaxiality maintain a constant and the
ARr and ARz are most likely as the linear functions of e . Thus , the relationship can be exposed as follows :

ARr = fx(R<r)ep 0)
ARz = fAR<r)n (2)

Where fj(R<r) and f2(R<r) are functions of the true stress triaxiality . If ARr / ARz is defined as the ratio of radial
increment to longitudinal one of a void , from eq. ( 1 ) and ( 2 ) , it can be obtained as :

ARr
(3)
ARz "f2(Re)

Using least square method , from Fig. 7 , the relationship can be derived :

^ = 1 . 3 2 ^ - 1 (4)
ARz

It should be mentioned that there are two critical values of the stress triaxiality from eq.4 : A R r / A R z > 0 ,
when Ro- > 0.76 , i. e. the void begins to enlarge along radial direction ; and A R r / A R z > 1 , when R c > 1.52 ,
i.e .the void grows along the radial direction faster than that along the longitudinal direction ; and as the stress
triaxiality gets very high , the void will grow much faster along the radial direction than that along the longitudinal
direction .

Eq.4 may meet satisfactorily with the void behavior in crack tip field estimated from 3-D computation . The result
of the reference ( McMeeking , 1989 ) has been analysed in this paper . The 3-D void growth was calculated and
shown in Fig. 8 . Throughout the loading process , a3 is approximately equal to a, , and they grow at about twice
the rate of a2 , i.e , ——- = 2.0 . The stress triaxiality can be obtained from eq.4 as Rer = 2.37 , and it can meet the
value of the stress triaxiality in crack tip field (Zhang etal., 1989 ) .

1 1 1 1 I 1

/
/
^
t»y
Ar©>\
a,
" CRACK VOID / ^s
/ °
- / D0-D

y yS 33-a0 1
a
y / °
- / / j£i ara0 1
^^*^^—■——-~ 32-ap
a
-1 ° . . 1
3
J/a 0 a 0

Fig. 7 The void growth with the stress triaxiality Fig. 8 3-D viod growing in the crack field
(McMeeking, 1989)
 67
Fig.7 also shows that f,(R<r) can be selected as a quadratic function of the stress triaxiality from the computer
simulation by the least square method , while f2(R<r) as a linear function of stress triaxiality .

The growth of a void with different original radius , R0 = 1.25 , 2.5 , 5.0 pm was studied for notched specimen
with p = 2.0 mm . Fig.9 and Table 1 show the void enlargement with different original radius R0. It is shown that
ARr / ARz is independent of original radius R0 , and the void increment is proportional to the original radius R 0
R0 = 5

Table 1 The voids enlargement with

different original ratio R 0

dRr dRz dRr

R0 de Rn dRz
P 0

1.25 3.892 5.178 0.7516

2.5 4.122 5.382 0.7659
5.0 4.196 5.553 0.7556
Average 4.037 5.371 0.7577
Error <4.0% <3.0% <0.81%

Fig. 9 The void enlargement with

different original ratio R0

Disscussion

The relationships of the void enlargement with the stress triaxiality from different references are not in agree-
ment with each other . The references ( Skockey et al . , 1978, 1980 ;Barnby et al . , 1984 ) indicated that V«
ln(V/ VJ
( defined as Ve = — , where V , V0 is the instant and initial relative volume of the void , respectively , e0
p o
and £p is nucleation and instant equivalent plastic strain , respectively ) was the linear function of the stress
triaxiality , i. e., Ye = a + b Ra ; a , b were different in the three references . The three papers are checked over, it
is found that they used the stress triaxiality from HRR structure which is higher than the real one in crack tip field
of plane strain state ( Zhang et a l . , 1989 ) , so the lower value was estimated for the enlargement of voids by them .

In fact, Rice (1969) investigated a void enlargement in high stress triaxiality field and concluded that:

^=0.2Kexp (lR<r)dep (5)

As the stress triaxiality is considered as a constant, it is found that:

Ve = 0.S5exp ( ^Ra) (6)

i.e., R - T Model leads to V« as an exponential function of the stress triaxiality Re .

Fig. 10 shows the critical void growth by the study and from the results of above references . Obviously , the void
enlargement not only depends on stress triaxiality , but also on effective plastic strain . Although the value of Ve
during the process of void growth may be underestimated from R - T Model, the critical void growth ratio is not
far away from that estimated from modified R - T Model, as pointed out by Zheng ( 1983 a , b , 1985 , 1986 ) .
68

t v«
Ve . _ Experiment results
20

[ Shockey et al. ,1978 ]

10 [ Shockey et al., 1980 ]

[ Barnbyet a l . ,1984 J

R<x

Fig. 10 The relation of void growth with the stress triaxiality

CONCLUSIONS

The computer simulation of void growth of the paper can estimate, to a considerable degree , the real void growth
of the material. The void enlargement in the longitudinal direction is , in general, different from that in the radial
direction , which is related to the stress triaxiality . According to the computer simulation ( shown in Fig . 7 ) , the
void enlargement along the radial direction can evaluated by using a quadratic function of the stress triaxiality ,
while that in longitudinal direction can be considered as a linear function of the stress triaxiality .

The variation of the void shape during the process of void growth is an important character in the damage process
of the material. Within the scale of the stress triaxiality investigated of Steel 40Cr , the ratio of radial increment to
longitudinal one of a void can be considered as a linear function of the stress triaxiality , and the critical value of
the stress triaxiality of the void beginning to enlarge along radial direction and growing along the radial direction
faster than that along longitudinal one is 0.76 and 1.52 , respectively .

The void growth obtained from tensile specimens is independent of the void original radius Ro , and can meet sat-
isfactorily with void enlargement in the crack tip field from 3-D computation .

REFERENCES

Barnby, J. T . , Y. W., Shi, and A. S., Nadkarni ( 1984 ), On the void growth of C - M n structure steel ducting plas-
tic deformation, InU.Fract. , 25, 273 .
MeMccking, R.M( 1989 ) , Numerical calculations for problems of ductile fracture , Proc.ICF7 , 3^ 1971-1999 .
Rice,J.R. and P. M. Tracey , ( 1969 ) On the ductile enlargement of voids in triaxal stress fields , J.Mech.Phys.Sol-
ids_, 17,201-217 .
Shockey , D. A. , et. al . ( 1978 ) , A computational fracture model for SA533 Grade B class 1 steel based upon
micro fracture processes , EPRI NP-701-SR .
ShockeyJD.A., K. C. Dao , L. Seaman , R. Burback , D. R. Curran ( 1980 ), Computational modelling of
microstructure fracture processes in A533B Pressure Vessel teel, EPRI NP-1398 .
Thomson,R.D. and J. W. Hancock , ( 1984 ) Ductile failure by void nucleation , growth and coalescence , Int.J.
Fract,, 26, 99-102.
Wang, K . ( 1990 ) ,Master Thesis, Northwestern Polytechnical University , China .
Zhang,K.S.and C. Q. Zheng ( 1989 ) , A computer simulation of ductile fracture initiation in TPB specimen - an
application of V GC criterion , J,Engin.Fract.Mech„ 33 , 671-677 .
Zheng , C. Q. and J. C. Radon ( 1983a ) , The formation of voids in the ductile fracture of a low alloy steel, Proc of
Int Symp on Fracture Mechanics , (Beijing), 1052-1056 .
Zheng, C. Q. and J. C. Radon ( 1983b ) , The corretion of triaxial state of stress and the failure strain , Proceedings
of ICF International Symposium on Fracture Mechanics ( Beijing ), 1057-1062 .
Zheng , C. Q. and J. C. Radon ( 1985 ) , The fromation of voids in the ductile fracture of a low alloy sreel, Joural
of Northwestern Polytechnical University, 3 ,409-418 .
Zheng, C. Q., L. Zhou and J. M. Liu ( 1986 ) , Fracture behavior of ductile steels under triaxial stress state , Pro-
ceedings of 9th Congress on Material Testing and the 3rd Danubia-Adria Symposium ( Budapest, Hungary ) ,
86-91.
WS1a7

NUMERICAL AND EXPERIMENTAL INVESTIGATIONS OF

DUCTILE STEELS INCLUDING DAMAGE

H. ALTENBACH

Institut fur Werkstofftechnik und - prufung,

Technische Universitat "Otto von Guericke"
Magdeburg,
PSF 124, Universitatsplatz 2, D-O-3010 Magdeburg
ABSTRACT

Numerical and experimental investigations of ductile steels in-

cluding damage can be realized only by so-called hybrid tech-
niques, using the framework of continuum mechanics, experimental
experiences and computer simulation. In the paper are reviewed
some developments in continuum damage mechanics. It is shown,
that the purly phenomenological models couldn't solve the prob-
lem of modelling material behavior including damage. After a
short discussion of creep damage problems there are given short
recommendations for interdisciplinary modelling in the case of
ductile steel's behavior including damage.

KEYWORDS

Damage; ductile behavior; creep; steel; hybrid methods

INDRODUCTION

In dependence of the thermo-mechanical, environmental and other

conditions in the material turns out ductile plastic damage,
creep damage, embrittlement or fatigue. The theoretical descrip-
tion of damage or its experimental investigation is difficult
(especially under complex or non-simple loading conditions
etc.). The main reason for these difficulties is connected with
characterization of the material's microstructure at each loa-
ding stage. The describtion based on the existence of specific
arrangements of diclocations, microcracks, microvoids or other
defects and faults, and several mechanisms of the material's
behavior (for example deformations in ductile metals are accom-
panied by nucleation, growth and eventual coalescence of voids).
At present many approaches to describe the deformations of mate-
rials including damage exist. They are reviewed in several pa-
pers (Krajcinovic, 1984; Lemaitre & Chaboche, 1985; Kachanov,
1986; Murakami, 1987; Fischer, 1987; Hult, 1988).
69
70
The open problems can be solved only by hybrid methods. It
means, that is necessery to use the theoretical framework of the
continuum or solid mechanics, the experimental experiences of
the material sciences or experiences of the physics of solids
and computer simulation techniques. The feature of this paper is
a discussion about the modelling of the behavior of materials
including damage.

CLASSIFICATION OF MODELS

At present we can observe a rapid development of mechanical

models including damage. At first, we can divide the models into
several classes, for example (Koutoul et al., 1989)

(a) phenomenological models,

(b) microscopic models and
(c) statistical models.

The development of these models is connected with the following

questions:
(1) method of damage description,
(2) formulation of damage evolution equations,
(3) relation between the evolution equations and the traditional
constitutive equations,
(4) the formulation of a criterion of the final material's state
and
(5) experimental (physical and/or numerical experiments) verifi-
cation of the problems (1) - (4).
The answers on these quetions can be found only by interdisci-
plinary methods, based on mechanics, physics and material scien-
ces. Taking into account the models (a) - (b), we can employ
different approaches to deduce the equations or relations for
the material behavior:

(A) purly empirical or

(B) half-empirical and
(C) physically-based.
Other classifications are possible: in dependence of the testing
methods (destructive, non-destructive), of the class of mate-
rials (metals, polymers^ minerals, ceramics, glasses, compo-
sites, concrete etc.), of the type of material behavior and the
damage process (ductile»plastic damage, elastic brittle damage,
creep damage etc.) or of the kind of external conditions (loa-
ding, temperature etc.).

PURLY PHENOMENOLOGICAL MODELS

Phenomenological models based on the concepts of rational mecha-
nics. The basic assumption is the postulate of a continuum (Al-
tenbach, 1990). In the classical approach the continuum is
structureless, homogeneous etc. With regard to the real situa-
tion in the material (there are exist inclusions, defects, voids
etc.), the classical assumption should be extended.
 71
The basic equations of continuum mechanics can be divided into
material-independend and material dependend equations (Palmow,
1984). The first group is more importend for structural mecha-
nics. The classical material-dependend equations consider con-
stitutive and evolution equations. The constitutive equations,
charakteristic for the given material, describe the time-rela-
tions between the phenomenological field variables (Krawietz,
1986). In the framework of rational mechanics the set of consti-
tutive equations (Palmow, 1984) can be expressed in the simplest
form
S (X, t) = S {E t # , T t # } (1)
t# t5
h (X, t) = h {E , T *} (2)
1
t*
F (X, t) = F {E *, T**} (3)
t3 t#
H (X, t) = H {E \ T } (4)
S, E - stress and strain tensor, respectively, h - heat flux
vector, F, H - Helmholtz free energy and entropy, respectively,
T - temperature, X - position-vector, {...} - time-functionals
(during the material's history)
The situation changes, if we had to describe a material with
internal processes (development of plastic or damaged zones
etc.). Continue the continuum mechanics approach, in this case
we should involve so-called internal variables. The equations
(1) - (4) now include the new variables and we get in regard
with the thermomechanics including internal variables (Coleman &
Gurtin, 1967) a new system of constitutive equations
S (X, t) = S {E t # , Tt5K, A ( k ) t * l } (5)
h (X, t) = h {E t # , T**, 4 (k) t* T> (6)
0^ t * * t
F (X, t) = F {E t # , T t # , A (k) t*x ' (7)

H (X, t) H {E t # , Tt5*, A (k) t * .> (8)

set of internal variables (the mathematical character of

Vk) variables
the is different, for example scalar-value, vector-
value, tensor-value variables), k = 1, 2, ..., p; p - number of
internal variables
For the completeness of the system (5) - (8) we need some evolu-
tion equations. They should describe the evolution of the inter-
nal processes. So we can express the evolution equations in the
following standard form
d^ ( k ) /dt = f(E't* "(k)
t*
rt* (9)
Often the internal variables are dievided into variables for
rheological processes and variables for damage processes. Some
examples of damage variables are shown in the tabl. The solution
of damage problems, using the equations (5) - (9) is very diffi-
cult. At first, there are numerical problems for solution
methods (simultaneous calculation of the unknown mechanical and
72
damage Type of Example Remarks:
mathematical
object Author, year
scalar - continuity ID isotropic damage
tensor of L. Kachanov, 1958
rank 0 damage D isotropic damage; Rabotnov, 1959
dependence different behavior in tension and
from loading compression;
hD Ladeveze, Lemaitre, 1984

vector - vector of non-propotional loading orthotro-

tensor of continuity pic behavior; L. Kachanov, 1974
rank 1 damage vector many planar cracks;
Krajcinovic, 1983

tensor of non-symmetric orthotropic material;

rank 2 damage tensor Murakami, Ohno, 1981
symmetric orthotropic damage;
damage tensor Cordebois, Sidoroff, 1981
symmetric equivalent long-time damage;
damage tensor Pavlov, 1988
tensor of crack field;
crack density Vakulenko, M. Kachanov, 1971

tensor of non-symmetric orthotropic damage;

rank 4 damage tensor Chaboche, 1982
effective anisotropic damage;
damage tensor Chow, Wang, 1987

field quantities, partition of the two problems). At second,

there exist many problems with the verification and identifica-
tion of general constitutive and evolution equations.

CREEP DAMAGE MODELS, BASED ON ENGINEERING CONCEPTS

Most of the traditional investigations of creep damage models
are based on the scalar-value damage variable, introduced by
Rabotnov. This variable gives the best results in the case of
isotropic materials with isotropic damage. The results of creep
tests for some light alloys, polymers etc. show some effects,
which are not included in the classical models. Such an effect
is for example different behavior in tension and compression.
The following equations, based on an energetic variant of the
creep theory (Altenbach & Zolochevsky, 1990), include three
invariants of the stress tensor

I^(S) = S-I, I 2 (S) = S-S, I 3 (S) = (S'S)-S (10)

and a creep potential
S e = S 0 + aS + gS1 (11 )
with
S = BI 1 ? S 0 2 = A ^ 2 + CI 2 , S ^ = D ^ 3 + K ^ I g + EI 3 (12)
 73
A, B, C, D, E, K - parameters for the given material; a, g -
numerical coefficients (characteristics of the "weight" of the
Invariants S and S 1 )

Using the potential formulation and an associated flow law, we

get the constitutive equations in the following form
dE/dt = d E Q / d t U A ^ I + CS)/S Q + aBI
(13)
r 2 9
+ g f D I ^ I + BS'S + (K/3)(I2I + 2I1S)]/S1Z}
dEe/dt = f(Se) (14)

Finally, including damage into the creep process, from the equa-
tion (14) we get

dEe/dt = f(Se)/[(33|c/(Q# - 6)]m (15)

6 is the specific dissipation energy (S 6 [0, 13*]) and m is a

property for the given material. S can be related with Rabot-
nov's damage parameter. The evolution equation for 8 can be
determinated in the following form

dB/dt = f(Se)Se[3#/(8)(c - 8 ) ] m (16)

In a similar way the damage should be included into the consti-

tutive equations. The function f we can identify by experiments.

The system of constitutive and evolution equations contents 6

material's parameters. There are several possibilities to deter-
minate these parameters in general and for special cases by some
so-called basic experiments (uniaxial tension, uniaxial compres-
sion, pure torsion etc.). This problem is solved and proofed for
isotropic undamaged materials (Zolo^evskij, 1988), but also for
damaged materials (Altenbach & Zolochevsky, 1990).

DAMAGE MODELS FOR DUCTILE STEELS

A succesful describtion of the behavior of ductile materials

including damage is possible on the base of two damage models
(Sun et al . , 1989). The first model connects the nucleation,
growth and coalescence of microvoids with the macroscopic con-
stitutive behavior. Starting from the von Mises yield criterion
we can develop new plastic potentials. The first model was com-
posed for pourous solids (Gurson, 1977). This model deals with
the void volume fraction. The coalescence in the final state of
the material was taken into account involving a splitted func-
tion of void volume fraction (Tvergaard, 1982). In analogy with
the classical plastic potential theory it should be included
into these models anisotropy and hardening.

The second model is founded on an equation for the isotropic

increase of voids (Rice & Tracey, 1969). In this case the void
radius is the variable, introducing the microscopic effects into
the model. This model should be extended to more realistic void
shapes.
74
The ductile damage models are applicated to rupture and damage
development analysis (Sun et al.. 1989; Regener & Schick, 1990).
These analysises are possible only by using hybrid techniques
(destructive testing methods, numerical simulation, continuum
modelling). At present there are big differences between the
accuracy of numerical calculations and testing data. So it is
necessery to derive simple equations for prediction of load-
diameter change curves or stress-strain curves.

REFERENCES

Altenbach, H. (1990). Zu einigen Aspekten der klassischen Konti-

nuumsmechanik und ihrer Erweiterungen. Technische Mechanik.
±1, 95-105
Altenbach, H. & A.A. Zolochevsky (1990). Eine energetisch be-
grundete Variante der Theorie des Kriechens und der Langzeit-
festigkeit fur isotrope Werkstoffe mit komplizierten Eigen-
schaften (submitted to ZAMM)
Coleman, B.D. & M.E. Gurtin (1967). Thermodynamics with internal
state variables. J. Chem. Phys.. 47, 597-613
Fischer, F.D. (1987). Schadigungsmechanik - Ein modernes Konzept
zur Beurteilung des Bruchverhaltens. Berg- Huttenmannische
Monatshefte, 132, 524-534
Gurson, A.L. (1977). Continuum theory of ductile rupture by void
nucleation and growth: part I. J. Engng. Mat. Tech., 99, 2-15
Hult, J. (1988). Stiffness and Strength of Damaged Materials.
ZAMM. 68, T31-T39
Kachanov, L.M. (1986). Introduction to Continuum Damage Mecha-
nics. Nijhoff, Dordrecht
Kotoul , M., Z. Bilek, J. H^ebic'ek and P.Polcar (1989). Applica-
tion of Damage Mechanics to Numerical Fracture Simulation.
Acta Technica. KSAV. N° 5, 579-598
Krajcinovic, D. (1984). Continuum Damage Mechanics. Appl. Mech.
Rev., 37, 1-6
Krawietz, A. (1986). Materialtheorie - Mathematische Beschrei-
bung des phanomenologischen thermomechanischen Vernal tens.
Springer, Berlin
Lemaitre, J. et J.-L. Chaboche (1985). Mecanique des materiaux
sol ides. Dunod, Paris
Murakami, S. (1987). Progress in Continuum Damage Mechanics.
JSME - Intern. J.. 30, 701-710
Palmow, W.A. (1984). Rheologische Modelle fur Materialien bei
endlichen Deformationen. Technische Mechanik, 5, Heft 4, 20-31
Regener, D. & E. Schick (1990). Schadigungsentwicklung in einem
ductilen Werkstoff. Neue Hutte (in press)
Rice, J.R. & D.M. Tracey (1969). On the ductile enlargement of
voids in triaxial stress fields. J. Mech. Phys. Solids. 17.
201-217
Sun, D.-Z., D. Siegele, B. Voss and W. Schmitt (1989). Applica-
tion of local damage models to the numerical analysis of duc-
tile rupture. Fatigue Fract. Engng. Mater. Struct., 12, 201-
212
Tvergaard, V. (1982). On localization in ductile materials con-
taining spherical voids. Int. J. Fract.. 18, 237-252
Zolo^evskij, A.A. (1988). Kriechen von Konstruktionselementen
aus Materialien mit von der Belastung abhangigen Charakteri-
stiken. Technische Mechanik, 9, 177-184
WS1a8

AN ANALYSIS ON DUCTILE FRACTURE OF AL ALLOYS

H. MIYAMOTO, M. K1KUCHI AND H. OTOYO

Faculty of Science and Technology

Science University of Tokyo
Noda-shi, Chiba, Japan

ABSTRACT

The microscopic process of ductile fracture in the process zone of Al alloy,

2017-T4, is studied. By considering two kinds of microvoids, the finite
element analyses based on Modified Gurson's model are carried out. The
first void {5 urn.) Is assumed to nucleate following stress-controlled
nucleation, and the second void (0.08 u m.) following strain-controlled
nucleation. The approximate method( Tvergaard ,1982) is used with finite
deformation theory. Using the void volume fraction obtained from the
experiments the parameters fc , fp are evaluated, and the nucleation and
growth of voids and coalescence with the crack are simulated. Several
distributions of the large inclusions are considered, and among them the
distribution of large inclusions are simulated to the results of FRASTA and
some improvements are obtained compared with the previous results.

KEYWORDS

Fracture; Process Zone; Modified Gurson's model; FEM analysis;

Stress-controlled Nucleation; Strain-controlled Nucleation.

INTRODUCTION

As is well known Fracture Mechanics (Linear Elastic Fracture Mechanics,

LEFM, at present) was introduced by G. Irwin and P. Paris about 35 years
ago. Then it was extended to Elastic Plastic Fracture Mechanics, EPFM,
successfully by J. R. Rice and J. W. Hutchinson. The experimental method
to obtain characteristics, Fracture Toughness Kc , Jc of fracture
parameter K, J, respectively, are standardized in several countries, and
the fracture mechanics grew up to the important practical technology for
preventing and predicting the fracture of the metals and the metal
structures. It is used efficiently and successfully for designing and
inspection of the aeroplane and the nuclear pressure vessel.
But, "the fracture mechanism Itself" is not yet clarified until now. As is
well known, LEFM is only efficient outside the small-scale yielded zone and
inside the K-field, and EPFM, outside the process zone and inside the H-R-R
75
76
field. Therefore, in order to approach to the secret of the fracture
mechanism, it is necessary to step into the process zone. This paper is
one of the test to clarify this secret from the standpoint of the continuum
mechanics, and this will be called tentatively as Process Zone Fracture
Mechanics, PZFM.

Such kind of research is a topics of nonlinear fracture mechanics at

present, and among them the papers due to Needleman and Tvergaard, Aravas
and McMeeking are famous. Recently, P. F. Thomason and J. W. Hutchinson
discuss these problems. In Japan, there is the research group leaded by
Prof. H. Kitagawa, Osaka University, and Prof. M. Sakata, Tokyo Institute
of Technology.

The flow of the fracture mechanics is shown in Tab. 1.

The new books ( J. W. Hutchinson ,1987; P. F. Thomason ,1990) introduce the

fracture of the voided material. The papers introduced until now treat the
problems from the continuum mechanics side, but in near future the secret
of the fracture are expected to be clarified from the standpoint of both the
fracture mechanics and the fracture physics.

Now, the behavior of microvoids, the central mechanism of the ductile

fracture, will be considered in more detail.

At first, large voids (the primary voids) nucleates, under stress-

controlled nucleation from large inclusions or particles (0.5-50 //i, In our
case the mean diameter of inclusion in Al alloy 2017-T4 are 5.8 /im) at
relatively low load. Due to our experiments mean diameter I) of the first
voids Increases with the increase of the load J, but it has the limit Dc,
and at this point the carrying capacity of the matrix begin to drop. The
volume fraction at this point is fc. Then Dc dose not become larger by
increasing the load, and the material waits for the occurrence of the
localization.(Fig.1)

On the other hand, small voids (the secondary voids) nucleate from the
smaller inclusions or particles (0.05-0.5 p. m and in our case 0.0876 # m)
under plastic-strain controlled nucleation and grow at higher strain. Due
to the experiments ( Ohji et al. ,1980), during the first voids keeping
their radius at Dc, the secondary voids grow between the grown up first
voids and connect them.

By coalescing the primary voids by the secondary voids, the ductile

fracture will be completed and the dimples will be appeared on the fractured
surfaces. The void volume fraction at this instant is fp. But the
details of the mechanism is not entirely clarified.

The main difference between this paper and the previous paper ( Kikuchi e_t
al.,1990) is taking account of the action of both the primary voids (stress
controlled nucleation) and the secondary voids (strain controlled
nucleation) at the same time. Similar problem( Needleman and Tvergaard,
1987) was treared.

The determination of the fc, fF is carried out due to the data of the first
voids, as the character of the matrix to the void is the same for both the
first voids and the second voids. At the same time the authors expects to
know the behaviour of the second voids at fc and fF by the FEM simulation.
 77
CONSTITUTIVE EQUATION OF VOIDED MATERIAL AND
DETERMINATION OF PARAMETER

Constitutive Equation of Voided Material

As the constitutive equation of the voided material, the Modified Gurson's

model is used as the last paper( Kikuchi et al.,1990). The plastic
potential is given as follows:

* = 7V-2'*^osh ( ( Li^l ) _ (1+(qif . )J)=0 (

v
M £ (J M

where the matrix flpw stress is &M , the macroscopic Mises stress is
O e =(3/2 s 1 jS 1 j) 1 / 2 , in terms of the stress deviator s 1 j = < 7 i j - d±\
^ k k ^ * an(* (7 kk^^ *s t n e m a c r o s c ° P i c mean stress.
For f* =f, q 1 s q 2 s l . the expression (1) is that derived by Gurson. The
additional parameter q^ and q 2 and f* are the modified parameter due to
Tvergaard, and in this paper put q 1 =1.5 and q2=l-
To account for the final fracture of the material, f are modified as
follows:
f
,= | XSfc:
(2)
I f c + K (f-f c) f>fc.

.where K will be determined as the macro-carrying capacity will be lost

at f*=f*u. that Is, at f=f F , f* =f* u and from eq. (2),f*u =fc+K(fF -fc),
we obtain

K = —f V f c (3)
fr ~ f C
In this case fc, fp will be determined from the experiments.
Now, the increase of the void volume fraction consists of the void growth
and nucleation, that is,
=
* (*/ «rowth + (f) i«c|„i|M (4)

As the matrix is plastically incompressible, we obtain

( O «row|h = ( 1 - f ) ePKK (5)

The nucleation of the new void is given by the next equation.

(f) o«cl..tlon = B (C7 M + OKK) / 3 + D e \ (6)

The first term is used to model nucleation controlled by the maximum normal
stress on the particle matrix interface! Needleman and Rice ,1978), and the
second term models plastic-strain controlled nucleation. Further, void
nucleation is assumed to follow a normal distribution(Chu and Needleman
,1980). The stress-controlled nucleation is specified by
78
B=
i ^ r e x p < T (—i;—} > • D=0 (7)

and for the plastic strain-controlled nucleatlon

£N
D ■ - j ^ z r exp (-i- ( £PM ; )2) . B=0 (8)
S N ^ ? 2 SN
,where f
l N , lf »/
N • N : void volume fraction of void nucleating particle,
<7N * £ N mean stress and strain for nucleation,
S fl , SN' : corresP°n(ling to standard deviation.
The nonzero values of D and B in (7) and (8), respectively, are only used if
((7 M + O kfc/3) or S ? M e x c e e d their current maximum in the increment
considered.

Determination of Parameters

The determination of parameters fc, fF and fN in (2), (3), (7), (8) will be
stated. Tvergaard and Needleman used fc=0.15 and fj,=0.25 In their papers
for the ductile fracture of Cu and steel.
By using the experiments on Al-alloys, the fc, fp and fN of 2017-T4 are
determined as follows.

The growth of the primary voids of 2017-T4 are obtained from the SEM, as
shown in Fig.l of CT-specimen.( Miyamoto et al.,1986). The mean diameter of
the voids are shown on the ordinate and the J-value on the abscissa. The
mean diameter of the first void D increases due to the increase of the load
(J-value), until at D=Dc = 11.63 urain 2017-T4, the increase of the void
stops and this corresponds to the £ g=0, ( Brown and Embury,1973), and Dc
is smaller than the dimple diameter Do. Then by increasing J, the
localization occurs in the matrix, and the secondary voids grow between the
primary voids, and the coalescence of the dimples appear on the fractured
surface. There can be seen many small voids on the fractured surfaces with
the large voids. The mean diameter of the dimple Do is composed of the
diameter of the Do+1.3do, where do is the mean diameter of the secondary
voids.
The void volume fraction at fp can be obtained due to Do. The mechanism
how the micro void bring about the last process of the ductile fracture
can't be cleared from this data only.

By calculating the number of dimples per 1mm2 on the photographs of SEM,

and assuming the voids number per unit volume, the fc and fp obtained
by using the Dc and Do value. The value of f^ are obtained from the
diameters of the inclusions on the polished surface of the specimen before
the test. These values are shown in Tab.2.

The secondary inclusions (0.05-0.5 //m) cannot be clearly seen by using SEM,
the observation is carried out by using TEM on the surface of the electronic
polished specimen. The secondary particles are composed of Cr and Cu
compounds whose mean diameter are 0.0876 urn. From the fractured surface of
the secondary voids, their diameters become 0.748 /^m at fracture (Tab.2).
 79
Analysis of Ductile Rupture Mode at a Crack Tip,

Finite element method mesh near the crack tip are shown in Fig.2.
Considering the void volume fraction fN due to the experimental results of
SEM, two examples of the distribution of the large inclusions are shown in
Fig.3(a) and 3(b), respectively. The radius of curvature of the crack
tip is assumed 2 u m,and the dimension of the large inclusion is a square
with the side of 6 u m. As the dimension of the process zone is 120 n m due
to a experiment in the previous paper(Miyamoto et al.,1986), the
arrangement of the crack and voids in Fig.3(a)and 3(b) can be thought to be
inside the process zone.
The nucleation criterion of both the primary and secondary voids are shown
in Tab.2. By using two kinds of the nucleation strain £ N = 0 , 3 a n d °-6»
two models are evaluated.
The FEM analysis is carried out by assuming the plane strain state based on
the finite deformation theory.
The number of elements and nodes is 766 and 805, respectively. By the
symmetry shown in Fig.2, the calculation is carried out only on the upper
half. Matrix properties are specified by E=71.8(GPa), Q n =272(MPa),
V =0.3.
The stress-strain response of the matrix is given by

a M = 2 . 3 1 a . ( 0.0095 + e \ )0248 (9)

Table 1. Flow of Fracture Mechanics

LEFM EPFM PZFM

ELASTIC EL-PLASTIC EL-PLASTIC

DEFORMATION INFINITESIMAL INFINITESIMAL FINITE
DEFORMATION DEFORMATION DEFORMATION

DENSE DENSE VOIDED

MATERIAL
BRITTLE DUCTILE DUCTRILE

F.C. K=K C J = Jc f=fr

CT0D CT0D

Table 2. Dimensions of void and f N. fc and f F and a N. e N. S N

2017-T4

diameter D and d void volume fraction <7N SN

p. m f e N SN'

inclusion D=5. 57 f N =0.021

Primary at f c Dc=ll. 63 fc=0.169 3.1(7. 0.10a.

void
at iT Do=12.78 fr=0. 206

inclusion d=0.0876 fN'=0.013 0.3

or 0. 10
Secondary 0.6
void
at fr do=0.748
80
15 A
A tC'1279
0
6 <?* n 63
o
10
E
A : Average of
Q (
dimple diameter
o : Average of
5 ■ ^D=0.16.J 5.57 void diameter

2017
m
Fig.l. Relation of void diameter Fig.2. mesh near the crack tip.
and J value.

1
—. D Q_
(a) (b)
Fig.3. Distribution of the large inclusions.

REFERENCES

Brown, L.M. and J.D.Embury(1973). The initiation and growth of voids

at second phase particles, Proc. 3rd Int. Conf. on Strength of metals and
alloys, 164-169, Inst. of Metals, London.

Chu.C.C. and A.Needleman(1980). J.Engng.Mat.Tech.. 102,249-256.

Hutchinson, J.W. (1987). Micro-mechanics of damage in deformation and

fracture, Department of Solid Mechanics. Technical University of
Denmark.

Kikuchi.M, H.Miyamoto, H.Otoyo and M.Kuroda(1990). Study on ductile

fracture of Aluminum Alloys, JSME., 523A, 217-225.

Miyamoto.H, K.Machida, H.Okayasu and T.Kawazoe (1986). Study of the

process zone at the crack tip.
In: Mechanical Behaviour of Materials-V (M.G.Yan, S.H.Zhang, Z.M.Zheng).
Vol.1, pp.39-50. Proc. 5th, Int. Conf. Beijin, China.

Needleman.A and V.Tvergaard (1987). An Analysis of Ductile Rupture Modes

at a Crack Tip. J.Mech.Phy.Solids, 35, 2, 151-183.

Needleman.A and J.R.Rice (1978). Mechanics of Sheet Metal Forming

(D.P.Koistinen and N.M.Wang), pp.237-267, Plenum Press, New York.

Ohji.K, K.Ogura, K.Ohmori and T.Nomizu(1980). Observation of Microvoid

and Critical Condition for its Initiation in Ductile Fracture of High
Strength Materials, Jour.Soc.Materials Science, Japan, 29,321, 550-555.

Thomason, P.F.(1990). Ductile Fracture of Metals. Pergamon Press.

Tvergaard.V (1982). Material Failure by Void Coalescence in Localized

Shear Bands. Int.Jour.Solid Structures, 18,8, 659-672.
WS1a9

FINITE ELEMENT ANALYSIS ON NEAR-TIP FIELDS

UNDER MIXED MODE CONDITIONS

K. KISHIMOTO*, N. T A K E U C H I " and S. AOKI"*

•Department of Mechanical Engineering for Production,

Tokyo Institute of Technology,
O-okayama, Meguro-ku, Tokyo 152, Japan
**Imaging Technology Research Center, Richo Company Ltd.,
Nakamagome, Oota-ku, Tokyo 143, Japan
***Department of Mechanical Engineering Science,
Tokyo Institute of Technology
O-okayama, Meguro-ku, Tokyo 152, Japan

ABSTRACT

A large deformation finite element analysis has been performed to study

the stress and strain fields near the crack-tip under mixed mode conditions.
The effects of microvoids on plastic flow are taken into account by using
the continuum constitutive model introduced by Gurson. Influence of hydrostatic
stress and strain hardening exponent on the near-tip field is examined.

KEY WORDS

Ductile fracture; mixed mode; hydrostatic stress; strain hardening exponent

INTRODUCTION

Structural members are often subjected to complex loading and the tip
of an existing crack is deformed under mixed mode loading. Crack propagation
in ductile materials usually occurs when the blunted crack tip coalesces with
adjacent microscopic voids. With increasing mode II component, crack due to
shear fracture appears at the sharpened corner of the crack tip and the
occurrence of the share type fracture affects the critical value of the J
integral at fracture initiation (Aoki et al., 1990).

The authors (Aoki et al., 1987: Kishimoto et al., 1989) have performed a
finite element analysis on the mixed mode crack-tip fields. Since the void
growth is very dependent on the stress triaxiality and plastic properties of
the material, the fracture behavior would be influenced by these factors. In
this paper, influence of stress state (plane strain and plane stress) and strain
hardening exponent of the material on the near-tip field is examined by using
a large deformation finite element method based upon Updated-Lagrangian
method. The presence of the void is taken into account by using Gurson's(1977)
constitutive equation. Numerical results of the near tip stress and deformation
fields as well as the void volume fraction are presented.
81
82
NUMERICAL METHOD

The large deformation finite element program developed by the authors(1984)

is used. Figure 1 shows the finite element mesh used for computation. In the
figure, d0/2 is the radius of curvature of the initial crack tip and later we
refer to a linear distance between A and B in a deformed state as a crack
tip deformation length d in which A and B are the intersecting points of the
straight flanks and the curved notch surface. In the computation the
displacement at the nodes on a peripheral circle far from a crack tip (R
= 12000rfo) is specified by

d (1)
0 0Jd0 L Wo / Wo

where R0 and 0o are polar coordinates in an undeformed state with an origin

O. o0 is the tensile yield stress in terms of Cauchy stress. Kj and Ku are
stress intensity factors of Mode I and II, respectively and %f (Af=J,Jj) is
the known function of R0 and 0o for each mode. Mixed mode conditions
expressed by a ratio of Kn to Kj are specified as KJJ/KJ=0 and 1.732 in
the present computation. These ratios correspond respectively to (l)0=9O°and
(2)0=30° where <f> is the angle between the uniaxial tensile loading direction
and the crack plane in the inclined crack problem.

As for the rate of void nucleation, we employ the following equation proposed
by Needleman and Rice(1978)

kk
fnucleation - F\°m + ^2 3 (2)

where / denotes the the volume fraction of microvoids, Om the effective

Mises stress of the matrix material, and o ^ the macroscopic (average) true
stress. Zero initial void volume fraction /=0 is assumed and the constants
associated with microvoid nucleation are specified as Fi=0.01 and F2=0. The
stress-strain relation of the matrix material is modeled by power hardening
rule. The computation has been performed for the cases of the strain hardening
exponent N=0.1 and 0.3 under the plane strain or plane stress condition.

2470 NODES
4784 ELEMENTS

(a) Whole configuration (b) Minute subdivision

Figure 1. Finite Element Mesh.
 83
An increase in the void volume fraction / brings softening of the material
and makes the macroscopic hardening rate H fall. According to an analysis
by Rudnicki and Rice (1975), shear localization occurs when H reaches a
critical value Hcrit. Although this condition refers to a uniformly strained
specimen that has been subjected to proportional loading, we adopt this
condition here for the purpose of simplicity and determine the region where
the shear localization condition H^Hcrit is satisfied.

NUMERICAL RESULTS

Figure 2 shows the deformed shape of the crack-tip for the case of strain
hardening exponent N=0.1 and 0.3. In the mixed mode loading, contrastive
deformations appear at the upper and lower regions of the crack-tip, i.e.,
sharpening and blunting. The deformed shape of the crack-tip is influenced
by strain hardening exponent.

Y/do
/v
4

N = 0.1 . 2
N = 0.3 *"*>.
N = 0.1
N = 0.3
-4 -2_ 0
)fj v. ' 45
1//
-2*-*T

Plane Strain - Plane Strain

- Plane Stress -4 Plane Stress

(a) 0=90° (Mode I) (b) 0=30° (Mixed mode)

Figure 2. Crack-tip deformation (Jappl(d000)^6.3)
Blunted
Dinged crack-tip Dinted Blunted
refi on crick-tip field HBH field \ field

(a) 0=90° (Mode I) (b) 0=30° (Mixed mode)

Figure 3. Circumferential stress H Q (JV=0.1, Jappl(d000)^6.3).
84
The variation of the normalized circumferential stress O Q (=0 QI00) is shown
in Fig.3 for AT=0.1. As shown by Aoki et al. (1987), the stress field near
the crack-tip may be divided into for regions; (1) the K field, (2) the HRR
field, (3) the blunted crack-tip field, and (4) the damaged region. The

10

\ ^=30* [6 =-60* )

0.5
10

Figure 4. Hydrostatic stress variation (AT=0.1, Jappl(d000)i=?6.3)

Y/d
2 ^
i

5 / s>
n
1 / s'
1 / 20

~^<S*x> . /
x
,
-2
,
-1 0 2

20 ~~

1 /
< — ' - ,
(a) AT=0.1, plane strain (c) AT=0.3, plane strain

(b) Af=0.1, plane stress (d) AT=0.3, plane stress

Figure 5. Equivalent plastic strain (%, Jappl{d00 ^^63).
 85
variation of the hydrostatic stress is also shown in Fig.4. In mixed mode
loading, the level of hydrostatic stress is low and the difference of the results
between plane strain and stress becomes small.

The distributions of the equivalent plastic strain £ P .are plotted in F i g . 5 for

mixed mode cases. Owing to the significant sharpening of the crack-tip, the
concentration of plastic strain at the upper region is significant for JV-1.0.
As shown in Fig. 6 the concentration of microvoids at the upper region
appears only for AT=1.0 of the plane strain state. This is attributable to the
fact that the hydrostatic stress is low in the mixed mode loading.

The regions in which the macroscopic work hardening rate satisfies the
condition H<Hcrit is shown in Fig. 7. It is noted that this region has not
appeared in the plane stress state under the present computational conditions.

If we assume that void type fracture initiates at the place where the
localization condition is satisfied, we may conclude that the fracture of this
type initiates at the midthickness of the specimen in which the plane strain
state is predominant. One the other hand, the plastic strain concentration
would result in the shear type fracture near the surface of the specimen in

X/d

(a) N=0.1y plane strain (c) AT=0.3, plane strain

Y/d Y/d
A
v
2
2
-».o—-«. ^ 2 -°^"~
1

/
X/d
?.^ x
Wf -1
-r>
TOX)/

■jj 3.0
/ i
J p
1

-2 -2 ^-20—"
(b) # = 0 . 1 , plane stress (d) # = 0 . 3 , plane stress
Figure 6. Void volume fraction (%, Jappl(do°o)^**.!).
86
which plane stress state is predominant. This results agree with the experimental
observations (Aoki et al., 1990) that cracks due to shear fracture initiated
at the sharpened corner of the crack tip near the surfaces of the specimen,
and another crack due to dimple fracture occurred at the blunted corner of
the crack tip near the midthickness of the specimen. The present results also
suggests that the shear type fracture tends to occur at the sharpened corner
of the crack-tip for the material with lower plastic hardening exponent.
Y/d

(a) AT=0.1 0=90° (c) #=0.1 0=30°

—Y i
1.0 -0.5 0 ^ 5 1.0 Y/d

X/d

(b) AT=0.3 0=90° (d) N

=Q-3 ^=30°

Figure 7. Region where the localization condition is satisfied.

REFERENCES
Aoki, S., Kishimoto, K., Takeya, A. and Sakata, M.(1984). Effects of
microvoids on crack blunting and initiation in ductile materials. Int. J.
Fract., 24, 267-278.
Aoki, S., Kishimoto, K., Yoshida, T. and Sakata, M.(1987). A finite element
study of the near tip deformation of a ductile material under mixed mode
loading. J. Mech. Phys. Solids, 35> 431-455.
Aoki, S., Kishimoto, K., Yoshida, T. Sakata, M. and Richard, H.A.(1990).
Elastic-plastic behavior of an aluminum alloy under mixed mode loading.
J. Mech. Phys. Solids, 38, 195-213.
Gurson, A.L. (1977). Continuum theory of ductile rupture by void nucleation
and growth: Part 1 Yield criteria and flow rules for porous ductile media.
Trans. ASME Ser.H, J. Engng. Mat. Tech., 99, 2-15.
Kishimoto, K., Yoshida, T., Aoki, S. and Sakata, M.(1989) Finite element
analysis on hole growth near a crack tip under mixed mode conditions.
In: Proc. 2nd Int. Conf. on Computational Plasticity, Models, Software
and Applications Part II, (D.R.J. Owen et al. Eds.), Pineridge Press,
pp.1183-1194.
Needleman, A. and Rice, J.R.(1978). Limit to ductility by plastic flow
localization, In: Mechanics of Sheet Metal Forming,(D.P. Koistinen and
N.M. Wang, Eds), Plenum, pp.233-267.
Rudnicki, J.W. and Rice, J.R.(1975) Conditions for the localization of
deformation in pressure-sensitive dilatant materials. J. Mech. Phys. Solids,
23, 371-394.
 WS1b1

THERMODYNAMICAL REFERENCE MODEL OF METALLO-THERMO-MECHANICS

B. RANIECKI* and 0. BRUHNS**

Institute of Fundamental Technological Research, Polish Academy of Sciences,

Swietokrzyska 21, 00-049 Warsaw, Poland.
•*
Ruhr University, Institute of Mechanics I, D-4630 Bochum 1, Postfach 102148,
Germany

ABSTRACT
Thermo-mechanics of phase transitions in metallic materials (or metallo-ther-
mo-mechanics, cf. Inoue, 1987) aims at formulation of basic coupled field e-
quations for reliable computer simulation of stresses and deformations gen-
erated in solids in the course of heat-treatment operations, welding or
chilling of castings. In the paper the concepts of classical thermodynamics
are used to develope general framework for possible simplest constitutive
model that takes into account the average intrinsic stresses that are pro-
duced within the colonies of individual phases. The ideal metallic element
considered here reduces to a mixture of "ideal solid solutions" in the limit
when all shear stress effects are neglected. The work complements the erlier
studies of Giusti, 1983 and Inoue etal., 1985.

KEYWORDS
Plasticity; phase transformations in solids.

NOTATION
A -B ♦ A.B. or A ^ B . . ; A B * A. .B jk or A. . ^
(! a) means "do not sum over repeated indexes a',' and superimposed dot de-
notes differentiation with respect to time. Greek subscripts (superscripts)
denote properties of phases, whereas Latin capital- properties of components.

FREE ENERGY OF ELASTIC-IDEAL-PLASTIC SINGLE PHASE HOMOGENEOUS

MATERIAL ELEMENT
Consider single phase multicomponent elastic ideal-plastic metallic element.
To specify its specific free energy $ a (phase a) use the following two exper
imental facts: i) above Debey temperature the specific heat c a at constant

87
88

elastic strain e e (infinitesimal strain) of a phase a is practically func-

tion of its chemical composition x" alone (K= l...r denotes a component num-
ber, x" is weight fraction of a component K in the phase a ) , ii) elastic be-
haviour of most of metallic solids may be approximated, with rather good ac-
curacy, by linear relationship between T =a /p a and e e at eyery temperature
T (here a and paare usual Cauchy stress tensor and mass density of the phase
a , respectively). Ideal plastic models do not account for the free energy
locked in the alloy element due to possible development of micro-stresses,
defects creation etc., which is normally small fraction of the total plastic
work. In effect one gets

♦a(T,4,X«)=0.5 e ^ - (T-T0)B£(x°).A C«(X-)(T-T 0 ) -

<*\
-c^(x£)T ln(T/T0)-T su(x£)+ u a (x£) (1)

Here, *a
s ( x j and u (x») represent specific entropy and specific internal en-
ergy at natural state where £^=0, 2^=0 and T=T 0 (reference temperature). The
former term includes also so called entropy of mixing (cf.,e.g.,Kestin,
1979, Reed-Hill, 1964). 3° denotes tensor of elastic thermal stresses at
e =0, expressed in units of work per unit of mass per °K (energetic elastic
thermal stresses), and L is tensor of isothermal elastic stiffness also ex-
pressed in terms of units of work per unit of mass. Two basic thermal equa-
tions of states are

T = v(3<|>'u/3e
-a
c
L e c - v (T-T
-a')= —a-a u /0)B°(x")= L°e c -v (T-T
-a v K' -o-a u / 0)BN (x",e )
-a K -a'
(2)
s°= (- 3*a/3T)= c°(x£) ln(T/T0) + 0.5 • £ • £ , £ * £ ( X||)M£ +
*°

where sa is specific entropy and $ is thermal stress tensor. The solution

of (2), with respect to e e is
+
£ - Mala (T-To) •.(T.xJ) ; a, = M ^ x " ) (3)

where a" is secant (engineering) thermal expansion tensor defined in the

chosen natural state, M is isothermal elastic compliance of phase a (in-
verse of L ). The change in the total free energy when unit of mass of com-
ponent K is dissolved in the phase a is represented by the chemical poten-
tial yj! defined by (^ and T are fixed)

y
K= fK +
* ° - * fKXK ; f = 3 a 3x
K ( * / K>
f4)

K=l

Two basic assumptions i) and ii) imply independence of J^ on T, linear tern-

 89
perature dependence of L

>* - !£<*;> - (T-To)^(xaK) ; I. = 5 j ( * ^ < x M (5)

and definite nonlinear temperature dependence of oT (cf.,(3) 2 ).

MULTIPHASE, MULTICOMPONENT METALLIC ELEMENT

We shall now consider n-phase (a=l...n) r-component (K=l...r) metallic ele-

ment that is enclosed by a diathermal wall impermable to the matter. Its o-
verall chemical composition C K is fixed. However, the individual phases are
treated as homogeneous elastic ideal-plastic subsystems open to the flow of
matter. Their weight fractions c a , chemical compositions x? and common tem-
perature T are varying in time due to possible internal diffusion of some
components associated with the formation of phases and heat exchange.
The mass balance gives

I ca(t)x£(t) = C K ; I x°(t) =1 (6)

Thus, in the set {x£,ca} containing n(r+l) variables there are only r(n-l)
variables independent. In what follows we shall use the summation convention
according to which the summation should be performed over all repeated (twice
or more) Greek or upper case Latin indices occurring in product terms.
Denote by <J> the overall specific free energy of a multiphase element. The
discussed simplified reference model is characterized by the following addi-
tional assumptions

♦ (T,e,b£,ha) = c V ( T , e J , x J ) ; e£ - L - e£ f (7)

where, b?= {x°J,ca} is the set of metallography internal parameters, h ={ejj }

is the set of inelasticity internal variables, £ is an overall total
strain, e p is intrinsic strain due to plastic flow and phase transitions
(averaged over the colony of the phase a),and <|r has the form (1) for all
phases with common reference temperature. More generally, one should take in-
to account other metallography internal parameters such as mean grain size
of the colony of a phase, parameters representing the shape and distribution
of grains etc., as discussed by Tomota and Tamura (1982).
One can further follow the general thermodynamic framework developed by Hill
and Rice (1973) with slight modification resulting from constraints (6).
Using the technique of Lagrange multipliers (here A„ and A ) one can define
a set of affinities
f° = A AKx£ ; f£ = caf£ + Aa+AKca ; f£=0*a/3x£) (la) (8)

which together with basic thermal equations of state s=c a s a , j^cax (T^O/P*
where a_ is overall Cauchy'sstress tensor, and p is mean mass density of an
element) enables to write the fundamental Gibbs equation in the form
90

d* =-sdT + dW° ; dW°= x .de -c°x •dE pf +f°dc 0 +f°dx" (9)

— — —ci —ot is i\
where, dW° represents the increment of work in the conceptual reversible
process, s a and x are intrinsic specific entropy of the phase a and intrin-
sic stresses (averaged over the colony of the phase, cf.(2)),respectively.
By writing thermal equations of state for s and x_ in the rate form, it can
be shown that the discussed model predicts Voigt estimates for overall elas-
tic stiffness, overall specific heat at constant £ and overall elastic ther-
mal stresses. Moreover, these quantities have the same type of temperature-
dependence as the corresponding quantities for single phase.
At unconstrained equilibrium under fixed e e and T, we have f a =0 and f?=0,
—a l\
what implies that chemical potential y£ of every component (K is fixed) must
be the same in each phase.
Combining (9) with the first law of thermodynamics,du=dq+j/de (u-internal
energy, u= ♦+ Ts, and q is the heat supply), one arrives at The expression
for the entropy production

s-q/T = D/T= T.£ - W° ; D= c a T -e p f - f a c° - f?x? * 0 (10)

^ -a -a K K
where D is the rate of energy dissipation that cannot be negative on account
of second law of thermodynamics. Equation (10) immediately suggests a rea-
sonable choice of the set of irreversible forces Y K T ,-f »-f„} and thermo-
dynamic rates y ={ e p , c a , *£}. To complete the set of all constitutive
—Ot l\
equations that would enable to describe the evolution of all state variables,
when £(t) and T(t) are prescribed, one needs 6*n +n(r+l) kinetic relations
between Y and y. The kinetic relations couple the kinetic equations of for-
mal theory of phase transformations (Christian,1965) with the rate equations
of the intrinsic plastic flow. The available experimental data (cf. review
of Denis et al.,1985) concern mainly simple uniaxial stress state and still
much of experimental work has to be done (at the border of mechanics and
metallography) to deduce meaningful kinetic relations. Here, we shall try
provisionally to formulate them in general "mixed" form. The generalized
internal plastic flow rule at the presence of solid-solid phase transforma-
tions can be written in the form e P = e P + e p, where e P represents the usual
r
-a —a —a —a
plastic flow within the colony of the phase a. This flow is regarded as rate
independent and ideal plastic. To simplify the issue we assume that the yield
condition of the phase a depends merely on intrinsic stress T acting in this
phase. Let Fa(x ,st)=l (st= {T.c3 ,x")> 3=1...a..n, K=l..r) be the yield con-
—01 n IN
dition of the phase a, where F is homogeneous function of order one with re-
spect to T . Whenever F a <1 the local plastic strain must vanish E P = 0 , and
-<* —a
when —a
x and'St' are such that F =1 the local rplastic flow rule is
i£=A°Fa (F053F0/3la) (!a) (11)
a
where undetermined multiplier X must be non-negative to satisfy (10) when
all c a =0 and x£=0. It should be determined in the usual way, with the aid of
local consistency relation Pa=0.The second tensor £^ p describes thermodynam-
ic cross effect "transformation induced intrinsic plasticity". To encompass
 91
p
existing models of this effect we shall express e* in terms of c and x,
(instead of f p and f£)
K
assuming, in the first instant, that the relation is
linear,

(12)
B K
In general, J^ and J^g can be functions of all state variables and have to be
specified in every particular case in such a way that the constraint rela-
tions (6) and the inequality (10) are satisfied. The general form of kinetic
equations for internal flow of matter within the multiphase element is

(13)
The first two terms occurring in (13) represent the kinetics of usual temper-
ature-induced phase transformations, and the last terms indicate that "strain
induced phase transformations" can be interpreted as the thermodynamic cross
effect.
The application of a reference model specified within the presented frame-
work will require careful estimation of initial values of intrinsic stresses,
sa
y T?*\» t n a t develop in the new phase (say, a=(i)) at the very beginning
of its formation (say, at time t9 when cv 's0) from the parent phase a=(i-l).
This stress does not need to coincide neither with the instantaneous overall
stress nor with instantaneous intrinsic stress of the parent phase
Equivalently, one can try to estimate the initial "phase distor-
tion" of the new phase. Any choice of is significant hypothesis which can
be verified, for instance, by trial and error when comparing the experimen-
tal data with the theoretical one, or it can be estimated by use of special
micro-mechanical models.
To show implications of specific model, consider 3-axial resemblance of typ-
ical uniaxial experimental program concerning isothermal decomposition of a
parent phase (a=l) into new harder phase (a=2) under small constant overall
stress T = T+, applied before beginning of the transformation (at time t<t
and such that F <1. Denote by "prime" the deviatoric
parts of appropriate tensors, and by AT_* the initial intrinsic extra stress
in the new phase Assume provisionally that: a) both
phases have the same isotropic elastic properties, b) is constant
for t> Under these additional simplifications the
model predicts that plastic flow in the parent phase starts when weight frac-
tion of the new phase is where F, is the
ratio of external stress and the yield stress of the parent phase at simple
tension, provided that Huber-Mises yield condition is adopted. The overall
strain due to transformation is where G is
the elastic shear modulus. The normalized function m for different c is
shown in Fig.l. The thick solid line shown in this figure represents the ex-
perimental data collected by Leblond elt al_. ,(1989), for the bainitic trans-
formation in A.533 steel. The discrepancy seems to be acceptable for C Q S O . I S .
Using Greenwood-Johnson formula for total strain amplitude, the parameter n
92

Fig.l

can be expressed in terms of yield limit Y at simple tension of weaker phase

(parent phase) and the volume dilatation AV/V associated with the phase tran-
sition, n= 56AV/(2YV). For austenite-pearlite transformation AV/V=3.6-10~3
(Gautier et al., 1987). Taking 6/Y=600, one gets n=5.4. Hence, plastic flow
in the austenite occurs when F^> 0.16. The average stress deviator in the
in the pearlite colony at the early stage of transition is T J O X U ? ^ " * ' ^ !*•
At the termination of the phase transition it relaxes to T±.

REFERENCES
Christian, J.W. (1965). The Theory of Transformation in Metals and Alloys.
Pergamon, Oxford.
Denis, S., E. Gautier, A. Simon and G. Beck (1985). Stress-phase transforma-
tion interactions- basic principles, modelling and calculation of inter-
nal stresses. Material Sciences and Technology, j_, 805.
Gautier, E., A. Simon and G. Beck (1987). Plasticite de transformation dur-
ant la transformation perlitique. Acta Metal!., 35, 1367.
Giusti, J. (1983). A model of thermo-mechanical behaviour of metals with
phase changes. Mechanics Research Communications, 10, 3, 163.
Hill, R. and J.R. Rice (1973). Elastic potentials and the structure of in-
elastic constitutive laws. SIAM J. Appl. Math., 25, 448.
Inoue, T. (1987). Metal 1 o-thermo-mechanical coupl ings. Berg und Htitten-
mannische Monatshefte, 132, Heft 3, 63.
Inoue, T. and Zhi-Gang Wang (1985). Coupling between stress, temperature
and metallic structures during processes involving phase transitions.
Material Sciences and Technology, 1, 10, 845.
Kestin, J. (1979). A Course in Thermodynamics, Vol. 1. Hemisphere Publishing
Corporation, New York.
Leblond, J.B., J. Devaux and J.C. Devaux (1989). Mathematical modelling of
transformation plasticity in steels I: Case of ideal-plastic phases.
International Journal of Plasticity, 5_, 551.
Reed-Hill, R.E. (1963). Physical Metallurgy Principles. Van Nostrand Company,
Princeton, New Yersey.
Tomota, Yo. and I. Tamura (1982). Mechanical behaviour of steels consisting
of two ductile phases. Transations ISIL, 22, 665.
WS1b2

BEHAVIOR AND MODELIZATION OF AN AUSTENITIC STAINLESS STEEL

IN CYCLIC VISCOPLASTICITY, FROM 20 TO 700°C

P. DELOBELLE

Laboratoire de Mecanique Appliquee associe au CNRS - LA 04

Faculte des Sciences et des Techniques
La Bouloie - Route de Gray
25030 BESANCON CEDEX (France)

ABSTRACT
The objective of the present paper is, on the one hand, to set forth the
diversity of mechanical properties of an austenitic stainless steel over
a large temperature domain (20 < T < 700°C), including its monotonic,
cyclic (uni-directional and bi-directional tension-torsion tests, both in
and out of phase) and viscous characteristics, and, on the other hand, to
present the possibilities of a unified model having internal variables
(developed during the past 4 years) with regard to the presented experi-
mental observations.

KEYWORDS
Stainless steel, mechanical properties, cyclic properties, viscoplas-
ticity, bi-directional loadings, unified model.

INTRODUCTION
The industrial materials used in certain components of modern instal-
lations (the nuclear industry in the present case) are often submitted to
mechanical and thermal loadings and the knowledge of the behavior and the
development of the anisothermic laws proves to be indispensable for the
prediction of the life duration of the installations. However, before
performing and modelizing real anisothermic tests, where the thermal and
the mechanical loadings evolve cyclicaly and simultaneously, the identi-
fication and the phenomenological modelization for different isotherms of
the physical mechanisms taking part in the strain, is necessary. This
article presents the results relative to this first step, in the case of
an austenitic stainless steel.

EXPERIMENTAL METHODS
The specimen of stainless steel are obtained form slabs cut out of 30 mm
thick plates and hyper-quenched from 1200°C. The weight composition of
this low carbon steel, with controlled nitrogen content is given in
Table 1.

Table 1. Weight composition of the steel

C P Si Mn Ni Cr Mo N B Co Cu
<0.03 <0.021 0.44 1.084 12.3 17.54 2.47 0.075 0.001 0.15 0.17

Differents machines have been used to perform the tests, notably : hydrau-
lic and electrodynamic tensile-torsion machines controlled by computer.
93
94
EXPERIMENTAL RESULTS
Figure 1 shows the evolution of the flow stress 3" for a constant strain
rate, hzz = 6.6 10" s" , and different strain levels, as a function of
the temperature. A plateau appears between 300 and 550°C. Figure 2, curve
b, represents, for a constant shear strain rate, eT = 5 10 s"1, and for
an V. Mises equivalent plastic strain (Kcp/2) * 2.2 10" 3 , the evolution
of the equivalent stabilized stress {Kb/2) as a function of the
temperature. The behavior is very different from that observed in Fig. 1
and a significant peak is seen, having a maximum around 550°C and whose
width is contained between 200 and 600°C, that is, approximately the zone
corresponding to the plateau of the preceeding figure. Note that such a
maximum has already been observed for a 304 and a 316 stainless steels
[1-2].

| o ; c t » 7N m - 2] $ T - 6 > 6 1- 0V
o tests
—model
D
LTD ^ ^ > ^
S45JK ^ * o o—cr-Ck,
ko ^v/X
r50 N
^ ^-"'—-"r.--

n --^-•-■.•J.uL,_;;;;;^
0 WO 200 300 400 500 600 TOO 800
ml

Fig. 1 Variation of the flow stress ~ with the temperature.

Tests and simulations.
Fig. 2 Evolution of the equivalent cyclic stresses, a) first
cycle, b) stabilized cycle (ID), c) 90° out of phase
stabilized cycles, as a function of the temperature. Tests
and modelization.
In terms of strain rate effects (in a ratio o f 10 3 ), Figure 3 shows that
the sensitivity coefficient n of the stabilize d stress to the strain rate
(Aa**ab(1.5 10"3 s"1))/(AaJJab(l.5 10 - 6 s -1 )) can be positive or negative
depending of the temperature of the test. The negative value is observed
in the intermediate temperature domain (300 < T < 500°C) and corresponds
exactly to that of the peak mentioned earlier . At low temperatures, this
coefficient is positive, which is due to a cold viscosity effect. For
higher temperatures, T > 600°C, the sensi tivity is naturally positive
since the thermally activated recovery effects lead to an increase of the
viscosity with the temperature.

For the 2D cyclic loadings, it is shown [2-4] that a supplementary harde-

ning appears, which is mostly a function of the degree of phase difference
cp between the strain components and the ratio R = em /cm between the
maximum amplitudes of these components. This hardening is maximum when cp =
90° , R = 2/ >/3, and is a strongly decreasing function of the temperature
(Fig. 2, curve c, for Ac? = 2 . 2 . 10" 3 ).
 95
As for the viscous properties, the viscous component TJ^ (a = 1J-'a, where'a
is the applied stress and a the sum of the contributions of the different
internal stresses) is measured as a function of the temperature by the me-
thod of inverse relaxation [5] (strain dip test technique), during a test
conducted at a constant strain rate cT = 6 . 6 10"4 s"1 . Figure 4 shows, for
different strains c, that ^ increases with ~c and passes through a minimum
around 300°C.

L 0£ [»7Nm-2]
U-tetts
to-ati.5K>y) K-model
17.12SPH

9 100 2po"~3po" 400 500 6p3 700 800 T fc]|

Fig. 3 Evolution of the stabilized stress ratio for two fixed

strain rates in a ratio of 101 Experiments and
modelization.
Fig. 4 Evolution of the viscous stress *a with the temperature
for three levels of strain. Tests and simulations.

Figure 5 presents the results of several creep tests for different tempe-
ratures and stresses and corroborates the results presented in fig. 4 :
cold and hot viscosity effects, loss of viscosity at intermediate tempe-
rature. For the tensile-torsion ratchet [6], the test parameters are such
that 50 Mpa, A£^e/2 - ± 0.35 % and h\% = ± 4.6 10v5 ,-1 The
ponse to this type of loading consists in the appearance of a progressive
axial strain ezz (fig. 6) due to the axial and shear stresses and in a cy-
clic hardening in the direction of the shear component. In the limits of
experimental accuracy the stress for the stabilized cycle corresponds to
the stress obtained in pure torsion for the same strain amplitude (fig.2).
?%
V
T.eootj

Fig. 5 Simulation of different creep tests.

50 100 ISO 200 250 300 350 'd)
Fig. 6 Evolution of the progressive strain
er = f(N). Tests and modelizations.
96

In conclusion, the mechanical properties of this alloy can be summarized

in table 2.
Table 2. Mechanical properties of the 17-12 SPH steel.
cold creep no or very little time thermally activated high
dependent strain temperature creep
ratchet (ID and 2D) little ratchet (ID and thermally activated rat-
2D) chet (ID and 2D)
little cyclic harde- very significant cy- fairly important cyclic
ning (ID) clic hardening (ID; hardening with time de-
pendence
strong supplementary progressive diminution weak supplementary (2D)
hardening (2D) due of the supplementary hardening due to the
to the phase diffe- 2D hardening phase difference of the
rence or the stresses stresses with time de-
pendence
positive sensitivity negative sensitivity positive sensitivity of
of the stress to the of the stress to the the stress to the strain
strain rate(monotonic strain rate (monotonic rate (monotonic and cy-
and cyclic) and cyclic) clic)
20 < T < 200°C 200 < T < 550°C T > 550°C

MODELIZATION
Without entering into the details of the formulation of this model, its
different components are reviewed together with their associated micro-
structural parameters [3] [7-8]. A synoptic diagram is presented in
Table 3.

Different physical properties appear in the viscoplastic state equation on

which depend the strain rate, namely : the critical velocities of the
Luders bands, the variation of the stacking fault energy with the tempe-
rature and the effective diffusion coefficient. This adimensional equa-
tion is identified over the domain 20-700°C.
Three tensorial variables a, a ,a appear in this kinematic model
which are associated with the internal stresses induced by the interac-
tions at different distances between the mobile dislocations and the sub-
structure. There are thus three interaction distances, respectively short,
medium and long. The amplitude of the progresive strain (2D ratchet) can
be adjusted by acting on the position of the a variable by the interme-
diary of the evasnescent terms (combination of normal [9] and radial [10]
evanescences).
The scalar variables Y and Y+ essentially depend on the accumulated plas-
tic deformation and represent the variations of the density of the free
dislocations and the substructure dislocations with the strain and tempe-
rature. Note that these variables condition the increase of the asymptotic
states of the kinematic variables. The partial memorization of the pre-
strains is realized by the introduction of non-hardening surfaces [11-12]
and reflects the stability, in relation to the strain, of some developed
substructures such as ; twinned zones, subgrain boundaries, tilt boun-
daries, .. . The loss of stability, with respect to time, of these
substructures is described by the presence of the recovery term in the
variables a, Y and Y + .
 97
For the 2D cyclic loadings, the supplementary hardening caused by the
rotation of the stresses is certainly due on the one hand, to the activa-
tion of new secondary gliding systems favorably oriented with respect to
the stress components and, on the other hand, to the interactions between
the different activated systems. The scalar variable Y is thus introdu-
ced, describing the increase in density of dislocations due to the activa-
tion of secondary systems [3].
In the intermediate temperature domain, there exists significant agreement
in attributing the physical origin of a negative loading rate sensitivity
to the dislocation-point defects interactions. For this alloy, the reo-
rientation at short distances has been proposed [7-8] : reorientation in a
FCC crystal of the point defects configurations in the stress field of the
dislocations (Snoek-Schoeck mechanism). A scalar component y( can be
attributed to each interaction (i) which kinetic equation predicts, in
agreement with experience, a first order time hardening, exponentially
evanescent with the strain.
For higher temperature, T > 600°C, the interstitial atoms migrate to long
distances to precipitate in a heterogeneous manner along the grain boun-
dary. A formulation has been proposed.
Figure 1 to 6 compare the predictions of the model with respect to the
experimental results. The agreement is satisfactory and the new notable
possibilities of the model are : the description of the strain rate effect
on the stabilized cycle and the description of the 2D loadings : ratchet
and out of phase experiments.

CONCLUSION
In conclusion, except for the ID ratchetting (which is overestimated by
the present model) the mechanical characteristics of this steel between 20
and 700°C, summarized in table 2, can be described by the incorporation of
the phenomenological modelization of the physical mechanism taking part in
the strain, into a unified viscoplastic model.

REFERENCES
N. Ohno, Y. Takahashi and K. Kowabara, J. Eng. Mat. Techn.. Ill, (1989),
106-114.
S. Murakami, M. Kawai, K. Aoki and Y. Ohmi, J. Eng. Mat. Techn.. 111.
(1989), 32-39.
P. Delobelle and R. Lachat, to appear Rech. Aerosp. (1991).
A. Benallal and D. Marquis, J. Eng. Mat. Techn.. 109. (1987), 326-336.
A.A. Solomon, Rev, of Sci. Inst.. 40, (1969), 1025-1030.
P. Delobelle, J. Nucl. Mat.. 166. (1989), 364-378.
P. Delobelle, in "Constitutive Laws of Plastic Deformation and Fracture".
edited by A.S. Krausz and al., Kluwer academic publishers, (1990), 253-261
P. Delobelle, Rev. Phvs. Appl.. 25, (1990), 977-999.
J.L. Chaboche, Int. J. of Plasticity. 2, n° 2, (1986), 149-188.
H. Burlet and G. Cailletaud, Eng. Compt.. 3, (1986), 143-150.
JL. Chaboche, K. Dang Van and G. Cordier.SMIRT V.L1/13 (1979).
N. Ohno, J. of APPI. Mech.. 49, (1982), 721-727.
98
Table 3. Synoptic diagram of the model

Viscoplastic state equation

- f
I N(Y )
1
1
Viscous Properties N(Y ) = ..

Secondary ki- Primary kinematic variable, a.. Scalar va-

nematic va- a.. - g(a..,a< 1 .>,a< 2) ,..yy T) riable Y*
riables a|J} , describing
allowing trie the asymp-
description totic sta-
of : te of the
- the form of kinematic
the cyclic, variables
loops o... c< n ) ;
- the 2D rat- Y 4 ih( Y ',t:
chet (i ) VP P
- the ID rat-
chet

HCyclic and monotonic hardenings

r-JY = k(Y, Y s a t , I, T^ => Y
Y+ = k + (Y + , Y s a t + , £, T) => Y+

Memory effect of the pre-

strains
Y s a t - ... Ysat

Recovery effect directly due

to time
I

Model Responses : Hardening effect due to the

monotonic loadings (ten- phase difference of the
sile, creep, relaxation, stresses
time effects...) Y_ = . . . => Y
cyclic loadings (cyclic
hardening, memorization
of the prestrains...) Dislocations-point defects
strain rate effects interactions
bi-directional cyclic
loading <f>
2D ratchet
ID ratchet (overestima-)
ted) Effect of the microstructural
instability due to the hetero-
genous precipitation
Yp r = . . . => Y p r
WS1b3

A STUDY OF THE MACROSCOPIC PLASTIC SPIN IN POLYCRYSTALS

E. VAN DER GIESSEN1^ and P. VAN HOUTTE*

^ e l f t University of Technology, P.O. Box 5033, NL-2600 GA DELFT, The Netherlands
*Katholieke Universiteit Leuven, Department MTM, de Croylaan 2, B-3001 HEVERLEE, Belgium

ABSTRACT

This paper addresses a micromechanical study of the macroscopic plastic spin in polycrystalline materi-
als due to texture development. The large strain analyses are carried out using a Taylor-Bishop-Hill the-
ory for plasticity due to crystallograpic slip in cubic polycrystals. Results are presented for planar
stationary deformation processes of initially isotropic aggregates as well as pre-textured materials.

KEYWORDS

Large strain plasticity; crystal plasticity; plastic spin; micromechanics.

INTRODUCTION

Currently, the macroscopic description of the anisotropic behaviour during large strain is one of the most
challenging tasks in the area of constitutive modelling of elastic-plastic materials. In particular this per-
tains to deformation-induced anisotropy in polycrystalline metals due to the progressive development of
texture. An important class of large deformation plasticity theories is founded essentially on the work of
Mandel (1971), in which a clear distinction is made between the continuum and the underlying substruc-
ture. This leads to the concept of the plastic spin which governs the evolution of the orientation of ani-
sotropy. This concept is now recognized to be a key instrument in the description of anisotropy in large
strain plasticity (e.g. Loret, 1983; Dafalias, 1985).

Within a purely phenomenological framework, the constitutive description of the plastic spin has been
studied in some detail over the last years, limiting attention to either kinematic hardening as an extremely
simple prototype of anisotropic hardening or to persistent initial anisotropies (e.g. Loret, 1983; Dafalias,
1985; Van der Giessen, 1989). The various approaches have been critically reviewed from a thermody-
namic and micromechanical point of view in (Van der Giessen, 1990b). Very recently, the first attempts
to incorporating deformation-induced anisotropy due to texture development in polycrystalline materials
into large strain continuum plasticity theories have appeared (Raniecki and Mr<5z, 1989; Van der Giessen,
1990a). The formulation of the constitutive laws related to texture development is a formidable and yet
largely unaccomplished task which is severely hindered by the limited understanding of, amongst others,
the macroscopic plastic spin.

99
100
The origin of the macroscopic plastic spin in polycrystalline materials is well-known to be attributed to
crystallographic slip (e.g. Mandel, 1971,1982; Dafalias and Aifantis, 1990). Several attempts are now
being undertaken to link these microscopic phenomena to macroscopic constitutive descriptions, e.g. by
means of an analytical multiple slip model for two-dimensional texture development and plastic spin
(Van der Giessen and Van Houtte, 1990). These phenomenological considerations are supplemented by
direct micromechanical analyses using polycrystal models. Such models (e.g. Van Houtte, 1989) rigor-
ously account for texture development and indeed have been used extensively in the past to explain the
complex phenomenology of crystallographic texture. In principle, such models therefore provide a rig-
orous description of the associated plastic spin, but this has not yet been effected. It is the purpose of this
paper to present some preliminary results of such a detailed study for cubic polycrystals.

THE MACROSCOPIC PLASTIC SPIN

Phenomenological plasticity

Whatever the form in which the material anisotropy manifests itself to us, its origin lies in the micro-
structure of the material. On the basis of this observation, an important class of phenomenological large
strain plasticity theories have explicitly endowed the continuum with a so-called substructure in the form
of a set of three vector directors (see e.g. Besseling, 1968; Mandel, 1971). The key proposition made in
such theories is that the kinematics of the continuum and that of the substructure are distinct entities. In
addition to the usual decomposition of strain-rate D into elastic and plastic parts De and D^, respective-
ly, this leads to an analogous decomposition of the continuum spin XV:

D = De + Dp, W=We + Wp. (1)

e e
Here, W can be further decomposed as W = W* + GO* in terms of the spin of the substructure W* and
a contribution af resulting from elastic deformations which can usually be neglected in metals. The plas-
tic spin Wp represents the spin of the material relative to the substructure. Via the substructure spin ©*,
the plastic spin is of key importance in the rate constitutive equations for vectorial or tensorial state quan-
tities which describe the anisotropy or, in turn, depend on it. In addition to constitutive equations for the
plastic strain-rate If like in any plasticity theory, constitutive equations must now be supplied also for
the plastic spin Wp (Mandel, 1971).

For polycrystalline metals, the prime source of anisotropy is texture development during large strain
deformation processes. The development of constitutive equations for the macroscopic behavior taking
into account this type of deformation induced anisotropy is one of the main challenges of phenomeno-
logical plasticity theories today. Whatever the precise formulation of the theoretical framework, consti-
tutive equations for the associated plastic spin are a necessary ingredient but have been left virtually
untouched sofar. Here we shall study this from a micromechanical point of view. A first step towards a
study of the plastic spin, is the identification of the substructure that is relevant to the kind of anisotropy
considered. Here we confine attention to crystallographic anisotropy which is due to the gradual rotation
of crystallographic directions towards a common axis; morphological anisotropy will be neglected. For
a single crystal, the crystal lattice is the obvious substructure; but the extension to a polycrystalline
aggregate is not at all trivial. Mandel (1982) has proposed a kinematic definition of the substructure: the
spin of the substructure in a polycrystalline aggregate is defined as the volume average of the spin of the
individual lattice orientations. We shall now proceed to analyse this in detail using the Taylor model.

The Taylor model

The Taylor model provides a description of the plastic deformation of polycrystalline materials on the
basis of the plasticity of single crystals by crystallographic slip on discrete slip systems. Detailed discus-
 101
sions of the basic underlying assumptions of this theory and methods of solution are given in many
review papers (see e.g. Asaro, 1983; Van Houtte, 1988); we shall discuss here only those aspects that are
most relevant for the present study.

First let us consider a single crystallite having n possible slip systems characterized by the unit vectors
ns and bs (s = 1,... n) normal to the slip plane and in the slip direction, respectively. Here we consider
cubic materials, where /i = 12 for the {111}<110> slip systems for FCC and « = 24 for the
{ 1 1 0 } ( 1 1 1 ) + {112}(111> slip systems of BCC. Neglecting elasticity, the imposed deformation rate,
or velocity gradient, L is then decomposed as

L = L* +LP ; or D = Tf and W = W* + Wp , (2)

where generic symbols D and W denote symmetric and skewsymmetric parts, respectively, and where

Lp = Dp+wr= £rA®",
s= 1

is the plastic deformation rate caused by the slip rates fs. Wp is the plastic spin of the crystallite, while
the spin W* of the crystal lattice ensures that the imposed spin W is accomodated. For the solution of
the n slip rates fs from the five equations in (2b) we adopt the Taylor-Bishop-Hill approach discussed
by Van Houtte (1988). Now consider the entire polycrystal consisting of m crystallites and denote quan-
tities associated with the kxh crystallite_by a superscript k. As suggested by Mandel (1982) we define the
average, or macroscopic, plastic spin V? of the polycrystal as

w' = IJTv,wj, v= £ v 4 .
V
(3)
A=1 *=1

where Vk is the weigth factor for crystal k. This definition is in keeping with the principal assumption of
the Taylor theory that the deformation within the polycrystalline aggregate is homogeneous, i.e.
DJ = D , V* = 1, ...m.

All computations to be presented use an aggregate consisting of m = 294 crystallites. The initial orienta-
tions constitute a uniform coverage of Eulerian orientation space so that the aggregate represents an ini-
tially isotropic material (see e.g. Van Houtte and Aemoudt, 1976). The numerical analysis is based on a
time step At such that A eg = e^A t = 0.05/V3 , where e] = ( 2 / 3 ) tr D2.

EFFECT OF CRYSTAL STRUCTURE

In this paper we shall study the behaviour under a class of homogeneous 2D plane strain deformation
processes which are characterized by the following components of the velocity gradient L = D + W
with respect to a global Cartesian coordinate system *•:

D
n = -°n = l- Dn = W u ~ ^ l , ^3 = 0 0 = 1 , 2 , 3 ) . (4)

The deformation process can be envisaged by considering a block of material that is first deformed in
simple shear along the redirection to a shear strain y and then deformed by planar isochoric stretching
("rolling") to a stretch X in the jc2-direction (see insert in Fig. 2). The components in (4) are taken to have
constant values in time and we introduce the parameter K = ( D ^ - Du) / (2D 1 2 ) as a measure of the
amount of rolling relative to the amount of shearing. Pure rolling corresponds to K -» ±°o_while K = 0
corresponds to pure simple shear. For these planar deformations we consider here only the WPX2 compo-
nent of the macroscopic plastic spin according to (3).
102

In Fig. 1 we first consider the macroscopic plastic spin during purely simple shear (K = 0) up to shears
of y = 10. Simple shear is the primary component of deformation during torsion, and the development of
texture during shear has been studied extensively (see e.g. Gil-Sevillano et ai, 1975; Van Houtte and
Aemoudt, 1976; Harren etal.t 1989). It is seen from Fig. 1 that initially, at y = 0 , the plastic spin vanishes,
since the material was taken to be initially isotropic, but the plastic spin increases quickly due to texture
development In the early stages of the process, say y < 1.5, the plastic spin is observed to be virtually
identical for FCC and BCC polycrystals, but for larger shears the behaviour is quite different. For BCC
crystals, the plastic spin approaches the imposed continuum spin at large shears, due to the fact that the
majority of crystals have reached their final crystal orientations in the ideal textures. For FCC polycrys-
tals the orientation of a significant number of crystallites attain stable loops in orientation space and they
never stop rotating. For this reason, the plastic spin does not reach its limiting value Wl2 but severly
oscillates around a value of about 0.1 Wl2.

1.00

0.75

5? 0.50

0.25

0.00
0 2 4 6 8 10

7
Fig. 1. Macroscopic plastic spin, normalized by imposed spin Wl2, during simple shear
for different crystal structures.

In Fig. 2 we present some results for simultaneous simple shear and rolling of cubic materials for various
values of K > 0. Comparing with Fig. 1 it is observed that the plastic spin for K = 0.5 deviates only slight-
ly from the result for pure simple shear, K = 0. For increasing value of K, SO that the contribution of roll-
ing becomes increasingly important, the plastic spin development is strongly accelerated. It should be
noted here that by plotting the results as in Fig. 2 the effect of simultaneous rolling is emphasized; if the
macroscopic plastic spin is plotted against the effective strain ee, the results for K = 2 and 5 are much
closer. Also note that the plastic spin in the FCC polycrystal tends to oscillate violently at larger values
of K and that the difference between FCC and BCC plastic spins decreases with increasing K.

EFFECT OF INITIAL TEXTURE

The cases considered in the previous section relate to an initially isotropic material. In many practical
applications however, some initial texture is usually present due to prior deformations during e.g. pro-
cessing. The influence of initial texture is of particular importance when the principal directions of the
subsequent deformations are significantly different from the major texture orientations induced previ-
ously. These matters have been largely ignored in phenomenological considerations sofar.

Figure 3 shows results for a case where the initially isotropic material is first rolled in either the*! or the
j^-direction to a strain of ee = 1 (i.e., X « 2.4) and is deformed subsequently by purely simple shear. Evi-
dently, texture development occurs during the prior rolling process, but the macroscopic plastic spin
remains negligible, | Wi2/^e\ < 10 ~ 10 - u P ° n subsequent shearing we see from Fig. 3 that the plastic spin
 103

1.00
Y 1
bid —t 0.75
^1* ^1
/ ii

0.50
X
\/
0.25

0.00

Fig. 2. Macroscopic plastic spin during simultaneous simple shear and rolling for
different cubic crystal structures vs. the shear y/A.

does not vanish initially as in the case of an isotropic material (Fig. 1), but attains a considerable fraction
of the imposed spin. It is of particular importance to note the directions of the initial plastic spin. In the
case of material that has been pre-rolled in the ^-direction, the initial plastic spinning is in the same
direction as the imposed spin, although the associated initial texture deviates considerably from the ideal
shear texture. The opposite effect is observed for the case where rolling has occurred in the j^-direction.
These phenomena rely on the fact that the crystallites possess multiple slip systems; in fact, the slip sys-
tems that are active during simple shear are predominantly different from the ones that were active dur-
ing the prior rolling process. It is also seen from Fig. 3 that the memory of the initial rolling texture has
essentially vanished after shears of about 2.5, although it appears that for very large shears the plastic
spin is slightly larger than for the initial isotropic material (cf. Fig. 1).

<_2

-0.5
r ^ ^ rolled in x, direction
BCC

_L_
-1.0
0 1 2 3 4 5
7

Fig. 3. Macroscopic plastic spin during simple shear of cubic polycrystals which have
been pre-rolled to zg = 1.
104
CONCLUSION

In this paper we have only considered the effect on plastic spin of crystallographic texture according to
the Taylor theory. It is expected that Taylor's assumption of homogeneous plastic strain within the poly-
crystal may have a dominant influence on the phenomena obtained here. Some insight in this effect may
be obtained with the aid of a self-consistent analysis (e.g. Molinari etal, 1987). Other potentially impor-
tant effects, which have been omitted here, are twinning in FCC crystallites, presence of of different crit-
ical resolved shear stresses on different slip systems, latent hardening and strain-rate sensitivity. These
aspects are currently under investigation.

Acknowledgement The work of EvdG was made possible by a fellowship of the Royal Netherlands
Academy of Arts and Sciences.

REFERENCES

Asaro, R.J. (1983). Micromechanics of crystals and polycrystals. Adv. Appl. Mech., 23,1-115.
Besseling, J.F. (1968). A thermodynamic approach to rheology. In: Proc. IUTAM Symp. on Irreversible
Aspects of Continuum Mechanics, Vienna 1966 (H. Parkus, L.I. Sedov, eds.), pp. 16-53. Springer
Verlag, Wien.
Dafalias, Y.F. (1985). The Plastic Spin. / . Appl. Mech., £2,865-871.
Dafalias, Y.F. and E.C. Aifantis (1990). On the microscopic origin of the plastic spin. Acta Mech., 82,
31-48.
Gil-Sevillano, J., P. Van Houtte and E. Aemoudt (1975). Deutung der Schertexturen mit Hilfe der Taylor-
Analyse, Z. Metallkd., 66.367-373.
Harren, S., T.C. Lowe, R.J. Asaro and A. Needleman (1989). Analysis of large-strain shear in rate-
dependent face-centred cubic polycrystals: correlation of micro- and macromechanics. Phil. Trans.
R. Soc. Lond., A 328,443-500.
Loret, B. (1983). On the effects of plastic rotation in the finite deformation of anisotropic elastoplastic
materials. Mech. Mater., 2,287-304.
Mandel, J. (1971). Plasticity Classique et Viscoplasticite\ CISM Lecture Notes No. 97, Springer-Verlag,
Udine.
Mandel, J. (1982). Definition d'un repere privilege" pour retude des transformations an&astiques du
polycrystal. / . Mic. Thio. Appl, \, 7-23.
Molinari, A., G.R. Canova and S. Ahzi (1987). A self consistent approach of the large deformation
polycrystal viscoplasticity. Acta Metall., 35.2983-2994.
Raniecki, B. and Z. Mr6z (1989). On the strain-induced anisotropy and texture in rigid-plastic solids. In:
Inelastic Solids and Structures (M. Kleiber, A. KOnig, eds.). Pineridge Press, Swansea (in print).
Van der Giessen, E. (1989). Continuum models of large deformation plasticity-Part II: A kinematic
hardening model and the concept of a plastically induced orientational structure. Eur. J. Mech. Al
Solids,%,%9-\W.
Van der Giessen, E. (1990a). A model of anisotropically hardening materials based upon the concept of
a plastically induced orientational structure. In: Yielding, Damage and Failure of Anisotropic Solids
(J.P. Boehler, ed.), pp. 187-198. Mech. Engrg. Publ., London.
Van der Giessen, E. (1990b). Micromechanical and thermodynamic aspects of the plastic spia Int. J.
Plasticity (to appear).
Van der Giessen, E. and P. Van Houtte (1990). An analytical 2D multiple slip model for continuum
texture development and plastic spin, (submitted for publication)
Van Houtte, P. (1988). A Comprehensive Mathematical Formulation of an Extended Taylor-Bishop-Hill
Model Featuring Relaxed Constraints, the Renouard-Wintenberger Theory and a Strain Rate
Sensitivity Model. Textures and Microstructures, 8. & 9,313-350.
Van Houtte, P. and E. Aemoudt (1976). Considerations on the crystal and the strain symmetry in the
calculation of deformation textures with the Taylor theory. Mater. Sci. Engng., 23,11-22.
WS1b4

NON-COAXIAL CONSTITUTIVE EQUATION IN FINITE DEFORMATION

(). WATANABE

Institute of Engineering Mechanics, University of Tsukuba

Tsukuba, Ibaraki 305, JAPAN

ABSTRACT

Issues related to constitutive modeling in finite deformation are discussed. In the present study,
hypoelastic models in rate form with anti-symmetric spin tensors are shown to be converted to the
linear stress-strain relation using corotated quantities, and clarified are the utilized stresses, strains
and rotations in their constitutive models. Also discussed are non-coaxiality in constitutive equation
based on the material spin model by introducing non-coaxial spin tensors progressing with
deformations. The simple shear problem is taken as an example to demonstrate the effects of non-
coaxiality.

KEYWORDS

Constitutive equation; Hypoelasticity; Finite deformation theory; Non-coaxiality; Simple shear

FUNDAMENTAL RELATION

The deformation gradient tensor F can be written by the polar decomposition theorem:
F=R-U=V*R, (1)
where V and U are symmetric left and right stretch tensors, respectively, and R the orthogonal
rotation tensor. The tensors U and V possess the common eigenvalues and diagonalized as follows
V=R E -A-R£ U=RL-A-R£ (2)

where A is diagonal tensor, and R E and R L are the orthogonal tensors with unit eigenvectors, and
the notation ( ) T indicates transpose. The velocity v and its gradient L are related to
I^F-F-^vV, (3)

where V is the gradient operator, and the notations ( *) and () _ 1 indicate material time derivative
and inverse, respectively. By decomposing L to the symmetric and anti-symmetric parts, we find
the stretching tensor I) and the spin tensor W defined by
I>=L S =^(L + L T ), W=La=^(L-L-1),
where the notations ( ) s and ( ) a indicate the symmetric and anti-symmetric part in the parenthesis,
respectively. The continuum spin W expresses the angular velocity of a unit vector attached to the
105
106
continuum. The spin tensor of stretch tensors U and V (Hill, 1978)
W^RE-RI W L = R L < , (5)

express the angular velocities of the eigenvectors. Substituting Eq.( 1) into Eq.(4) yields the tensors
D and W as a function of U and R by
T
D=R*(lMJ V R , W=WR+R*(U*U VR7, WR=R*RT. (6)

The tensor WR is called the material spin expressing the angular velocity of a unit vector measured
from the intermediate unrotated configuration after the right stretch U. The relations among rotation
tensors and spin tensors are given by (Chu, 1985)
RE=R-RL, WE=WR+R-WL-RT. (7)

Analogous definition may be adopted for the spin (U*U~ )a related to the deformation U may be
expressed by rotation rate (Storen-Rice, 1975) as
As-Rl-ttMJ- 1 ).. (8)
From Eqs.(6) and (7), we have
W=R*R T +R*(R S *RI)*R T =(R*RS)**(R-RS) T . (9)
The continuum spin W consists of angular velocity due to the successive rotations R s and R.

COAXIAL CONSTITUTIVE EQUATION

Constitutive Equation with Spin Tensor

The standard linearly hypoelastic constitutive equation using Jaumann derivative is expressed by
using the 'continuum' spin W as follows:
Tj=2u0I)+A0(trl))I, with tj-T-W«T+T«W. (10)

The tensor T is Kirchhoff stress, and Uo and Xo are material constants of Lame, and I is the unit
tensor of the second order, and (tr I)) means inner product of I) and I. The constitutive equation
including plastic deformation is usually obtained by replacing the stretching tensor I) by the elastic
part, and plastic component may be calculated by using the same approach of flow theory in small
strain range. In this paper, we restrict our attentions to constitutive equation for elasticity. Eq.( 10)
is a special case of hypoelasticity (Truesdell and Noll, 1965) by excluding the concept of frame of
reference, and the response can be described by quantities in the present configuration, but
oscillatory stresses in simple shear problems are reported. Another rate-type constitutive equation
for elastic response is proposed (Green & Naghdi, 1965 and Green & Mclnnis, 1967) by using the
'material' spin as follows:
TG=2u0I)+A0(trl))I, with TO-T-WR-T+T-WR. (11)
This constitutive equation is based on an intermediate unrotated configuration uniquely defined in
terms of the rotating R entering the polar decomposition of the deformation gradient F, and causes
no-oscillatory stresses in simple shear problem. The other alternate rate-type constitutive equation
is expressed by using Eulerian stretch spin WE as follows:
TH=2u 0 im 0 (trD)I, with TH-t-WtfT+T-WB. (12)
These three equations are defined in rate-form for describing elastic response. Taking the trace of
Eqs.(10),(ll) and (12) and considering the nature of inner product of tensors, we have the same
constitutive equation for mean component, regardless of the utilized spin tensors:
tr f o=tr Tj=tr f H=tr t=3K0(tr I)), (13)

where K0 is bulk modulus defined by K O =A 0 +2/3U 0 . By subtracting Eqs.(10),(ll) and (12) from
Eq.( 13), then we obtain the following deviatoric constitutive relations:
fG=2u 0 D\ with f G = t - W R - T + T - W R , (14a)
where the notation () indicates deviatoric component defined by

Constitutive Equation with Rotation Tensor

By introducing the rotation tensors, the stresses and strains are defined as follows

The material time derivative of these rotated stress tensors are related to the objective stress rates as

Equation (14) can be regarded to the rate-form of the following linear stress-strain relation.

If we retain the stretching tensor I)' in the equation, we have from Eqs.(14) and (17):

These strains in Eq.(18) are all path-dependent quantities, and does not satisfy the requirement of
the strain (Hill, 1968). If we introduce the following strains derived from orthogonal
transformation of R, (R*RS) and RE, respectively:

then we have the stress T' as a function of the newly defined strains in Eq.(20):

Substituting Eqs.(20) and (16) in Eq.(18), and taking material time derivative yields

Equation (22) indicates change rate of stress and strain from the corotated coordinate systems with
rotation of R, (R - R s ) and RE, respectively, and can be converted using spin tensors as follows:

The stretching tensor I) in each constitutive equation can be calculated as follows:

Some Criteria

The primary criteria we shall demand these constitutive modeling to satisfy are: (1) The model
108
should be valid for hyperelasticity requirement, which means the utilized stress and strain are
conjugate with respect to internal work rate (Storen & Rice 1967, Atluri 1986); (2) The model
should obey the so-called Prager's criteria, which implies that the second stress invariant remain
constant when the objective stress rate vanishes. Rotated stresses and strains in their modeling are
easily shown to be conjugate with respect to internal work rate.
TR:ER=Ts:Es=TE:E^r:!)'. (25)
If Eq.(21) holds, stress T' and strain measures in Eq.(20) are coaxial resulting in:
T:e R =e R :T', T:e s =e s :T, T':e^e E :T'. (26)
And also we can show that stress T' and strain measures in Eq,(20) are also conjugate with respect
to internal work:
T^e^T^es^^e^T-D'. (27)
Each of constitutive equations can be easily proved to satisfy Prager's requirements for stress
invariance, since the objective rates employ the an ti-symmetric spin tensors. There exists no
difference for the above mentioned two criteria among these three constitutive models.
Let us compare constitutive equation of simple material (Truesdell and Noll 1965) derived in the
following general form:
t

RT(t)-T(t)-R(t)= 6 (U(f)),
f = -~ (28)
where t and V are the present and past time, respectively. While the present rotation generally
affects the stress, past rotation are without influence, and the total history of the right stretch tensor
U up to the present time affects the stress in simple material. Each of constitutive equation (14) or
(19) can be reduced to contain the rotation R in the following:

R T (t)'T(t)'R(t)=l ( I K O ' U - ' ^ d f for spin W R ,

(29a)

R T (t)-T(t)-R(t)=RL (t)-| I R[(f)-(U(0-U-'(t')),-R L (f)df|-R[(t) for spin W,

(29b)

R T (t)-T(t)-R(t)=R s (tM I RS(f)'(D(0'U- , (f)) I »Rs(t , )df]'R|(t) for spin WE.

(29c)

+
The rotation R L and R s in Eqs.(29b,c) are calculated by using Eqs.(2) and (8) as follows:

RL(t)=RL(U(t)), R s (t)= <D(t , )'U- I (t , )).'Rs(t , )df.

(30)
It may easily found that rotation R L only depends on the current configuration, and rotation R s is
derived from the recursive formula and path-dependent Constitutive model (29a) based on material
spin WR is the most simple form, while effects of past loading history are affected by rotation R L
and R s in models (29b,c).

NON-COAXIAL CONSTITUTIVE EQUATION

Theoretical Development

Let us discuss constitutive equation based on the material spin W R where stress T R and strain E R
are related linearly and can be regarded as coaxial relation. By introducing non-coaxial rotation Q,
which is assumed to progress with deformation, non-coaxial constitutive equation can be obtained
by the analogous manner of Eq.(19) as
 109
Q-(Q T -TR'-Q)--Q T =2 M OER. (31)

Eq.(31) can be modified to the following rate equation using spin tensor:
TR-WQ-TR+TR-WQ=2U0ER with W Q - Q - Q T . (32)

However, if w e introduce the following stress and strain:

VQT-TR-Q, EQ-QT-ER-Q, (33)

then, substituting Eq.(33) in Eq.(31) yields the following coaxial relation:

TQ=2U0EQ. ( 3 4 )

The non-coaxial anti-symmetric rotation spin W Q is proposed (Dafalias, 1985, Zbib & Aifantis,
1988) as follows:
W 0 =k 1 (T R -ER)a+k 2 (T R 2 -E R ) a + • • , (35)

where k p k ? ... are material constants. W e only assume the first term o f Eq.(35),
W < ^ M V E R ) a = ^-(T R .E R ) a ,
2
Mo 2u0 (36)
where k is material constant. Substituting Eq.(36) in Eq.(32) yields the non-coaxial relation.
I^MO^+^TR-ER^TR-ER-TR+ER-TR).
4
Mo (37)
Orthogonal transformation o f Eq.(37) and including the mean component relation (13) yields
TG=2M0I>+Xo(trD)I+-lc-(T2-I)-2rM>-T+I)-T2).
4
Mo (38)
Replacing T R by ( 2 u 0 e R ) in Eq.(38) yields the following equation:
tG=2Mol> + Ao(trD)I+kMo(eR-D-2eR-D-e R +D-e R ). (39)

The inverse relation for constitutive equation (18) is given by

2MO (40)
Employing the similar manner used in Eq.(31), w e have the non-coaxial constitutive equation,

P-(I**VP)--P l = o 1 - 1 *
2Mo (41)
where P is non-coaxial rotation. Eq.(41) is reduced to the following relation:
E R - W P * E R + E R * W P = J - T R with W p - I M * .
2Mo (42)
Non-coaxial spin tensor W p may be assumed to be the following form:
Wp=-h-(fR.ER)a= -|L(tR-ER)a,
2Mo 4*O (43)
where h is material constant. Substituting Eq.(43) into Eq.(42) yields
E R = ^ T R V h - ( E R - f R-2E R -f R - E R + T R - E R ) .

Considering Eq.(13), the constitutive model referred to the present configuration is derived by
,)=
97rtG • ^(trtG)I+^-(eR-tG-2eR-tG.eR+TG-eR).
2Uo OK0)Ll0 4UD (45)
Simple Shear Problem

Zbib & Aifantis (1988) analyze the simple shear problem using non-coaxial constitutive equation
with the continuum spin W, and conclude that the stress-strain response by various other spins
YVR or W s can be predicted with proper choice of non-coaxial parameter when the shear strain is
less than 2. In the present study, based on the non-coaxial constitutive equation (38) with the
material spin VVR, the solutions to the shear stress and axial stress versus shear strain are illustrated
in Figs.l and 2. The discrepancy between non-coaxial spin model and the other spin models
become dominant, when shear strain e/2 is greater than 2.
110

Fig.l Shear stress vs. shear strain response for hypoelasticity

based on various spin

Shear strain e/2

Fig.2 Axial stress vs. shear strain response for hypoelasticity

based on various spin

REFERENCES
Atluri, S. N. (1986). An endochronic approach and other topics in small and finite deformation
computational elasto-plasticity,£ww/;e-(/S Symposium on Finite Element Methods for
Nonlinear Problems, (ed. Bergan et al.), 143, Springer.
Chu, E. (1985). Aspects of strain measures and strain rates. Acta Mechanica, 59, 103-112.
Dafalias, Y. F. (1985). A missing link in the macroscopic constitutive formulation of large plastic
deformations. Plasticity Today, (ed. Sawczuk, A., Bianchi, G.), 135-151, Elsevier.
Hill, R. (1968). On constitutive inequalities for simple materials-1.7. Mech. Phys. Solids, 16, 229.
Hill, R. (1978). Aspects of invariance in solid mechanics. Advances Appl. Mech., 18, 1-76.
Green, A. E. and B. C. Mclnnis (1967). Generalized hypo-elasticity. Proc. Roy. Soc. Edinburgh,
A57, Part 111, 220-230.
Green, A. E. and P. M. Naghdi (1965). A general theory of an elastic-plastic continuum. Arch.
Rational Mech. Anal, 18, 251-281.
Storen, S. and J. R. Rice (1975). Localized necking in thin sheets. J. Mech. Phys. Solids, 23,
421-441.
Truesdell, C. and W. Noll (1965). The non-linear field theories of mechanics. Handbuch der
Physik, (ed. S. Flugge), 111/3. Springer.
Watanabe, O. (1988). The stress-strain relation of elasticity under finite deformations. Trans.
JSME. 54-497 A. 100-110.
Watanabe, O. (1988). Finite deformation theory of elastoplasticity, Trans. JSME, 54-501 A. 992-
1001.
Zbib, H. M., and E. C. Aifantis (1988). On the concept of relative and plastic spins and its
implications to large deformation theories, part I: Hypoelasticity and vertex-type plasticity.
Acta Mechanica, 21,15-33.
WS1d

MICROSTRUCTURAL ASPECTS OF CRACK EXTENSION

IN A CRYSTALLINE MATERIAL
—A MOLECULAR DYNAMIC STUDY—

H. KITAGAWA and A. NAKATANI

Department of Mechanical Engineering, Osaka University,
2-1 Yamada-oka Suita, Osaka, 565, Japan

ABSTRACT
The molecular dynamic (MD) simulation is applied to analysis of the crack opening and propaga-
tion in a crystalline material. Special attention is placed on investigation of the process how the
local phenomena on atomic scale at the crack tip propagates, leading to extension of the crack.
After investigation of the basic features which the MD simulation of the crystalline material pre-
dicts concerning dynamics of the crystal lattice defects such as the dislocation, transformation
or twinning, the mode I type crack opening process is analyzed for bcc and fee crystals under
various lattice orientations with different potentials.
KEYWORDS
Computational Mechanics; Molecular Dynamics; Crack Opening; Twinning; Dislocation
Emission; Cleavage.
INTRODUCTION
Most of substantial properties of crystalline material are structure-sensitive, that is, they have
strong sensitivity to inhomogeneity of the microstructure. It means that structural analysis is
necessitated for evaluation of such material properties. There seems to be essential difficulty to
solve the microstructural problem by means of the continuum approach, because it is impos-
sible to represent full details of the dynamics of micro-inhomogeneity in the phenomenological
constitutive equations. One of the most reasonable procedures is mechanical analysis of the
hierarchically lower (finer) structure, that is, computer simulation of dynamics of the elemen-
tal process which is ground for structure-sensitivity. For this purpose, the molecular dynamic
(MD) simulation is the most elemental and it has possibility to treat the dynamics of the crystal
defects, such as vacancy, dislocation and twinning. In this paper, MD simulation is applied to
analyze the local process at the crack-tip and effects of the crystal structure and the lattice
orientation on the local process concerning the crack opening and advance are investigated.
MODEL AND METHOD
Model
Mode I type opening of crack in a single crystal block is investigated by numerical simulation
based on the molecular dynamics. The crack of 2a in length is supposed to be placed at the
center of a plane strain block of 2w in width and 4w in length, subjected to uniaxial tension
with constant edge speed, as shown in Fig. 1(a). The crack-tip region is modeled by a collection
of atoms which is surrounded by an anisotropic elastic medium.

Ill
112

(a) Specimen (c) Near tip mesh (d) Initial atomic configuration

Fig. 1. Mode I type opening of crack in a single crystal block under plane
strain.

Boundary Condition of MD Model

The velocity of the atoms which are touched to the surrounding medium is prescribed at each
instant of MD-analysis. The velocity is estimated formerly by the infinitesimal elastic analysis
of the same problem as shown in Fig. 1(a), using FEM-Model shown in Fig. 1(b). Figure 1(c)
depicts the near tip mesh which corresponds to the shaded region of Fig. 1(b). The surrounding
region of the crack tip is model by a singular element. The elastic medium is assumed to have
anisotropic properties corresponding to the single crystal with the initial atomic configuration
of the MD model.
MD Analysis
Equation of Motion of Atomic Collection. The constant temperature molecular dynamic
model proposed by Nose (1984) is used, in which a virtual system acted as a heat bath of one
degree of freedom contacts the classical physical system constituted by iV^-atoms with no internal
structure. The motion of the atoms is governed by

d2
„ «. _ v - 9 $ fm d * m
m
'l^--F'--^-Cm,lT> (1)

where q{ and rrii(i = 1 , 2 , . . . , JV") are coordinates and mass of the atom i, respectively. Fi is
force acting on the atom i, which is estimated from the potential energy $ of the i^-atomic
system and the properties of the heat bath. C, 5 are the characteristic variables which describe
the state of heat bath and Q is constant corresponding to its mass. T and k are the prescribed
temperature and Bolzmann constant, respectively.
 113
MD Computation.
The initial positions of the atoms are guessed from the displacement field estimated by the
infinitesimal strain analysis of the centrally-cracked block using FEM. The initially prescribed
displacement at the edge of the block is Aw which corresponds to the average strain eo = Aw/2w.
The initial velocity of each atom is given, being assumed to obey the Maxwell's distribution of
velocity at the prescribed temperature T. The Eqs.(l) and (2) are solved numerically from
these initial condition to give a time series data of the coordinates and velocity of the atom.
A pre-relaxation calculation is performed before time integration during an appropriate time
interval t*, in which the atoms locating at the boundary are held to be constant place.
Interatomic Potential
Two-Bodv Potential. A simple representation of the interatomic interaction is obtained
by introduction of the two-body potential. In this case, the potential energy function $ in the
right-hand side of Eq.(l) is described by sum of pair potentials in spherical form which represents
the interaction of two atoms, such that,

* = £££*(*;), (3)
in which qi3 is the distance between the atoms i and j .

iV-Bodv Potential. JV-body potential proposed by Finnis and Sinclair (1984), abbrev. FS
potential, is one of the best representation considering the multi-body interaction and it is
regarded to be a first approximate solution of the Schlodinger equation. Moreover, it has simple
mathematical structure and does not require substantial change of the algorithm of solution
based on the pair potential. If the FS potential is used, the total potential energy in Eq.(l) is
described by sum of pair term $ p and iV-body term $ # , such that,

$ = <I>P + $ W , (4)

respectively,

*p = \ET, **(*>)> (5)

N N
*N = - £ f(pi), Pi = J2 fa*)' (6)
•=1 j=l

We choose f(p) = y/p. The function <f>* and p are determined so as to fit the experimental data
concerning, for example, lattice constants, elastic constants, cohesive energy, vacancy formation
energy, and so on.
Bcc Crystal Model
The dependence of the crack opening and propagation behaviors on the lattice orientation of the
bcc crystal is studied using Johnson potential. The lattice orientations and conditions analyzed
are shown in Figs. 2(a)-(d) and Tables 1. As shown in Fig. 1(d), two atomic layers are set in
z-direction and periodic boundary condition are applied. Though interaction between the layers
is considered, the motion of atoms are restricted in zy-plane in order to be satisfied with the
plane strain condition. Time is normalized such that to = Roy/m/e(= 3.9685012 x 10~ 14 (s)),
where Ro ( = 2.6166387 x 10" 10 (m)) and e (= 4.0317194 x 10~ 20 (J)) are the interatomic distance
and potential energy, respectively, at the stationary points of Johnson potential, and m(=
9.27376 xl0" 2 6 (kg)) is the mass of Fe-atom. In comparison purpose, analysis using FS potential
is performed for the case of Ori. 2 in Fig. 2., in which the initial strain eo = 1.04 x 10~ 3 , the
relaxation time t* = 100 to and the strain rate eto = 4.17 x 1 0 - 6 .
114

Fig. 2. Lattice orientation. The Miller indies in parentheses and brankets

denote the cleavage plane on crack and the direction along its tip,
respectively

Table 1. Condition in Analysis for bec crystal

Case Orientation T(K) N r*/*o eo e x t0 r/t0
Case 1 Ori .1 300 4640 29.62 1.04 x 10~ 3 4.48 x 10" b 10
Case 2 Ori .1 800 4640 30.65 1.04 x 10"3 4.17 x 10" 6 10
Case 3 Ori .2 300 4614 24.84 1.04 x 10"3 8.33 x 10"7 100
Case 4 Ori .3 300 4645 29.62 1.04 x 10" 3 4.17 x 10"6 10
Case 5 Ori .4 300 4614 24.84 1.04 x 10-3 4.17 x 10-6 100

Fee Crystal Model

In plane strain state, any deformation of the fee crystal which is symmetric with respect to xy-
plane requires that at least two slip systems are activated simultaneously. Then, it is hard for
the crystal to glide, the atom of which has no degree of freedom in ^-direction. Locally relaxed
plane strain model is introduced, where eight layers of atom with three degree of freedom are set
in z-direction and periodic boundary condition is applied on the upper- and lowermost layers.
The case of the lattice orientation shown in Fig. 2(b) is analyzed, using the TV-body FS type
potential which Ackland et a/.(1987) proposed for copper. Cu atoms (N = 5080) whose mass
is m = 1.05522 x 10" 25 (kg) are placed in the area of r* = 12a0 (a0 = 3.615 x 10" 1 0 (m), the
lattice constant of Cu) in radius, and MD analysis is carried out under the condition to =
6.816732 x 10" 14 (s), e 0 = 1.04 x 10" 3 , t* = 100t0, et0 = 6.816732 x 10" 6 .

RESULTS
Crack Evolution in Bee Crystal
Dependence of Lattice Direction. Typical configurations of the atoms around the crack-tip
evolving in bee crystal are shown in Fig. 3. In Case 1, the crack opens with tip of wage-like
shape and advances straight, trailing transformation zones expanding in both sides vertical to
the cleavage-like cracked plane. If temperature is high, as seen in Case 2, vacancies appear
just ahead of the crack. In Case 3, the edge dislocations issue from the tip in [ i l l ] - and [ I n -
directions, and the crack open with little advance. Thus, blunting of crack is recognized. In
contrast to Case 1, the transformation zones are spreading firstly in the directions inclined by
±30° from the crack plane in Case 4, and after the crack branches in [110]- and [110]-directions,
one of them grows. Then, the shape of the transformation zone changes into subdivided slip and
twinning areas bounded along the {110}-planes. Such a process in the crack-tip zone has been
reported by Gehlen et al. (1972), Gehlen (1973) and deCelis et al (1983). In Case 5, brittle
advance of the crack appears, involving the twinning deformation along (121)- and (121) planes.

Influence of Potential Function in Blunting Crack. Atomic configurations at t = 300*o and

600tfo obtained by Johnson and FS potentials are shown in Fig. 4. Dislocation emission from
the crack tip is observed in both cases, in contrast to Mullins's comment(1984) that Johnson
potential is inadequate for plastic blunting analysis resulting from dislocation emission. This
results shows that if the model includes sufficient number of atoms, simple Johnson potential is
feasible for simulation analysis of ductile behavior like plasticity. Figure 5 shows the trajectories
of atomic motion from t = 500*o to 700*0- Angular sector regions emitting from the crack-tip
are recognized and motion of atoms are nearly uniform in each sector. The sector boundaries
 115

Fig. 3. Typical configurations of the atoms around the crack-tip evolving

in bcc crystal.

(b) Result using FS potential (b)Result using FS potential

Fig. 4. Atomic configurations of bcc crystal Fig. 5. Atomic trajectories bet-
for the case of Ori. 2 in Fig. 2. ween 500*o and 7001 0
with different potentials. every 20 to steps.
116
are consist of slip or twinning planes. This result seems to give a microstructural ground for
the reasoning of Rice et a/.(1990) on singularity of the crack-tip deformation field based on
asymptotic analysis and its FEM simulation.
Local Process in Fee Crystal
Sequential changes of atomic configurations are shown in Fig. 6. The atoms belonging to the
even-numbered layers in the initial configuration are shaded. In this lattice orientation, three
sustained slips in the forward(A), backward(B) and parallel(C) directions to the crack surface are
principally possible under plane strain condition and all these are consequence of simultaneous
activation of plural slip systems which have components of z-directional displacement being
cancelled totally. The simulation result shows that dislocation emission occurs in B-slip firstly
and then in A-slip involving atomic motion in ^-direction and narrow zones containing crystal
defects appear emitting from the crack-tip. But C-slip is not activated in contrast to reasoning
by Rice et al. (1990). Main reason to this contradiction is that the crack does not act as a
dislocation source to C-slip.

(a)* = 300*o (b)*=400l 0 (c) I = 50010

Fig. 6. Atomic configurations of fee crystal.

CONCLUDING REMARKS
Molecular dynamic simulation has been applied to investigation of local process in near tip field
of the crack with mode I type opening under plane strain condition. Dependence of crystal
structure and lattice orientation on crack evolution have been discussed, remarking influence of
representation of the interatomic potential. Successful simulation has been carried out for plane
strain slip and twining deformation of fee crystal by means of introduction of local relaxation on
atom movement in ^-direction. It should be important to have presented that MD simulation
gives reasonable predictions of local elemental process which is observed as plastic behavior in
macroscopic level, corresponding well with results obtained by, for example, a crystal slip theory.
REFERENCES
Ackland, G.J., G. Tichy, V. Vitek and M.W. Finnis (1987). Simple AT-body potentials for the noble metals
and nickel. Phil. Mag. 4,56., 735-756.
deCelis, B., A.S. Argon and S. Yip (1983). Molecular dynamics simulation of crack tip processes in alpha-
iron and copper. J. Appl. Phys., 54, 4864-4878.
Finnis, M.W. and J.E. Sinclair (1984). A simple empirical JV-body potential for transition metals. Phil.
Mag. A, 50, 45-55.
Gehlen, P.C., G.T. Hahn and M.F. Kanninen (1972). Crack extension by bond rupture in a model of bec
iron. Scripta Metall., 6_, 1087-1090.
Gehlen, P.C. (1973). Crack extension in a model of a-iron. Scripta Metall., 7, 1115-1118.
Johnson, R.A. (1964). Interstitials and vacancies in a iron. Phys. Rev. A., 134, 1329-1336.
Kohlhoff, S. and S. Schmauder (1989). A new method for coupled elastic-atomistic modeling. In.Atomistic
simulation of Materials (V. Vitek and D.J. Srolovitz, ed.) , pp.411-418. Plenum Press, New York.
Mullins, M. (1984). Computer simulation of fracture using long range pair potentials. Acta Metall., 32.
381-388.
Nose, S. (1984). A unified formulation of the constant temperature molecular dynamics methods. J. Chem.
Phys., 81, 511-519.
Rice, J.R., D.E. Hawk and R.J. Asaro (1990). Crack tip field in ductile crystals. Int. J. Frac, 42, 301-321.
WS1C2

SIMULATED FINITE ELASTIC PLASTIC BEHAVIOUR

OF FCC SINGLE CRYSTALS WITH A SPECIAL REGARD TO
THE DENSITY EVOLUTIONS OF THE VARIOUS DISLOCATIONS FAMILIES

P.Franciosi, M.Benblidia
Laboratoire PMTM CNRS, Univ. Paris Nord, 93430 Villetaneuse,
France

ABSTRACT

A numerical model based on previous extensive experimental and theoretical analyses of single
crystal plasticity has been developed in order to investigate, in addition to the usual
phenomenological and crystallographic parameters, the evolution with strain for various
loading conditions, of the dislocation microstructure and of its statistical organisation on
the various crystallographic systems of the considered - here FCC - lattice.

Several loading simulations of differently oriented single crystals are here compared in
terms of the relative effects of the main physical parameters accounted for (dislocation free
path lentgh or interaction product hardening effect for example). A special attention is paid
to the correlations between the flow and hardening features and the characteristics of the
dislocation density anlsotropy evolution with the plastic strain, an original representation
of which is presented.

KEYWORDS

Crystal plasticity, dislocation microstructures, numerical simulations

INTRODUCTION

From extended experimental and theoretical studies of low temperature single crystal
plasticity, a numerical simulation code has been developed, integrating the microstructural
features of the crystalline plasticity at the dislocation density scale. The bases of this
code have already been presented in several papers for both the microstructural (Franciosi,
1985, 1987) and the mechanical (Franciosi and Zaoui, 1989, 1991) parts. The main ones can be
summarized as follows:

- the single crystal hardening law expresses the critical shear stress .rate t 8 on any g slip
system in terms of the various dislocation family density variations 0 , such that:

* 8 - (Mb)2( E A g k 0 k + a Z I A g j ( h , k ) p h ^ k ) / 2 t 8 (1)
k-1 h-lk-1

with P k « P k + P* - P (* k/A k) qz k + t k /bD, z k «* k /A k (2)

K
m max c c
In (1), I A. | is a dislocation interaction coefficient matrix, the anlsotropy of which is
governed by a single A parameter depending on the material stacking fault energy, & is the
current mobile dislocation segment length, and A the critical length at which the macroslip
Y can become non zero. The power law in (2) represents the current active fraction of the

117
118
dislocation segment length distribution on the k system.

- the microslip associated to the dislocation multiplication p prior to the macroscopic slip
threshold on the g system is neglected but not the hardenin g % h e n $8?H),p8«0 and Y 8 - 0 ) . The
steady state is reached on g when *8-fc8 so that p 8 «0 and p 8 »& 8 »t 8 /bD, 't.he main free path D of
the dislocations being assumed cpnSjtant. The second term in (1) represent the dislocation
{ n f o f n / i t -n
interaction ^nnrn>tii/<t-Aana 1 t-1 ap'
c densities
products a ftJ ' nonnn > a o a a ir4 1wglissile,
«necessarily
ma/- t*11 aa4 1a the
t-Vi r*nn
f- r-1Kn "t 4 nn weight
ocontribution O ^ oh "
M fof nf

which being ajusted with the a scalar

- the code is expressed in a finite elastic plasticity formalism under the assumption of
uniform stress, strain and associated rate fields. Mixed and regular loading conditions can
be locally prescribed so that for any (i,j) pair of indices either the (nominal) stress rate
component s.. or the (total) velocity gradient component L ^ is prescribed, leading to a set
of 9 constitutive equations of the form: jl

Wik -^V8 (3)

where, for plastic straining only by slip, |Q| is the current elastic plastic moduli tensor
and y t n e slip rate on the active g system.

- the flow criterion is assumed of the generalized Schmid law form, so that all the slip
systems of the structure obey to:

T* < T 5 = T8, T8 < T8 (4)

with strict equalities between the critical (CRSS) and the applied (ARSS) resolved shear
stress rates for only the m active ones. . ,.
- the relation between (2) and (A) assumes 2 « T /T

ANALYSIS OF THE CODE PREDICTIONS

The Influence of the microstructural main parameters

The main microstructural parameters of (1) and (2) here discussed are: the anisotropy A of
the IAI dislocation interaction coefficient matrix; the weigth a of the interaction product
contribution to hardening; the main free path D of the dislocation motion; the sharpness q of
the dislocation segment length distribution on each g system.

The respective influence of these parameters are shown, for values sets reported in Table 1,
on the figure 1, a, b, c and d in terms of stress strain curves and, on the figure 2 and 3 a,
b, c and d in terms of total primary and total interaction products dislocations

N N N
total k total V, U
• I Pk P Z Ephp (5)
IP
k=l h=lk=l

densities respectively, for a tensile test along a <110> direction.

[a a 1

/
/
/
l\
1^> 2
VI 50 /
s^ooy
/
/

\ ^ ^ \
3
kl_ T~TT. . . .el
\fi^~-~
r__..
°0
el
0 10 2 0 3 0 40 50 0 10 2 0 3 0 4 0 5 0 0 10 2 0 3 0 4 0 50 0 10 2 0 3 0 4 0 5 0

Fig. 1. Simulated stress strain curves in <110> tension for the table 1
A, a, D, q parameter (a,b,c,d) values, from left to right respectively.
 119
Table 1: the A,a,D,q parameter values used in all the simulations

(a) (b) (c) (d)

A 1 2 3 2 2 2

a 105 103 105 106 105 105

D 100 100 50 100 300 100

q 8 8 8 2 8 12

0 2 4 6 10 3 /cm 2 0 2 4 6 10 3 /cm 2 0 2 4 6 l0 3 /cm 2 0 2 4 610 3 /cm 2

Fig. 2. Simulated stress versus total primary dislocation density curves in
<110> tension according to the A, a, D, q parameter values

a MPa • a MPa o MPa

16
/ / sol
1 6
12 / ° ^ 3 0 0
1 0 0 ^
6 / / «
r /**
4 // .
T r T
f — - 1 0 — P IP I I . .Pi?
106/cm2
0
2 10b/c 2l0 6 /cm 2 0 a o
Fig. 3. Simulated stress versus total interaction products dislocation density
curves in <110> tension according to the A, a, D, q parameter values

From the stress strain curves, the hardening slope increases in both I (single slip) and II
(double slip) stages when A, a or q increases, and when D decreases, while the stage I length
decreases. The used "simple", unconstrained, tension description is the one of the table 2a.

Table 2: the stress and total strain rates loading conditions of the
simulations, in simple tension (a) and in constrained tension (b)

0 0 0 * 0 0

0 0 * 0 * 0

0 0 * D

(a) (b)
120
The first linear stage on the curves of the figure 2 correspond to the preyield primary
dislocation multiplication on all the systems supporting a non zero ARSS. From the macroyield
point, these curves show two stages as the stress-strain ones. The parabolic shape of the
stress versus total (glisslle on octahedric systems plus sessile on cubic ones) interaction
product curves on the figure 3 mainly contributes to the stage 11 hardening, and is
insensitive to D or q.

The loading description effect

The figures A and 5 compare the simulated behaviour in tension for the two loading (s,L )
conditions reported in the Table 2, still in terms of stress-strain curves and stress versus
total primary (5a) and versus total interaction products (5b) dislocations, for a <110> and a
<111> oriented crystals (A«2,a«100,D-10 ,q«8 from the Table 1 first column). From the
stress-strain curves, while the difference is weak for the <111> stable axis between the
simple and the constrained tension, the stage 1 desappears for the <110> axis for a
constrained tension. The real behaviour being not homogeneous as assumed in this code, one
can expect it to be a combination of these descriptions. Experimental curves to compare with
can be found (for example for copper) in Vorbrugg et al (1971). Again, while on the figure
5a, the existence of a stage I of single slip is associated to the delay in the interaction
product multiplication due to the initial single slip stage, on the figure 5b, the
interaction product multiplication mainly relates to the stage 11 hardening, as expected from
theoretical analyses (Friedel, 1955) and known from observations (Essmann, 1963, Steeds,
1966).

o MPa / , a MPa /
16 simple tension 16

/..,
12 12 X:onstrained
/ / tension
110
8 / / 8

4 4 / S^™
r ' J f
z\
0
^.. ..ss
0 10 2 0 3 0 4 0 5 0
0
0 10 20304050

Fig. 4. Compared stress strain curves for <110> and <111> oriented tensile
tests in simple and constrained tension, according to table 2

20
o MPa / o MPa a MPA j o MPa
16
111
/
/ i / / 111
12 * simple tension ^ / constrained tension
I
H 110 n
I! //n o 110//
,/
U

110
4

0
I
^-*—-^—'"
/ 111
p
T
' p* p 10 6 /cm 2
_jj™ PT Pj p 10 6 /cm 2 |
0 2 2
3 6l0 3 /cm C i 2 :1 C 3 6 10 3 /c * « 1 2 3
Fig. 5. Stress versus total primary and versus total Interaction products
dislocation density in <110> and <111> simple and constrained tensions
 121
Detailed analysis of a <123> tension simulation

The code also allows to follow the specific parameters of each crystallographic system the
plastic straining mode is concerned_ with. The figure 6 reports some of these parameters one
can access to, in the case of a <T23> simple tension test, say the slip amplitude on the
active systems and the major primary and interaction product density evolutions with strain,
here denoted in using the Schmid and Boas notation, summarized on the figure 7 (the
corresponding stress-strain curve has been plotted on the figure 4).

p* p 10 6 /cm 2

ze j

y xi ,_e|
10 20 30 40 50
The evolution of the main slip amplitudes (a), the main primary
dislocation densities (b) and the main interaction product glissile (c)
and sessile (d) densities in the case of a <l23> simple tension

The access to the individual systems parameters allows to analyse the relation between the
global behaviour and the anisotropy at the scale of the elementary mechanisms.

In order to mainly illustrate original possibilities of such a code where the crystal
behaviour is described so as to follow the various dislocation population evolutions, the
figure 7 shows superposed <111> and <100> pole figures for the <T23> simple tensile test

The system slip direction and plane notation

1 = Oil
2 - Oil
3 - 101
4 - T01
5 - HO
6 - 110

A - Til
B - 111
C - Til
D - ill

X - 100
Y - 010
Z - 001

Scale of the figure 7

1 - 10^
2 - 10«|
3 - 10^
4 - 10?
5 - lo'

Fig. 7. The microstructural <111> and <100> pole figures for the <l23> simple
tension, showing the interaction product density evolution on each
(111) and (100) plane of the FCC structure
122
presented on the figure 6. In addition to the rotation of the crystal, these pole figures
indicate the relative increase of the dislocation interaction products densities on each of
the four <111> slip planes and of the three <100> planes of the FCC structure, on which
accumulate respectively glissile and sessile (Lomer Cottrell locks) junctions involved in the
substructure formation.

In this example the dislocations have been gathered with respect to the slip plane they
belong to. Similar plottings can be realized in gathering them with respect to their <110>
Burgers vectors or, for the interaction products, with respect to their physical orientation.
The substructure anisotropy evolution with the plastic strain can so be globally visualized.

CONCLUSION

The here presented simulation of the evolution with strain of the dislocation microstructure
organisation in the crystal lattice - even if purely statistical - can be very helpfull in
the understanding of the correlations between these microstructures, their anisotropic
characteristics and the associated macroscopic behaviour. For example, such a study of the
dislocation density characteristics at the onset of twinning for low stacking fault energy
materials, recently performed (Franciosi et al, 1990), has brougth new enlightments on the
twinning initiation criterion expression.

This code can also be considered as a model for aggregates in the sense of grain collections
all assumed to support equivalent loading conditions of the previously described type (the
extremal - static and Lee - models, here in a finite transformation version, correspond to a
fully prescribed stress rate or strain rate tensor respectively). The average behaviour for
the aggregate in terras of the previously specified phenomenological, crystalline or
microstructural parameters can be followed as for isolated crystals.

However, these statistical representations of the dislocation distribution evolution with

strain in single or polycrystal are not directly reliable to their spatial organization. But,
with the help of simple assumptions on the way the dislocations multiply and pile up in the
lattice, some possible correlations are expectable. These developments are on progress.

REFERENCES

Essmann U., (1963). Die versetzungsanordnung in plastisch verformten kupfereinkristallen,

Phys. Stat. Sol, 3, p932
Franciosi P., (1985). The concepts of latent hardening and strain hardening in metallic
single crystals Acta Metall, 33, 9 pl601
Franciosi P., (1987). On work hardening relations for constitutive models, Proceedings of the
8th RISO conference, Roskilde, Denmark
Franciosi P., Zaoui A., (1989). Crystal hardening and the issue of uniqueness, Advances in
Plasticity Proceedings of Plasticity 89 Tsu, Japan, Pergamon Press p561
Franciosi P., Zaoui A., (1991). Crystal Hardening and the issue of Uniqueness, Int. J. of
Plasticity, to be published
Franciosi P., Tranchant F., Vergnol J., (1990). Dislocation microstructures and twinning
initiation in Cu-Al alpha FCC single crystals, Proceedings of the 9th ICOTOM, Avignon,
France, to be published
Friedel J., (1955). On the linear work hardening rate of FCC single crystals Phil Mag, 46
pll69
Steeds J.W., (1966). Dislocation arrangment in copper single crystals as a function of
strain, Phil Mag., p343
Vorbrugg W., Goetting H.Ch., Schwink Ch., (1971). Work hardening and surface investigations
on Cu single crystals oriented for multiple slip, Phys Stat Sol., 46, p257
WS1C3

COMPUTER SIMULATION OF INTERNAL FRICTION PEAKS ASSOCIATED

WITH INTERACTION BETWEEN CARBON ATOMS AND DISLOCATIONS
IN Fe-Ni-C MARTENSITE DURING LOW TEMPERATURE AGING

Y. Liut, K. Ullakko and J. Pietikainen

Laboratory of Engineering Materials, Helsinki University of Technology,

Espoo, Finland

ABSTRACT

Based on the process which has been proposed for the low temperature aging of Fe-Ni-C martensite, carbon atoms
diffusing to and interacting with dislocations, the computer simulation of internal friction peaks of the Fe-Ni-C
martensite during low temperature aging was performed. The Koehler-Granato-LUcke string model was used for
the simulation to describe the process of interaction between dislocations and carbon atoms. A model is proposed
for considering the diffusion of carbon atoms to dislocations at low temperatures. In this case the relaxation
strength is temperature and heating rate dependent In addition, by the accurate determination of the peak position
from computer simulation, it was found that the position of the internal friction peak situated at the temperature
of about 210 K is shifted with frequency. The activation energy of this process is determined to be 0.79 eV.

KEYWORDS

Aging; carbon atoms; computer simulation; dislocation; low temperature; martensite.

INTRODUCTION

The aging and tempering processes of martensites with subambient Ms temperatures have been studied
extensively during the last thirty years. It has been found by MOssbauer measurments (Genin et al., 1968,
DeCristofaro et al., 1978), X-ray diffraction studies (Chen et al., 1980a, b), electron microscopy (Nagakura et al.,
1979, Taylor et al., 1989), internal friction method (Prioul et al., 1979) and calorimetric measurements (Grggoire
et al., 1990) that carbon redistribution can take place at temperatures as low as 230 K. Three processes namely
relaxation, aging and tempering have been subdivided (Sherman et al., 1983, Olson et al., 1983). The relaxation
stage characterized by a slight resistivity decrease takes place at temperature below 200 K (Sherman et al., 1983).
Dilatometric and internal friction experiments have also shown that an isothermal martensitic transformation
exhibiting C curve behavior occurs in this temperature range (Rodrigues et al., 1984). The aging stage
interpreted in terms of a carbon clustering occurs in the temperature range from 220 K to room temperature (RT),
in agreement with the early works of Winchell and Cohen (1962) showing an increase of hardness. The carbide
formation starting at temperatures above RT is named the tempering stage. Recently, it has been found that the
pinning of dislocations by carbon atoms can occur in virgin martensite at temperatures as low as 170 K (Prioul et
al., 1986) and the carbon clustering can start at temperatures as low as 200 K (Uwakweh et al., 1990).

t On leave from Institute of Metal Research, Academia Sinica, Shenyang, China.

123
124
The internal friction behavior of lenticular martensite during low temperature aging has been studied extensively
by Prioul et al. (1979,1985,1986) and Rodrigues et al. (1984). It has been found that there are two peaks which
could be due to the interaction between carbon atoms and dislocations, the first peak at about 210 K can be
interpreted in terms of pinning of dislocations by carbon atoms, the other peak at about 250 K which has
Snoek-like relaxation features (Prioul, 1985) could be explained by the Schoeck-Seeger theory (Schoeck and
Seeger, 1959).

In the present study the computer simulation of the internal friction peaks has been performed. Based on the
Koehler-Granato-Lticke (K-G-L) string model (Koehler, 1952, Granato et al., 1956, Liicke et al.t 1981), a model
has been proposed to describe the process when the carbon starting diffusion to dislocations. In this case the
relaxation strength is temperature and heating rate dependent The Snoek-like relaxation peak situated at about 256
K was simulated by a normal Debye peak. In addition, by the accurate determination of the peak position from
computer simulation, it is found that the position of the internal friction peak situated at the temperature between
170 K and 230 K was shifted with frequency, which disagrees with the early experimental results (Prioul, 1985).
The activation energy of this peak is determined to be 0.79 eV. This is almost the same value as what was
determined by the Mossbauer method for Fe-C martensite (Uwakweh et al.% 1990).

EXPERIMENTAL PROCEDURE

The alloy used in the internal friction measurements was Fe-28Ni-0.2C. The specimens were austenitized at
1150°C for 1 hour and water quenched. A surface layer was then removed in order to eliminate possible effects of
decarburization. After machining to the size of about 1 x 1 x 36 mm 3 , the specimens were polished to die size of
0.7 x 0.7 x 36 mm 3 using acid HF. The Ms temperature of this alloy is about 230 K and the morphology of the
martensite is lenticular with a mainly dislocated substructure. The samples were fixed in an inverted torsion
pendulum using two threaded heads before cooling to 82 K. The cooling rate was 14 K per minute. After one
hour holding at 82 K the specimens were heated to room temperature with a rate of 1.5 K per minute. The strain
amplitude was less than 10"5 and different frequencies between 0.2 Hz and 1.5 Hz were used. The data was
acquired and processed by a micro-computer.

MODELS

The theory of internal friction due to dislocation damping has been studied by numerous authors during the past
thirty years. In Koehler's model (1952) it is assumed that the dislocation is fixed at certain places by pinning
points and under the influence of external periodic shear stresses the free dislocation segments or loops between
the pinning points undergo forced vibration. Based on the vibrating string model proposed by Koehler, Granato
and Liicke (1956) derived a theory for the damping of a specimen containing dislocations. The damping described
by the logarithmic decrement § is given by

5 =4 fill— (i)

with

(2)
K 12C

* = *i (3)
96
Where A is the relaxation strength, A is the dislocation density, L is the loop length of the dislocation line
segments, C is the line tension or dislocation energy per unit length, G is the shear modulus, b is the Burger's
vector, a) is the angular frequency of the applied stress and T is the relaxation time.

Since the quantities C, A, G and b vary only slightly with temperature, the observed dependence of 6 and the
modulus can come only through the temperature dependence of L or T if the Granato-Lucke theory is applicable.
In the case of low temperature aging process of dislocated martensite, when diffusion of interstitial atoms occurs
at low temperatures, the most significant change in the dislocation structure of a specimen is the change in the
loop length due to the adding of the point defect pinners and it will affect the value of 8. With these conditions,
 125
equation (1) can be written directly in terms of the number of pinners added to a dislocation segment during low
temperature aging. Thus, if nQ is the original number of pinners per unit length of the dislocation line, LQ is the
original loop length, nd is the number of defect pinners added per unit length, and L d is the average loop length
with the added pinners, then

Al = - ^ - (4)
1+ M
no
Thus Eq. (2) becomes

A = JLG*LAt-!4-Y (5)
K
12C li + M l

Using an elastic interaction potential suitable for a point defect and an edge dislocation, Cottrell and Bilby (1949)
have found that the number of defects n(t) which have arrived at a unit length of dislocation at time t is given by

,(t) = 3 ( * ) U ( ^ (6)

in which NQ is the initial number of defects per unit volume, A is the interaction potential constant, D is the
diffusion coefficient of the defect in the lattice, t is the time measuredfromthe starting time at which NQ is fixed,
k is Boltzmann constant and Tis the temperature. If we take

D = DQEXP{-E/kT) (7)

where E is the activation energy for the diffusion of the interstitial atoms, and combine Eqs. (5), (6) and (7), then

A = BALl- 1 — (8)
I 2 \^
lJMEXP(-E/kT^T\
\ IkT 'J I
in which B and BQ are constants. From Eq. (8) it can be seen that the relaxation strength A is the function of the
temperature and the heating rate. This is in accordance with the experimental results (Prioul, 1985) which shows
that when increase the heating rate the relaxation strength increases. If the heating rate is kept constant then the
Eq. (1) can be written in the form

S = BAL% 1 &3_ (9)

1+ £0_EXP(-E/kT) 3

where CQ is constant.

EXPERIMENTAL RESULTS AND DISCUSSION

The internal friction behavior of the lenticular martensite in the alloy of Fe-28Ni-0.2C during low temperature
aging is shown in Fig. 1. It can be seen that the internal friction curve consists of four peaks situated at about
110,170,210 and 256 K seperately in the case of 0.41 Hz vibrating frequency. Thefirstpeak which is due to the
isothermal martensitic formation and which has been studied in details by Delorme (1971) and Rodrigues et al.
(1984), and the second peak which is newly found (Liu, et a/., 1990) are not discussed in this paper. The main
attention of this paper is paid to the last two peaks. As proposed by Prioul et al. (1985,1986) these peaks have
relations with both dislocations and carbon atoms. The 210 K peak is explained due to the movement of
dislocations under the periodically alternating external stress and their pinning by carbon atoms, the peak at
256 K is suggested to be caused by the short distance movement of the carbon atoms among the octahedral lattice
126
sites in responding to a screw dislocation stress field.

/ \

cc .004
>
5 -002

100 200 300

TEMPERRTURE ( K )

Fig. 1 Internal friction of the alloy Fe-28Ni-0.2C during heating

from 82 K to 350 K

Considering the facts that the carbon atoms are mobile at temperatures as low as 170 K (Prioul, et al, 1986) and
the clustering can occur at temperatures as low as 200 K (Uwakweh et al, 1990), the carbon atoms may start to
diffuse to dislocations at this temperature range. Then the internal friction evolution of this process, dislocation
damping and adding of more pinners (carbon atoms) to the dislocations during heating, can be described by Eq. (9)
which can aslo be written in the form

1 -Sech (10)
U
2 k\T rp)J
1 + [£0L£XP (-£/*r)l

where Q is the interaction energy between carbon atoms and dislocations, T p is the peak temperature. Based on
the fact that the 256 K peak is due to an relaxation process which assumed can be interpreted in terms of the
Schoek-Seeger theory (Prioul, 1985), the simple form of Debye relaxation (Liicke and Granato, 1981) can be used
to describe this process. To make the work less complicated, three Debye peaks were also employed to simulate
the first two peaks and the background. The simulation result is shown in Fig. 2.

100 150 200 290 300 350 400

TEMPERATURE ( K )

Fig. 2. Computer simulation of the internal friction curve

 127
The values of the activation energy obtained directlyfromfittings are about 0.25 ± 0.02 eV for the 210 K peak
and 0.23 ± 0.02 eV for the 256 K peak. It is interesting that the obtained activation energies of these two
processes have almost the same value within the error limit Comparing with the value of about 0.78 eV
obtainedfromother methods (Sherman, et al., 1983, Prioul, 1985 and Uwakweh et al, 1990), these values are
rather small. For the value of the activation energy is related directly to the peak width and for these two
processes have internal relationship in nature, it seems that finding a more unique form to describe these two
processes together could be expected to obtain the most reliable results. This form should include the factors of
pipe diffusion of carbon atoms and carbon clustering. On the other hand, from computer simulation the peak
position can be determined more precisely, especially in the case of multi-process. From the accurate
determination of the peak position the activation energy can also be determined more accurately. As a result of the
computer simulation it is found that the 210 K peak is shifted with vibrationfrequencyas shown in Fig. 3. This
result disagrees with the early results (Prioul, 1985) and suggests that the 210 K peak may also due to a kind of
relaxation process.

1000 / T

Fig. 3. The simulation results of the 210 K peak for five different vibrating
frequencies: A, 0.21; B, 0.26; C, 0.41; D, 1.03; E, 1.48 Hz.

The activation energy determined using the common method, as shown in Fig. 4, is 0.79 eV. This value agrees
with the value of 0.78 eV obtainedfromMOssbauer measurements (Uwakweh et al, 1990)

3T 1

2
I

1 A

oH • 1 1 1 1 ^H
4.6 4.7 4.8 4.9
1000/T

Fig. 4. Natural logarithmic plot of (O versus 1/Tp from the data of Fig. 3. An
activation energy Q = 0.79 eV is obtainedfromthe slope of this graph.
128

CONCLUSIONS

— The low frequency internal friction evolution of Fe-28Ni-0.2C lenticular martensite during low temperature
aging can be simulated by four peaks at about 110,160,210 and 255 K and a Debye shape background
— Considering the diffusion of carbon atoms to dislocations at low temperature, a model is proposed to describe
the internal friction evolution of this process. In this case the relaxation strength is temperature and heating
rate dependent
— The 210 K peak is shifted with vibrating frequency, the activation energy is determined to be 0.79 eV.

ACKNOWLEDGEMENTS

The Academy of Finland is kindly acknowledged for financially supporting this work.

REFERENCES

Chen, P.C., B. O. Hall, and P. G. Winchell (1980a). Atomic displacements due to C in Fe-Ni-C martensite.
Metall. Trans. A. 11 A. 1323-1331.
Chen, P. C. and P. G. Winchell (1980b). Martensite lattice changes during tempering. Metall. Trans. A, 11A.
1333-1339.
Cottrell, A. H. and B. A. Bilby (1949), Dislocation theory of yielding and strain aging of iron. Proc. Phys. Soc.
(London) A62. p. 49.
DeCristofaro, N., R. Kaplow, and W. S. Owen (1978). The kinetics of carbon clustering in martensite. Metall.
Trans. A, 2A, 821-825.
Delorme, T. F., (1971). Thesis, Lyon, France.
G6nin, J. R. and P. A. Flinn (1968). MOssbauer effect study of the clustering of carbon atoms during the
room-temperature aging of iron-carbon martensite. Trans. TMS-AIME. 242. 1419-1430.
Granato, A. and K. LOcke (1956). Theory of mechanical damping due to dislocations. /. Appl. Phys. 22, p. 583.
Grdgoire, P., C. Dagbert, P. Pahuta, J. Galland, and L. Hyspecka (1990). Effect of carbon content on ageing and
tempering processes in Fe-Ni-C virgin martensite. Proc. ICOMAT-1990, Sydney, Astralia,Afateria/j Science
Forum, Swizerland, 56-58.213-218.
Koehler, J. S. (1952), Imperfections in Nearly Perfect Crystals, edited by W. Shockley et al. (Wiley, New York,
1952), p. 197.
Liu, Y., K. Ullakko and J. Pietikainen (1990). Anelastic relaxation of ferrous martensite at low temperatures.,
March. 1990. Tempere, Finland. Report 7-90,14:9.
LUcke, K. and A. V. Granato (1981). Simplified theory of dislocation damping including point-defect drag. I.
theory of drag by equidistant point defects. Phys. Rev. B 24,6991-7006.
Nagakura, S. and M. Toyoshima (1979). Crystal structure morphology of the ordered phase in iron/carbon
martensite. Trans. 7/Af,2Q, 100-110.
Olson, G. B. and M. Cohen (1983). Early stages of aging and tempering of ferrous martensites. Metall. Trans. A,
14A. 1057-1065.
Prioul, C, M. Canard, L. Hyspecka, J. Plusquellec and P. Azou (1979). Internal friction associated with a reheat
transformation in Fe-Ni-C alloys. Scripta Metallurgies H, 523-526.
Prioul, C. (1985). Snoek like relaxation in Fe-Ni-C virgin martensite. Journal de Physique. £lQ, 665-668.
Prioul, C. and L. Hyspecka (1986). Carbon dislocation interaction in virgin Fe-Ni-C martensite. Proc.
ICOMAT-1986. JIM. Nara, Japan. 337-342.
Rodrigues, C. A. V. de A, C. Prioul and L. Hyspecka (1984). Isothermal martensitic transformation in Fe-Ni and
Fe-Ni-C alloys at subzero temperatures. Metall. Trans. A, 15A. 2193-2203.
Schoeck, G and A. Seeger (1959). The flow stress and its dependence on impurities. Acta Met. 2,469-477.
Sherman, A. M., G. T. Eldis and M. Cohen (1983). The ageing and tempering of Iron-Nickel-Carbon
martensites. Metall. Trans. A. 14A. 995-1005.
Taylor, K. A., L. Chang, G. B. Olson, G.W. Smith, M. Cohen, and J. B. Vander Sande (1989).Spinodal
decomposition during aging of Fe-Ni-C martensite. Metall. Trans. A, 20A. 2717-2737.
Uwakweh, O. N. C, J. Ph. Bauer and J. -M. R. G6nin (1990). MOssbauer study of the distribution of carbon
interstitials in iron alloys and the isochronal kinetics of the aging of martensite: the clustering-ordering
synergy. Metall. Trans. A, 21A, 589-602.
Winchell, P. G. and M. Cohen (1962). The strength of martensite. Tans. ASM. 55. 347-360
WS1C4

MULTIAXIAL CREEP OF A DIRECTIONALLY SOLIDIFIED ALLOY:

EFFECTS OF LATTICE ROTATION

N. OHNO* and T. MIZUNOt

* Department of Mechanical Engineering, Nagoya University,

Chikusa-ku, Nagoya, 464-01 Japan.
t Nagoya Guidance and Propulsion Systems Works,
Mitsubishi Heavy Industries, Ltd., Komaki, 485 Japan.

ABSTRACT

Combined tension-torsion creep tests of directionally solidified IN7 38LC at

850°C are first discussed to find features which become noticeable with the
advance of creep deformation. Analysis based on the crystallographic slip
theory of finite deformation then shows that crystalline lattice rotation
explains the experimental features; it is mostly responsible for the change
of the noncoaxiality between creep rate and stress in combined tension-
torsion creep, and partly for the earlier appearance of tertiary creep under
combined tension-torsion than under pure tension and torsion.

KEYWORDS

Directionally solidified alloy; multiaxial creep; lattice rotation; slip

system; finite deformation.

INTRODUCTION

Nickel-base directionally solidified and single-crystal alloys have been

used recently as materials for gas turbine blades. However, multiaxial
inelastic behavior of such materials has been investigated only in a few
works so far, in contrast with many works for uniaxial behavior.

The present authors et al. therefore carried out combined tens ion-torsion
creep tests of directionally solidified IN738LC at 850°C to examine creep
anisotropy of this material in multiaxial stress states (Ohno et al., 1989,
1990). Analyzing the experiments on the basis of the crystallographic slip
theory, they found that the minimum creep rates are well simulated if the
{lll}<112> octahedral slip system is combined with the {l00}<110> cubic
system. The former has been observed to be active in creep (Leverant and
Kear, 1970; Pasley et al., 1970, 1971; MacKay and Maier, 1982; Hopgood and
Martin, 1986; Sheh and Stouffer, 1988), while the latter has not been
reported for creep (Pope and Ezz, 1984; Sheh and Stouffer, 1988).

129
130
In the previous papers (Ohno et al., 1989, 1990), phenomena which become
noticeable with the advance of creep deformation were not discussed. A
possible micromechanism which brings about such phenomena is lattice
rotation. Since directionally solidified alloys consist of columnar grains
growing parallel in the solidification direction, their mechanical behavior
is governed directly by the micromechanisms of single crystals. Therefore,
when deformation is large, lattice rotation is a potential micromechanism
which may influence markedly on the inelastic behavior of directionally
solidified alloys.

In the present work, first, the experiments (Ohno et al., 1989, 1990) are
discussed to find features which become noticeable as creep proceeds. Then,
to study the effects of lattice rotation on them, the experiments are
analyzed on the basis of the the crystallographic slip theory of finite
deformation.

EXPERIMENTAL FEATURES

Thin-walled tubular specimens of IN738LC solidified in the axial direction

were subjected to constant true tensile stress 0 and torsional stress T at
850°C (Ohno et al., 1989, 1990). The stress state in the tests was
specified in terms of the equivalent stress of Mises, 0 , and the angle of
stress, 0, defined as

O = (0 2 + 3 T 2 ) 1 / 2 , (1)
eq
6 = tan-1(0//3T). (2)

The creep curves obtained under 0 = 300 MPa are shown in Fig. 1, where the
equivalent strain of Mises for isotropic materials, £ , is taken for
eq
convenience in the ordinate. With tensile strain e and shear strain Y, £ eq
is expressed as

eq J<J 2 *2 1/2
ez + y / 3 ) ± x d t . (3)

9=60°

9=45°

.9=30°

Oeq
• 350MPa
A 300MPa
■ 250MPa

10 20
Time (hr) Shear Strain r / / 3 (%)

Fig.l. Creep curves by experiments Fig.2. Strain trajectories by

«* 300 MPa). experiments.
 131
We see from the figure that the change of creep rate with £ depends on the
stress state: While steady-state creep prevails up to £ - 10 % in the
eq
tensile creep test (9 = 90°), tertiary creep becomes noticeable around £ -
eq
5 % in the combined tension-torsion creep tests of 0 = 60° and 6 = 30°. In
the torsion creep test (8 = 0°), on the other hand, tertiary creep is not
observed except just before creep rupture.
The noncoaxiality between stress and creep rate tensors also changes, with
dependence on the stress state, as creep deformation proceeds (Fig. 2). Let
us define the angle of creep rate to be

0 = tan 1[£/(Y//3)]. (4)

Then, i f we deal with a Mises-type i s o t r o p i c m a t e r i a l , we have 0 = 0 ; i . e . ,

t h e d o t t e d l i n e s in F i g . 2 a r e t h e c r e e p s t r a i n t r a j e c t o r i e s t o be
predicted. However, t h e t r a j e c t o r i e s observed in the experiments are not
such s t r a i g h t l i n e s . In the t e s t s of 0 = 45° and 0 = 60°, f i r s t 0 > 0_, and
e v e n t u a l l y 0 - 0 . _In the t e s t of 0 = 30°, on the other hand, f i r s t 0 - 0 ,
and then s l i g h t l y 0 > 0 e x c e p t j u s t b e f o r e r u p t u r e . Moreover, the
t r a j e c t o r i e s in t h e t e s t s of 0 = 0° and 0 = 90° were observed t o nearly
coincide with the abscissa and the o r d i n a t e , r e s p e c t i v e l y , though they a r e
not shown in Fig. 2, (see Fig. 7 ) .

MODEL FOR ANALYSIS

z t
Directionally solidified nickel-base
alloys consists of columnar grains f f /
growing parallel in the solidifica-
tion direction, for which the [001] J s . y
direction is preferred. Hence the
thin-walled tube was modeled simply Go
as shown in Fig. 3, where x, y and z
denote the radial, circumferential
and axial directions of the tube,
respectively, and £, f| and £ indicate
the crystalline axes. In this simple
model, only two kinds of columnar
grains, Go and Gi»s» alternate in the
circumferential direction. In the
grain Go the crystalline axes are Go G45 ~ u G45
directed in the x, y and z direc-
tions, while in G45 they rotate by Fig.3. Model for analysis.
45° with respect to the z direction.

To specify creep rate of the grains Go and Gi+5, let us consider three kinds
of slip systems, i.e., the {lll}<110> octahedral, the {lll}<112> octahedral,
and the {l00}<110> cubic system, reported to be active in plastic and/or
creep deformations of nickel-base single crystals (Pope and Ezz, 1984; Sheh
and Stouffer, 1988; Walker and Jordan, 1989). Then, on the basis of the
crystallographic slip theory of finite deformation (see, e.g., Asaro, 1983),
creep rate and spin tensors of each grain are expressed as follows:
12 12 6
•(k)a(k)
(k) (k)
yr ( k ) a ( k ) (5)
I y'octl«octl +
I oct2 oct2 +
I cub cub
k=l k=l k=l
132

ft =ftS+ ft*, (6)

fts= 2
y ; (k)
u, (k)
y ; a,2 (k)
i ; a> ,(k)
, L, Toctl octl + , L, Toct2 oct2 + , L, Tcub cub'
(k) (k)
(7
K } )
k=l k=l k=l
where the subscripts octl, oct2 and cub stand for the {lll}<110> octahedral,
the {lll}<112> octahedral, and the {l00}<110> cubic system, respectively;
• (k )
Y n ( Q = o c t l , o c t 2 , cub) denotes the s l i p r a t e in the s l i p system
specified by the subscripts (k) and 0: Q3 and ft* indicate spins due t o s l i p
(k) (k)
and r i g i d rotation, respectively; a and 0) are defined in terms of the
(k) (k)
s l i p direction vector b ^ and the s l i p plane vector n _ as
Q Q
(k) 1
1 ,,Ak)Q. (k) . „dOxx-UK
w ( k ) ^ (k) (k)6a.(k) ,Q.
a = - ( b2 ^ (Qb Q0 n + n ® b ) ,
® ^" +
Qn ^ Q s > b ^ ) ,
Q Q (8)

(k) (k)
U)^ i l((bbx ^ , ® n ^ /
= T -- nn Q^ '®^ bb Q^ ' )) .. (9)
2 C Q
(k) (k)
The spin due to rigid rotation,ft*,rotates b and n :
*(k) O**^) '<k> - O* ^ ) M M
b
Q = f t * b Q ' n
Q = Q
* n
Q ' (10)
•(k)
For Yn $ we assume a simple power law

Y ( Q } = sign[T(k)]-K |T (k) | n Q (Q = octl, oct2, cub), (11)

(k) (k)
where T = tr((XX ), and K and n are material constants.

Then, combined tension-torsion creep of the d i r e c t i o n a l l y s o l i d i f i e d t h i n -

walled tube modeled as shown in F i g . 3 can be analyzed, if we take into
account appropriately the interaction between the neighboring grains Go and
GJI5. In t h e p r e s e n t work, s i n c e we d e a l w i t h c o n s i d e r a b l y l a r g e
deformation, i t may be appropriate to assume

L = L ._, L = L ._, (12)

zz:0 zz:45 yz:0 yz:45
where L and L are components of velocity gradient tensor L, and the
zz yz ^
subscripts 0 and 45 denote the grains Go and Gi*5, respectively.

MATERIAL CONSTANTS (SIMULATION ON MINIMUM CREEP RATE)

The simulation on minimum creep rate in the framework of small strain (Ohno
et al., 1989, 1990) is reported here again for convenience in Figs. 4 and 5.
The material constants used in this simulation were
-23 -24 -24
K ^ = 1.07X10 , K ^ = 4.91X10 , K ,_ = 2.37X10
octl oct2 cub
n . = n . =n = 9.2,
octl oct2 cub
where units are MPa (stress), hr (time), and mm/mm (strain). As seen from
Figs. 4 and 5, if we assume only one kind of slip system to be active, the
experiments are not simulated accurately. However, the combination of the
{lll}<112> octahedral and {l00}<110> cubic systems is very successful.
 133

U11X112>

iq 60' A
Ml11)<110>

AB/M111)<112>+<100)<110> ^ -<iiixii2>+nooxno>
/ A / Experiment
30' h 0*
/ / \ ,(100X110> /•
/ / V Experiment
O»Q /; O

III
•/; A
10" //
F / ^ « i i X112> \
o
A
oDUMra
300MP o
/; D

a 250MP, <100X110>
/-nooh
t I L
30* 60* 90' 90'
tan- 1 (o/^T) tarT1(o/73T)

F i g . 4 . Dependence of c r e e p r a t e on F i g . 5 . N o n c o a x i a l i t y between c r e e p
stress state. r a t e and s t r e s s .

RESULTS OF ANALYSIS AND DISCUSSION

C r e e p c u r v e s a n d c r e e p s t r a i n t r a j e c t o r i e s r e s u l t e d from t h e p r e s e n t
a n a l y s i s a r e shown i n F i g s . 6 a n d 7 , r e s p e c t i v e l y . The a n a l y s i s w a s
performed for O = 300 MPa. The c o m b i n a t i o n of t h e {lll}<112> o c t a h e d r a l
eq
and {l00}<110> c u b i c systems was assumed, b e c a u s e i t s i m u l a t e s a c c u r a t e l y
t h e minimum c r e e p r a t e d a t a ( F i g s . 4 , 5 ) .

-6=90°

e=90* e=60*

20 / /
e=30°
5 / / / . ' 0 6=0°
8\, / / / ,^s^ ^y^ ■
d 10 - / / / ,*y^ ^^--'''
:
/// jS^'^<^ '"s=m

i^r\ . . i—x—■—.—.—i—. e=o°

0 500 1000
Shear Strain y/tt (%)
Time (hr)
Fig.6. Creep curves by analysis Fig.7. Strain trajectories by anal-
based on {lll}<112> and ysis based on {lll}<112> and
{l00}<110> slip systems {l00}<110> slip systems, to-
(O = 300 MPa). gether with experiments,
eq
(O _ = 300 MPa).
eq
134
As seen from Fig. 6, acceleration of creep rate occurs in the creep curves
of 0 = 60° and 30°, whereas rather steady-state creep prevails under 9 = 90°
and 0°. This trend is the same as in the experiments (Fig. 1 ) ; thus, the
theory is partly successful in simulating the creep curves in Fig. 1. The
strain trajectories resulted from the analysis, on the other hand, agree
well with the experiments (Fig. 7); i.e, along the trajectories of G = 60°
and 45° the noncoaxiality between creep rate and stress becomes smaller and
eventually vanishes, while it becomes noticeable gradually in the case of
6 = 30°.

In the present analysis, only lattice rotation is the internal change,

because the creep equation employed, eq. (11), does not include any internal
variable. Therefore, the acceleration of creep rate and the change of the
noncoaxiality in the analysis is brought about through lattice rotation.

ACKNOWLEDGMENT

The authors appreciate the financial support by the Ministry of Education of

Japan under a Grant-in-Aid for Scientific Research C (No. 01550070) in the
fiscal year of 1989. The second author, T. Mizuno, was associated with the
present work while studying as a graduate student at Nogoya University.

REFERENCES

Asaro, R.J. (1983). Micromechanics of crystals and polycrystals. Adv. Appl.

Mech., 23, 1-115.
Hopgood, A.A. and J.W. Martin (1986). The creep behaviour of a nickel-based
single-crystal superalloy. Mat. Sci. Eng. , 8^2, 27-36.
Leverant, G.R. and B.H. Kear, B.H. (1970). The mechanism of creep in gamma
prime precipitation-hardened nickel-base alloys at intermediate tempera-
tures. Metal. Trans., 1_, 491-498.
MacKay, R.A. and R.D. Maier (1982). The influence of orientation on the
stress rupture properties of nickel-base superalloy single crystals.
Metal. Trans. A., 13, 1747-1754.
Ohno, N., H. Kawaji, H. and T. Mizuno (1989). Creep of a nickel-base
directionally solidified alloy under combined tension and torsion. In:
Advances in plasticity 1989 (A.S. Khan and M. Tokuda, eds.), pp. 357-360.
Pergamon Press, Oxford, New York.
Ohno, N., T. Mizuno, H. Kawaji and I. Okada (1990). Multiaxial creep of a
nickel-base directionally solidified alloy (1st report, Experiments and
analysis on minimum creep rate). Trans. JSME. Ser. A., _56, 2288-2296.
Paslay, P.R., C.H. Wells and G.R. Leverant (1970). An analysis of primary
creep of nickel-base superalloy single crystals. ASME J. Appl. Mech.,
32,759-764.
Paslay, P.R., C.H. Wells, G.R. Leverant and L.H. Burck (1971). Creep of
single crystal nickel-base superalloy tubes under biaxial tension. ASME J.
Appl. Mech., 2§# 623-626.
Pope, D.P. and S.S. Ezz, S.S. (1984). Mechanical properties of Ni3Al and
nickel-base alloys with high volume fraction of Y'. Int. Met. Rev., 29,
136-167.
Sheh, M.Y. and D.C. Stouffer (1988). Anisotropic constitutive model for
nickel-base single crystal superalloys. NASA report CR-182157, NASA.
Walker, K.P. and E.H. Jordan (1989). Biaxial constitutive modelling and
testing of a single crystal superalloy at elevated temperatures. In:
Biaxial and multiaxial fatigue (M.W. Brown and K.J. Miller, eds.), pp.
145-170. Mechanical Engineering Publications, London.
WS1c6

SIMULATION OF L A T E N T H A R D E N I N G

IN R A T E - D E P E N D E N T FCC POLYCRYSTALS

Y . Z h o u , K . W . N e a l e and *L.S. T o t h
Faculte des sciences appliquees
Universite de Sherbrooke
Sherbrooke, Quebec, Canada J1K 2R1
t Institute for General Physics
Eotvos University
1445 Budapest, P.O.B. 323, Hungary

ABSTRACT

A strain hardening model for rate-dependent FCC crystals is proposed based on experimental
observations previously reported for FCC single crystals. This model includes both the self-hardening and
latent hardening of the slip systems. The anisotropic hardening of the latent systems is assumed to arise
from the differences of interaction strengths between glide dislocations and forests. With this hardening
model and a rate-sensitive crystal plasticity theory, the deformation behaviour of rate-dependent FCC
polycrystals can be predicted from the deformation response of the constituent single crystals. As an
example, the uniaxial tensile behaviour of pure aluminum polycrystals is simulated using the proposed
model. The effects of latent hardening on poly crystal deformation, especially on flow stress and the
formation of tensile textures, are discussed.

KEYWORDS

Plastic deformation; FCC polycrystals; strain-hardening; textures; rate sensitivity; crystal models.

1. I N T R O D U C T I O N

It is well known that strain hardening in polycrystals results from the interaction between dis-
locations and obstacles, as well as from interactions among dislocations themselves. Such hardening
involves dislocation density, dislocation movement, the nature of the polycrystal as well as the deforma-
tion conditions. Because the exact relationship between flow stress and dislocation interaction has not
yet been quantitatively obtained, simulations of strain hardening in polycrystals are generally based on
experimental observations for the deformation response of single crystals.

So far, various models have been proposed to simulate strain hardening in polycrystals on the basis
of the hardening of single crystals [1-4J. During polycrystal deformation, more than one slip system is
activated simultaneously, and the slip in each slip system has an effect on the hardening of all systems.
Accordingly, the rate of increase of flow stress in slip system s, fya, can be expressed as

rs, = X><l7,l (1-1)

where hst are the hardening moduli and j t is the shear rate on slip system t. For FCC crystals possessing
12 {111} < 110 > slip systems, hst is a 12 x 12 matrix. The diagonal elements of h3t are the self-hardening
moduli and the off-diagonal ones are the latent hardening moduli.

The manner in which one specifies the hardening matrix h3t is the subject of the various hardening
theories. For example, Taylor [1] proposed an isotropic hardening theory in which the active and latent

135
136
systems harden equally, i.e., hat = const, for all s and t. On the other hand, Asaro et al. [4] used the
following hardening law for rate dependent FCC crystals

h,t = h{ya)q.t (1-2)

where h(ya) is a single slip hardening modulus, ya is the sum of the slips on all the systems, and qst is
a matrix describing the latent hardening behaviour of the crystal. For coplanar slip, qtt = 1, and for the
others, qsi — q > 1.

In accordance with the dislocation forest intersection theory [5] and experimental observations re-
ported for FCC single crystals [6-9], a strain hardening model is proposed for rate-dependent FCC crystals
in this paper. With this hardening model and a rate-sensitive crystal plasticity theory, the deformation
behaviour of rate-dependent FCC polycrystals can be predicted from the deformation response of the
constituent single crystals. Here, the stress-strain curves for Al polycrystals are simulated and compared
with experimental observations. The effects of latent hardening on flow stress and tensile textures are
discussed.

2. S T R A I N H A R D E N I N G M O D E L

The magnitude of latent hardening is generally specified by the ratio (LHR) of the flow stress of
the latent system (r/) to that of the primary one (r p ) after a certain amount of primary slip. T h a t is,
LHR = TI/TP. The LHR's have been investigated for various FCC crystals, such as Al [6,7], Cu [7,8]
and Cu — Al [9]. The main results of these investigations can be summarized as follows:

All latent systems harden more due to the primary slip than do the primary systems themselves.
Within the strain stage I (7 < 1 — 3%), the LHR's increase with increasing strain, reach some
maximum values, then decrease gradually. Beyond stage I, all the LHR's stabilize at values larger
than unity. Differences in the LHR values are observed from one latent system to the other. The
lower the stacking-fault energy of the crystal, the higher is the latent hardening. For example,
the LHR's of Cu are higher than those of Al. However, the LHR's seem to be rather insensitive
to alloying, at least for Cu — Al alloys. In alloy crystals, a reduction in temperature results in a
considerable decrease of the LHR's. However, in pure crystals, the LHR's are essentially constant
for all temperatures. The temperature sensitivity of flow stress is independent of both the history of
deformation and the slip systems, i.e., it is independent of the nature of the dislocation distributions.
With a change of strain rate, the variation of the LHR is rather small. Moreover, both the latent
and primary systems exhibit a similar strain-rate sensitivity.

It is known, from dislocation theories [5], that the level of flow stress is the sum of a thermal
activation term ( r , ) and another component (rg). The short-range obstacles responsible for r, are forest
dislocations, although impurities may make a significant contribution when the flow stress is small. There
are several approaches to explain the origin of rg. The first one ascribes rg to long-range stresses set
up by the accumulation of primary dislocations [10]. A second theory suggests that rg is due to forest
intersections [5], whereas a third states that rg is a result of the stress needed to bow out segments of the
dislocation network pinned by interactions with parallel dislocations [11]. As LHR's less than unity are
predicted with the long-range stress theory, most investigators [7-9] believe that the forest intersection
theory is appropriate for latent hardening. Also, the constancy of LHR's in coplanar systems cannot be
explained by the mesh length model.

With the help of the forest intersection theory [5], the hardening anisotropy among latent systems
can be explained as the differences in the strengths of the interaction between glide dislocations and
forests. From this point of view, the LHR's of coplanar and colinear slip systems of a F C C crystal
should be close to unity after stage I, since their dislocations cannot form junctions with those in the
primary system. For systems where Burgers vectors are at 90° to the primary slip direction, an attractive
node ("Hirth lock" [7]) would tend to form. Since the corresponding reduction in energy is small, their
LHR's would be systematically lower than those of other intersecting systems. Systems in which the
dislocations would form sessile junctions ("Lomer-Cottrell locks" [7,8]) with the primary ones would
be the most hardened latent systems. The second most hardened latent systems are those in which the
dislocations would form glissile junctions with the primary ones. These predictions are in good agreement
with experimental observations [6-9].

According to the experimental observations and the dislocation forest intersection theory, the fol-
lowing strain hardening model is proposed in the present work for rate-dependent FCC polycrystals. In
this model, the hardening anisotropy among latent systems is considered to arise from differences of the
interaction strengths between glide dislocations and forests.
 137

For a FCC crystal, the rate sensitivity of slip can be described by a power-law relationship between
the shear rate 7, and resolved shear stress r, on slip system s [12-14]:

r. = r o . s g n ( 7 . ) l ? i r = r0.^-\^-\"- (2-1)
7o 7o 7o
Here m is the strain-rate sensitivity index, 70 is the reference shear rate and To, is the reference shear stress
for system s, which depends on the effects of strain hardening. The strain hardening model proposed
here is as follows
dr09 = J2hst\dyt\ (2-2)

In this relation, dyt is the increment of shear slip yt on slip system t of a crystal and hti is the matrix of
hardening moduli of the slip systems. The form of h$t is the same as (1-2), but the matrix qtt is chosen
in the following form for the 12 {111} < 110 > slip systems (listed in [14]) of FCC crystals:

a b e d
b a d e
q,t (2-3)
c d a b
d c b a
where
S S S R L L'
S S S 6 = L S L
.S S S. L L R.
S L L R L L
L R L d= L R L
L L R L L S
Here S < R < L; S = I is the latent hardening ratio (LHR) of the coplanar or colinear systems in
which the dislocations cannot form any junctions with those in the corresponding active system; R is
the LHR of the systems where the Burgers vectors are at 90° to the active system so that an attractive
node (Hirth lock) would be formed causing these systems to harden more rapidly than the coplanar or
colinear systems; and L is the LHR of other intersecting systems in which glissile or sessile junctions
(Lomer-Cottrell lock) would be formed between the latent dislocations and the primary ones. The values
of R and L are higher at the beginning of deformation (7 < 1 — 3%) and then decrease to constant
values greater than unity with further deformation. In addition, for a pure FCC crystal, the matrix
qst is supposed to be unaffected by strain rate, strain-rate sensitivity or temperature, as suggested by
experimental observations [8,9].

3. TENSILE BEHAVIOUR OF RATE-DEPENDENT FCC POLYCRYSTALS

With the strain hardening model described above, the uniaxial tensile behaviour of pure aluminum
polycrystals has been simulated using a rate sensitive crystal plasticity theory [13,14]. In this theory,
the rate sensitivity of slip is expressed by (2-1) and the corresponding constitutive equation relating the
strain-rate tensor D to the stress tensor <r is

il/m-1 (3-1)
2r
s 0«

We assume that m and 70 are constant during deformation and that they are the same for all the slip
systems of the crystal. Here m* = b* x n a is the Schmid tensor for the slip system s, and b* and n a
denote the unit slip direction and unit slip plane normal of the slip system s in the current configuration.
In the simulations, the polycrystal is modelled using 800 grains with random orientations in the
initial undeformed state. A uniaxial tensile strain is imposed on the polycrystal. The parameters involved
in (2-1) and (2-2) describing latent hardening are specified according to experimental observations of Al
single crystals [6,7]. The calculation steps are as follows. First, the strain increment state for each grain
is set equal to the macroscopic strain increment. Then (3-1) is solved using an iterative Newton-Raphson
scheme to determine the deviatoric stress state, the shear slip rate distribution and the lattice rotation
138

of each grain. Finally, the stress deviatoric state of the polycrystal is obtained from the average of that
over all the grains. Various values of strain-rate sensitivity m were employed in the simulations. Here we
only present results for the case m = 0.005.

In order to emphasize the effects of latent hardening on polycrystal deformation, the uniaxial
tensile behaviour of pure Al polycrystals with isotropic hardening has also been simulated. In this
calculation, the parameters are taken to be identical to those for Al, except that qst = 1 for all s and t.
The following discussion is based on a comparison between the predictions of the latent hardening and
isotropic hardening models.

Stress-Strain Response

The numerical results show that the predictions of the true stress-natural strain curves of pure Al
polycrystals are in excellent agreement with the experimental data [151. Figure 1 shows the difference
between the stress-strain curve of the Al polycrystal with latent hardening (Curve 1) and that with
isotropic hardening (Curve 3). It can be seen that latent hardening agrees best with the experimental
data. It leads to a higher true stress for a given strain, compared to the isotropic case, even though the
LHWs of Al are not high numerically. As mentioned previously, the LHR's of a FCC crystal in the
strain stage I are much higher than those in the other stages. This effect of initially higher LHWs affects
the crystal behaviour not only in the initial stage of deformation, but also at larger strain. If we suppose
that the LHWs in stage I are the same as those in the other stages, the stress response obtained is the
second curve of Fig. 1. A comparison of Curve 1 with Curve 2 shows that the initial LHR results in an
increase of the flow stress of the polycrystal at larger deformation.

10.00 n

s
l l l I l l l l I | l I l l l l l l l | l l l I l l l l I | l I I I
0.00 0.10 0.20 0.30
Natural Strain

AAAAA experimental data

Fig. 1 Predictions of the true stress-natural strain curves for a pure Al poly-
crystal with (1) latent hardening (the LHWs in strain stage I are higher
than those in the other stages), (2) latent hardening (the LHWs in
strain stage I are equal to those in the other stages) and (3) isotropic
hardening (m = 0.005).

The anisotropy of strain hardening results not only from the anisotropy of the interactions between
dislocation sets, but also from the anisotropy of the respective densities of these sets [7-9]. T h e LHWs
are known to be related to the ratio of the dislocation density (pp) in the primary system to that (pi)
in the latent system by a quadratic relation. At the initiation of plastic flow, the primary density pp
strongly increases at first and then varies more slowly with deformation [7]. In contrast, the latent density
pi has a more gentle variation [7]. As a result, the relative multiplication rate for the latent dislocations
is expected to rapidly become of the same order of magnitude as that for the primary dislocations. If we

decrease for a larger 7. After the completion of stage I, the LHWs would remain constant.

Due to the stronger initial anisotropy caused by latent hardening, each grain of the polycrystal
would rotate more rapidly towards its stable orientation, which implies that an initially higher LHR
would change the slip distributions in the slip systems. From this point of view, the initial latent
hardening also affects the polycrystal behaviour at larger deformation.
 139
Grain Rotations

In Fig. 2 the inverse pole figure of the tensile axis for the Al polycrystal is shown for a tensile
strain en = 1.0. Here it can be seen that the tensile texture is comprised of two main components: a
stronger < 111 > fibre and a weaker < 106 > fibre. With an increase of deformation, the < 111 > fibre
component remains constant, but the grains whose < 106 > direction is aligned with the tensile axis tend
to rotate around the transverse axis.

(001) (011)

(111)

Fig. 2 Simulated tensile-axis inverse pole figure for the Al polycrystal with
latent hardening (e = 1.0, m = 0.005).

(001) (on)

(111)

Fig. 3 Simulated tensile-axis inverse pole figure for the Al polycrystal with
isotropic hardening (e = 1.0, m = 0.005).

For the case of isotropic hardening (Fig. 3), the final tensile texture includes two fibres: < 111 >
and < 001 >. A decrease of the m-value has the effect of increasing rates of grain rotation. When
m = 1, there is no lattice rotation. These results are the same as those for the case with no hardening.
A comparison of Fig. 2 and Fig. 3 shows that latent hardening affects not only the lattice rotation rate
of each grain, but also the formation of tensile texture. With latent hardening, the final texture (for
m = 0.005 and en = 5.0) is comprised of the stronger < 111 > fibre and the weaker < 103 > fibre, about
140

20° away from < 001 >. Such a shift of the texture component was predicted by Asaro and Needleman
[4], but has not yet been observed experimentally [16,17]. The larger the m-value, the closer the axis of
the latter fibre is to < 001 >. When the m-value is equal to 0.5, the stronger component of the tensile
texture is still the < 111 > fibre, but the weaker one becomes the < 001 > fibre. In the case of m = 1,
the lattice rotation rate is not exactly equal to zero but is nevertheless very small, and a slight < 111 >
fibre texture is formed only at very large deformation.

4. CONCLUSIONS

Based on experimental observations reported for FCC crystals, the strain hardening behaviour
of rate dependent FCC polycrystals has been simulated in the present work and the effects of latent
hardening have been examined. The conclusions drawn from this study are as follows:
The strain hardening of a slip system in a FCC crystal involves self-hardening which results from
its own shear slip, and latent hardening which arises from the shear slips in the other systems.
According to the possibility of junction formation between latent dislocations and the primary
ones, the LHWs may be divided into three groups: S < R < L, where S = 1 is the LHR of the
coplanar or colinear systems, R is that of the systems in which the Burgers vectors are at 90° to
the primary slip direction, and L is that for the systems where glissile or sessile junctions would
be formed between latent dislocations and the primary ones. An initially high latent hardening
influences not only the crystal behaviour at small deformation, but also that at larger deformation.
Also, latent hardening increases the lattice rotation rate of individual crystals and affects the
components of the tensile texture.

ACKNOWLEDGEMENTS

This work was supported by the Natural Sciences and Engineering Research Council of Canada
(NSERC) and the Government of the Province of Quebec (Programme FCAR).

REFERENCES
1. G.I. Taylor, J. Inst. Metals 62, 307 (1938).
2. K.S. Havner and A.H. Shalaby, Proc. R. Soc. Lond. A358, 47 (1977).
3. D. Peirce, R.J. Asaro and A. Needleman, Ada Metall. 30, 1087 (1982).
4. R.J. Asaro and A. Needleman, Ada Metall 33, 923 (1985).
5. G. Saada, Eledron Microscopy and Strength of Crystals, Interscience, New York (1963).
6. U.F. Kocks and T.J. Brown, Acta Metall. 14, 87 (1966).
7. P. Franciosi, M. Berveiller and A. Zaoui, Acta Metall. 28, 273 (1980).
8. P.J. Jackson and Z.S. Basinski, Can. J. Phys. 45, 707 (1967).
9. E.J.H. Wesseles and F.R.N. Nabarro, Acta Metall. 19, 903 (1971).
10. A. Seeger, Dislocations and Mechanical properties of Crystals, Wiley, New York (1957).
11. D. Kiihlmann-Wilsdorf, Trans. Met. Soc. A.I.M.E. 224, 1047 (1962)
12. J.W. Hutchinson, Proc. R. Soc. Lond. A348, 101 (1976).
13. K.W. Neale, L.S. Toth and J.J. Jonas, Int. J. Plasticity 6, 45 (1990).
14. L.S. Toth, K.W. Neale and J.J. Jonas, Proc. R. Soc. Lond. A427, 201 (1990).
15. U.F. Kocks, Metall. Trans. 1, 1121 (1970).
16. M.G. Stout and J.A. O'Rourke, Metall. Trans. 20A, 126 (1989).
17. D.J. Jensen, A.W. Thompson and N. Hansen, Metall. Trans. 20A, 2803 (1989).
WS1C7
FINITE ELEMENT ANALYSIS ON INITIAL AND SUBSEQUENT YIELD
SURFACES OF BCC POLYCRYSTALLINE AGGREGATES

Masaki SHIRATORI* and Toshiro MIYOSHI**

* Department of Mechanical Engineering and

Materials Science, Yokohama National University,
Tokiwadai, Hodogaya-ku, Yokohama, 240 JAPAN
** Department of Precision Machinery Engineering,
University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113
JAPAN

ABSTRACT

At first the elastic-plastic constitutive equations for BCC single crystals

have been formulated. It was assumed that plastic deformation occurred by
slip only. The polycrystalline aggregate was modeled by the assembly of the
finite elements each of which represented a crystal grain with a prescribed
orientation.
The rolling textures have been simulated and it has been found that each
texture has the specific initial and subsequent yield surfaces. Further,
the relation between the texture and the Rankford value has been studied.
It is found that the proposed method is effective to study about the effect
of microscopic mechanism of plasticity on macroscopic deformation.

INTRODUCTION

The authors proposed a method for simulating the elastic and elastic-plastic
behavior of polycrystalline aggregates from that of single crystals by means
of finite element method (Miyamoto et al., 1971). Afterwards, there are
many studies reported about this topics (for example, Gotoh et al., 1985,
and Havlicek et al., 1989), but in most of them the simulations were
carried out about FCC metals because the mechanism of the slip deformation
is more simple. The BCC metals are of much interest from the practical
point. In this paper the authors have studied about the effect of
microscopic slip deformation of BCC metals on the macroscopic elastic-
plastic behaviors by means of the proposed finite element method.

CONSTITUTIVE EQUATIONS

A polycrystalline aggregate consists of crystal grains with its own

crystallograghic orientations. In the proposed finite element model it is
assumed to be an assembly of finite elements each of which represents a
crystal grain. The plastic deformation is assumed to occur only by the slip
of the crystal grain which is described by that of a single crystal with 48
slip systems in the case of the BCC metals. And the slip is assumed to
follow the Schmid's law.

141
142
N N
dx = Hs'(l|dY|) , T g = x c + Hs'(l|dy|) (1)

Another assumption for the work hardening is that

< = H s ' < • \mi+ - v Hs

' < • i*8i+i + KV = 2 (2)

where m: number of the grain, i: number of the slip system, T m and T m :

v
si+ si-
critical shear stress on the slip plane toward and backward the slip
direction respectively.
The latter hardening model is called the type 1 while the former the type 2.
From the above assumption, the constitutive equation is expressed by the
following equations:

{do} = [D ]{de} for elastic elements

D
{do} = [Dp]{de} for plastic elements
where
[De] = [*]T[C][$]
[Dp] = [1»]T[C]([I]-[T]J[™]-1[T]T[C])[$]
[ T M ] r Hs'[S p ] N + [T]N[C][T]J
where [C]: elastic stiffness matrix for the single crystal, [ <J> ]:
transformation matrix of stress and strain components from specimen-fixed
global to grain-fixed local coordinates, [I]: unit matrix, [T]^ : active
components of the matrix [T] which expresses the resolved shear stresses on
the 48 slip systems, Hs'[SP] : matrix which expresses the latent hardening
on the active slip planes.

METHOD OF ANALYSIS

A BCC polycrystalline aggregate has been modeled by an assembly of the

finite elements each of which represents a crystal grain. Fig. 1 shows the
element breakdown. A triangular prism with linear shape functions has been
used as the basic element, each of which represents a crystal grain
with its own three dimensional crystallograghic orientations. Fig. 1
shows that there exists five cubes, composed of a pair of grains, in the x,
y, and z directions, respectively. In order for the aggregate to simulate
the isotropic body or the texture with specific orientations, random numbers
with the specific probabilistic distributions have been initiated to
represent the characteristic orientations in each grain. The
structures simulated are (1) the isotropic body, and (2) the rolling
textures of the low carbon steel. The isotropic body has been modeled by
applying the uniformly random orientations in each grain.
On the other hand the rolling texture of (hkl)[uvw] is modeled by defining
the orientations of each grain in such a way as (hkl) and [uvw] express the
rolling plane and the rolling direction, respectively.
Fig. 2 shows the boundary condition. The normal displacements on the planes
of x=0 and y=0 have been fixed, and the uniform normal loads, LOADX and
LOADY, have been applied to the specimen in the direction of x and y,
respectively, as shown in the figure. The ratio of LOADY/LOADX=tan0 has
been fixed in one elastic-plastic analysis to realize the proportional
loading. By changing the value of 0 from 0° to 360° with each 15° step, one
 143
could obtain the yield surface. The material constants used in the analysis
are as follows:
elastic stiffness: C1U237, C12=141, C44=116 (GPa)
critical resolved shear stress: Tc = 16.7 (MPa)
work hardening rate: Hs f = 137 or 1370 (MPa)
The real value of the work hardening rate of the mild steel is about 137
MPa, but the value of 1370 MPa has also been used in the simulation
in order to demonstrate the effect of the work hardening remarkably.

lYVVVV^ LOADY
NIVIVSr
S <r VVVV VS A\
MNN Vf JS^ A
/ VA W
AA
I N NT UAAAA/
mFr
SLNN \yy AA7
^flfl
\W-
CK /y / /
CK / / / /
LOADX

"U XI iZJ n r i jf

Fig. 1 Finite element model of the Fig. 2 Boundary condition

polycrystalline aggregate

RESULTS OF THE SIMULATION

Cyclic Behavior for Uniaxial Tension-Compression

At first the cyclic stress vs. strain behavior of the polycrystalline

aggregate against the uniaxial tension and compression has been simulated.
An isotropic model of the aggregate has been simulated, and the two types of
the hardening law have been compared. Fig. 3 shows the result of the stress
vs. strain curves when the cyclic tensile strain of 0.1% and compressive
strain of 0.05% has been applied. The stress °x in the vertical axis is
defined by the mean stress, that is, the applied load devided by the area
where the load is applied. The solid and dotted curves in Fig. 3 correspond
to the hardening models type 1 and 2, respectively, assumed in the previous
section. Macroscopically, these two curves seem to express the kinematic
and isotropic hardening behaviors. The result of the simulation shows that
there is good correspondence between the microscopic and the macroscopic
hardening models.

Ox/Tc

1
-° ex<xio-')

HS*= 1370 (MPa)

Fig. 3 Cyclic stress vs. strain curves of the isotropic body
for the two hardening models
144
Initial and Subsequent Yield Surface

The next problem analyzed is that of the initial and subsequent yield
surface. In order to obtain the initial yield surface, the proportional
loading has been applied to the specimen in the manner, explained in the
previous section. The initial yield point is defined as that at which the
maximum resolved shear stress on the slip planes reaches the critical
shear stress Tc for the first time. By rotating the angle 0 of the
proportional loading the yield stresses corresponding to 0 can be obtained,
and they are plotted on the stress 7r-plane. The open circles in Fig. 4
shows the results. In the figure, (a), (b), and (c) show the results of
the isotropic bo»dy (uniformly random model), and the rolling textures of
(111)[211], and (112)[110], respectively. The solid line expresses a circle
with the radius of CJ/T C s 2.0 which is the theoretical curve obtained for
the ideal isotropic body. In Fig. 4(a) it is observed that the simulated
initial yield surface for the isotropic model is nearly on this theoretical
curve. On the other hand Fig. 4(b) and (c) show that each texture has its
own yield surface with the characteristic anisotropy.
The subsequent yield surface has been obtained by the following procedure.
At first the uniaxial tensile load, LOADX, is applied to the specimen until
the strain e x reaches to the prescrived value shown in the figure. The
direction of x corresponds to that of the principal stress Oi/ic in Fig.
4. The load is removed in the next step (unloading), and then, the

Os/Tc
t o e - 0 (%)
|4 A e x =0.02 (%)
| ■ e x =0.05 (%)

Oi/Tc 02/Tc

(a) Isotropic body

(b) Rolling texture of (111)[211] (c) Rolling texture of (U2)[1T0]

Fig. 4 Initial and subsequent yield surfaces on the stress 7r-plane

for the type 2 hardening model
 145
proportional loading is applied in the direction of 0 . In this case the
subsequent yield point is defined as that at which the resolved shear stress
on the slip plane reaches the flow stress Ts on that slip plane for the
first time. Each slip plane has the memory of the flow stress according to
the work hardening law stated in the previous section. The open triangular
and rectangular marks in Fig. 4 show the results of the simulation. These
are the results for the work hardening rate of Hs'= 137 MPa. The results of
the isotropic model, Fig. 4(a), is something curious, although the results
of the rolling texture, Fig. 4(b) and (c), seems to be reasonable. This may
be attributed to the following reasons on the simulation procedure. In the
isotropic model the uniform random numbers are applied to express the
crystallograghic orientations of each grain. The number of grains are not
enough to express the fully isotropic behavior of the polycrystalline
aggregate in the model shown in Fig. 1. Another reason may lie in the
definition of the yielding point. On the macroscopic point of view, the
yielding point should be defined as that at which a large scale slip
deformation starts instead of the definition previously described. Further
investigations are necessary to make clear these points.

Rankford Value of the Rolling Texture

The Rankford value has a close relation to the deformability of the rolled
thin plate in the deep drawing. It is defined by r= e w / e t where e w and
£ are the strains in the directions of width and thickness of the
specimen, respectively. In this section the Rankford values of the rolling
texture have been simulated. _
The rolling textures simulated are those of (111)[110] and (001)[100]. Fig.
5 shows the finite element model and the boundary condition used in the
analysis. The orientation of the rolling direction against the load
direction has been changed from 0° to 180° with every 15° step to simulate
the anisotropic properties of the Rankford values within the rolling plane.
The r-values have been obtained according to the definition of r by applying
uniaxial tensile load to the specimen until the average strain of the
loading direction reaches the prescribed values shown in Fig. 6. Fig. 6
shows the results simulated, that is, the dependence of r-values on the
angle of load direction from the loading direction. The results show that
the distribution of r-values highly depends upon the orientation of the
rolling texture, and that the proposed method is effective to simulate the
r-values_. If we compare the two simulated textures, the rolling texture of
(111)[110] is preferable to that of (001)[100] from the viewpoint of
the deformability in the deep drawing because r is larger than unity for any
angles in the former case while it is less than unity for the latter case.

x
(a) (b)

Fig. 5 (a) Finite element model and (b) boundry condition

for the analysis of Rankford values of rolling textures
146

-i— i - i 1 1 1 1 1 1 1 1 1 i r -i 1 1 11 1 1 1 1 1
10
4 '.fXy-o^cryA P-^-o^o^A (y^-^^r^c^
3
2

0.25
0.5

0.1
o i i i i i i i i i i _i
0.1
o
A /
1
30
1 A
60
1 1
90 120 150 180
30 60 90 120 150 180
Angle from rolling direction (deg.) Angle from rolling direction (deg.)
oe=0.1% A£=0.5%ne=1.0% o e = 0 . 1 % A e=0.5% D e = l . 0 %

(a) (ll"l)[110] texture (b) (001)[100] texture

Fig. 6 Dependence of Rankford values on the angle of

loading direction from the rolling direction

CONCLUSIONS

In this paper the authors have simulated the macroscopic elastic-plastic

behavior of the BCC polycrystalline aggregate based upon the slip
deformation of a single crystal through the proposed finite element method.
The summary of results obtained are as follows:
(1) The macroscopic cyclic hardening behavior against the uniaxial tension
and compression can be simulated well through the microscopic hardening
model.
(2) The initial and the subsequent yield surfaces of the isotropic body and
the rolling texture can be obtained through the analysis.
(3) The Rankford values of the rolling texture can be estimated easily by
the proposed method.
(4) The proposed method is useful to investigate the microscopic mechanism
of plasticity.
Finally the authors would like to express their thanks to Dr. S. Nagashima
and Mr. K. Nagawa for the valuable contributions in writing this paper.

REFERENCES

Gotoh, M., and Tanaka, M. (1985). A Computer Simulation of Elastic-Plastic

Behavior of Thin Metal Plates with Texure by Means of Polycrystalline Plate
Model, Transactions of the JSME, 151, 1098-1106.
Havlicek, F., Tokuda, M., and Hino, S. (1989). Contribution of Finite
Element Method for Understanding Polycrystalline Plasticity, Advances in
Plasticity, Proc. of Plasticity '89, Pergamon Press, 613-616.
Miyamoto, H., Shiratori, M., Miyoshi, T., and Oto, M. (1971). Interpretation
of Mechanical Properties of Metals in Terms of Microstructure, Bulletin of
the JSME, 14, 893-900.
WS1C8

STUDY ON MICRO-MACRO TRANSITION IN POLYCRYSTALLINE PLASTICITY

BY FINITE ELEMENT METHOD

M. TOKUDA and F. HAVLICEK

Department of Mechanical Engineering, Mie University,

Kamihama-cho 1515, 514 Tsu, JAPAN

ABSTRACT
An aim of this research work is to investigate interrelations between the
micro-mechanisms and macroscopic inelastic behaviours of polycrystalline
metallic materials under general loading conditions. The results may give us
the reliable and important background to formulate for engineering applica-
tions inelastic constitutive equations in physically understandable forms.
Based on the mathematical simulations which incorporate basic microscopic
features of plastic deformation as simple and realistic as possible the
finite element model is used to evaluate the polycrystal microscopic and
macroscopic responses to various loading conditions which are represented by
proportional,cyclic, and complex deformations.

KEYWORDS
Polycrystalline plasticity; slip systems; plastic accommodation parameter;
complex loading path; finite element method.

INTRODUCTION
In the present time, it is very difficult to experimentally observe the
inelastic deformation of single grain components embedded in the polycrystal
aggregate, especially, the development of non-uniform stress/strain dis-
tributions accompanied by slip activations in each polycrystal constituent -
the phenomena which are responsible for macroscopic behaviour of polycrys-
tals. Only some experimental techniques limited to the observations of slip
lines which appear on the surface of the multicrystal specimen can provide
partial information on the single crystal activity during polycrystal in-
elastic deformation.

In this research work, the microscopic deformation behaviour of grain com-

ponents in the polycrystal metallic materials was investigated by using a
mathematical model of a polycrystalline aggregate incorporated in the finite
element method. The selected types of loading paths are used including

147
148

proportional, cyclic, and complex (combined loading with the rotation of the
principal stress/strain axes) deformations. The two-straight segments path
with the right angle corner in the deviatoric strain vector space proposed
by Ilyushin (1963) is employed as a typical complex deformation process. In
this paper, based on several computational results obtained, the focus is
put on (1) the slip system development within a grain of the polycrystal
aggregate, representing the microscopic activity of the single crystal
component, (2) the variation of the accommodation parameter, representing
the micro-macro transition, and (3) the integral macroscopic response of the
studied polycrystalline aggregate under the selected loading paths. As the
definition of the accommodation parameter a the following form is accepted

s 4 j = s*j + a G (e*J - e[j) , (i,j=l,2,3), (1)

where s*. and e*^. are the stress deviator and the plastic strain deviator,

respectively, of the grain component, s.. and e^. are the averaged macro-
scopic stress deviator and the plastic strain deviator, respectively, of the
polycrystalline aggregate, and G is the macroscopic elastic shear modulus.
To follow the self-consistent approach, the stress and strain states in the
grains are represented by their averaged uniformly distributed values.
Historically, there are several proposals on the realistic value of the
accommodation parameter a, ranging from 0 to +«>, but which value is suitable
from the engineering application point of view is still uncertain. Using the
definition of a from eq.(l), the physical meaning of this parameter is
expressed through the relation between the microscopic and macroscopic state
variables, and thus is closely related with the interaction mechanism among
crystal grain components. Therefore, in its consequences, this parameter is
associated with the state around yield surface corner which appears at
loading point during polycrystal deformation. It means that this accommoda-
tion parameter is very important to control the localized deformation of
polycrystalline metals (the initial stage of ductile fracture) as well as
the increasing rate of ratcheting strain which is observed in the cyclic
deformation processes under the combined loading conditions.

MATHEMATICAL MODEL OF SINGLE CRYSTAL COMPONENT AND POLYCRYSTAL

The mathematical models of single crystal component and polycrystal are the
same as those used in the previous paper (Havlicek et al., 1990), and thus
only the fundamental ideas are summarized here. As the single crystal model
is concerned, (1) the plastic deformation is caused only by a slip, (2) the
slip is treated by the slip systems which are determined by the crystal-
lographic structure, (3) the activity of the slip system is controlled by
the Schmid law, (4) the critical resolved stress is changed according to the
linearized Taylor-type hardening law, (5) the slip strain-slip stress rela-
tion is selected as the rate-dependent type based on the thermo-activated
motion of dislocations. As the polycrystal model is concerned, additionally
it is assumed that (6) the polycrystal is composed of 23 single crystal
grains whose shapes are regular hexagons as shown in Fig.l and deforms under
the plain strain condition, (7) the orientations of grains are selected to
be distributed randomly in order to preserve the initial isotropy of the
polycrystal model, (8) the grain boundaries are considered to be surfaces of
zero thickness across which the crystallographic structure changes its
 149

orientation. The material constants for each single grain are determined by
considering the pure aluminum (Metal Databook, 1974).

COMPUTATIONAL RESULTS FOR DIFFERENT STRAIN PATHS

According to the Ilyushin's idea, the deviatoric strain vector e is defined

as follows

e = e1nr (1=1,2,... ,5), (2)

where n. are the set of the orthonormal vectors, and

ei/(V2a) = enCOs(/3+7r/6) - e22sin(J3),

e2/(v/2cx) = ei iCos(fi+7T/6) + e22sin(fi),

es/fv^a) = ei2 , e4/(V2a) = e 2 3 , es/U2oc) = e 3 i.

Under the plai n strain condition in which the strain deviator components ei i

Fig.l Polycrystal model composed Fig.2 Strain path in deviatoric

of 23 crystal grain strain vector space
components

and ei2 are given arbitrary and e 3 3 = e 2 3 = e 3 i = 0, e 2 2 = -e ire 33= -e n

and if we select a = V(2/3), fi = TT/6, ei = (2/V3) e n , e3 = (2/V3) ei 2 , e2 =

e4 = e 5 = 0 then,

e = (2/v/3)[ei1ni + e 1 2 n 3 ] . (3)

Therefore, the arbitrary plain strain state can be expressed in terms of the
two-dimensional vector defined by eq.(3), and thus the strain path can be
illustrated by the hodograph of this vector in the two-dimensional vector
150
space of strain (ei,e 3 ). The magnitude of the stress vector |e| equals to
the Mlses-type equivalent strain. The strain paths used for the computation
are represented in the vector space in Fig.2 in which the path 1 is the
proportional deformation along the ei-axis, the path 2 is the cyclic defor-
mation along the ei-axis, the path 3 is the shear deformation along the e 3 -
axis, the path 4 the two-segment strain path with the right angle corner
whose segments are parallel to the ei-axis and the e3-axis, respectively.

The corresponding stress states can be expressed in terms of the following

two-dimensional stress vector

d = V3 [On/2 ri! + 0i 2 n 3 ]. (4)

The magnitude of the stress vector Id I equals to the Mlses-type equivalent

stress. Figure 3 shows the |d| - |e| relation with the variation of the
accommodation parameter obtained by the computations when the polycrystal
model deforms along the ei-axis. The accommodation parameter was estimated

by using the averaged plastic strain eT^ of the representative grain (the
grain with No.12 in the center of the polycrystal model, see Fig.l). Figure
4 shows the development of the slip lines in the representative grain No.12.

Equivalent plastic strain |e^| xlO

Fig.3 Variations of stress and Fig.4 Slip line developments in grain

accommodation parameter for No.12 for proportional
proportional deformation deformation (loading point
numbers correspond to numbers
used in Fig.3)

As it is seen from these two figures, the accommodation parameter decreases

rapidly at the beginning of the deformation, and then, the decreasing rate
becomes much more smaller after the slip lines develop over the whole grain.
In another loading case, Fig.5 shows the stress ^3 d n / 2 - strain (2/V3) e?i
 151
relation and the variation of the accommodation parameter a when the
polycrystal model deforms cyclically along the ei-axis. From this figure, a
= 0.4 - 0.5 may be recommended for the stress analysis for the cyclic
deformation; this value is greater than a for the proportional deformation.
As for the complex loading condition, Fig.6 shows the stress-strain relation
when the polycrystal deforms along the two-segment path with the right angle

Fig.5 Variations of stress and accommodation parameter

for cyclic deformation

Fig.6 Stress-strain relations for Fig.7 Variations of accommodation

shear and complex parameters for shear and
deformations complex deformations

corner (see Fig.2). Namely, it is interesting to point out that the mechani-
cal polycrystal model used here can reproduce the fading memory phenomenon
which has been observed in many experiments.
Figure 7 shows the variations of accommodation parameters for these two
strain paths. As in the proportional deformation, the accommodation
parameter except the small transition region in which the loading path
changes its direction can be treated as constant in the stress analysis even
when the polycrystal is subjected to the complex deformation. On the micro-
scopic level, Figs. 8 and 9 show the slip line developments in the
representative grain No.12 for these two strain paths. Figure 8 provides
152
only their development after the right angle corner of strain path. As seen
from the Fig.8, slip lines continue to develop even though the observed
macroscopic equivalent stress decreases just after the corner. Further with
the increasing plastic deformation these slip systems gradually become
nonactive, and approximately from the state when the macroscopic equivalent
stress starts once again to increase the plastic deformation in the grain
mainly develops on new slip systems corresponding to the pure shear deforma-
tion as it is inferred from comparison of Figs.8 and 9.

Fig.8 Slip line developments in the Fig.9 Slip line developments in the
grain No.12 for the complex grain No.12 for the shear
deformation (loading point deformation (loading point
numbers correspond to numbers correspond to
numbers used in Fig.6) numbers used in Fig.6)

CONCLUDING REMARKS

In this paper, the relation between the micro-mechanisms and macroscopic

deformation of the polycrystal aggregate was discussed on the basis of the
computational results obtained by the finite element model. The several
interesting data not only regarding the microscopic and macroscopic states,
but also their mutual interaction can be acquired for the model polycrystal-
line structure under the proportional, cyclic as well as complex loading
conditions. Generally speaking, this approach can provide an unique informa-
tion on inelastic polycrystal behaviours and their microscopic underlying
phenomena, and therefore can help to construct reliable constitutive equa-
tions.

REFERENCES

Ilyushin,A.A.(1963).Plasticity, Foundation of General Plastic Theory,

Izdat.Akad.Nauk,Moscow
Metal Databook (1973). Japan Society of Metals, Maruzen Publishing Co., Tokyo
[in Japanese].
Havlicek,F.,J.Kratochvil,M.Tokuda,V.Lev (1990).Finite element model of
plastically deformed multicrystal.Int.J.Plasticity, 6, 281-292.
 WS1c9

COMPUTER SIMULATION OF THE EFFECT OF GRAIN SIZE ON THE PROPERTIES OF

POLYCRYSTALLINE SPECIMENS BY FINITE ELEMENT METHOD

C. WEI*, R. G. QIAN**, S. LIN*, and J. M. XIAO*

* Department of Materials Physics, ** Department of Mathematics and

Mechanics, University of Science and Technology Beijing,
Beijing 100083, The People's Republic of China

ABSTRACT

The effects of grain size and strain on the flow stress of polycrystalline
are simulately calculated by using crystal elasto-plastic finite element
method in this paper. The stress distributions in the crystallines with
different grain sizes are given. The present calculated results are in
aggrement with that calculated by the Hall-Petch formula and related
experimental ones.

KEYWORDS

Polycrystalline, grain size, mechanical properties, crystal elasto-plastic

finite element, computer simulation.

INTRODUCTION

Polycrystals consisted of grains which due to a mutual interaction

process, cannot deform freely during deformation process. Higher stresses
are therefore required to deform polycrystals than are needed for isolated
single crystals that can deform by glide on a single slip system. This
polycrystalline strengthening connects to macroseopic deformation process
which normally are considered to be independent of the grain size. Beyond
this an additional factor affecting the strengthening of polycrystals is
that of the size of the grains. This grain—size dependent contribution to
the strength is demonstrated by the well-known experimental observation
that the low temperature strength of polycrystalline specimens normally
increases when grain size decreases.

A major part of the theoretical and experimental work in this field in the
last 50 years has concentrated on the macroscopic deformation of
polycrystalline specimens with the main aim of understanding strain-stress
relationship and the texture development during cold deformation. But in
the last 20 years much attention has been paid to the effect of grain size
on the yield stress and the flow stress of polycrystalline specimens. An

153
154
important part of this work has been to interpret empirical strength—
grain size relationship on the basis of the microstructural observation of
the surface and the bulk behavior. The strength of polycrystalline
specimens can be related to interaction phenomena, which is in terms of
macroscopic and microscopic strain accommodation processes required to
maintain strain continuity across the grain boundary, taking place during
elastic and plastic deformation. A number of empirical equations of the
strength-grain size relationship have been proposed(Petch, 1953, Meakin
and Petch, 1963, Thompson and Baskes, 1973, Kocks, 1970). The structural
information in the equations is obtained mainly from surface relief
patterns and from bulk structures observed by transmission electron
microscope of thin foils.

This paper deals with the computer simulation of strength—grain size

relationship by calculating model and crystal elasto-plastic finite
element method proposed by Wei et al.(1984). By this method, which is
different from traditional experimental methods, will become more possible
to discover the whole process during the deformation of polycrystals and
the strengthening function of grain size.

THE SPECIMENS FOR CALCULATION

The geometry of polycrystalline specimen is a plate of 2.7mm in width, 1mm

in length and 0.1mm in thickness, as shown in Figure 1. Three crystallo-
graphphic orientations of the grain among polycrystals are illustrated in
Figure 2. The polycrystalline specimen consists of grains which have a
periodic arrangement of three orientations shown in Figure 2. Five
specimens with the grain sizes of, respectively, &.05, 0.1, 0.15, 0.3 and
0.45mm were used in calculation. The load condition is tensile along the
specimen axis(constant displacement tensility). In order to simulate the
deformation processes by crystal elasto-plastic finite elememt, the
specimen is divided into 320 elements of triangular prim mesh with six
nodes. The elastic moduli Cu = 108200MPa, C/2.=61300MPa, C22=28500MPa, and
the slip shear moduli Gi =15MPa (for one active slip system), Gjt=100MPa(for
one more active slip system) of aluminum were chosen. At IBM-PC/AT
computer, the executing time of the program was about twenty minutes for
one load step.

THE CALCULATED RESULTS

The results of computer simulation are as follows:

Figure 3 gives the tensile stress-strain curves of three single crystals

oriented as in Figure 2 and their cooresponding polycrystals with
different grain size. The curves for polycrystals are within those for the
single crystals. The curve of the single crystal with a favourable
orientation is the highest. Because of the presence of grain boundary in
the polycrystals, their curves become more complicated. The complexity is
corresponding to the complexity of slip processes during the plastic
deformation.

Figure 4 gives the curves of the true tensile stress versus the grain size
dl/a- at different true strain, simulated by computer. From Figure 4 it is
found that the true stress is linear with the grain size. The calculated
results are in agreement with that calculated by the Hall-Petch formula
and related experimental ones(Al-Haidary etal., 1983). The slope of 6—d^
 155
curves varies with the strain. It is clearly known that the work-hardening
processes during the polycrystal deformaton play an important role in
strengthening of polycrystals. Because of the contribution of the work-
hardening rate, the strength difference between polycrystals with
different grain size increases with the true strain when the strain is
from 0.002 to 0.02, but this difference decreases when the strain is
larger than 0.02.

The polycrystalline specimens are far from homogenous. Figures 5 and 6

give, respectively, the distributions of the stress in the direction of
the tensile axis and the hydrostatic stress in the cross section of the
polycrystalline specimens. It is shown that the boundary makes the stress
sharply up or down near the boundary dependent on the orientation of the
grains and the orientation difference between the adjacent grains in the
polycrystalline specimens. Because of the periodic arrangement of the
grains in the polycrystalline specimens, the stress distributions are also
periodical. The amplitude of stress in tensile direction is larger than
that of hydrostatic stress.

CONCLUSIONS

The effect of grain size on strength of polycrystalline specimen is

simulated. The results are in good agreement with the Hall-Petch formula
and experimental data.

The slope of 6—d** curves varies with the true strain in the case of
small strain. The slope at larger strain is larger than that at small
strain because of the contribution of strain hardening.

The prescence of grain boundary makes the stress markedly up or down

depenpent on the orientation of grains and the orientation difference
between adjacent grains in polycrystals. the smaller the grain size is,
the more homogeneous the distribution of stress in polycrystalline
specimen is.

REFERENCES

Al-Haidary, J.T., Petch, N.T., et al.(1983). Phil. Mag., 47, 8 % .

Kocks, U.F.O970). Matell. Trans., 1, 1121.
Meakin, J. and Petch, N.J.0963). Report ASD-TDR-63-324, U.S Air Force W-P
AFB, OH, 243.
Petch, N.J.U953). J. Iron Steel Inst.. 174, 25.
Thompsom, A.W., Baskes, M.I. & Flanagan, W.F.U973). Acta Metal. 21, 1017.
Wei, C , Qian, R.G., Lin, S. et al.(1984). Acta Mech. Solid Sinica, 2, 375.
156

h- — z' j tniH,— ta-

t

IT
/
'i f / ( f ./ (

li
A B C A B c

1 ,vm
T

Fig.l Polycrystalline specimen Fig.2 Orientation of grains

2-r f

2-0 f

1.5 f

1° i

stmirt'o"4;

Pig.3 Stress-strain curves

 157

4
uS 4i 6

Fig.4 Plot of flow stress 6 vs grain size d

(calculated values)

<?0|
strain
o.a
"•" o.\y
% — •
■
0.06

%—o
yt*\t

(ipliimj*

Fig .5 Plot of flow stress <S vs grain size d

(experimental values)
158

|5 StfWSCMPoJ [3 5treSSCMftt)

1 l
If
r*<N

1
1 '
<
'i 1
■K/w,A\ r'-iM
w \t\ W
\Z
V/v II »

■i ii 1111111■ 1 1 • 1 1 1 ■ i • i > - • ■ ■ 1 1 1 1 ■ i ■ 1 1 1 1 1 1 1 ■ • ■ > > ■ i ' > 1 1 1 1 1 * II

j
II I II I III II III M M l Itll H U H ||| l|| I ||| || |l| 11 |||||
'2 \<j 24- JO 4% 53f O 6
42 II 1$ 24 30 3f> 42 48 54
d sa o. 45mm.
A = o.fo m*t

Fig.6 Distribution of tensile stresses with various

grain sizes(d-0.45, O.lOmm)

stress CMfti)
itfre«CMP»>

***!
M
M, l4 V
ikKJ .
WH
I I M I l H i l l H i l l l II l | | | 11|| i H i | i l l n i l || | M | | | | i f I I M < | I I M I I I I I 11 I 11 M I 11 | I I | 111 11 M I I I I
IJIIIIIIMIM
\2 fe & 30 3b 42 6 tt T$ 2<t 30 $6
J c r 0.4JT HI*.

Fig.7 Distribution of hydrostatic stresses with various

grain sizes (d=0.45, O.lOmm)
WS1d1

TRANSFORMATION PLASTICITY AND ITS

APPLICATION TO CERAMICS TOUGHENING

HWANG Keh-Chih SUN Qing-Ping *

Department of Engineering Mechanics,

* Department of Materials Science and Engineering,
Tsinghua University, Beijing 100084, P.R. China.

ABSTRACT

A constitutive Model of transformation plasticity is suggested based on micromechanics and

thermodynamics consideration. The model takes into account both the dilatation and shear effects
of phase transformation, and is capable of describing the plastic, pseudoelastic and shape memory
behavior of structural ceramics during transformation under different temperatures. The
constitutive element used, taken as a representative material sample, contains transformed grains or
precipitates, as second phase inclusions embedded in an elastic untransformed matrix. Under some
reasonable basic assumptions, the expressions of free energy are derived in a self-consistent manner
by use of Mori-Tanaka's method, taking account of the interaction between the transformed inclu-
sions. In the framework of Hill-Rice's constitutive theory with internal variables, the transforma-
tion criteria and incremental stress strain relations are derived. Theoretical predictions of the sug-
gested constitutive relations are compared with the available experimental data of Mg-PSZ and
Ce-TZP polycrystalline ceramics, and good agreement is obtained between theory and
experiments. Moreover, the constitutive relations are used to predict toughening effect of transfor-
mation for ceramics and lead to excellent coincidence with experiments.

KEYWORDS

Transformation plasticity; ceramics toughening; internal variables; constitutive model.

INTRODUCTION

A comprehensive understanding of the constitutive behavior of transformation toughened ceramics

has essential importance in the explanation of toughening phenomena and in stress strain calcula-

159
160

tion of ceramics structures. Since the fundamental work on transformation toughening (McMeek-
ing et al., 1982, Budiansky et al., 1983), most of the research work on this subject is concerntrated
on how to take the transformation shear effect into account properly in the constitutive description
(Lambropoulos, 1986, Chen et al., 1986, Reyes-Morel et al., 1988a,b). Although some new scientif-
ic findings in those works helped us get more insight into the physical nature of the transformation
plasticity, there are obvious shortcomings (Sun et al., 1990). So reconsidering the desciption of
transformation constitutive behavior in a new approach becomes necessary. The aim of this paper
is to give a continuum description of the plastic and pseudoelastic behavior during forward and re-
verse transformation by a micromechanics and thermodynamics method. The results are finally
discussed and compared with experimental data of PSZ and TZP ceramics.

MICROMECHANICS CONSTITUTIVE RELATIONS

Microstructure of the Constitutive Element and Basic Assumptions

For the martensitic transformation of partially stabilized zirconia (PSZ) and tetragonal zirconia
polycrystal (TZP) ceramics considered in this paper, the constitutive element consists of a great
number of untransformed t-Zr0 2 or c—Zr02 grains (as the matrix) and the transformed
m-Zr0 2 grains as dispersed second phase inclusions of volume fraction f embedded coherently in
the elastic matrix. The temperature 6 is uniformly distributed in the element and the external
macroscopic stress (£) or strain (E) is applied on the boundary. In the macroscopic plastic
deformation process accompanying transformation the material sample experiences a
microstructure evolution, the volume fraction f changes and each transforming particle experience
a chemical free energy change, surface energy change and a stress-free transformation strain e".
The microscopic stress, strain and the volume of the matrix and inclusions are denoted by <T,E,V
and V;, respectively. The elastic compliance tensor of the matrix is assumed to be equal to that
of the particles, and so is equal to the macroscopic overall elastic compliance tensor M of the ele-
ment. The transformation strain s," is composed of volumetric and deviatoric parts z and z9* ,
where e is the constant lattice volume dilation during t-^m transformation (i.e., e = £ d(.)t
whereas B* , because of its strong deviatoric stress-biased feature (Chen et al., 1986, Reyes-Morel
et al., 1988 a,b, Sun, 1989), is assumed to depend on the average deviatoric stress s in the matrix
by
£=As"/cM (1)

where a = (-s s ) * , A is a material constant and can be considered as a measure of the con-
straint of the elastic matrix and the effect of twinning. By using the self—consitent Mori-Tanaka
method (Mura, 1982, Mori and Tanaka, 1973, Sun et al., 1990), the s can be calculated accord-
ing to

where < > represents volume average, J?1 = 2JJ(5V — 7)/(15(1 — v)),and n,v are elastic shear
 161
modulus and Poisson's ratio.

Free Energy of the Constitutive Element

In this section, we first derive the elastic strain energy of the constitutive element and then give ex-
pressions for the change in chemical free energy and surface energy and the energy dissipation dur-
ing transformation. Finally we formulate the expression of complementary free energy. For simplic-
ity, we assume that the transformed particles are equal sized spheroids.

Elastic Strain Energy. Taking into account the interaction between the inclusions by Eshelby's so-
lution (Eshelby, 1957) and Mori-Tanaka method (Mori and Tanak, 1973, Sun et aL, 1990), we
finally abtain the elastic strain energy W of the constitutive element per unit volume

w-5Vfwsu-/iv«,/3+3*1<«'V/2 i+i/w,<«:>,,<«:>,,
+ 3B 2 (£") 2 ] (3)
where B = K(4v — 2) / (1 — v), K is the elastic bulk modulus.

Chemical Free Energy and Surface Energy. The total change in chemical free energy per unit vol-
ume of the element is

Where G (0) and G (0) are chemical free energy of m and t phase, respectively. The total change
in surface energy is
A = A / = 6y f/ a (5)
where a is the diameter of the grain and y is the surface energy change per unit area (y = y
o p p m
-7.).

Energy Dissipation During Transformation. Because the transformation in PSZ and TZP are
thermoelastic in nature (Reyes-Morel et al., 1988a,b), the forward and reverse transformations by
motion of the t-m interfaces are usually to meet the resistance of the lattice friction and thus cause
energy dissipation, which will result macroscopically in the stress hysteresis between forward and
reverse transformation. Through the limitted amount of experimental data analysis and for simplic-
ity of mathematical treatment, we tentatively assume that the total energy dissipation W per unit
volume is proportional to the cumulated volume fraction / ( = J \df\) of transformation in the
whole deformation history, thus we have
W=Df (6)
where D is a microstructure-dependent material constant.

Complementary Free Energy of the constitutive Element. From Eqs.(3),(4) and (5) we can formu-
late the expression of the complementary free energy \J/ of the constitutive element per unit volume
162

by

-\f\fy«rv> r,<^> r^^y^-AJ-^G^m (7)

Thus, from the thermodynamics internal variable constitutive theory (Rice, 1971, 1975), it is clear
that the thermodynamic state of the constitutive element is completely defined by the variables
E ,Gyf and < z". > , in which f and < e!" > are obviously the internal variables describing
1/ 1/ Vj 1/ V |

the microstructure change of the material during transformation, that is, the dependence of the ma-
terial response on loading history can be replaced by a dependence on the current values of internal
variables.

Constitutive Law for Non-proportional Loading

When transformation proceeds (/V 0), the second law of thermodynamics requires (denoting time
rated( ) / d t b y ( ))

a v,
Substituting Eq.(6) into (8) andusing relation

and eliminating f, we obtain the forward and reverse transformation yielding functions F and F ,
respectively
F/(£/;/,0,<<>K/) = | ^ ( 5 ( ; - / B 1 < < ; > K ( ) + 3^(rm-/B/i)-Co(fl) = O (10)

where C o(0) = D o + A Q + AG ,^m(9) + 1,

C,(fl)-C#(e)-2/)#,?I= -5^2/3-3S2(«")2/2
The incremental stress—strain relations for forward transformation, for example, can be readily ob-
tained by the usual routine of internal variable constitutive theory (Rice, 1971,1975)
E =E' + EP
B\J/ • d^f . 9\\/
~ ~ -S„ + * j+ <«' > „ (11)
•i */ // ' B2. 9<e >

'"^w +fc'X+ ^ / O
where / can be determined by the consitency condition F = 0.

DISCUSSION AND CONCLUSIONS

 163

Macroscopic Yielding Character of the Material

Based primarily on the energy changes that accompany transformation the macroscopic
constitutive relations of materials are derived by a micromechanics and thermodynamics internal
variable approach, providing the role of microstructure, temperature etc. in the macroscopic plastic
behaviors. Because both the shear and dilatant effect of transformation strain are taken into ac-
count, the derived yielding condition has the characteristic of pressure sensitivity which agrees with
experimental observations (Chen et al., 1986). From Eq.(lO) we can see that the certer of the yield-
ing surface moves with the average residual stress in the matrix (<a'>v — — fB < B1" >
1/ U ' I

— fB2eP S ). Because B x andJ?2 are negative, the material will exhibit a softening response since
Co(0) is independent off. However, the published experimental stress-strain curve showed a hard-
ening rather than softening response. Thus, to describe the hardening phenomena, a simple method
is to assume that C increases linearly with f. Replacing C (6) by C (0,/) — C (0)+ <xB (eP ) /
, where Bo = 4/i(l + v) / (1 - v) + nh\{2% - 20v) / (5(1 - v)),hQ =A/ 3s",then the yielding will
have the characteristic of both kinematical and isotropic hardening, that is, under uniaxial stress
the material may exhibit hardening or softening depending upon the values of B l yB 2 and a.

Comparison with Experiments

In the present, only experimental data under uniaxial compression is available. Under such propor-
tional loadings the constitutive law of Eqs.(lO) and (11) are greatly simplified. Then, taking
hg = 1.4, a = 1.16 for TZP and/j o = 1.3, a = 1.2 for PSZ, the theoretical predictions of Eqs.(l),
(10), and (11) agree well with the experiments (Sun, 1989, Sun et al.,, 1990). Moreover, the present
model is used to predict the toughening effect of PSZ and TZP, and good agreement is also
found(Sun, 1989).

Description of Pseudoelasticity and Shape Memory Effect

Martensitic transformations can be induced by the application of stress as well as by changes in

temperature. This interchangeability of temperature and stress as state variables affecting the trans-
formation is clearly reflected in the present model. The transformation stress (Eq.(10)), through de-
pendence on AG i_tm depends on temperature 0. This character of dependence on temperature
makes the forward transformation stress increase with temperature and, at a given value of D , the
stress-strain relation exhibits conventional plasticity at low temperatures and pseudoelasticity at
high temperatures (Reyes-Morel et al, 1988a, b). Thus the present model can also by used to des-
cribe the pseudoelastic and shape mamory behavior which is typical of thermoelastic martensitic
transformations.
164

REFERENCES

Budiansky, B., J.W.Hutchinson and J.C.Lambropoulos (1983). Continuum theory of dilatant

transformation toughening in ceramics. Int. J. Solids Struct., \% 337-355.
Chen, I.W. and P.E. Reyes-Morel (1986). Implications of transformation plasticity in Zr0 2 -con-
taining ceramics: I, shear and dilatation effects. J. Am. Ceram. Soc, 69,181-189.
Eshelby, J. D. (1957). Determination of the elastic field of an ellipsoidal inclusion and the related
problems. Proc. R. Soc, London, A, 241, 376-396.
Lambropoulos, C. (1986). Shear, shape and orientation effects in transformation toughening. Int.
J. Solid Struct., 22,1083-1106.
McMeeking, R. and A.G. Evans (1982). Mechanisms of transformation toughening in brittle mate-
rials. J. Am. Ceram. Soc, 65, 242-246.
Mori, T. and K. Tanaka (1973). Average stress in matrix and average elastic energy of materials
with misfitting inclusions. Acta metall., 21^, 571-574.
Mura, T. (1989). Micromechanics of Defects in Solids. Martinus Nijhoff, The Hague.
Rice, J.R. (1971). Inelastic constitutive relations for solids: An internal-variable theory and its ap-
plication to metal plasticity. / . Mech. Phys. Solids, \% 433-455.
Rice, J.R. (1975). Continuum mechanics and thermodynamics of plasticity in relation to microscale
deformation mechanisms. In: Constitutive Equations in Plasticity (A.S. Argon, ed.), pp.23-79.
MIT Press, Cambridge, MA.
Reyes-Morel. P.E. and I.W. Chen (1988a). Transformation plasticity of Ce02-stabilized
tetragonal zirconia polycrystals: I, stress assistance and autocatalysis. J. Am. Ceram. Soc, 71^,
343-353.
Reyes-Morel. P.E., J.S. Cherng and I.W. Chen (1988b). Transformation plasticity of Ce0 2 -stabi-
lized tetragonal zirconia polycrystals: II , Pseudoelasticity and shape memory effect. J. Am.
Ceram. Soc, 71_, 648-657.
Sun, Q. P. (1989). Micromechanics constitutive theory of transformation plasticity and toughening
analysis of ceramics. Ph.D. Thesis, Department of Engineering Mechamics, Tsinghua University,
Beijing, China.
Sun, Q.P., K.C. Hwang and S.W.Yu (1990). A micromechanics constitutive model of transforma-
tion plasticity with shear and dilatation effect, to appear in J. Mech. Phys. Solids.
WS1d2

FINITE ELEMENT CALCULATION OF THE MICROMECHANICS

OF A DIFFUSIONAL TRANSFORMATION

J.F. GANGHOFFER*, S. DENIS*, E. GAUTIER*. A. SIMON* and S. SJOSTROM**

* Laboratoire de Science et Genie des Materiaux Metalliques CNRS UA 159,
Ecole des Mines, Pare de Saurupt, 54042 NANCY Cedex, FRANCE
** Department of Mechanical Engineering, Linkoping University,
58183 LINKOPING, SWEDEN

ABSTRACT

A micromechanical model for diffusional transformations has been

developped. We use two different descriptions of the transformation, namely
a spherical growth of nuclei of the new phase and a random progression
model. An external stress state is applied to the unit cell (3D F.E. mesh),
resulting in a transformation plastic strain, the evolution of which we
study versus the progress of the transformation.

KEYWORDS

MICROMECHANICS, PHASE TRANSFORMATIONS, FINITE ELEMENT MODELS,

TRANSFORMATION PLASTICITY.

INTRODUCTION

In the present work we study the mechanical behaviour of a material

submitted to an external stress state on a microscopic scale (the scale of
the phases) and determine as a main result the evolution of the induced
transformation plastic strain (transformation plasticity).
The occurence of transformation plasticity can be explained by two basic
mechanisms (Gautier et al., 1987), i.e. i) orientation of the product phase
by the stress state and ii) anisotropic plastic accommodation of
transformation strains.
We have undertaken finite element simulations on one hand for a
transformation occuring with nucleation and growth for which only mechanism
ii) needs to be considered (Sjbstrbm et al. 1989) and on the other hand for
a martensitic transformation where mechanism i) has also to be considered
(Simonsson et al., 1990). In this paper, we focus on the results obtained
in the case of a diffusional transformation (austenite -► pearlite).

MICROMECHANICAL MODEL OF A DIFFUSIONAL TRANSFORMATION

The model has been described by Sjbstrbm et al., 1989. The unit cell is a
3D cubic finite element mesh of a volume element in which the
transformation will develop. The cube is submitted to an external load
during the progress of the transformation. The transformation strain is
165
166
isotropic. We describe the transformation progress by letting successive
elements transform, changing thereby their specific volume and mechanical
properties. The transformation progress is described in two different ways
corresponding to two different scales of modelling i) a spherical growth
transformation and ii) a random progress of the transformation.
i) It corresponds to an initially regular pattern of pearlite nuclei within
the material. All nodules have nucleated at the same time and continue to
grow simultaneously at the same rate. The transformation starts in the
center of the cube and spreads, by letting the layer of surrounding
elements transform at each transformation step, simulating by this an
increase of nodule radius. The boundary conditions used are : the octant
symmetry due to spherical growth, and rectangularity of the cell simulating
the presence of neighbouring cells. We have used linear mesh subdivisions
and three mesh sizes: 4x4x4, 6x6x6 and 10x10x10 elements.
ii) In this case there is no marked division of the transformation into a
first nucleation phase and a second growth phase : new particles are formed
during the whole transformation process in a completely random manner. The
pearlite particles are represented in the model in their final size state.
Each transformation step corresponds to the transformation of one element.
(the unit cell represents the whole specimen). Most of the runs have been
done with the same boundary conditions as in case i). We performed also a
run with free boundaries. Calculations have been done for both 4x4x4 and
6x6x6 meshes, leading to 64 and 216 transformation steps respectively.

DESCRIPTION OF THE RUNS

The F.E. code used for the calculations is ASKA. Most of the runs have been
done on the CRAY-XMP 48 computer at the Swedish National Supercomputer
Center in Linkoping.
The external loading is applied at first, before the transformation starts.
At each transformation step, the total strain over the unit cell will be
defined as the displacements of the faces divided by the cube length. The
total strain eij can then be decomposed into its different contributions :
. . e, ex c.. . tr, 1 . .. tp ,_x
eij = eij + v6ije + eij , (1)
where eij ' is the elastic strain due to external loading
tr 1
e ' is the isotropic transformation strain for a completed
transformation
v is the volumic transformed fraction
eij is the transformation plastic strain, i.e. the transformation
plasticity deformation.
From equation (1), the transformation plastic strain can be computed after
each transformation step. The runs performed are listed in Table 1.
The case we model corresponds to an isothermal pearlitic transformation of
an eutectoid steel at 673°C. The calculations have been performed with an
elastoplastic material model, using linear isotropic hardening. Yield
strengths (25 MPa for austenite, 110 MPa for pearlite) and hardening
constants (3800 MPa and 8300 MPa respectively) have been measured for the
-5 -1
deformation rate of 2x10 s . The transformation strain measured by
tr 1 -3
dilatometry is e ' = 1.2 x 10
We present here only the results for an uniaxial external stress state
(CK, = 20 MPa).
 167
Table 1. Identification of the runs

Run number Run Code Type of model Bound. Cond. Mesh Mech. Prop
1 Sp41200b Sph symm 4x4x4 beg*
2 Sp61200b Sph symm 6x6x6 beg
3 Sp61200e Sph symm 6x6x6 end*
4 Spl01200b Sph symm 10x10x10 beg
5 Sp61200S Sph symm 6x6x6 -
6 Spl01200S Sph symm 10x10x10 -
7 Spl01200e Sph symm 10x10x10 end
8 rs41200b ran symm 4x4x4 beg
9 rs61200b ran symm 6x6x6 beg
10 rf61200b ran free 6x6x6 beg
11 rs61200e ran symm 6x6x6 end
* Mechanical properties given either at the beginning ('beg') or at the end
('end') of the transformation step.

RESULTS AND DISCUSSION

From the F.E. calculations, we have chosen to show at the present time only
the transformation plastic strain versus the progress of the
transformation. We will point out : the influence of the size of the mesh
i.e transformation step, the influence of the way the change in mechanical
properties is imposed, the influence of boundary conditions. In last part
we shall analyse the influence of the transformation progress description
and compare our results with experimental results.

Spherical growth model

Influence of transformation step

A comparison between runs 1,2,4 (4x4x4, 6x6x6 and 10x10x10 subdivisions,

mechanical properties given at the beginning of the transformation step)
shows that the influence of the size of the mesh is quite large (fig. la).
At the very beginning of the transformation, the initial slope is similar
for the three runs ; this is due to the very small size of the first
transformation step (the largest is for the 4x4x4 subdivision and is about
1.56%). Considering the behaviour in the last steps, the slope is quite
near zero for the 4x4x4 mesh but increases with the size of the mesh.

0,0 0,2 0,4 0,6 0,8 1,0 0,0 0,2 0,4 0,6 0,8 1,0
transformed fraction transformed fraction
tP/
Fig. 1. ba e 11 (vj for Sp41200b (run 1
for Sp61200s (run 5
Sp61200b (run 2} Spl01200b (run 4)
Spl01200s (run 6 ) .
168
This is related to two depending factors : the large amount of phase
transformed in the last step and the allocation of the mechanical
properties at the beginning of the step. For the 4x4x4 mesh, the high
mechanical properties of the new phase (hard pearlite) are given to the
remaining austenitic elements representing about 42 % (volumic fraction),
leading to very small plastic deformations. This effect lowers when the
size of the mesh increases, since the last transformation step decreases
also at the same time. Since the size of the mesh determines both the
finite element discretization error and the size of the transformation
step, we have separated both effects by prescribing same mechanical
properties to both phases. Results of runs 5 (6x6x6 mesh) and 6(10x10x10
mesh) (fig. lb) are quite identical, so we can conclude that pratically no
influence of F.E. discretization occurs in this case.

Influence of the way of imposing mechanical properties

The comparison between runs 2 and 3 (fig. 2) shows that imposing the change
of mechanical properties at the end of the transformation step leads to
much higher values of the transformation plastic strain than changing the
mechanical properties at the beginning of the step. As expected, the
difference between the 'beg' and 'end' cases becomes less important for the
finer mesh as can be evidenced from runs 4 and 7 (fig. 2 ) .

transformed fraction
Fig. 2. eiS(v) for Sp61200b (run 2), Sp61200e (run 3)
Spl01200b (run 4), Spl01200e (run 7)

To reduce such mesh influence in a very significant way, it should be

necessary to make calculations with very much finer meshes. Maintaining
step size less than 5 % would require a 59x59x59 finite element mesh which
is quite prohibitive from the point of view of computer processing time.

Random progression model

Influence of the transformation step

The comparison between runs 8 and 9 (fig. 3a) shows that the influence of
the transformation step, even if it is not negligible, is much smaller than
for the spherical model. This is mostly due to the transformation step
which is constant for a given size of the mesh and small (1.56 % and 0.46 %
for the 4x4x4 and 6x6x6 mesh respectively). There is only a deviation
between both curves at the end of the transformation (7.8 % ) .
 transformed fraction transformed fraction
Fig. 3a £i?(v) for rs41200b (run 8), rs61200b (run 9)
b etp(v) for rs61200b (run 9), rs61200e (run 11)
11
Besides the effect of the step, these results include also the effect of
the transformation order. In order to evaluate the influence of the order,
calculations have been performed with two different random sequences in the
case of a 4x4x4 mesh. They lead to a maximum difference of 3.3 % in the
transformation plastic strain during the transformation.

Influence of the way of imposing mechanical properties

The influence of the mechanical properties allocation is given on fig. 3b

by the comparison of runs 9 and 11. At the beginning of the transformation
this influence is small. As for the spherical model, the results of case
'end' lie above those of case 'beg'. As the transformation progresses, the
deviation between the curves is progressively reduced and tends to reverse.
Some finer analysis on internal stress states and local plastic strains are
necessary in order to explain that behaviour.

Influence of boundary conditions

Quite small difference appears between runs with symmetry and free face
boundary conditions as evidenced by comparing runs 9 and 10 (fig. 4 ) . One
can then conclude that randomness is represented in a correct and
sufficient manner.

Comparison between models and experiment

Fig. 5 shows a comparison between the results obtained for the spherical
model and those obtained for the random model. For the spherical model, we
have represented the two cases : run 4 (properties given at the beginning
of the step) and run 7 (properties given at the end). For the random model
we have used the result of run 11 (properties given at the end). A
relatively good agreement between the two types of models is observed. If
we consider that further calculations with finer meshes would probably
decrease the influence of mechanical properties allocation, we can conclude
that both models, even using a different original representation of the
transformation (at different scales) should represent the same macroscopic
behaviour. At last, the comparison between our calculated results and the
experimental data (fig. 5) shows acceptable values of the transformation
170
plastic strain till 30 % of transformation. But the slopes of the curves
are quite different : experimental results show a near linear variation.

0,0 0,2 0,4 0,6 0,8 1,0 0,0 0,2 0,4 0,6 0,8 1,0
transformed fraction transformed fraction
Fig. 4. eif(v) for rs61200b (run9) Fig. 5. eigv) for Spl01200b (run4)
and rf61200b (runlO) Spl01200e (run7) rf61200b
(runll) and experiment

CONCLUSIONS

From the results obtained by these F.E. calculations, we can draw the
following conclusions :
- The spherical growth model still presents a noticeable influence of the
size of the transformation step.
- The random progression model is satisfactory since a less marked effect
of transformation step, mechanical properties allocation and boundary
conditions occurs. It shows a good agreement with the present results of
the spherical growth model.
- The functional dependence of e with the volume fraction of pearlite is
non linear in all cases. This seems reasonable since the plastic strain
hardening effect opposes to linearity.
A better understanding of the differences between calculated and
experimental behaviour involves the study of plastic zones evolution and
development of local stresses during the transformation. Moreover, a recent
result of the simulation, considering the same mechanical properties of
both phases, shows an evolution of transformation plasticity close to
linearity. This can lead to a different modelling of the mechanical
behaviour of the phases that takes into account a contribution of creep.

REFERENCES

GAUTIER, E. and A. SIMON (1987). Transformation plasticity mechanisms for

martensitic transformation of ferrous alloys. In : Phase Transformations'87
(GW Lorimer, ed.), pp. 285-287. The Institute of Metals, London.
SIM0NSS0N, K., S. SJ0STR0M, J.F. GANGH0FFER, S. DENIS, E. GAUTIER, A. SIMON
(1990). On the mechanical description of martensitic transformation using
continuum mechanics FE calculations. In : European Mechanics Colloquium
263. Vienna Austria.
SJ0STR0M, S., S. DENIS, E. GAUTIER, A. SIMON (1989). FEM Calculation of the
micromechanics of a diffusional transformation. In : International
Conference on Residual Stresses (G. BECK, S. DENIS, A. SIMON ed.), pp.
416-423. Elsevier Applied Science, London and New-York.
WS1d3

D E S I G N OF MATERIAL LAWS FOR N A T U R A L A N D ARTIFICIAL

M U L T I P H A S E MATERIALS
BY MICROMECHANICAL CONCEPTS

H.J.BOHM 1 , F.G.RAMMERSTORFER 1 and F.D.FISCHER 2

1
Institute of Light Weight Structures, Vienna Technical University,
Gufihausstr. 27-29, A-1040 Vienna, Austria
2
Institute of Mechanics, University of Mining and Metallurgy,
Franz Josef Str. 18, A-8700 Leoben, Austria

ABSTRACT

A semianalytical micromechanical approach is used for arriving at macroscopic material

descriptions for phase transforming materials. Some aspects of the overall behavior of
long fiber reinforced metal matrix composites are investigated by computational mi-
cromechanics.

KEYWORDS

Micromechanics; phase transformations; multiphase materials; metal matrix compos-

ites.

PHASE TRANSFORMING MATERIALS

Phase transforming materials play an important role in many technical applications,

among them the quenching of steel components, the toughening of ceramics by Zr02
and the shape memory eflFect displayed by certain alloys. In materials undergoing a
phase transformation both a parent phase and one or more product phases are present,
which may share the same chemical composition but differ in their microstructure, their
volume and, in the case of martensitic transformations, their shape. The interaction
between the microregions occupied by the these phases gives rise to microstresses which
can influence the overall behavior of the material. The macroscale stress-strain relations
of such phase transforming materials take the form

a = E : £el = E : (etotal — Ctherm — Cplast — Ccreep ~ ^TRIP) , (l)

where STRIP stands for the macroscopic transformation-induced strains. The main
emphasis in the present chapter lies on the evaluation of this transformation term, a
micromechanical approach being followed.
171
172
In each microregion the phase transformation can be described in a local coordinate sys-
tem by a transformation tensor e'T, compare e.g. Wechsler et al. (1953) for martensitic
transformations and Mitter (1987) for diffusional transformations, see fig.l.

A Austenite A Austenite
M Martensite P Pearlite

Martensitic Diffusional
Transformation Transformation

F i g . l . Sketch of microregions under martensitic and diffusional

transformations.

In the following only martensitic transformations will be considered. Thermomechan-

ical investigations of an elastoplastic material have shown (Tanaka and Fischer, 1991)
that for a local transformation condition not only the load stress tensor o x , but also
the local interaction eigenstress tensor aeq and the stresses <rn developing during the
transformation of a microregion have to be taken into account (all stresses are given
with respect to the global coordinate system). The balance of the energies before and
after the complete transformation of a given microregion thus takes the form

G* - ((TL + (Teq + ^n) I (Re'TRT) = AG , 0 < K < 1, (2)

where G?(T) and G™(T) are the chemical free energies of the unstressed parent and
product phases, respectively, AG is a threshold energy and R describes the coordinate
transform from the local (x') to the global (x) system. The actual microstress state
cr = <TL + (TCq + o'n and the metallurgical structure are, therefore, coupled phenomena,
as already pointed out qualitatively by Inoue et al. (1981).

In order to arrive at a macroscopic material description from such micromechanical

considerations, suitable internal variables can be introduced. The contributions of all
microregions, each with its own orientation of the local coordinate system, its own stress
state and its own material state, must be taken into account by appropriate averaging
 173
procedures. A typical example for this approach is the introduction of a transformation
fraction £(x,2) as an average over a mesodomain (a group of microdomains), which, in
the case of plastic interaction, leads to an an additional transformation plasticity term
in the macroscale material law as proposed for steels by Franitza (1972) and thoroughly
discussed by Leblond et al. (1986). This term takes the form

iTRIP = ~k6f(0£sL , (3)

where k is a numerical constant, 6 stands for the volume change during transformation
and S£ is the deviator of the macroscopic load stress tensor. Various expressions of the
monotonic function /(£)> 0 < f < 1, have been proposed in the literature, see e.g. Denis
et al. (1989). This concept has been expanded via a micromechanical model by Fischer
(1990), which also takes into account the shape changes 7 characteristic of martensitic
transformations.

In a natural extension of this strategy the expression for STRIP can be combined with
a "macroscopic" kinetic equation for £(x,<), which depends on the averages of the local
stress state {&) and of the transformation tensor ET(£) = (ReJpR T ), where ET is a
function of £ because a ^-dependent weight function is used in the averaging procedure.
Recently, Tanaka and Fischer (1991) have derived the following kinetic equation for
martensitic transformations by using a consistent micromechanical approach:

r^e = ~kV ^ ( ( < ? r _ G ))f+kVEH0

* '■{a) ■ (4)

Here k and V are material constants. This promising concept is now being implemented
into numerical procedures.

MICROMECHANICAL T R E A T M E N T OF METAL MATRIX

COMPOSITES

The use of numerical methods in micromechanical analyses of composite materials is by

now a well established practice for the investigation of both long fiber (Adams, 1989)
and short fiber (Tvergaard, 1989) reinforced composites. By applying the finite element
method to an appropriate unit cell, the microscale distributions of stresses and strains in
periodic composites can be modelled at considerable detail for a wide range of material
models, material properties and reinforcement volume fractions. While the assumption
of a periodic arrangement of the reinforcing phase may give rise to inaccuracies in
the interfacial stresses (MacKay, 1990) and in the stress distributions in the plastic
range (Brockenbrough and Suresh, 1990), no other approach can currently deliver a
comparable level of insight into microscale effects and their influence on the overall
material behavior.

For the present work a unit cell corresponding to a hexagonally packed fiber arrangement
with a fiber volume fraction of 47.5% was employed for two-dimensional generalized
174
plane strain analyses, the finite element method being used. Thermoelastic fibers and a
thermo-elastic, thermo-elastic-plastic or a thermo-visco-elastic-plastic matrix were mod-
elled, the material data corresponding to a B / A l metal matrix composite (MMC). For
the matrix a v.Mises type plasticity either without hardening or with kinematic harden-
ing and, where appropriate, a steady state (secondary) strain hardening creep law were
employed. The following examples show some of the capabilities of this computational
micromechanics approach in the investigation of long fiber reinforced composites.

All production processes for MMCs feature a cooldown stage from high solidification
or consolidation temperatures, as a consequence of which the pronounced thermal ex-
pansion mismatch between reinforcement and matrix gives rise to microstresses in both
fiber and matrix. These self-equilibrated microstresses, which can considerably influ-
ence the macroscopic thermomechanical properties of the composite, were investigated
in the course of the present study by modelling the cooling down of MMCs with both
thermo-elastic-plastic and thermo-visco-elastic-plastic matrices.

In both cases the computed residual stresses were found to considerably exceed the
matrix yield stress. The experimental evidence in this respect is mixed, but at least
some of the results reported in the literature appear to be more in line with a partially
elastic residual stress state of the matrix (e.g. Masutti et a/., 1990). This behavior may
be due to stress relaxation at room temperature as discussed by Krempl and Yeh (1990)
or to metallurgical effects (Wolff, 1990).

Fig.2. Computed thermal cycling behavior of a virgin MMC and

a cooled-down MMC.

The axial residual stresses in the cooled-down matrix are typically tensile and there are
pronounced tensile hoop stresses around the fiber, which act as clamping stresses. In the
 175
authors' simulations of the thermal cycling of unidirectional MMCs, the influence of this
stress state is clearly evident upon comparison with the behavior of a virgin (i.e. initially
stress free) composite, see fig.2. The residual stresses shift the temperature at which
plastification occurs to higher values and give rise to a practically closed hysteresis, the
stress state at the end of the cycle being nearly identical to the initial residual stress
state.

Fig.3. Computed mechanical cycling behavior in fiber direction of

a virgin MMC and a cooled-down MMC.

These results are in good qualitative agrement with experimental data, e.g. Masutti et
al. (1990). When the axial mechanical cycling of the same composites was modelled, the
virgin composite showed a pronounced elastic range while the residual stresses in the
cooled-down material caused it to plastify immediately upon tensile loading, compare
fig.3.

As pointed out by Kural and Min (1984), the residual stress state and thus the ther-
momechanical behavior can be modified by continuing the cooling down of the MMC
below room temperature and then heating it up again. The authors' computational
investigation of such processes showed that the thermal and axial mechanical cycling
behavior of an MMC can be "adjusted" this way between the responses corresponding
to the virgin and the cooled down states. It should be noted, however, that this does not
hold for the transversal mechanical cycling behavior, which, being a matrix dominated
property, is much more sensitive to the residual stress state.
176
ACKNOWLEDGEMENT

The financial support of this investigation by the Austrian Federal Ministry of Science
and Research within the project "Computer Aided Material Development", project
number GZ 49.518/5-24/87, is gratefully acknowledged.

REFERENCES

Adams, D.F. (1989). Micromechanical analysis of composite materials: Application to

practical problems. Technomic Publishing, Lancaster, PA.
Brockenbrough, J.R. and S. Suresh (1990). Plastic deformation of continuous fiber-
reinforced metal-matrix composites: Effects of fiber shape and distribution. Scr.
Metall.Mater. 24, 325-330.
Denis, S., E. Gautier and A. Simon (1989). Modelling of the mechanical behavior of
steels during phase transformations: A review. In: Int. Conf. Residual Stresses,
ICRS2 (G.Beck et al. ed.), Elsevier Applied Science, London, 511-521.
Fischer, F.D. (1990). A micromechanical model for transformation plasticity in steels.
Ada Metall.Mater. 38, 1535-1546.
Franitza, S. (1972). Warme- und Umwandlungsspannungen in langen Kreiszylindern.
Ph.D. Thesis, T.U. Braunschweig.
Inoue, T., S. Nagaki, T. Kishino and M. Monkawa (1981). Description of transformation
kinetics, heat conduction and elastic-plastic stress in the course of quenching and
tempering of some steels. Ingenieur-Archiv 50, 315-327.
Krempl, E. and N.M. Yeh (1990). Residual stresses in fibrous metal matrix compos-
ites. A thermoviscoplastic analysis. Report MML 90-3, Mechanics of Materials
Laboratory, Rensselaer Polytechnic Institute, Troy, NY.
Kural, M.H. and B.K. Min (1984). The effects of matrix plasticity on the thermal
deformations of continuous fiber graphite/metal composites. J. Compos.Mater. 18,
519-535.
Leblond, J.B., G. Mottet and J.C. Devaux (1986). A theoretical and numerical ap-
proach to the plastic behavior of steels during phase transformations, Parts I and
II. J.Mech.Phys.Sol. 34, 395-409, 411-432.
MacKay, R.A. (1990). Effect of fiber spacing on interfacial damage in a metal matrix
composite. Scr. Metall.Mater. 24, 167-172.
Masutti, D., J.P. Lentz and F. Delannay (1990). Measurement of internal stresses and
of the temperature dependence of the matrix yield stress in metal matrix composites
from thermal expansion curves. J.Mater.Sci.Lett. 9, 340-342.
Mitter, W. (1987). Umwandlungsplastizitat und ihre Berucksichtigung bei der Berech-
nung von Eigenspannungen. Gebr. Borntrager, Berlin.
Tanaka, K. and F.D. Fischer (1991). A continuum mechanical approach to the kinetics
of martensisitc transformation. Paper submitted to Ada Met.
Tvergaard, V. (1989). Analysis of tensile properties for a whisker-reinforced metal-
matrix composite. DCAMM Report 382, Technical University of Denmark, Lyngby,
Denmark.
Wechsler, M.S, T.A. Liebermann and T.A. Read (1953). On the theory of the formation
of martensite. Trans. AIME 197, 1503-1515.
Wolff, E.G. (1990). In: International Encyclopedia of Composites (S.M.Lee, ed.), Vol.1,
511-521. VCH Publishers, New York, NY.
WS1d4

HEAT F L O W AND INELASTIC STRESSES INCORPORATING SOLIDIFICATION

— An Application to Strip Casting Process by Twin Roll Method —

T. INOUE and D.Y. J U

Department of Mechanical Engineering, Kyoto University

Sakyo-ku, Kyoto 606, J a p a n

ABSTRACT
T h e purpose of this paper is to describe the temperature and stresses incorporating solidi-
fication under steady material flow, and the application of the theory to simulate the strip
casting process by the twin roll method is presented. Interaction of the t e m p e r a t u r e fields
between the strip and the cooling roll is taken into account by the substructure method
when solving the heat conduction equation. A simulation method for the deformation
and stress/strain in the strip bounded by the traction-free boundaries was also developed
by employing an elastic-viscoplastic constitutive relation relevant to describe both solid
and liquid states. In order to verify the methods of simulation, calculated t e m p e r a t u r e
and thickness of the strip were compared with the experimental d a t a for Sn-Bi alloy using
a developed continuous casting system.

KEYWORDS
Solidification; viscoplastic stress; thin slab casting by twin roll method;

INTRODUCTION

Solidification is one of common phenomena occurring in some kinds of material processing

such as casting, welding and surface coating, etc. In order to forecast thermo-mechanical
behaviour during the processes, finite element schemes have been proposed for the heat
conduction equation coupled by the latent heat generation due to phase transformation,
and elastic-viscoplastic stress/strain fields were calculated for continuous casting process
(Williams, 1979; Inoue and Wang, 1988; Inoue and Sanari, 1989; J u , et_al., 1990).
T h e paper motivates to develop the numerical simulation technique for t e m p e r a t u r e in-
corporated with solidification and viscoplastic stress/strain in the entire domain including
liquid and solid as well as mushy zone in twin roll continuous casting system in steady
operating condition. Considering t h a t some difficulties still remain in identifying the
temperature and stresses in the strip developed in the previous papers (Inoue and Sanari,
1989) where the temperature distribution in cooling mould or roll were ignored for sim-
plicity, the substructure method is used for the analysis of heat conduction in the roll and
strip. An elastic-viscoplastic constitutive equation relevant to describe the behaviour of
both liquid and solid is employed for stress analysis, and deformation on the free boundary

177
178
is also simulated. Discussion is presented on the comparison of the numerical simulation
with the experimental data.

M O D E L I N G O F T W I N ROLL SYSTEM AND G O V E R N I N G EQUATIONS

Modeling

T h e twin-roll continuous casting system is schematically illustrated in Fig. 1(a), and, due
to the symmetry to the central line, a half part of the model shown in Fig. 1(b) is treated
for the analysis.
Free boundary
Molten steel
-Steel roll
Steel shaft

Strip

Roll
Cooling water
Cupper roll sleeve
Cast strip Free boundary

(a) (b)

Fig. 1. View of twin roll casting system and the model for simulation.

The material in the pool between the solidified shells is an incompressible viscous fluid.
The form of the velocity field is assumed such that

Vv = C&y/r* - (ym - y)> ■ bl Vx = D0-Vy (1)

(b-x-bo)* '
under the boundary condition t h a t Vy = ru on roll surface , and Vx = 0 along x — 0, and
that VQ = ru> at y > ym, where UJ is the angular velocity of the roll. T h e parameters C0
and D0 in eq.(l) are determined from the incompressibility condition

rb rb <jy
/ Vydx = rbQu , Vx = / ——±dy . (2)
Jo Jo ox
Kinetics of solidification
Solidification of liquid into solid, or, in general, phase transformation of materials, is es-
sentially a microscopic phenomena associated with nucleation and growth of a new phase.
To take into account the phenomena from continuum mechanics viewpoint, we follow an
assumption t h a t a material point undergoing solidification consists of a mixture of solid
and liquid elements. To identify the volume fraction of solid phase £ s during solidification,
use is made of a phase diagram. A Sn-Bi alloy with low melting t e m p e r a t u r e is employed
for the experiments as an example, and, when adopting the lever rule, the volume fraction
£ s is determined as

T>T,
6 = l {(T- T,)/m,}/{CBi + (T - T,)/m,)} if TS<T <T,
if T<T. .
 179
where T3 and T\ represent the solidus and liquidus temperature, and m\ is the gradient of
T[ with respect to C# t content, where C# t is t h a t of this material.
Heat conduction equation

In the steady continuous casting process, t h e material flow is preferably described in a

spatially fixed Eulerian coordinate system x with velocity V . A heat conduction equation
including latent heat generation la from solidifying element with volume fraction £s leads
to (Inoue, and Wang, 1988)

pcV - grad T — div(kgrad T) — plsV • grad (5 = 0 , (4)

for the strip, and the equation for the roll without phase transformation is expressed as

pcV • grad T — div(k grad T) = 0 . (5)

Here, />, c and k are respectively the density, specific heat and heat conductivity of the
material being represented by the mixture law. T h e boundary condition of t e m p e r a t u r e
can be written as

-kngradT = h(T -Tw) on Sh , -kn grad T = TF(T4-T*) on Sf . (6)

in which h is the heat transfer coefficient on the boundary 5^, T and F are the Stefan-
Blotzmann constant and the emissivity on the boundaries 5 / with unit outward normal ?i,
while Tw is t h e t e m p e r a t u r e of coolant.
Inelastic constitutive equation

Elastic-viscoplastic stress analysis is necessary to evaluate proper modes of stress and

deformation in the global domain of t h e strip including viscous liquid and solid (Inoue and
Wang, 1988). Total strain r a t e e is given by the sum of t h e elastic and inelastic strain
rates e e and e \ as well as the thermal strain rate e* and the strain rate im representing
dilatation caused by phase change,

e = e e +e'+e T + em , (7)
where the elastic strain is

1 4- v v
e* = -?rO-1,(tro)\ . (8)
Here, E and v denote Young's modulus and Poisson's ratio depending on temperature.
The constitutive relation of the thermal strain rate il and the transformation strain rate
C m due to solidification yields

eT = atl ; em = ft.l , (9)

where a and /3 denote the coefficient of thermal expansion and dilatation due to solidifi-
cation, respectively.
In order to formulate t h e inelastic strain r a t e e* for t h e description of t h e behavior of solid-
ifying material from liquid to solid, a unified viscoplastic model by Perzyna type(Perzyna,
1971) is employed,
180
where cry = ay0 -f H'e stands for static flow stress being dependent on t e m p e r a t u r e , and
H' is harding coefficient. In the liquid state, (Tyo and H' is assumed to be zero so t h a t
inelastic strain rate is reduced to

*■■ = £ . . (H)
T h e constitutive equation (7) with the viscoplastic strain rate (10) was confirmed to de-
scribe the behaviour of viscous fluid as well as viscoplastic solid (Perzyna, 1971).

A L G O R I T H M O F NUMERICAL CALCULATION
Substructure method for t e m p e r a t u r e

T h e finite element formula of heat conduction equation (4) for t h e strip is obtained by
applying the Galerkin method with the boundary conditions (6);

\H'\{T) = {Qm} + { « / } + {Q'k} , (12)

and t h a t for the roll leads to

[HR]{T} = {Qh} + { Q f t . (13)

Here, [Hs] and [Hr] are the stiffness matrices considering material flow. {Qm} is the latent
heat vector, and {Qj} and {Qh} mean vectors of the heat radiation and heat transfer.
{Qsh} and {Qrh} are heat input vectors through the contact surface with the strip and the
roll, respectively, which are defined as

{Qtt = J hRTR[N)TdS ; {Q%} = J h,Ts[NfdS , (14)

where Ts and Tr are the temperature on the contact surface belong to the strip and the roll.
In the initial step of the numerical analysis, t h e t e m p e r a t u r e of the roll Tr is assumed to be
uniform, Substituting the Tr temperature into eq.(12) leads to the t e m p e r a t u r e Ts of the
strip. When the t e m p e r a t u r e Ts of the strip on t h e contact boundary is introduced into
eq.(13), we can again solve the t e m p e r a t u r e distribution Tr in the roll. Such a iteration
algorithm is successively repeated for eq.(12) and (13) until the convergence of the solutions
is satisfied.
Analysis of elastic-viscoplastic stresses

Based on the elastic-viscoplastic constitutive equation (7), finite element equation for stress
analysis of the strip (but, not of t h e roll) is reduced to

[K}{u] = {Ft} + {Fm} + {Fi} , (15)

where [K] is the stiffness matrix, {it} denotes the deformation rate vector, and {Ft} and
{Fm} represent force vectors of thermal expansion and phase transformation dilatation,
while {Fi} is the inelasticity force vector. T h e meniscus and the surface of the strip below
roll outlet are traction-free boundaries. Especially, the material on the boundaries tend
to expand due to the viscoplastic deformation to reduce in the incorrect thickness of the
plate. Such a deformation profile is assumed to be represented by the shape function in
the forms:

y-f(x,t) = 0 , x-g(y,t) = 0 . (16)

 181
with the time parameter t. The material-time derivative of the functions reads

".-'-£♦£"•' V - x - ^ + ^-V
Vx x dt + dyv*
(17)

Since the shape functions are independent on time t in the steady state, the functions are
now expressible by polynomials:

f = a0 + axx + a2x2 + 9 = bo + biy + ky 2 + (18)

At the beginning of numerical calculation, the deformation velocity be solved by eq.(15)
and a new velocity field is obtained as the combination of the velocity of casting and the
deformation velocity. The coefficients of above function (18) is identified if the velocity
Vx and Vy on the free boundary is introduced into eq.(17). Such processes are iterated to
reduce the convergent value of the coordinate of the boundary.

RESULTS OF NUMERICAL ANALYSIS AND DISCUSSIONS

The procedure developed above are now applied to the simulation of the thin slab casting
process under some operating conditions. The results are summarized as follows. Figure
2 represents the finite element descritization of the whole region of the strip and roll, and
the velocity field based on eqs. (1) and (2) is plotted in Fig.3.

50 10 30 20 10 0 20 15 10 5 0
Distance from center x, mm Distance from center x, mm

Fig. 2. Finite element division. Fig. 3. Velocity field.

Simulated results of steady temperature distribution both in the strip and roll is shown in
Fig.4(a) for the casting speed of 77.2mm/s with T0 = 190°C at the meniscus, and Fig.4(b)
depicts the volume fraction of solid phase, in which the line indicated by fs = 1.0 shows
the solid front. Measured temperature distribution by thermocouples along the central
line is plotted by circles in Fig.5, while the solid line indicates the calculated temperature.
It may be suggested from the figure that the simulation gives fairly good agreement with
the experiment.
The stresses distributions at several locations are given in Fig. 6. The distribution at the
very end of the strip can be seen to grow up again, which may become the origin of residual
stresses. The deformation on free boundary is shown in Fig. 7 with the measured data
of the thickness.
182

To=190 X
To=190 *C

} Calculation

N
V=51.1mm/s

50
20 40 60 80 100
Distance f r o m center x , mm Distance from meniscus y,

Fig. 4. Distribution of temperature (a) Fig. 5. Variation of t e m p e r a t u r e

and volume fraction of solid (b). along t h e central line.
«20 10 0

20h

3 40

*
E
60
E
o Roll outlet
Z 80
c V0=77.2mm/s

I 100 • Measured data

30 20 10 0
Distance from center x, mm
10 5 ""' 0
Distance from center x. mm
Fig. 6. Stresses distribution Fig. 7. Deformation on free boundary
at several locations.

REFERENCES
Inoue, T. and H. Sanari, (1989). Simulation of temperature and inelastic stresses in a
Solidifying slab during twin-roll casting process. Proc. Int. Conf. Advances of
Plasticity, T s u , 57-60.
Inoue, T. and Z.G. Wang (1988). Thermal and mechanical fields in continuous casting
slab — A steady state analysis. Ing. Arch., 58, 265-276.
Ju, D. Y., T . Inoue, and N. Yoshihara (1990). Solidification mode and viscoplastic stresses
in aluminum cylinder during vertical semi-continuous direct chill casting process. Proc.
Int. Conf. of Technology of Plasticity, Vol. 2, Kyoto, 1095-1100.
Perzyna, P (1971). Thermodynamics theory of viscoplasticity. Adv. Appl. Mech., U, 313-
354.
Williams, J. R., R . W . Lewis and K. Morgan (1979). An elastic-viscoplastic thermal stress
model with applications to t h e continuous casting of metals. Int. J. num. Meth. Engng,
14, 1-9.
WS1d5

FUNDAMENTAL STUDY ON THE RE-CRYSTALLIZATION OF

SUS304 STAINLESS STEEL BILLET FOR TUBE EXTRUSION

M. AKIYAMA* and M. YAMASHITA**

* Precision Technology Development Department, Division of

Research and Development, Sumitomo Metal Industries Ltd.,
1-8, Fuso-cho, Amagasaki, 600, Japan
** Steel Making and Rolling Plant, Steel Tube Works,
Sumitomo Metal Industries Ltd.
1, Nishino-cho, Higashi-Mukojima, Amagasaki, 660, Japan

ABSTRACT

Fundamental research work was carried out on the re-crystallization

behaviour of a cast round SUS304 stainless steel billet for extrusion. In
order to obtain smooth external surface of an extruded tube, it is
necessary to have sufficiently fine grain in the mother billet. For this
purpose, some metal working on the cast billet is necessary, and from the
viewpoint of minimum yield loss by turning, which is for the preparation of
extrusion, cold working through a round die is the best one. In the
present paper, material property of a cast SUS304 billet was first tested
and axi-symmetric rigid-plastic finite element analysis was then carried
out by taking this result into account. Next, test billets were subjected
to cold working through a round die and then some heat treatment were given
to these billets to observe the grain size before extrusion. The grain
size distribution was compared with the distribution of equivalent strain
obtained by the analysis. In the end, the surfaces of extruded tube were
observed to reach a conclusion that at least 5% area reduction is necessary
for obtaining a smooth surface on an extruded tube.

KEY WORDS

SUS304: cast billet: cold metal working: heat treatment: re-crystallization

hot extrusion: axi-symmetric rigid-plastic finite element analysis.

BACKGROUND
Hot extrusion process is known as a major process for manufacturing
stainless and high-alloy steel tubes. Cast billets for hot tube extrusion
have been subjected to hot rolling. One of the purposes of hot rolling is
to get sufficiently fine grain for extrusion. There are reports in which
it is stated that grain size on the billet affects the external surface
quality of the extruded tubed). However, there are very few research work
in which attention is focussed on the fundamental and quantitative analysis
on the process through which the grain in the cast billet becomes finer.

In the present work SUS304 billet is taken as an example to carry out

quantitative analysis by FEM to know the distribution of the equivalent
strain in the billet after cold work. Before the extrusion the billet is
heated and the coarse grain becomes finer due to re-crystallization.
Prediction of the grain size before extrusion is, therefore, necessary.

183
184

80 1
a 1
70 Ll y I
n=21.0kq/nm 2 f
^ 60

T.P. position ^> 50

in a billet
u, 40
«/»
O)
£ 30 TP-0
in
* 20 TP-M
140
25H L^OtO.05. h25J * 10

0
0 10 20 30 40 50
" 5 R 1|5 ' /ST.?. True strain (%)

Fig. 1 Stress-strain relationship at room temperature of SUS304

specimens taken from a cast billet

MATERIAL PROPERTY
Tensile testing

Before carrying out finite element analysis, it is important to know the

material property, i.e. the stress-strain relationship at room temperature.

A round cast SUS304 billet used is illustrated at the upper left corner of
Fig. 1. It was suspected that there might be difference in the material
properties between the outside and inside portion of the billet, and two
specimens were taken from the outside surface and the other from the middle
part of the billet. If the material properties are almost the same, it may
be concluded that the material property is almost uniform in the billet.

The specimen for tensile testing is also illustrated at the lower left
corner of Fig. 1. The testing was carried out at room temperature.

Stress-strain relationship

The true stress-true strain relationship obtained through the testing is

shown on the right hand side of Fig. 1. The solid line is for the specimen
taken from the middle portion and the broken line is for that taken from
the outside surface. There is little difference between the two lines when
the amount of true strain is less than 20%. Slight difference is observed
between the two when the amount of true stain becomes larger than 20%, but
it may be concluded that the difference is still small.

However, the present process is a cold process through a solid round die,
and total plastic strain may not exceed 40%, as there is a limitation of
reduction in diameter due to adhesion, press force and the buckling of the
billet during cold work. Because of this reason, the average reduction in
area cannot exceed 10%.

It was concluded, therefore, that the fundamental material property was

uniform over the cross section. The difference between the two lines are
at most a few percent when the true strain is about 40%, and the difference
may not give a significant influence on the re-crystallization behaviour as
the total strain is large. If the analytical and experimental results show
some critical effect, analysis will be carried out taking into account the
difference between the two lines.
 185
* 162 Element , 190 Nodes J
a5
: Ik
II II j I J H d
s
I

Example of
187*-182* force chart
a-5'

E 50
0 0.05 0.1 0.15 0.2
Time (sec) Coulomb friction coefficient (u)
Fig. 2 Axi-symmetric rigid-plastic finite element analysis for
deciding the Coulomb friction coefficient

FINITE ELEMENT ANALYSIS

Preliminary analysis

For the re-crystallization behaviour, elastic strain may have little

influence and the dominant factor may be the plastic strain of which value
must be much larger than that of elastic strain. Therefore, rigid-plastic
analysis was adopted. It is incidentally simpler and requires less
computational time compared with the elastic-plastic analysis.

The basic set of equations for the analysis is shown by equation (1) <2>.

Ki v + p K2 (1)

where Ki, v, p • K2 • v, f are the stiffness matrix, the velocity vector to

be calculated, the penalty term and the external force vector respectively.
The set of equations were solved and then equivalent strain rate was
calculated to update the equivalent plastic strain £ by adding the
ecruivalent strain rate I multiplied by time increment A t as it is shown in
equation (2).

Enew eoid + e • At (2)

In carrying out the analysis, it is important to know the Coulomb friction

coefficient [i between the die and the billet. The calculated results by
changing the value of \i were compared with an experimental result.

The axi-symmetric finite element mesh used in the analysis is shown on the
upper left side of Fig. 2. It is clearly indicated in Fig. 2 that as the
friction coefficient increases, the amount of press force increases.

In order to get the actual friction coefficient, an experimental work was

carried out using a billet and a die of the same sizes as were used in the
analysis, i.e. a billet of 187mm outside diameter and a die of 182mm inside
diameter. The length of the billet was 3m. The chart for the press force
is indicated at the lower left of Fig. 2. It is observed that there is
little fluctuation of press force and the state of friction between the
billet and the die is very stable.

A comparison of analytical results and experimental result was given in

Fig. 2. The result show that the value of friction coefficient is 0.08.
In the following analyses, this value is used.
186

30
+ ♦♦ + + + a - 7°
a~ 6°
♦1
+ j
a = 4° +/ \
20 a =3°

JA
a =2°
187*-182$
/ A
p = 0.08
10
.-z^'-—

50 91
Distance from b i l l e t centre (mm)

Fig. 3 Distribution of equivalent strain in the radial direction

in a cold worked billet

Main analyses

The die geometry was first discussed and then the distribution of
equivalent strain in the cross section was examined.

It was intuitively predicted that the geometry of die, in the present case
the half die angle a, had a strong influence on the distribution of
equivalent strain in the radial direction, especially in the vicinity of
the external surface of the billet. It was also expected that the press
force required would change according to the change of a. Press force is
one of the important factor in the experiment, as the maximum capacity of
equipment is decided by the maximum press force. The value of a which
gives smaller press force is, therefore, preferable.

In Fig. 3 analytical results are indicated. The abscissa is the distance

from the billet centre after the cold work, and the ordinate the equivalent
strain. The value of equivalent strain does not change significantly in
the central portion even if the value of |i changes. The value of the
equivalent strain at the centre is almost the same as the value of the
reduction in area changes. In the vicinity of external surface, however,
the distribution of equivalent strain is affected by a, and the influence
is larger as the position is closer to the billet surface.

In order to obtain finer grain by re-crystallization, it is better to get

larger amount of plastic strain. The quality of the extruded tube surface
highly depends on the grain size in the vicinity of the billet surface, It
is, therefore, recommended to use a die of which half angle a is larger.

However, the minimum press force 172Ton was given when the value of a is
equal to 4 degrees. When the value of a is less than 4, the press force
sharply increases and the occurrence of buckling of billet is suspected.
It is assumed that 4 degrees is a critical die angle. When the value of a
is 5, the calculated press force is 175Ton. The calculated press forces
are 200Ton and 223 Ton for ot=6 and 0t=7 respectively. From the viewpoint of
smooth operation, the die of which half angle a=5 degrees is preferable.

Experiments were carried out using a die of which a was 5 degrees. If the
surface quality of extruded tube was unsatisfactory, the reduction in area
would be increased, but a the first stage 18% equivalent plastic strain at
the billet surface was regarded to be enough.
 187

3 0 2 4 6 8 10 12 14 16 18 20
Tensile plastic strain (%)

Fig. 4 Examples of the relationship between tensile strain and

the grain size after heat treatment

FUNDAMENTAL EXPERIMENTS OF RE-CRYSTALLIZATION

Tensile testing
In order to understand the fundamental behaviour of re-crystallization, a
set of tensile testings was carried out followed by a heat treatment. The
specimens were cut and the micro-structure was observed. The diameter of
specimens was 14mm and the gauge length was 50mm. i.e. JIS No.4 specimen.

The specimens were then subjected to tensile testing at room temperature.

The tensile strains given were 2%, 4%, 6%, 8%, 10%, 15% and 20%. The
maximum value 20% was chosen by the analytical result of the equivalent
strain at the external surface of the billet.

The stress-strain curves were again compared between the specimens, some of
which were taken from the external surface and others were taken from the
inside portion of a billet, but no significant difference was observed.

Relationship between tensile strain and grain size after heat treatment

The specimens were then subjected to heat treatment. They were heated to
1250°C and kept for 10 minutes and then put in water. The temperature was
chosen as it is the maximum temperature to which a billet for extrusion is
heated. The round cross sections of the specimens were observed.

In Fig. 4, the relationship between the tensile plastic strain and the ASTM
standard grain number is indicated. The amount of plastic strain and the
grain size after heat treatment has a positive relationship and the larger
the plastic strain becomes the finer the grain is.

It is clearly indicated that the relationship is piecewise linear, which

means that the ASTM standard grain number increases proportionally to the
plastic strain given to an as cast material. As this relationship is very
simple, it is very easy to apply this relationship to a practical use.

As the relationship between the plastic pre-strain and the grain size after
heat treatment has been obtained, and also as it is possible to calculate
the distribution of plastic strain by cold press, it is now possible to
predict the distribution of grain size in the radial direction just before
extrusion. Therefore, by observing the extruded tube surface, the optimum
amount, or the threshold value, of cold work will be determined.
188

-Q °
C
c 2 I 0 : Experimental
: Calculated
h
^ ^
— ■ "
—
0 " r = 91mm
■8 o O after cold work
C
rd
r = 86mm \
for extrusion \
-1 L
"
§0
1
20 40
1 —;
60 80
>\ 1
100
Distance from b i l l e t centre (mm)

Fig. 5 Comparison of grain sizes on an actual extrusion billet

and the predicted values by the fundamental analysis

PREDICTION OF GRAIN SIZE ON A BILLET FOR EXTRUSION

By using the above described result, prediction was made on the

distribution of grain size of a billet to be extruded. The diameter of the
mother cast billet was 187m and that after cold work was 182mm. The
distribution of equivalent plastic strain is shown in Fig. 3.

After the cold work, the billet was reduced in diameter to 172mm by turning
and then heated to 1250°C by an induction heater. When the temperature
reached to the aimed value, the billet was put into water. After cooling,
a round slice was cut from the billet and micro-structures were observed.

The results are shown in Fig. 5. The abscissa of Fig. 5, is the radial
position from the centre, and the ordinate the grain size. Open circle
shows the measured value and the solid line is the predicted value. A good
agreement was obtained between the predicted value and experimental value.

RESULTS

As the final step of the present research work, extrusion were carried out
using billets which were cold worked under different conditions of area
reduction. The size of the mother cast billet was 187mm and the values of
area reduction was 3, 4, 5 and 7%. As a comparison, a cast billet was also
tested. The outside and inside diameters of extruded tube were 66.5mm and
56mm. After de-scaling, the outside surface of the tubes was observed.

The surface quality was good for those extruded from billets of 5 and 7%
area reduction, but it was poor for those extruded from a cast billet. A
half of the tubes extruded from billets of 3 and 4% area reduction had poor
surface quality. Therefore, the area reduction of 5%, or to be more strict
18% equivalent plastic strain at the surface of the billet, may be the
minimum value to ensure the good surface quality of extruded tubes.

REFERENCES

(1) e.g. Sakane T, et al., Proc. of the ISIJ autumn meeting, 1986, pp-194
(2) Zienkiewicz O.C. (1977) The Finite Element Method, p-607-644, McGrow
Hill
WSlel

ON THE COMPUTATIONAL PREDICTION OF

PLASTIC STRAIN LOCALIZATION

Viggo Tvergaard
Department of Solid Mechanics
The Technical University of Denmark, Lyngby, Denmark

ABSTRACT

The analysis of plastic flow localization in shear bands is here discussed with special focus on the
effect of the nucleation and growth of microscopic voids. Constitutive relations for porous ductile
materials are often used for such investigations, and here predictions of an isotropic hardening model
as well as a kinematic hardening model will be discussed. Numerical cell model analyses of localization
are used to evaluate the capabilities of the approximate constitutive relations. Furthermore,
computations for nonuniformly strained solids showing flow localization in shear bands will be
discussed.

KEYWORDS

Voids; ductile fracture; localization; shear bands.

1. INTRODUCTION

Localization of plastic flow in shear bands is frequently observed in ductile solids. Initially the
deformations tend to vary smoothly in the solid, but at some stage a different deformation pattern
may develop, involving highly localized deformations. Subsequently, the strains grow large inside the
shear band(s) without contributing much to the overall deformation of the sohd, and this often results
in shear fracture.

For a uniformly strained elastic—plastic solid localization occurs at a bifurcation point, which
coincides with loss of ellipticity of the equations governing incremental equilibrium. It is well known
that the value of the critical strain for loss of ellipticity is very sensitive to the constitutive law. The
classical elastic—plastic solid with a smooth yield surface and normality is very resistant to
localization, but more realistic critical strains are predicted if the material develops a yield surface
vertex or if softening due to material damage is accounted for. In the present paper the effect of the
nucleation and growth of micro—voids on localization predictions will be discussed in some detail.

Investigations of ductile fracture mechanisms are often based on porous ductile material models as
that proposed by Gurson (1977a,b). This material model will be briefly presented here together with
kinematic hardening versions of the model, and the effect of these different models on localization
predictions will be discussed. Furthermore, results of numerical cell—model analyses will be used to
illustrate the approximations involved in localization predictions based on ductile porous material
189
190
models. Finally, examples of finite element solutions are presented, showing plastic flow localization
based on the constitutive relations for void containing materials.

2. SIMPLE LOCALIZATION ANALYSIS

The basic phenomenon of plastic flow localization can be studied by a relatively simple model
problem for solids subject to uniform straining, as illustrated in Fig. 1. T h e localized shearing is
assumed to occur in a thin slice of material with reference normal nj , while the strain fields outside
this band are assumed to remain uniform throughout the deformation history. T h e quantities inside
and outside the band are denoted by ( )b and ( )° , respectively, and a Cartesian reference
coordinate system is used. Since uniform deformation fields are assumed both inside and outside the
band, equilibrium and compatibility inside the solid are automatically satisfied, apart from the
necessary conditions at the band interface. These conditions on displacement gradients and tractions
are

u
i.j = u
i.j + c n
i j (1)

(Ti)b = (Ti)0 (2)

where cj are parameters to be determined, while T* = (r'J + r^JuJk)nj are the nominal tractions
on the interface, expressed in terms of the contravariant components rU of the Kirchhoff stress
tensor on the deformed base vectors.

The incremental constitutive relations are of the form

f ij = LiJkUi?kl (3)

where ?/kl is the Lagrangian strain tensor. When these relations are substituted into the incremental
form of (2), using the incremental form of (1) to express ^kl i the result is the following set of
incremental algebraic equations for the unknown parameters ci

(AiQl)b n q c i = [(Aiql)o - (Aiql)b]u?,q (4)

where A1(fl denotes the expression (using the reference metric tensor gij)

Aiql = [LkJPq(gi + u j k ) ( g ' + u> p ) + r<Ugli]nj (5)

If there is an initial inhomogeneity inside the band, such as a higher void volume fraction or a higher
concentration of void nucleating particles, the incremental equations (4) are inhomogeneous, since
(A*ql)b differs from (A*ql) 0 , and thus the equations describe the gradual evolution of localization.
In such cases localization is said to occur when straining stops outside the band (elastic unloading).

If there is no initial inhomogeneity, equations (4) are homogeneous, so that a non—trivial solution for
ci can only occur at a bifurcation point. The first such bifurcation into a shear band mode coincides

Fig. 1. Shear band in a uniformly strained solid.

 191
with the loss of ellipticity of the equations governing incremental equilibrium, and the corresponding
critical band inclination is that of the characteristics (Hill, 1962; Rice, 1976).

3. DUCTILE POROUS MATERIAL MODELS

A material model suggested by Mear and Hutchinson (1985) for a porous ductile solid, and extended
by Tvergaard (1987a) to account for void nucleation, makes use of a family of isotropic/kinematic
hardening yield surfaces of the form $(<r1J,a1J,orp,f) = 0 , where f is the current void volume
fraction, 0-iJ is the average macroscopic Cauchy stress tensor and a*J denotes the stress
components at the centre of the yield surface. The radius (7p of the yield surface for the matrix
material is taken to be given by

<rF = (l-b)<r y + b aM (6)

where ay and <TJJ are the initial yield stress and the matrix flow stress, respectively, and the
parameter b is a constant in the range [ 0 , l ] . The constitutive relations are formulated such that
for b = 1 they reduce to Gurson's (1977a,b) isotropic hardening model, whereas a pure kinematic
hardening model appears for b = 0 . The approximate yield condition is taken to be of the form

~2
= — + 2qif* cosh 1 - ( q i f*)2 = 0 (7)
2<r,
FJ
4
where W = erij - aU , ae = ( 3 i i j 5 i J / 2 ) ^ and s i J = *U - GVa\i/Z . F o r f* = f and qi = 1
the expression (7) is that proposed by Mear and Hutchinson (1985), which coincides with that of
Gurson (1977a) for b = 1 . The parameter qi > 1 improves the predictions of the Gurson model at
low void volume fractions (Tvergaard, 1981, 1982a), while the function f*(f) is introduced to model
the more rapid loss of material stress carrying capacity during final failure by void coalescence
(Tvergaard and Needleman, 1984).

.p
The plastic part of the macroscopic strain increment rj i j and the effective plastic strain increment
•P
cjl for the matrix material are taken to be related by (Tvergaard, 1987a)

W inj = ( i - o <TF il (8)

.p
Using the uniaxial true stress natural strain curve for the matrix material e ^ = (1/Et — 1/E)(7j| in
(8) leads to

(y)
' M - E - E t (l-f)<rF

The change of the void volume fraction during an increment of deformation is taken to be given by

f = (l-f)GiJ^j + jCh^ + 3(A) IZ (10)

where the first term results from the growth of existing voids, and the two last terms model the
increment due to nucleation, either strain controlled or stress controlled (Needleman and Rice, 1978).

To avoid unrealistic oscillatory stress predictions for kinematic hardening (Dafalias, 1983; Loret,
1983), the ductile porous material model has been modified by Tvergaard and van der Giessen (1990)
to incorporate alternative stress rates involving corotation with the crystal substructure spin (the
elastic spin) rather than with the continuum spin. In terms of the Jaumann rate cr1) of the Cauchy
192
stress an alternative rate a1) is defined by

£ij = W + (G^<yjl _ **GJl)u;kl » <*%} = MGik9?j - mGlj)akl (11)

where p is an additional material function in the assumed constitutive law (lib) for the plastic spin.

The expression for the plastic part of the strain rate is taken to be of the form

•P 1 G F_ o,kl
* i j = JJ mijmkl a (12)

and the finite strain generalization of Ziegler's (1959) hardening rule, expressing the evolution of the
yield surface centre during a plastic increment, is chosen as

a " = ji £ H , ft > 0 (13)

(see further details in Tvergaard, 1987a; Tvergaard and van der Giessen, 1990). Finally, the
incremental constitutive law of the form (3) is derived from the assumption that the total strain rate
.E .P
is the sum of the elastic and plastic parts, T/ij = 77 ij + »/ i j .
The simple localization analysis of Section 2 (Fig. 1) has been used by a number of authors to study
localization predictions for the porous ductile material models. Fig. 2 shows a comparison of
predictions for isotropic hardening and kinematic hardening in a material under uniaxial plane strain
tension. This material has no porosity initially; but voids nucleate inside the band from a particle
volume fraction f{|} = 0.01 , with a mean nucleation strain 0.3 and standard deviation 0.1 . Thus,
localization develops here gradually, as determined by (4), and the minima of the different curves in
Fig. 2b indicate the most critical initial angle of inclination tfa of the slice of material containing the
inhomogeneity. Kinematic hardening has an effect similar to that of a rounded vertex on the yield
surface, leading to relatively early onset of localization (Mear and Hutchinson, 1985; Tvergaard,
1987a); but this early localization is somewhat delayed for p > 0 in (11). A more important effect of
taking p> 0 is that unrealistic oscillatory stresses inside the band are avoided in the
post—localization range (Tvergaard and van der Giessen, 1990), so that final void sheet failure is

Fig. 2. Shear band predictions by porous ductile material models, for

uniaxial plane strain tension, with strain controlled nucleation, 1^ = 0.01 ,
fj} = 0 , ffl = 0.3 , s = 0.1 . (a) Localization strains, (b) Fracture strains.
(From Tvergaard and van der Giessen, 1990).
 193
predicted at a realistic value of the maximum principal logarithmic strain €f inside the band (Fig.
2b).

4. NUMERICAL STUDIES OF VOID INDUCED SHEAR BAND FORMATION

Shear band bifurcation has been analysed in detail by Tvergaard (1981) for a power hardening
elastic—plastic solid containing a doubly periodic array of circular cylindrical voids. In this
micromechanical study full account was taken of the interaction between neighbouring voids and the
strongly nonuniform distributions of stress and strain in the matrix material. Due to symmetries, only
a characteristic unit cell around one void had to be analysed numerically, also in the bifurcation
analysis where the conditions (1) and (2) at the band interface were satisfied on the average between
two different periodic deformation patterns. It was shown on the basis of this detailed shear band
bifurcation analysis that too large localization strains are predicted by the Gurson model, but
reasonably good agreement is obtained by using qj = 1.5 in (7).

A somewhat analogous micromechanical analysis for a solid containing an initial inhomogeneity in a

slice of material has been carried out more recently by Tvergaard (1989). Here, only a single row of
uniformly spaced circular cylindrical voids are assumed along a particular material plane, and this
void sheet acts as an imperfection that promotes localization along the plane. The non—linear
interaction between neighbouring voids and the gradual development of plastic flow localization along
the row of voids has been studied numerically by a cell model analysis, which links the strongly
nonuniform stress and strain fields near the voids to the assumed uniform fields well away from the
void sheet. In terms of the porous material models this situation would be represented by a thin slice
of material containing initial porosity, with no porosity outside (analogous to Fig. 2). However, the
void volume fraction to be used inside the band is not well defined when there is only a single layer of
voids.

Fig. 3 shows cell model predictions for the onset of localization in uniaxial plane strain tension
compared with predictions of the Gurson model (b = 1 , qi = 1.5) , as function of the initial angle of
inclination VQ of the void sheet. The initial void radius and half spacing are denoted Ro and Do ,
respectively, and fj denotes the initial void volume fraction inside the band in the Gurson model
analyses. The comparison shows that the appropriate layer thickness to be used to calculate the
relevant void volume fraction is of the order of half the void spacing. Furthermore, the dependence of

0* 10* 20* 30* 40* 50* % 60*

Fig. 3. Localization strain vs. initial angle of inclination of void sheet. Cell
model analyses compared with Gurson model predictions. (From Tvergaard,
1989).
194

(Q) (b) (c)

Fig. 4. Deformed cell models and maximum principal logarithmic strain

contours for void sheet specified by KQ/DQ = 0.175 and ^0 = 30° ,
subject to stress ratio K . (a) K = —0.25 with no particle, (b) K = —0.25
with rigid particle inside void, (c) K = 0.25 . (From Tvergaard, 1989).

the critical localization strain on the band inclination found by the detailed cell model analysis is
reasonably well represented by the simple shear band analysis for the porous material model.

This micromechanical model has also been used to study the effect of the particles from which the
voids have nucleated. As an approximation sliding contact is assumed between particle and void
surface, and nucleation is taken to occur at zero strain. Figs. 4a and 4b show deformed cell models for
a negative ratio, K = — 0.25 , of the macroscopic transverse and tensile stresses, at stages well beyond
the onset of localization. In Fig. 4a the void flattens out and will eventually close up, whereas in Fig.
4b the particle size sets a minimum value of the smaller axis of the oval void, which gives rise to
significantly more rapid void growth and earlier onset of localization. On the other hand, in Fig. 4c
for K = 0.25 the void grows so rapidly due to the higher hydrostatic tension that a particle inside
the void would have no influence. Accelerated void growth due to particle pressure on the void surface
has also been studied by Fleck ei al. (1989), and it is noted that this effect is not accounted for in the
porous ductile material models.

The cell model studies discussed above and studies based on the simple localization analysis (1)—(5),
e.g. Fig. 2, refer to the idealized case of a homogeneously stressed solid. T h e more general case of
localization leading to shear fracture in non—uniformly strained solids is more complex, and this
usually requires a numerical analysis based on a material model that accounts for the effect of voids.
Several numerical studies of this kind have been carried out, e.g. the study of localization induced by
small—scale cavities between larger voids (Tvergaard, 1982b), the analysis of the cup—cone fracture in
a round tensile bar (Tvergaard and Needleman, 1984) or a study of ductile shear fracture at the
surface of a bent specimen (Tvergaard, 1987b). Fig. 5 shows results from the latter study, where
initially two shear bands have grown from wave—bottoms on the surface into the region analysed, but
only one of these bands has developed into a void sheet fracture. All these analyses make use of
quadrilaterals built up of crossed triangular linear displacement elements, which have been found able
to accurately represent shear bands as narrow as the element size provided that the mesh is chosen
such that localization wants to occur along diagonals or sides of the quadrilaterals (Tvergaard,
Needleman and Lo, 1981).

In the numerical analyses based on quadrilaterals with crossed triangles the compatibility of the
localized solution is exactly satisfied. As an alternative approach, non—compatible elements for
localization analysis have been developed (Ortiz, Leroy and Needleman, 1987; Nacar, Needleman and
Ortiz, 1989) by adding special shape functions to represent band—like deformation modes. These
 195

Fig. 5. Stretched surface section of a bent specimen with strain controlled

nucleation, fjyj = 0.04 , c^ = 0.3 , s = 0.1 , b = 0 . (a) Strain and void
contours soon after onset of localization. (b) Surface shear crack has
formed. (From Tvergaard, 1987b).

elements are much less sensitive to the mesh design, and localization predictions show reasonably good
convergence in spite of the lack of compatibility. As for the crossed triangles these alternative
elements also tend to resolve bands as narrow as the element size. A completely different approach to
localization analysis is that proposed by Triantafyllidis and Aifantis (1986), who used a non—local
continuum theory accounting for higher order gradients in the constitutive description in an attempt
to represent a characteristic length scale. This type of approach does lead to a shear band width that
is rather insensitive to mesh refinements. However, in most applications for metals, including the
numerical analyses mentioned above, the chosen mesh is not fine enough to resolve the actual band
width determined by material length—scales, and therefore no theories introducing larger
length—scales than the element size are needed. If solution by a sufficiently fine mesh is feasible, the
choice of element size can be directly used to set the minimum band width.

The fields around the tip of a sharp crack are an example of extremely non—uniform strain fields for
which the possibility of localization and void sheet fracture has also been analysed numerically. Under
quasi—static loading crack growth involving localized shearing between the crack tip and an adjacent
larger void has been found (Needleman and Tvergaard, 1987), and similar effects have been found in
a study of crack path meandering during dynamic crack growth (Tvergaard and Needleman, 1990).
Thermal softening and adiabatic shear band formation are potentially important mechanisms at high
strain rates that have been incorporated in these analyses of rapid crack growth.

REFERENCES

Dafalias, Y.F. (1983). Corotational rates for kinematic hardening at large plastic deformations. J.
Appl. Mech., 50, 561-565.
Fleck, N.A., Hutchinson, J . W . and Tvergaard, V. (1989). Softening by void nucleation and growth in
tension and shear. J. Mech. Phys. Solids 37, 515—540.
Gurson, A.L. (1977a). Continuum theory of ductile rupture by void nucleation and growth — I. Yield
criteria and flow rules for porous ductile media. J. Engng. Materials Technol., 99, 2—15.
196
Gurson, A.L. (1977b). Porous rigid—plastic materials containing rigid inclusions — yield function,
plastic potential, and void nucleation. Proc. Int. Conf. Fracture (ed. D.M.R. Taplin), 2A,
357-364.
Hill, R. (1962). Acceleration waves in solids. J. Mech. Phys. Solids, M), 1.
Loret, B. (1983). On the effects of plastic rotation in the finite deformation of anisotropic
elastoplastic materials. Mechanics of Materials, 2, 287—304.
Mear, M.E. and Hutchinson, J.W. (1985). Influence of yield surface curvature on flow localization in
dilatant plasticity. Mechanics of Materials, 4, 395—407.
Nacar, A., Needleman, A. and Ortiz, M. (1989). A finite element method for analyzing localization in
rate dependent solids at finite strains. Comp. Methods Appl. Mech. Engrg. 73, 235—258.
Needleman, A. and Tvergaard, V. (1987). An analysis of ductile rupture modes at a crack tip. J.
Mech. Phys. Solids 35, 151-183.
Ortiz, M., Leroy, Y. and Needleman, A. (1987). A finite element method for localized failure analysis.
Comp. Methods Appl. Mech. Engrg. 61, 189-214.
Rice, J.R. (1976). The localization of plastic deformation. Proc. 14th Int. Congr. Theor. and Appl.
Mech. (ed. W . T . Koiter), 207-220, North-Holland.
Triantafyllidis, N. and Aifantis, E.C. (1986). A gradient approach to localization of deformation. I.
Hyperelastic materials. J. Elasticity 16, 225—237.
Tvergaard, V. (1981). Influence of voids on shear band instabilities under plane strain conditions.
Int. J. Fracture, 17, 389-^107.
Tvergaard, V. (1982a). On localization in ductile materials containing spherical voids. Int. J.
Fracture, 18, 237-252.
Tvergaard, V. (1982b). Ductile fracture by cavity nucleation between larger voids. J. Mech. Phys.
Solids 30, 265-286.
Tvergaard, V. (1987a). Effect of yield surface curvature and void nucleation on plastic flow
localization. J. Mech. Phys. Solids, 35, 4 3 - 6 0 .
Tvergaard, V. (1987b). Ductile shear fracture at the surface of a bent specimen. Mechanics of
Materials 6, 5 3 - 6 9 .
Tvergaard, V. (1989). Numerical study of localization in a void—sheet. Int. J. Solids Structures, 25,
1143-1156.
Tvergaard, V. and Van der Giessen, E. (1990). Effect of plastic spin on localization predictions for a
porous ductile material. Danish Center for Appl. Math, and Mech., Report No. 402.
Tvergaard, V. and Needleman, A. (1984). Analysis of the cup—cone fracture in a round tensile bar.
Acta Metallurgica, 32, 157—169.
Tvergaard, V. and Needleman, A. (1990). Effect of crack meandering on dynamic, ductile crack
growth. Danish Center for Appl. Math, and Mech., Report (to appear).
Tvergaard, V., Needleman, A. and Lo, K.K. (1981). Flow localization in the plane strain tensile test.
J. Mech. Phys. Solids 29, 115-142.
Ziegler, H. (1959). A modification of Prager's hardening rule. Quart. Appl. Math., 17, 55—65.
WS1e2

FLOW LOCALIZATION OF ELASTO-VISCOPLASTIC TENSION BLOCKS

YOSHIHIRO TOMITA* AND TETSUYA NAKAO**

Faculty of Engineering, Kobe University, Nada, Kobe, Japan

**
Graduate Student, Kobe University

ABSTRACT

The thermocoupled flow localization of plane strain tension blocks, obeying

an elasto-viscoplastic constitutive equation with strain-gradient-dependent
flow stress, has been analyzed. The influence of finite element mesh size
and the size of the specimen on flow localization has been clarified.

KEYWORDS

Thermo-elasto-viscoplastic deformation; shear band; plane strain tension;

strain-gradient-dependent flow stress; finite element mesh size dependency;
size effect

INTRODUCTION

Flow localizations frequently accompany the large plastic straining of

materials. These a~e often recognized as prefracturing processes of ductile
materials and have been extensively investigated so far. However, most of
the investigations employed the classical constitutive equation, and hence
the flow localization zones were found to be essentially dependent on the
size of the finite elements. In other words, energy dissipation due to the
flow localization per unit length of the shear band depends on the finite
element mesh size. This must be a material property which may not depend on
the mesh size employed (Bazant et al., 1987).

In the present investigation, a thermo-elasto-viscoplastic version of the

rate-dependent constitutive equation (Tomita et al., 1990) is generalized
by introducing the strain gradient into the flow stress (Aifantis, 1984;
Zibib and Aifantis, 1988). The influence of the strain gradient in the flow
stress, mesh size and size of the specimens on the shear band type flow
localization is clarified by the full plane strain finite element
simulation of velocity and temperature fields of the block subjected to
tension.

CONSTITUTIVE EQUATION

We shall now discuss the constitutive equation employed in this

197
198
investigation. As discussed by Tomita et al. (1990), the thermo-elastic
constitutive equation and the constitutive equation for the viscoplastic
strain rate give the following relation for the the Jaumann rate of
Kirchhoff stress VS.., deformation rate tensor d. _, and the rate of change
4, 11 kl °
in temperature T:
VS. .=L . . . . d - ^vpp..-ie .., (1)
ij ljkl kl

wheree
30 . .
ij
p
P
ij 25 ij=Deijkipkr
1 dZ
3
i j - r ^ 6 i j " E 5T ° i j '

Hs me .J0/1* x 2G(1+V) ,3G„' ' N1 (2)

L (D
ijkl=Hl?3G i j k l + f f ; ( 3 6 l j 6 k l T T r r + g 2 ° i j Q kl ) ] >
H
°'ij"Hs+3G
%(J£e
x
Hs klxu3l <kA,+^\/. J+3,,),
ij kl -2 ij kl 7
ij

D . is the elastic stiffness tensor, a is the thermal expansion coeffi-

cient, T is the absolute temperature, E is the elastic modulus. V is
Poisson's ratio, G is the elastic shear modulus, e and e ^ are
representative viscoplastic strain and its rate, respectively, and
Hs=o/e /u). The parameter U) accounts for the degree of the noncoaxiality of
the viscoplastic strain rate to the stress tensor (Tomita and Shindo,1985).

Here, according to Zibib and Aifantis (1988), the above-mentioned thermo-

elasto-viscoplastic constitutive equation is generalized by introducing
higher strain gradient terms. Present investigation employs the simplest
model as

a=5(evP,gvp, T)-CV2evP> (3)

2
where 5 is representative stress, V is the Laplacian operator, C is
assumed to be constant. Then the hardening parameter Hs in Eq.(2) is

Hs=(o-CV2evp)/evp/aj. (4)

Introduction of Eqs.(3) and (4) into Eq.(2) yields the nonlocal

generalization of the thermo-elasto-viscoplastic constitutive equation.
Since the present constitutive equation is an elasto-viscoplastic one, the
problem associated with the condition of loading and unloading will not
arise. In order to increase the length of the time steps for stable
computation, a forward gradient method (Peirce et al., 1984) is applied.

METHOD OF ANALYSIS AND COMPUTATIONAL MODEL

The numerical procedure employs the well-established thermo-elasto-

viscoplastic finite element method (Tomita et al., 1990) along with the
constitutive equation derived above. The gradient term of representative
strain for an element was approximately estimated by the numerical
differentiation based on the values of the strain of neighboring elements.

Thermo-elasto-viscoplastic analysis is performed for the plane strain

blocks subjected to tension at both ends. Due to the symmetry of the
 199

S p e c i m en size Mesh d l v l s l on
Notation 1 . D . m A. B. C lognO T «C/C»

I A 0 0 A 0 0
1 A 0 1 A 0
1 A 0 4 A 0
I A 0 2 0 A 0 2 0
I A 6 0 A 6
1 A 6 1 A 6
u 2L u

_L
L ,|t
I A 6 4 A 6
I A 6 2 0 A 6 2 0
/ ^ /
I D 0 0 B 0
/ 1 CO O C 0

\S*
"X\ K I 0 0 I B 0

2W '-Shear ! 1 C 0 1 C 0
Band \ /2W5 1
I
0 6
C 6
0
0
B
C
6
6

/4* // 1 B 6 1 B 6

/ v
\ L/W=3 i
I C 6
n c o o
1
D
C
C
6
0

/ 1
V/
^s 111 C 0 0 10 C 0

A 1 n c o i
ID C 0 1
U
in
C
C
0
0
Mesh Division D C 6 0 n C 6
111 C 6 0 111 C 6
A:16X48, B:24X72. C : 3 2 X 9 6 n c 6 i 11 C 6
I1CC 1 m C 6
Specimen Size
I :W=W 0 , II:W=1.5Wo. II!:W=2Wo
Fig.l. Computational model and notation.

deformation, 1/4 of the block with finite element discretization shown in

Fig.l is investigated. Each quadrilateral shown here consists of four
crossed constant-strain triangular elements. Heat generated by viscoplastic
work is assumed to be discharged through convection to air at the side
surface. The remaining surfaces are assumed to be adiabatic boundaries. In
all calculations described here, representative stress a , absolute
V
temperature T, representative viscoplastic strain ? P and representative
viscoplastic strain rate e are related by

5=T (K(T)/K(T))(2.287+1.986tanh(31.16eVp))(|Vp/G )" (5)

c U y
K(T)=0.00214T2-2.632T+991.3

where T and e are material constants. The constitutive equation of the

temperature and strain rate independent limit well describes the
deformation behavior of the polycrystal. Material and computational
parameters are V=0.3, u>=1.0, G =0.001/S, T 60.84MPa, Cn=0.005, C=yCn
y c -6 X=59W/(mK). X =0.1256
E=1000T , m=0.005, T =T . =296.15K, a=11.6*10 air
c 0 air
*10 5 W/(m 2 K), p=7.87*103Kg/m3, U=(u/L)/e =1,106 W =0.032mm

RESULTS AND DISCUSSION

Here, we focus our attention on the effect of the strain gradient in the
flow stress, the finite element mesh size employed and the size of the
specimens on the flow localization behaviors. In order to clearly specify
the computational results, the notation shown in Fig.l will be employed
henceforth.

The effect of the strain gradient term in the constitutive equation on the
flow localization is investigated with four different C values in Eq.(3).
The normalized end displacement rate is set at U=l,10 . As predicted by
analytical investigation (Zibib and Aifantis, 1988), the nonlocal effect
stabilizes the deformation, and considerably postpones the growth of the
shear bands accompanied with a rapid drop in force with an excessive
distortion of finite element mesh. Henceforth, the value of C will be set
at 0 or C . The former stands for the local case and the latter represents
the nonlocal case.
200

(a)u«0.125 (b)u»0.15 (c)u«0.11 (d)u-0.125

Vp
Fig.2. Representative strain e distribution
in the shear band

In order to clarify the effect of finite element mesh size on the flow
localization, three different mesh divisions shown in Fig.l are employed
for specimen I. Regardless of the deformation rate, until flow localization
starts, the deformations predicted by the different mesh size are almost
identical. However, a different nature of the flow localization depending
on the mesh size is clearly observed in the local case. That is, in the
local case, refinement of the mesh size causes intense flow localization
with a rapid drop in force. On the other hand, since the refinement of the
mesh size makes it possible to estimate the more local strain gradient, the
stabilization effect increases as the mesh size reduces. This may cause the
reverse relation in the order of force-displacement curves with C=C as
compared with those of the local case. However, the difference observed in
the nonlocal case is smaller than that in the local case.

Figure 2 depicts the representative strain distribution along the

crosssection normal to the shear band. With reduction of the mesh size, a
more intense flow localization appears in (a) and (c). Meanwhile, (b) and
(d) show that the predictions of shear band thickness and strain
distribution are rather insensitive to the finite element mesh size. In the
local case, regardless of the mesh size, the mesh sets a minimum width for
the band, which essentially corresponds to the element size. Consequently,
it can be said that the strain gradient term in the constitutive equation
reduces the mesh dependency of flow localization behavior.

l
n r

0 .05 .1 .125 0 .05 .1.11

u u
Fig.3. Force tj vs displacement *u
 201

(c)u=0.11 (d) u=0.11

Fig.4. Deformed mashes and representative
strain e v p contours

F
Fig.5. Representative strain e distribution
in the shear band

The size dependency of the flow localization is investigated for three

different sized specimens, I, II and III, with the finite element mesh C
in Fig.l. Figure 3 shows the force a vs displacement ti. Figure 4 shows
the deformed meshes and representative strain contours. In order to
directly compare the results, the sizes of II and III are normalized to
that of I. Both patterns of meshes and strain contours for the local case
202
(a) are almost the same. This implies a size-independent feature of the
flow localization behaviors. As can be seen in the nonlocal case (b), the
more intense localizations appear as the size of the specimen increases.

This can be more clearly seen in Fig.5, which shows the representative
strain distribution across the shear band. The thickness of shear bands is
almost independent of the size of the specimen in nonlocal cases (b),
whereas strong dependence is observed in the local case (a). Of course, as
discussed by Tomita et al (1990), the thermal effect contributes to the
size dependent flow localizations. Hence, in the case with U=10 where the
thermal effect is active, more localized deformation is equally observed in
Figs.3-5 as the specimen size increases.

It should be mentioned that the difference in the magnitude of the

representative strain for the same displacement is attributed to the
almost identical thickness of the shear band. When the shear band develops
sufficiently with the same thickness for the different sized specimens, the
displacement arising from the shear localization with almost the same
inclination should be independent of the size. A more intense localization
is required to attain the same displacement u for the larger blocks. As
discussed in this paper, it is noted that the results presented above may
be slightly affected by the size-dependent nature of the Laplacian operator
in flow stress.

CONCLUSIONS

In this study, the thermocoupled flow localization of plane strain tension

blocks obeying an elasto-viscoplastic constitutive equation with a strain-
gradient-dependent flow stress was investigated. The effects of the strain
gradient in the flow stress, finite element mesh size, and size of the
specimen on the flow localization have been clarified.

ACKNOWLEDGMENTS

The present work has been partially supported by the Grant-in-Aid for
Scientific Research, Japanese Ministry of Education. Their support is
gratefully acknowledged.

REFERENCES

Aifantis,E.C.(1984). On the micro structural origin of certain inelastic

model, Trans. ASME, J. Eng. Mat. Tech., 106. 326-330.
Bazant,Z.P., F.B.Lin and G.Pijaudier-Cabot(1987). Yield limit degradation:
nonlocal continuum with local strain. Proc. Int. Conf. on Computational
Plasticity. Barcelona, ed. by Onate, E. et al., University of Swansea.
1757-1779.
Peirce,D., C.F.Shih and A.Needleman (1984). A tangent modulus method for
rate dependent solids. Comp. Struct., 18, 875-887.
Tomita,Y. and A.Shindo (1985). Bifurcation behaviors of thin square
elastic-plastic orthotropic plates subjected to diagonal tension. Proc.
Int. Symp. on Plastic Instability. 203-213.
Tomita,Y., A.Shindo and T.Sasayama(1990). Plane strain tension of thermo-
elasto-viscoplastic blocks, Int. J. Mech. Sci. , 32, 613-622.
Zbib,H.M. and E.C.Aifantis(1988). On the localization and post localization
behavior of plastic deformation. I On the initiation of shear bands, Res
Mechanica 23, 261-277.
WS1e3

GRADIENT DEPENDENT VISCOPLASTIC MODEL FOR CLAY AND NUMERICAL

EXPERIMENTS BY FEM

Fusao OKA and Atsushi YASHIMA

Dept. of Civil Engr., Gifu University, Gifu, Japan
Toshihisa ADACHI
School of Transportation Engr., Kyoto University, Kyoto, Japan
Elias C. AIFANTIS, Dept. of Mech. Engr. and Engr. Mech.
Michigan Technological University, Houghton, USA
Aristotle University, Thessaloniki, Greece

ABSTRACT
A gradient dependent viscoplastic constitutive model for water saturated
clay is proposed. A linear perturbation stability analysis is applied to this
model. We disccussed the instability of this model and the application to a
boundary value problem. Finally, we carried out a numerical experiment by
using a finite element method.

KEYWORDS
GRADIENT VISCOPLASTICITY; FINITE ELEMENT ANALYSIS; CLAY

GRADIENT DEPENDENT VISCOPLASTIC MODEL FOR CLAY

In relation to the strain localization problem, a new approach has been proposed where
strain gradients are introduced into the constitutive model(e.g. Aifantis 1987). Following
this approach, Oka et al.(1991) developed a gradient dependent viscoplastic model for
clay and showed the role of the second gradient of viscoplastic strain. In this section, we
introduced the second gradient of viscoplastic strain into the constitutive model of clay
Adachi and Oka (1982). These authors developed an elasto-viscoplastic constitutive model
for clay based on overstress type viscoplastic theory.
The viscoplastic flow rule is given by

<»=< w >i£ (i)

where e"* is the viscoplastic strain rate, (7^ is the stress tensor, / is the dynamic yield
function, $ is a material function accounting for the strain rate effect. (F = 0 denotes the
static yield function).
It has been found that the shear strength and deformation characteristics of clay de-
pends on the volumetric strain. The volumetric strain is a measure of the deterioration
of the granular material. We have, therefore, introduced the second order gradient of
volumetric strain into the constitutive model.
The yield function now includes a gradient term and it is expressed as follows:

203
204

where X is the gradient term, i.e. the second order gradient of the viscoplastic volumetric
strain, Ji is the second invariant of the deviatoric stress tensor Sij , a'm is the mean effective
stress and a1 is the strain hardening parameter. In the following, we will use Terzaghi's
effective stress a[-. The material function <&(F) is given by

• ( F ) = c • e * r { m ' ( ^ | | + ln£- - ± ± V + X)} (3)

c = c0exp{m'ln-?2-} (4)
^myO

and we assume that M*, m! and c are material constants. In Eq.(3)} a'mc is the initial
value of a'mi A is the consolidation index, K is the swelling index, e is the void ratio, and vp
is the volumetric plastic strain. The elastic strain rate is assumed to be obtained by the
isotropic Hooke's law.

TWO-DIMENSIONAL INSTABILITY ANALYSIS

In this section, we consider a two dimensional motion under plane strain undrained
conditions with axial stresses in order to determine the preferred orientation of the localized
zone where growth of the fluctuation occurs(the orientation of shear band)(Anand et al.
1987, Zbib and Aifantis 1988).
The plane strain undrained condition (e33 = 0 , €n + e22 = 0 ) implies

5 33 = 0, a'3=^±A (5)

„; _ °i + Q* nrr_ K - ^ l „ g g _ < - °'i (fj^nt\ (R\

m = 2
—2—' * 2 2' 2 —2— *l ' * '
In view of the undrained condition and the initial condition (vp = 0), Eq.(3) becomes

where p' = a'm and X' is the gradient term.

Next we consider the equilibrium equation, the undrained condition and the constitutive
equation in the perturbed configuration. The perturbations of stresses <ii, velocities v;,
volumetric viscoplastic strain vp are assumed to be as usual of a periodic form

a = < „l > = a*exp(iq(niXt) -\-wt)) <j* = < J, >

Vi = v*exp(iq(riiXi) + ut) . .
vp = vpexp(iq{niXi) + wt) *'
where rii is the component of the unit vector h which is normal to the shear band(Fig.l)
h = (—sin9, cos9) = (ni, n2) (9)
By using the equilibrium equations, the undrained condition and constitutive equations,
the following relation are obtained
%qa\n\ = 0, iqo^rii — 0, v\ri\ + v*2ri2 — 0 (10)
 205

A^l + A2o\ - H2vp* - H3X' - iqmvl = 0 (11)

uv?* = H'0al + tfja; - jyjtf - H'3X'. (12)
where IT/ , Hi and A; are material coefficients. We will consider two kinds of gradient
term X'\ One is related to an isotropic gradient effect and the other to a directional second
gradient.

Isotropic gradient(Zbib and Aifantis,1988)

When we assume isotropy, the gradient term can be expressed by the Laplacian as

X' = W . (13)

With the aid of £9.(8)3, we obtain

X' = - g V . (14)
and the corresponding eigenvalue equation reads obtained as

u> = -H'2 + Htf. (15)

For u = 0, the critical wave number qc is obtained as:
/a7 A(l + e) , / . , . , , Al x 27r , .
qc = \ —, <*i = —TT r, Ucntical wave length) = —. (16)
y a3 K(\ - K) qc
From Eq.(\b), it is seen that there is no preferred orientation of the band. Moreover, the
perturbation with the wave length / which is larger than lc never grows. In other words, it
is seen that for the stiff clay with the larger value of a1} the inhomogeneous solution with
small wave length grows rapidly compared with soft clay.

Directional second gradient(Oka,Yashima, Adachi & Aifantis 1991)

We consider a directional differential operator DO(2) expressed by

nd?_ , , d2 n,2j?_
DO(2) = " fdx\
e + 2 n1 W
2 ir-o- +
dxidx2 2
dx\ fc (17)

in which n' = ( n j , ^ ) = (—sin£,cos£) is a arbitrary unit vector.

In order to obtain the directional gradient term X\ we used this operator DO(2) for
volumetric viscoplastic stain. It is worthnoting that DO(2)(vp) is frame-indifferent. In this
case, the preffered orientation of the band is obtained (Oka et al 1991).

FINITE ELEMENT ANALYSIS USING A GRADIENT DEPENDENT

VISCOPLASTICITY THEORY

Higher order gradient terms have been introduced into the constitutive equations to
simulate localization phenomena in the media of infinite extent. However, there is still a
difficult problem to be solved when we apply a constitutive equation with gradient term
to solve a boundary value problem defined in a finite domain. Recently, Miihlhaus and
Aifantis (1989) pointed out the importance of this and proposed a variational principle. In
the present study, we assume the weak form of the dynamic yield function that contains
the second gradient of viscoplastic strain and the boundary condition in terms of the first
gradient of volumetric viscoplastic strain. In the present model, the dynamic yield function
corresponds to the volumetric component of the flow rule.
206
For the first gradient vp, we consider the flux Q associated with internal structure
change. We have

/ (/ - a n f - a 3 V V - g{i?))Wdv + / (Q - Vnvp)6vphds = 0 (18)

JV JSi

where Q is the microstructure flux, Si is the boundary where Q is defined, and 8vp is
the virtual volumetric viscoplastic strain associated with virtual displacement 8u during
the deformation process. In the psresent study, viscoplastic strain rate is assumed to
always occur. From Eq.(\$), we obtain the relation between the following equation for the
microstructure change flux Q.
Q = V„tf (19)
where V n is the normal gradient to the boundary.
For the total equilibirum equation, we use the well known virtual work theorem. When
we implement the proposed model into the FEM code, we need the boundary value of
Q. In this respect, we postulate that the flux Q is zero at the boundary between rigid or
elastic material and viscoplastic one. From a physical point of view, we could say that for
a material that never deforms plastically, the flux Q never flows into the material, and also
the flux Q never outflows from the viscoplastic material into rigid or elastic materials.
At the boundary where the stresses are specified, like a free surface of the ground, the
flux Q is also assumed to be zero. For the deformation analysis with consolidation, we
could use the same method as used by Oka, Adachi and Okano(1986). They combined
the finite element method with the finite difference method. The equation of motion of
the fluid phase is discretized by a backward finite difference scheme. The finite difference
scheme is also used to explicitly calculate the second gradient of viscoplastic strain. In
Figure 2, the finite difference grid for the rate of microstructural change flow is shown.
NUMERICAL EXPERIMENT
To examine the effect of gradient term, we have numerically analyzed the strain rate
constant compression test under undrained plane strain condition. A weak element is
introduced to enhance the growth of inhomoeeneity. In the weak element, the material
parameter C is three times larger than that in the perfect element. Figure 3 shows the finite
element mesh and the boundary conditions. The material parameters used for calculation
are as follows: Af*=0.865 ,C = 1.0 x 10~12 1/sec, initial mean effective stress cr'me =
1.5kgf/cm2, initial stress ratio = 1.0, m' = 25, A = 0.231 ,K = 0.05 , void ratio = 1.5,
elastic shear modulus G = 20kgf/cm2 , permeability coefficient = 1.16 x 10~ 10 m/sec,
a3 = 50.0, e22* average axial strain rate is 0.2 %/min. Figs. 4 and 5 show the distribution
of second invariant of the deviatoric the viscoplastic strain rate tensor j p = (Je^e^) for
two cases( with and without strain gradient) at the axial strain e22 of 2 %. It is seen that
the inhomogeneity grows with the increase of average strain and the localization intensity
in the case that the gradient term is introduced is larger than that in the case without the
gradient term. In Figure 6, we can observe the checker board pattern at larger average
strain of 2.8 %.
REFERENCES
Aifantis E.C.(1987), Int. J. Plasticity 3, 211-247.
Oka,F., Yashima, A., Adachi,T. & Aifantis, E.C.(1991), Proc. 3rd Int. Con}, on
Constitutive law for Engineering Materials, ed. by C. S. Desai 1991 Tucson.
Adachi, T. and Oka, F.(1982), Soils and Foundations, 22, 4,57-70.
Anand, L., Kim, K.H. and Shawki, T.G.(1987). J. Mech. Phys. Solids, 35,407-429.
Oka,F., Adachi, T. and Okano, Y.(1986), Int. J. Num. Anal. Methods in
Geomechanics, JL0, 1-16.
Zbib, H. M. and Aifantis,E.C.(1988), Res. Mech., 23,261-305.
Mulhaus,H. and Aifantis,E.C.(1990), MM Report ,17, MEEM Dept,
MTU, Houghton, MI 49931.
 207

1
V b4
Shear band

'U)

'(H- '(3)

n=(-sinO, cosO)

■43J-
2 p p
7 v = 3v z B ^ P . ) , B.= b ^ s .
o 1
Fig. 1 Graphic representation
of shear band Fig. 2 Evaluation of gradient term V v
p

lt>
lt>
lt>
\t>
lt>
ID
\t>
lt>
ll>
IO
impermeable
lt>
boundary
IO
lt> /
IO
ID>
IO

II>
Weak
«flr~7r~7n n r~zr~zn r~zr~kelement
Fig. 3 FEM mesh
208

. U -408 .377 13 .011

Fig. 5 Contours of Y P for
Fig. A Contours of t P for a = 50 , average strain
3
a~=0, average strain 2 %
J
2 % (with gradient)
(without gradient)

YYYYWWYYi
WnAAAAAAA
\\\\AAMAM
VWWWYYY\ for a~ = 50, average strain
WAAAAYAA •* 2.8 %
W\\AAAYW\
W\AAA/VVV\A
V\AAAA /
VW\A
(with gradient term )

\MAM/Y\AAA
\YYYWYYW\ x1(T* (1/sec)
\/i/[/W □ <0.3
{/p&i/i^^
hq [HP I/fed &8$sa/1
tf¥W™
r^**N *wvi \Z\ 0.3-0.5

I M I HT I HL/M B3 0.5-1.0

Jtf&oq_ _W| I pod/bn m >i.o

HrnHnsW/H
Fig. 6 Distribution of yp
WS1e4

ANALYSIS OF THE PLASTIC INSTABILITY AND FRACTURE

OF A THERMALLY AGED CAST DUPLEX STAINLESS STEEL

SUN YI, C. DUVAL and G. ROUSSELIER

Electricity de France, Departement MTC,
Les Renardieres, 77250 Moret sur Loing, FRANCE

ABSTRACT

The plastic instability and fracture of a cast duplex stainless steel is

analysed by applying the deformation gradient theory. The critical conditions
for the crack initiation in three different types of notched specimens are
derived and detailed finite element calculations are made. The theoretically
predicted critical values are in good agreement with the experimental results.
Also the predicted location and orientation of initiated cracks correspond
quite well with the experimental observations.

KEYWORDS

Ductile fracture, shear localization, duplex stainless steel, deformation

gradient theory.

INTRODUCTION

The long-term aging behaviour of cast duplex stainless steels has been
extensively studied since the last ten years. Recently, special attention is
focused on the fracture properties of these materials aged at the working
temperature (320°C) for a long period. At room temperature, the fracture
process is described as the formation of cleavage microcracks in the ferrite
phase and final fracture occurs by the linkage of these microcracks (Bonnet
et al., 1989). However, when tested at the elevated temperature (320°C), the
fracture mode is totally changed (Duval, 1990). In fact, very little secondary
damage is observed besides the main crack (Bonnet et al., 1989). The fracture
process is a sudden plastic instability process which exhibits many features
of shear localization. In simple tension test, fracture occurs while the
material still shows a strong positive strain hardening rate. Such kind of
phenomenon could be hardly explained by a bifurcation analysis with simple
209
210
classical constitutive equations. Recently, a different approach was proposed
(Aifantis, 1984, Coleman and Hodgdon, 1985) by introducing higher-order strain
gradients into the constitutive equation, which released the usual necessary
condition of the loss of ellipticity of the equilibrium equations. While the
introduction of the higher-order strain gradients is more intuitive than from
deduction, it seems quite effective and could model in certain extent the
influence of local nonhomogeneity. In the following we first outline some
basic equations in the deformation gradient approach, then we make a detailed
analysis of the crack initiation in three different types of notched
specimens. Finally we compare the analytical results with those of the
experiment. Good agreements are obtained.

GOVERNING EQUATIONS
—^ —* _i

We denote by v the spatial velocity vector, D the strain rate tensor, o the
Cauchy stress. When the plastic deformation is large, we can neglect the
elastic part. Then the constitutive equations for the isotropic von Mises
material are given as
~£=-pt+2\iD i (1)
u = T/Y

where
1/2
■ ( * * ■ * )

a' = ?- i tr (a)t ( (2)

Y = (2D : D)1/2

For the hardening relation, we add in the second-order deformation gradient

term (Aifantis, 1984)

T = T (Y, V 2 Y ) , (IT = hdy + c d (V 2 Y ) (3)

2
where V is the Laplace operator. The bifurcation analysis is carried out by a
linear perturbation method (Zbib and Aifantis, 1988). The perturbations Av and
Ap are taken of the form
Av" = cv exp (iq n.x + Wt)
(4)
Ap = cp* exp (iq "n.x + Wt)

where 0 < £ « 1, |v*| = 1 . With the incompressibility condition and the

equilibrium condition we have

~1 (h "w^ " ^ ( D-n)(D.^) + ut . v* + i p * ^

(5)
>
 211
The above equations can also be rewritten as

AY = 0 (6)

where Y = (v*p v*2> v*5, p) . The condition for the existence of non-trivial
solution is
det(A) = 0 (7)

For the axisymmetric case, we chose the cylindrical coordinates system

Xi = r, Xo = 9, x-r — z

with
D = D = D
12 21 23 = D 3 2 = 0 (8)

Let *P be the angle between "v* and r axis, then

n^ = -sin <P \
n2 = 0 > (9)
n, = cos y> /

A detailed calculation of (7) yields

h - cq2
W = - (10)

1
^IATT^T - )
where \

f W ) = | D 1 3 cos 2^ + - ( D „ - D n ) sin 2^1 (11)

From (11) we get

D
1 , 33 " Dll
- tan"-1 , D,,
13
* 0
2 2D 13

^1-in , D13 = 0
I <12>

, /'D,,
D
33 -" DD, •2
ll\
f
<^1> = f»

Combining (2) and (12) we can prove the following inequality

2
Y
1 £ 0 (13)
4f W
The condition for the growing of an inhomogeneous perturbance is w ^ 0. Notice
that the lower part of equation (10) is always bigger or equal to zero, so the
212
instability condition could be given as

h - cq 2 ^ 0 (14)

The perturbation will grow along the direction where

1
h c 2
w, . - q

fe" )
w =
max
" / i2 \ (15)

If we take c and q as material constants, the critical condition could be

given as
h = hc , <pc = ^ (16)

NUMERICAL RESULTS AND COMPARISON WITH THE EXPERIMENTS

Based on the above criterion, we analyse the fracture initiation in three

different types of notched specimens. The material used in the experiments is
an aged duplex stainless steel CD7 (Duval, 1990). The tests were carried out
at the temperature of 320°C. The geometries of the specimens are shown in
Fig. 1.
:
Notice that h is a decreasing function of y

h ^ h = cq 2

With the assumption

IV2 Yl
q2 » — H - ' (17)
Y
we can neglect the c term in (3) in the finite element calculation. The
justification of (17) could be given by direct experimental observation of the
distance between the deformation bands and the theoretical estimation of
|V Y |/Y term. However, it is only limited to the present notched specimens.
For the cracked specimens there exists a strong singularity of the deformation
fields in front of the crack. In this case it seems necessary to directly
incorporate the c term in the calculation. In the case of monotonic loading,
(16) could be rewritten as
(o
e > - « = CTc > *c - *1 (18)

where o„ is the equivalent stress and aQ corresponds to the instability

point in the experiment. The a value is then determined by the finite element
calculation. In the present study we determine a c by AE2 notched specimen
(fig. 1 ) . The result is aQ = 853 MPa. The finite element calculation for the
three types of notched specimens is carried out on EDF's programme ALI-BABA
with Lagrange large deformation formulation. One of the meshes used in the
calculation is shown in fig. 2.
 213
Table 1 gives the comparison between the experimental results and the theore-
tically predicted values with a = 853 MPa. A very good agreement is obtained.
The predicted location and orientation of the initiated cracks for the three
types of notched specimens are shown in fig. 3, which correspond quite well
with the experimental observations (Duval, 1990).

DISCUSSION

The good agreement between the predicted values and the experimental results
supports the application of the deformation gradient theory to the present
case. Although the physical meaning of the gradient term is not yet clear, it
seems quite reasonable to incorporate certain parameters which could reflect
the influence of local deformation patterns on the instability and fracture.
In fact, recent examination (Sun and Rousselier, in preparation) shows that
the gradient term relates to the local nonhomogeneity development. This might
concern some basic problems in deformation localization analysis.

In the above analysis the aging effect is not shown explicitly. It is believed
that such effect is implied in the variation of the parameters h, c and q. In
fact, the aging effect on the micromechanism of plastic deformation of the
ferrite phase, especially at elevated temperature, is not yel fully explained,
and further efforts are needed both in mechanical and metallurgical aspects.

REFERENCES

Aifantis, E.C. (1984). On the microstructural origin of certain inelastic

models. Trans. ASME. 3. Eng. Mat. Tech., 106, 326-330.
Bonnet, S. et al. (1989). Evolution of mechanical properties of various cast
duplex stainless steels in relation to metallurgical and aging parameters:
an outline of current EDF programmes. International Workshop: "Intermediate
temperature embrittlement processes in duplex stainless steels". Oxford,
Aug. 1-2.
Coleman, B.D. and M.L. Hodgdon (1985). On shear bands in ductile materials.
Arch. Rational Mech. Anal., 90, 219-247.
Duval, C. (1990). Mod61isation de l'endommagement des aciers austeno-ferriti-
ques vieillis. Ph. D. thesis. Ecole Centrale de Paris.
Zbib, H.M. and E.C. Aifantis (1988). On the localization and postlocalization
behavior of plastic deformation. I. On the initiation of shear bands. Res
Mechanica, 23, 261-277.
214

Table 1. The maximum load and diameter

contraction at instability of CD7
axisymmetric specimens.

2==iZ
Diameter Contraction
Maximum Load (kN)
at Instability (mm)
Specimen

theory experiment theory experiment 18* -0.05 M 0 * -005

AE2 75 75 0.39 0.39

AE4 72 72 0.60 0.61

AE10 65 65 0.79 0.81

vr-^c
18* -0.05 I 10* -0.05

7A:

MM
90

21 " = 10 R = 10 21

/ /
A
"Ii
18* -0.05 J l O * -0.05 22
1
/*—"X
J ' > 1/ _
90

Fig. 1. The geometry of the specimens.

Fig. 2 . The finite element mesh for A E 2 specimen.

8.0-

6.0"

4.0-
/ ^
2.0-

0.0-
44.2^K/
f
2.0- 1 1——i 1 r —
-2.0 0.0 2.0 4.0 6.0 8.0 10.0 -2.0 0.0 2.0 4.0 6.0 8.0 10.0 -2.0 0.0 2.0 4.0 6.0 8.0 10.0

(a) (b) (c)

Fig. 3 . Predicted location and orientation of initiated cracks.

(a) A E 2 specimen
(b) A E 4 specimen
(c) AE10 specimen.
WS1e5

A NUMERICAL MODEL OF TENSION TEST DURING DYNAMIC

RECRYSTALLIZATION COUPLED WITH PLASTIC INSTABILITY

A. BELKEBIR, P.-H. YI, F. MONTHEILLET and A. KOBYLANSKI

Ecole Nationale Superieure des Mines, Departement Mat&iaux

158, cours Fauriel 42023 SAINT-ETIENNE, CEDEX 2, FRANCE

ABSTRACT
Tension stress-strain curves during hot deformation of steels in the austenitic range exhibit a
particular shape which is sometimes difficult to interpret. This is due to the simultaneous
occurrence of dynamic recrystallization and the development of necking by plastic instability. In
order to study the possible interactions between these two mechanisms, analytical expressions
where first determined to describe the stress-strain relationships. A slice model was men used
for predicting the necking development during hot deformation.

KEYWORDS
Hot deformation ; dynamic recrystallization ; tension test; plastic instability.

INTRODUCTION
The main difficulty encountered in the processes of hot working is the loss of metal ductility
following some damage mechanism. One of the important uses of hot working tests is to
determine how ductility varies with chemical composition, microstructure, temperature, and
strain rate. In the tension test, ductility is characterized by the reduction of area at fracture Z.
However, during hot deformation of steels in the austenitic range, the value of this parameter is
simultaneously affected by the dynamic recrystallization (DRX) and the plastic instability which
causes a necking in the specimen ; Z is thus more difficult to relate to the material ductility.
In order to study how these mechanisms can affect ductility, a mathematical model of hot defor-
mation was used to describe the stress-strain curves in the form a = f (££,T) (0.6 < T/Tf< 0.8).
With the aid of a cumputer simulation, a slice model was used for predicting the necking
development in a specimen undergoing DRX at various temperatures and strain rates, and
theoretical load-elongation curves were calculated.

MATHEMATICAL EXPRESSIONS FOR STRESS-STRAIN CURVES WITH

DYNAMIC RECRYSTALLIZATION
The stress-strain curves during hot deformation of steels in the austenitic range exhibit a
specific shape which characterizes the occurrence of DRX (Jonas and Mc Queen, 1976). The
latter takes place when the strain is larger than a critical value 6c fig. 1 (Roberts, 1979). At high

215
216
strain rates, the flow stress rises to a maximum Gm for a strain e m , it then decreases to an
intermediate value GS between the yield stress G0 and the peak stress o m . At low strain rates, or
high temperatures, the flow stress exhibits several waves due to periodic cycles of softening an
hardening during deformation. The stress amplitude of these cycles decreases progressively to
the stationary value Gs.

In order to describe the experimental results of hot tension tests, mathematical expressions were
determined to represent the relationship between stress and strain with DRX exhibiting single or
multiple peaks. Some equations quoted in the literature (Palm, 1948 and Wray,1982) indicate
that the stress-strain relationship can be described by the following form :
G = (G0 - GS) exp (- a e) + GS (1)
where a is a material constant.
However, this equation does not represent the flow stress for T/Tf > 0.6 and for DRX with
multiple peaks. Therefore, other forms of stress-strain relationship are proposed (Yi et al.,
1990) here to describe the dynamic recrystallization exhibiting single or multiple peaks in the
temperature range 0.6 < T/Tf < 0.8.
In the case of a single peak :
G = f(e) exp (- a e) + GS (2)
where a is a material constant, and f(e) a function which characterizes the work hardening f(e)
is determined as follows : for e = 0, G = GOJ and f(e = 0) = GQ - Gs. Thus, a linear function
can be chosen:
f(e) = G 0 - GS + A e (3)
where A is a material constant.
The effect of strain rate can be included in (2) by the factor (e / ei) m , where m is the strain rate
sensitivity of the material, and 6i a reference strain rate (£i = 1 s_1).
Finally eq.(2) becomes
G = Gog(e)(e/ei)m (4)
where g(e) = [ ( G G - G S + A e) exp (- a e) + cs]/oQ (5)
When DRX exhibits multiple peaks, g(e) becomes
g(e) = [(G 0 - G S + A e) exp (- a e) h (e) + OS]/G0 (6)

where (7)
^"(^(e-eJltS.'eVt
and 2 7i/B is the period of the cycles on the stress-strain curve.
For any given temperature, the rheological parameters A, a, m, and B can be determined from
experimental stress-strain curves obtained by compression or torsion tests where necking does
not occur.

NUMERICAL MODEL OF THE TENSION TEST

A slice model was used (Fig. 2) to predict the necking development in a cylindrical tensile
specimen. Furthermore, the effect of stress triaxiality in the vicinity of the minimum cross
section was also introduced in this model according to the Bridgman (1944) approximation.
Given the initial length LG and the nominal radius R0 of the specimen, the parameters of the
system, when referred to the initial configuration (L0, AG, R0, ...)> are defined for a N slice
model as follows:
 217
Geometrical parameters Mechanical parameters
Thickness 5i =
t Strain *i =
**(*]
Cross section area Pi = £ Strain rate k = 5i
L-L0
Position Xi = &
Elongation = "XT"
e

Radius Ri =
£ Elongation rate e = L

If Oi is the uniaxial mean stress in the slice i, and Gn the measured nominal stress, the
equilibrium equations of the system reduce to :
C te
0i Ai = = = F = a n A0 (8)
Now, according to the Bridgman approximation,
(* = Ti a (9)
where a is the flow stress of the material defined by eq. (4), and Ti is the triaxiality factor of
stress defined by :

H 1+ ^) Ln ( 1+ :fe) (10
>
where T{ is the radius of slice, and pi the radius of curvature (Fig. 2).

From eqs (4), (8) and (9) we get

8i = § e (i =
On (e / £ i ) m *) (ID
and
(12)
where p. °i
1 1
[gteOTipi] /™ (13)
N
and Q = X Pk (14)
k=l

Finally eq. (14) becomes

d5;
^ = <P(Sk) (k
(k = 1, N ) , (i = 1, N) (15)

for e varying from 0 to emax by steps Ae where the 8i are determined by simple integration of
(15) and OTJG0 is calculated from (12).
To produce a necking in the specimen during the simulation, an initial geometrical defect is
introduced by giving the parameter p initial values lower than 1 in one or several slices.

RESULTS AND CONCLUSIONS

The results of the simulations were obtained from the following data : the material is a high
purity steel containing 0.021 % C, 0.034 % Nb, 0.0027 % S. The Theological parameters
(Table 1) were determined from experimental stress-strain curves exhibiting single peak
(950°C), or multiple peak (1100°C) DRX.
Fifty slices are used to represent the initial geometry of the specimen which has a length to
diameter ratio about 4. The thickness of each slice is §x = 0.2 (i = 1,50). A initial geometrical
defect is also introduced : the slices from i = 16 to 34 are affected ; the normalized length 5 of
this defect is 0.38 and the minimum of the parameter p is 0.99 at i = 25.
218

The conditions of the test simulations are for both temperatures e = 2x10~3 s"1, Ae = 10~2,
emax = 0.62 for 950°C, and emax = 0.70 for 1100°C.
Table 1. Rheological parameters of the material at 950°C and 1100°C.

Single peak DRX Multiple peak DRX

Temperatures (°Q 950 1100

G0 (MPa) 50.50 26.83

Gs (MPa) 42. 55.40
A (MPa) 729. 328.
a 3.44 11.4
m 0.1 0.1
0.2 0.12
1" 42.8

Figure 3 shows the variation of the normalized nominal stress On/o0 with respect to the
elongation e (curve a). To bring into evidence the influence of triaxiality, the calculation was
also carried out without Bridgman correction (curve b). The third curve c corresponds to a
sample without initial defect. The evolutions of the minimum section of the specimen are
depicted in Fig. 4. Localization occurs at e = 0.48 and 0.42 for the (a) and (b) cases,
respectively : this shows that triaxiality delays neck development by inducing propagation of the
defect to the neighbouring slices. The same conclusion can be drawn from Figs 5a and 5b,
which show the elongation dependence of the sample profile without (Fig. 5a) or with (Fig. 5b)
triaxiality effect.

The same results are illustrated in Figs 6 and 7 in the case of multiple peak DRX. The sample
profile are similar to the single peak one. Furthermore, it should be noted that the early
occurrence of necking due to the first softening stage is strongly slowed down by the following
strain hardening stage, so that instability takes place for about the same elongation as in the first
case.

The main conclusions of this work are the following :

(i) For the flow rule and the initial defect investigated, instability occurs significantly later than
dynamic recrystallization, in the two cases of single (lower temperature) or multiple peak
(higher temperature).
(ii) In particular, in the case of multiple peak DRX, instability does not occur during the first
stage of softening.
(iii) The model gives a rather good description of the hot tension curves. Nevertheless, it has
still to be improved by the introduction of a fracture criterion, in order to make theoretical
predictions of the reduction of area at fracture.

° m _.
T,<T 2
" ^ ^ ^ T,
F measured

.... 12 / i
/
A* £m
a, T
2 /
JJiL
0
h
\U ^ i j j s,
'ce i defined by:
1
thickness lf ; radius r ,-
position x { ; area A,

Fig. 1. Stress-strain curves during hot Fig. 2. N slice model used for the
deformation with dynamic simulation.
recrystallization.
 219

1.2
- Single peak
o 1.0

0.8

/ I
(c)
o \
.E 0.4
E
o
Z
0.2 [ (b)^
V va)
0.0 L i i i i i i i

0.0 0.2 0.4 0.6 0.8 0.2 0.4 0.6 0.8

Elongation e Elongation e
(a},(b) with initial defect. (a},(b) with initial defect.
(a) with triaxiality. la) with triaxiality.
(b) without triaxiality. fb) without triaxiality.
(c) without initial defect. (c) without initial defect.

Fig. 3. Load-elongation curves calculated Fig. 4. Variation of the minimum section

at 950°C, for steel containing of neck with elongation.
0.021 % C,0.034 % Nb and
0.0027 % S.

1.1 1.1
Single peak Single peak

e-0.00 e-0.00
1.0 1.0
0.08 0.08
of 0.16
>
«0.9 «)0.9
3
'•5
o
a:

0.8 0.8

0.7 0.7
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Initial position jflo Initial position xto

Fig. 5a. Specimen profile calculated without Fig. 5b. Specimen profile calculated with
triaxiality, for 5 elongations, and triaxiality, for 7 elongations, and
N = 50 slices. N = 50 slices.
220

1.2 1.4

i Multiple peaks Multiple peaks

~1-0
so.
c
(0
0.8 .2 0.8
CO O
0>

is
Q>
CO
L.
CO 0.6 f \ ,.0.6
E (c)
o E • \ \
.E 0.4 |0.4
E
o bs
Z
0.2 \(b) \(a) 0.2 ( b ) \ \ ^

0.0 1 . i i i I I n r\ I 1 I 1 I 1 I
0.0 0.2 0.4 0.6 0.8 0.0 0.2 0.4 0.6 0.8
Elongation e Elongation
(a},(b) with initial defect. (a),(b) with initial defect.
(a) with triaxiality. with triaxiality.
(b) without triaxiality.
without initial defect. 8 without triaxiality.
without initial defect.

Fig. 6. Load-elongation curves calculated Fig. 7. Variation of the minimum section

at 1100°C, for steel containing of neck with elongation.
0.021 % C0.034 % Nb and
0.0027 % S.

REFERENCES
Bridgman, P.W. (1943). The stress distribution at the neck of a tension specimen. Trans. Am.
Soc. Metals, 22, 553-574.
Jonas, J.J. and H.J. McQueen (1976). Recovery and recrystallization during high temperature
deformation. Mise en forme des mitaux et alliages, 99 -143, Editions du C.N.R.S., Paris.
Palm, J.H. (1948). Stress-strain relations for uniaxial loading. App. Sci. Res., Aly 198-214.
Roberts, V., H. Boden and B. Ahlblom (1979). Dynamic recrystallization kinetics. Metal
Science, March-April 195-205.
Wray, P.J. (1982). Effect of carbon content on the plastic flow of plain carbon steels at
elevated temperatures. Metallurgical Transactions A, 125-134.
Yi, P.H., F. Montheillet and A. Kobylanski (1990). Description et moderation du ph6nomene
de striction accompagant la recristallisation dynamique au cours d'essai de traction a chaud
d'aciers microallies. Archives of Metallurgy, vol 35, 311-327.
WS1e6

SHEET FORMING SIMULATION BASED ON

BARLATS PLANAR ANISOTROPIC YIELD CRITERION

Kwansoo Chung and Kirit Shah

Alcoa Laboratories, Alcoa Center, PA 15069, U.S.A.

ABSTRACT

Modeling of sheet metal forming processes requires an accurate description of anisotropic

material behavior. However, the majority of FEM simulations still assume isotropy, even
though sheet metals usually show anisotropic properties after they are fabricated by thermo-
mechanical processes. There have been some efforts to include anisotropy, but most of them
are limited to planar isotropy (equivalently/'through-thickness anisotropy"), and the efforts to
include planar anisotropy are still rare. This paper describes the finite element (FEM)
simulation results obtained using Barlat's six-component anisotropic yield function, developed
recently. A cup drawing test was modeled for a 2008-T4 aluminum alloy, using this new yield
function incorporated into ABAQUS. Good agreement was found between the FEM simulation
and the experiment. The result shows that a better mathematic tool is now available which can
be used to enhance the forming simulation of planar anisotropic metals.

KEYWORDS

ABAQUS; anisotropy; cup-drawing; earing; finite element simulation; 2008-T4 aluminum

alloy.

INTRODUCTION

To represent planar anisotropy, Hill's quadratic anisotropic yield criterion (1948) has been the
most popular choice. However, Hill's criterion does not model material behavior properly for
certain metals, including some aluminum alloys, because of "anomalous" behavior. Later,
various non-quadratic yield criteria were developed by several authors. Some of them were
developed using crystallographic calculations. However, most of them are not really useful to
represent planar anisotropy, especially for FEM applications. The reasons are various: some
are only for isotropy or for planar isotropy; some are for planar anisotropy but they do not have
shear components; the criteria using crystallographic calculations are not simple enough for
practical use in numerical applications.

Recently, Barlat et al. (1990) have proposed a new six component yield criterion for planar
anisotropy which is simple but does not have the limits of the other criteria. The yield criterion,
now called Barlat's criterion in this paper, has been shown to be consistent with yield surfaces
221
222
based on polycrystal models, which often exhibit small radii of curvature near uniaxial and
balanced biaxial tension stress states. In order to verify the performance of Barlat's criterion, it
was implemented into ABAQUS and a cup drawing test was simulated. Good agreement was
found between the simulation result and the experiment. This paper describes the brief
overview of Barlat's criterion, implementation of the new criterion into ABAQUS, numerical
simulation of a cup drawing test, and comparison of the predicted result with the experiment.
Detailed discussions are summarized elsewhere by Chung and Shah (1990).

BARLAT'S ANISOTROPIC CRITERION AND MATERIAL

CHARACTERISTICS

In Barlat's anisotropic criterion for three dimensional deformation, the yield function O is
defined as

*=|SrS2| + S
| 2-
S
3| + S
| 3-S.| =2
° (1)

s
where s is the effective stress referring to a material flow strength. ^1,2,3 are the principal
values of a symmetric matrix S^, defined with the components of the Cauchy stress a as

'i(cC-bB) hH gG 1
S„ R = hH |(aA-cC) fF (2)
gG fF i(bB-aA)J

where A = ayy - a „ , B = o a - a „ , C = axx - o w , F = o^, G = azx and H = o xy . In eq. (2),

a and p are variable indices for x, y and z; and the subscripts x, y and z represent the mutually
orthogonal axes of the orthotropic symmetry (the resulting anisotropic yield function is
orthotropic and independent of hydrostatic pressure). The material coefficients a, b, c, f, g and
h represent anisotropic properties. The exponent m is roughly associated with the severity of
the texture. As the severity of the crystallographic texture increases, the m value increases. A
higher m value has the effect of decreasing the radius of curvature of the rounded vertices of
the yield surface. Thus, this criterion can represent the small radius of curvatures of the yield
surface near the uniaxial and balanced biaxial tension ranges, as observed in polycrystalline
yield surfaces. The yield surface is convex, when m > 1 and it does not reduce to Hill's 1948
anisotropic criterion even when m=2.

The material data (m, a, b, c, f, g, h) can be calculated from known test results. In this work,
FEM simulations were performed using the mechanical properties of a 2008-T4 aluminum

Table 1. Anisotropic material data of 2008-T4 aluminum alloy.

m a b c f g h

tension data 11 1.223 1.014 0.9858 1.000 1.000 1.000

compression data 11 1.017 1.023 0.9761 0.9861 0.9861 0.8875

 223

500

J_ _L
0 0.1 0.2 0.3 0.4 0.5
Effective strain

Fig. 1. Stress-strain data of 2008-T4 aluminum alloy.

alloy sheet. This material has been extensively characterized in previous works (Lege et al.t
1989; Barlat et al., 1990), and the variation of the uniaxial yield stress with respect to the
loading direction has been measured both in tension and compression. These two sets of yield
stresses (tension and compression) were used to calculate two sets of anisotropic material data,
shown in Table 1. Assuming isotropic hardening, the material data were kept constant during
the simulation. The stress-strain data used to describe the plastic hardening behavior were
measured from the uniaxial tension test in the rolling direction. The stress and strain data are
plotted in Fig. 1. The data were considered piecewise linear for the simulation.

IMPLEMENTATION OF BARLATS CRITERION INTO ABAQUS

Barter's criterion was implemented into ABAQUS using the user subroutine UMAT (see
ABAQUS manual, 1989). Since ABAQUS uses the elastic-plastic formulation for metal
plasticity, the followingrelationwas used for the numerical treatment:

a = 2^i(D - Dp) + tar(D)I Dp = [ 2na(f:D)

=n£i7ln (3)
{h(a:n) + 2^io|f|}

where a is the conventional Jaumannrateof Cauchy stress and D is the total strain rate (Dp is
a plastic part). |i and X are two elastic Lame constants, and I is an identity tensor, h is the
slope of the hardening curve, J | = (2a m_1 )_1 H and n is a normalized tensor of % m

To derive the incremental form of eq. (3), which is needed in UMAT for the updated
Lagrangian formulation, every material element was assumed to move at a constant strain rate
during a time increment, and the simple forward gradient integration scheme was employed
along with a very small time increment. The increment of the stress by rotation was calculated
by ABAQUS, prior to the call to the subroutine UMAT.
224
GA 2693
28

Fig. 2. Geometry of cup drawing test.

The anisotropic symmetry axes of the yield surface (x, y and z) are embedded on each material
element, and, initially, they are aligned with the rolling, transverse and normal directions of an
initial blank sheet. During deformation, the anisotropic yield surface of each material element
rotates by the material rotation so that the anisotropic symmetry axes are all in different
directions during deformation. Using the keyword card *ORIENTATION, the rotation of
symmetric axes was executed by ABAQUS, outside of UMAT. When the keyword card
♦ORIENTATION is used, the quantities defined in UMAT - the stress which defines the yield
function in eqs. (1) and (2) and the incremental values of stress and strain ~ are expressed with
respect to the local coordinate system embedded on each material element. Under this
circumstance, ABAQUS traces material rotations and updates the difference between the local
coordinate system and the laboratory coordinate system at every step. Then, ABAQUS delivers
these quantities (stress and the incremental values of stress and strain) to UMAT after
transforming them from the values with respect to the laboratory coordinate system into the
values with respect to the updated local coordinate system at every step; therefore, the effect of
the yield surface rotation is taken care of.

In real material deformation, the anisotropic property which is initially orthotropic might lose
orthotropic symmetry during deformation, especially because of shear deformation, when
principal directions of loading are not aligned with the anisotropic symmetry axes. However, it
will take extensive study of anisotropic hardening to account for that phenomenon. Since
isotropic hardening was assumed in this work, initial orthotropic symmetry of anisotropy was
preserved during simulation.

CUP DRAWING TEST

After being implemented into ABAQUS using UMAT, the new anisotropic yield function was
tested for the cup-drawing test. The test geometry is axisymmetric, but non-axisymmetric
earing deformation is induced by the planar anisotropic material properties of the 2008-T4
 225

Blankholder force = 22.2 KN

40 Fric. coeff. = 0.01
O FEM, tension test data
D FEM, compression test data
39 h
A Measured
38 _L _L _L _L J_
45 90 135 180 225 270 315 360
Angle from rolling

Fig. 3. Predicted and measured earing profiles.

aluminum alloy. In order to account for material planar anisotropy, the FEM simulations were
performed with a three-dimensional, eight node brick element, type C3D8H.
With this solid element, bending effects were accounted for properly. The simulations were
performed with the following input parameters shown in Fig. 2: Rp = 48.59 mm, rp = 4.78
mm, Rd = 50.04 mm, rd = 6.35 mm, RD = 81.00 mm. Sheet thickness is 1.24 mm. During
the simulations, the maximum effective strain increment was kept less than 0.001.

The values of the blankholder force (BHF) and friction coefficient, r|, were not known from
the experiment, except that BHF was kept constant and just sufficient to prevent wrinkling.
Quaker 8IX lubricant was applied to the die surface only, and no lubricant was applied to the
punch surface in the experiment (see Lege et al.y 1989, for the details about the experiment).
FEM simulations were carried out with two values of BHF and r\. The values of BHF were
22.2 KN or 44.4 KN, which were 1% and 2% of the yield force (the value of the initial yield
stress multiplied by the initial flange area). 1% and 2% are the values normally used in cup
drawing to prevent wrinkling (Marciniak and Duncan, 1988). With the fixed BHF values,
materials under the blankholder are under realistic deformation conditions, which are in-
between plane stress and plane strain conditions. The values for ^ were selected to cover the
range reported from the strip test for aluminum alloys with a good lubricant applied to the die
surface and a dry condition between the blank and punch (Shah, 1989): T| (Blank/Punch) =
0.20, T] (Blank/Die) = 0.05 or 0.01, *1 (Blank/Blankholder) = 0.05 or 0.01.

In the cup drawing test, the material undergoes compressive deformation in the flange area due
to circumferential forces. Also, some stretching occurs in the radial direction of a cup. Since
two sets of material data were available which are based on tension and compression tests data,
FEM simulations were performed using both data shown in Table 1.
226

The measured cup height profiles were compared with the predicted profiles for the two values
of r\ and BHF. As expected, cup height was larger with a higher BHF or a higher T|, since
both of these create more stretching; however, the difference was not significant. In fact, the
effect of blankholder force and coefficient of friction on earing was not significant for the
specific range selected here. In Fig. 3, therefore, only the predicted cup height profiles
obtained for BHF = 22.2KN and *! =0.01 are compared with the measured profile. The two
predicted height profiles obtained using the tension and compression data are plotted in this
figure. The results show that the cup heights obtained from both data are in good agreement
with the measured value, even though they are slightly overpredicted. Also, the four predicted
ears located at 0° and 90° to the rolling direction agree well with the experiment. However, the
magnitude of earing is overpredicted for the result associated with the compression data, while
it is underpredicted for the result associated with the tension data. In fact, the average cup
height profile of the two predictions showed an excellent agreement with the measurement. The
improved agreement of the average profile complies well with the fact that real deformation in
the flange area involves not only circumferential compression but also radial stretching in the
cup drawing test.

SUMMARY

Barlat's planar anisotropic yield criterion was successfully implemented into ABAQUS using
the user subroutine UMAT. The ABAQUS modeling results of the cup drawing test using the
new anisotropic function showed good agreement with the experimental result. The average
value of the predictions obtained using compression test data and tensile test data provided
better earing prediction than either the one based on compression test data or the one based on
tension test data. This might be because the cup drawing test involves stretching as well as
compressive deformation. Thus, a better mathematical tool is now available which will improve
the forming predictions of planar anisotropic metals.

ACKNOWLEDGMENT

Dr. F. Barlat provided detailed discussions about his new yield criterion. He calculated the
material data used in this work. Mr. DJ. Lege and Mr. J.C. Brem supplied the experimental
data. Dr. R.C. Becker guided the use of ABAQUS. The authors would like to express sincere
gratitude to these people for their help.

REFERENCES

ABAQUS user's manual, Hibbitt, Karlsson & Sorensen, Inc., Providence, RI, Version 4.7.
Barlat, F., Lege, D.J. and Brem, J.C. (1990). A six-component yield function for anisotropic
materials. Int. J. Plasticity (accepted for publication).
Chung, K. and Shah, K. (1990). Finite element simulation of sheet metal forming for planar
anisotropic metals (submitted to Int. J. Plasticity).
Hill, R. (1948). A theory of the yielding and plastic flow of anisotropic metals. Proc. R. Soc.
Lond. A\9A, 281-197.
Lege, D. J., Barlat, F. and Brem, J. C. (1989). Characterization and modeling of the
mechanical behavior and formability of a 2008-T4 sheet sample. Int. J. Mech. ScL, 31, 549-
563.
Marciniak, Z. and Duncan, J. L. (1988). The mechanics of sheet metal forming, Notes of
Special Course.
Shah, K. N. (1989). Evaluation of the finite element code ABAQUS for analysis of sheet
stretching processes. Unpublished Alcoa Laboratories report, Alcoa Center, PA.
WS1e7

EVALUATION OF LIMITING DRAWING RATIO OF

LAMINATED COMPOSITE SHEETS BY FINITE ELEMENT SIMULATION

K. YAMAGUCHI, T. KAWAGUCHI, T. GOTO and K. MORI*

Department of Mechanical and System Engineering

Kyoto Institute of Technology
Matsugasaki, Sakyo-ku, Kyoto 606, Japan

ABSTRACT

To investigate the deformation characteristics of laminated composite sheet

metals, the rigid-plastic finite element (FEM) simulation of axi-symmetric
deep drawing is carried out under various drawing conditions. In the
simulation, the normal anisotropy of each material constructing a composite
sheet is taken into consideration. The influences of the combination of
materials and the thickness ratio of composite sheets on the limiting
drawing ratio (LDR), thickness strain distribution and drawing load are
examined. It is shown that for aluminum-steel two layer sheets, the LDR
increases with increasing thickness of the steel sheet. For a given
thickness ratio, the LDR of the laminated composite blank becomes larger
when the steel side of the blank contacts punch. This is qualitatively
consistent with experimental results.

KEYWORDS

Rigid-plastic FEM; Laminated composite sheet; Deep drawing; LDR.

INTRODUCTION

Laminated composite sheets have been increasingly employed as advanced

materials in automobile, aerospace and electric industries. In the
composite sheets, material properties change in the thickness direction.
Thus, the drawability of composite sheet strongly depends on the combination
of material properties of each layer sheet. As for the deep drawing of
composite sheets, some experiments have been done by Hawkins and
Wright (1971), Hiraiwa and Kondo (1985), and other investigators (Yoshida et
al., 1989). They have mainly investigated how the LDR varied with
thickness ratio of two different metal sheets. However, the shapes and
dimensions of punch and die, and the thickness ratio of laminated composite

at present, Department of Mechanical Engineering, Faculty of Engineering

Science, Osaka University, Machikaneyama, Toyonaka, Osaka 560, Japan
227
228
sheets used in these experiments are rather limited.

In the present paper, in order to investigate the deformation character-

istics of laminated composite sheet metals in detail, the rigid-plastic
finite element simulation (Mori et al., 1989) of axi-symmetric deep drawing
is carried out under various drawing conditions. The influences of the
combination of materials and the thickness ratio of a composite blank on
the LDR, thickness strain distribution and drawing load are examined for
aluminum-mild steel laminated sheets. In addition, the influence of setting
condition of blank (either the surface side of a composite blank contacts
punch or not) on the LDR is also examined.

FEM SIMULATION OF DEEP DRAWING OF LAMINATED COMPOSITE SHEETS

A laminated composite circular blank is drawn with a flat punch as shown in

Fig.1. The laminated composite blank consists of two sheets of steel and
aluminum. The blank is divided into four layers of elements in the
thickness direction. The thickness ratio of a composite sheet was changed
by giving material constants corresponding to each material. It was
assumed that there was no slip at the interface between the two materials.
As the model of the laminated composite sheets, mild steel (SPCC)-soft
aluminum (Al-0) and soft aluminium (Al-0)-half hard aluminum (Al-H/2) clad
sheets were used. The material constants of each sheet used are listed in
Table 1. In the FEM simulation, the frictional coefficients between the
tool and the material were assumed to be u=0.25 (no lubrication) on the
punch, and U =0.1 on the die and blank holder, respectively.

Table 1. Material constants(o=Fen).

Material

Mild Soft Half hard

steel aluminum aluminum
(SPCC) (Al-0) (Al-H/2)

F (MPa) 584.8 177.4 154-7

n 0.25 0.29 0.07

r-value 1.26 0.41 0.1

Fig. 1. Finite element mesh used for

deep drawing of laminated Fig. 2. Examples of calculated
composite sheet. distortion of meshes.
 229
THICKNESS STRAIN DISTRIBUTIONS OF DRAWN CUPS

To understand the deformation behavior of a composite sheet in deep drawing,

the influence of setting condition of a blank on the deformation of element
was firstly simulated. Figure 2 shows examples of the calculated distortion
of elements. It is seen that the deformation aspect is appreciably
different depending on whether the mild steel (SPCC) is located at the
punch or the die side. In order to examine such differences in deformation
aspects due to the setting condition of blank, the thickness strain
distribution of each layer was calculated. The calculated results are
shown in Fig.3. Since the success or failure of the deep drawing of sheet
metals depends on the magnitude of the thickness strain at the punch profile
portion, the discussion was focused to the thickness strain at the punch
profile portion. For (SPCC)-(Al-O) and (Al-H/2)-(Al-0) composite sheets,
the thickness strain concentration of the composite sheet at the punch
profile portion is less when the (Al-O) sheet is located at the die side
than when the (SPCC) or the (Al-H/2) sheet is located at the die side.

0.4 0.4
B. P.R. s.w.
0.2 Composite
shee t — _ _

o -0.2
\Jt Al-H/2 layer
(die side)

^/' Al-0 layer

(punch side)

-0.4 i 1 1 1

.3 0.2

-0.4 -0.4
0 10 20 30 40 50 0 10 20 30 40
Initial radius of blank mm Initial radius of blank mm

Fig. 3. Influence of setting condition of blank on thickness

strain distributions.
(B.:Bottom, P.R.rPunch profile, S.W.rSide wall of
drawn cup)
230
The degree of the thickness strain concentration at the punch profile
portion directly depends on the bending resistance at the die profile
portion and the strength of blank material at the punch profile portion.
The increase in drawing resistance due to the bending and unbending at the
die profile portion is remarkable when the sheet with larger flow stress is
located at the die side, i.e. at the outside of a drawn cup. On the other
hand, the decrease in the thickness of the material at the punch profile
portion is larger at the outside of the drawn cup because of the larger
elongation along the meridian direction. As the result, when the sheet
with larger flow stress and smaller n-value (work hardening exponent) is
located at the die side, the loading ability of the composite sheet
decreases. Therefore, in order to increase the LDR of composite sheet
metals, a blank should be set so that the sheet with smaller flow stress and
larger n-value is located at the die side. For (SPCC)-(Al-O) and (Al-H/2)-
(Al-0) composite sheets, for example, the LDR becomes larger when the (A1-0)
sheet is located at the die side.

LIMITING DRAWING RATIO OF COMPOSITE SHEETS

The punch load required for the deep drawing of a sheet metal is given as
the sum of forces caused by (1) pure radial drawing, (2) the frictional
resistance at the flange and die profile portions, and (3) the resistance
for bending and unbending at the die profile portion. If this punch load is
beyond the material strength, a fracture occurs at the punch profile portion
of the drawn cup. In the following, the influences of thickness ratio and
setting condition of a composite blank on the LDR are discussed based on the
magnitude of the punch load and the material strength.

Comparison of Drawing Load with Material Strength at Punch Profile Portion

In general, the circumferential strain of a drawn cup is approximately zero

at the punch profile portion. Thus, as the strength of the drawn cup, the
plane strain tensile strength of a composite sheet was adopted. Using the
uniaxial ultimate tensile strength 0-Q and average r-value of each sheet
constructing a composite blank, the tensile strength at plane strain
condition o is given by

The vertical component of the strength P* at the punch profile portion of a

drawn cup is approximately expressed by

P* = 2TT [ { R-r p + rpsin<J>+—1-| sin<J)} t-j op-| sin<J)

+ { R - r p + ( r p + t-| ) sin(t) + -t2sin(J)} t2ap2sin<l>]

where R is punch radius (=20mm), r p is punch profile radius (=4.mni), t 1 and t 2

are thicknesses of each sheet of a composite blank, respectively. The
contact angle between the blank and the punch or die is expressed as <t> which
is assumed to be the same at the punch and die profile portions. Since the
contact angle (J> is given in terms of punch stroke S, the vertical component
of cup strength P* becomes a function of the punch stroke. After the blank
completely contacts the punch and die profile portions, i.e. <l>=90, P*
becomes constant.
 231
Figure U shows the comparison of drawing load calculated by the FEM with the
material strength P* of a drawn cup. When the blank diameter dg is small,
the drawing load does not reach to the material strength and therefore the
drawing can be safely carried out. However, when dn becomes larger, a
fracture occurs at the punch profile portion, because the drawing load
exceeds the strength of a drawn cup. It is seen that when the mild steel
sheet (SPCC) is located at the die side, the LDR of the composite sheet
decreases.

Figure 5 shows how the maximum drawing load Pmax and the strength of cup
wall P* are affected by the combination and the thickness ratio of materials
constructing a composite sheet. The strength of cup wall obeys simple law
of mixture. Since the composite sheet is very thin compared with the
diameter of punch used, the strength of cup wall is hardly dependent on the
setting condition of the blank. While, the maximum punch load required for
drawing the composite sheet increases with increasing thickness of sheet
with larger flow stress. For a given thickness ratio, the maximum punch
load becomes larger when the sheet with larger flow stress is located at the
die side.

60
50
(SPCC) - (Al-0) Strength
(die side) (punch side)
40 3*

30

20
SPCC(punch side)
10 Al-0(die side)
-P
dn=80mm
i Uj
(SPCC) 0 0.3 0.6 0.9 1.2
(Al-0)1.2 0.9 0.6 0.3 0

T3
cd
(SPCC) - (Al-0) Strength -~"t
O (punch side) (die side)
15'
3
PL. \ Al-H/2(die side)
10 \ Al-0(punch side)
X
cd Al-H/2(punch side)
E
90mm P-. 5 Al-0 (die side)
do=88mm
do=80mm dQ=76mm
n
0 10 20 30 40 (Al-H/2) u 0 0.3 0.6 0.9 1.2
(Al-0) 1.2 0.9 0.6 0.3 0
Punch stroke S mm
Thickness ratio

Fig. 4-- Comparison of calculated Fig. 5. Influence of thickness

drawing load with material ratio on maximum drawing
strength P*. load Pmax of blank and
strength of cup P*.
232
2.0

Al-H/2(punch side)
Al-0 (die side)

SPCC(punch side)
Al-0(die side)
\
SPCC(die side) Al-H/2(die side)
Al-0(punch side) Al-0(punch side)

(SPCC),°9 0.3 0.6 0.9 1.2 (Al-H/2)0 0.3 0.6 0.9 1.2
0.9 0.6 0.3 0 0.9 0.6 0.3 0
(Al-O)'^ (Al-O) ' ^
Thickness ratio Thickness ratio
Fig. 6. Influences of thickness ratio and setting condition
of blank on limiting drawing ratio (LDR).

Influences of Thickness Ratio and Setting Condition on LDR

Figure 6 shows influences of thickness ratio and setting condition of the

composite blank on the LDR. The results of simulation obtained are
qualitatively consistent with experimental results of (Cu)-(SPCC) composite
sheets by Hawkins and Wright and Yoshida et al. The calculated results also
shows the similar tendency to the experimental results of (Al-O)-(Al-H) and
(Al-0)-(Brass) composite sheets by Hiraiwa and Kondo.

CONCLUSIONS

The deformation behavior of (SPCC)-(Al-O) and (Al-H/2)-(Al-0) laminated

composite sheets in deep drawing has been simulated by the rigid-plastic
FEM. The influences of material combination, thickness ratio and setting
condition of composite blanks on the thickness strain, drawing load and LDR
were investigated. It has been shown that the LDR of composite sheets can be
predicted from the comparison of the maximum punch load calculated by the
FEM with the strength of cup wall determined by the law of mixture. The LDR
of composite sheet metals can be improved when the sheet with larger flow
stress is located at the punch side.

Acknowledgment; The authors are very grateful to Associate Professor S.

Imatani and Instructor N. Takakura of Kyoto Institute of Technology for
their valuable discussion. The authors also would like to express their
gratitude to The Mechanical Industry Development & Assistance Foundation
(MIDAF) for Grant-in-Aid for Scientific Research.

REFERENCES

Hawkins, R. and Wright, J. C. (1971). Mechanical Properties and Press-

Formability of Copper/Mild Steel Sandwich Sheet Materials. J. Institute
Metal., 99, 357-371.
Hiraiwa, M. and Kondo, K. (1985). Press Forming of Clad Sheets. J. Japan
Soc. Technol. Plasticity., 26-291, 385-393.
Mori, K. and Yamaguchi, K. (1989). Finite Element Simulation of Deep Drawing
and Stretching of Laminated Composite Sheet Metals. Proc. 1st Japan Int.
SAMPE Symposium, 701-706.
Yoshida, F., Sakamoto, K, Komatsu, M., Ohmori, M. and Mori, K. (1989). Deep
Drawing of Clad Sheet Metals. Proc. 4-Oth Japanese Joint Conf. Technol.
Plasticity. 21-24.
WS2a1

THE NEWEST DEVELOPMENT ON PHYSICALLY BASED CONSTITUTIVE

MODELING IN DYNAMIC PLASTICITY

J.R. KLEPACZKO

Metz University, Faculty of Sciences, Laboratory of Physics and Mechanics of Materials,

De du Saulcy, F-57045 METZ, France

ABSTRACT
A review is presented on recent developments in constitutive modeling in dynamic plasticity of
metals and alloys. A consistent approach to modeling is based on description of microstructural
evolution represented by physically motivated internal state variables. The evolution of mobile as
well as immobile mean dislocation densities are taken into account. Thus, the rigorous formalism
has been introduced, which employs, besides the evolution of microstructure, the thermal activa-
tion strain rate analysis. The kinetics of plastic deformation of metals and alloys with FCC, BCC
and HCP lattices is discussed. The modeling of instantaneous rate sensitivity, rate sensitivity of
strain hardening and temperature sensitivity of flow stress is rigorously approached in terms of
kinetics of dislocation multiplication, glide and annihilation. Numerical calculations performed
for some FCC and BCC metals demonstrate capabilities of the formalism. It has been shown that
evolution of the mobile dislocation density permits for description of the short transients of flow
stress.

KEYWORDS

Dynamic plasticity ; dislocations; thermal activation; constitutive relations.

INTRODUCTION

During last decades a vast experimental evidence has been accumulated that pure metals as well
as alloys deformed plastically at different strain rates and temperatures undergo a complicated mi-
crostructural evolution. On the other hand interpretation of those experimental data via materials
science along with microscopy studies has gained our knowledge on related-to-microstructure
material behavior. As a consequence, in recent years the materials science approach is more fre-
quently applied to constitutive modeling in dynamic plasticity of metals and alloys. Such approa-
ch permits for rationalization of different material responses to imposed plastic deformation over
a wide range of strain rates and temperatures.

If a theory is based on a physically sound microscopic model, it must be formulated as a set of

equations, but experimental data are necessary to determine the constants which enter into equa-
tions. This approach is called the rational phenomenology and is quite effective in dynamic plas-
ticity. The physical framework along with fundamental assumptions is called a formalism. This
study presents one of many possible formalisms. The formalism presented here was proposed in
235
236
its simplest form some time ago, (Klepaczko, 1975), a more advanced characterization of the
formalism was given later (Klepaczko, 1987,1988). During recent years this approach to mode-
ling has been advanced further and the recent developments are reviewed in this paper.

THE FORMALISM

Plastic flow of metals is determined on the atomic scale by the motion of defects (dislocations).
The two types of dislocations are always present in the lattice, the mobile dislocations which are
carriers of plastic deformation, and immobile dislocations which accumulate and cause strain
hardening. Since the mobile dislocations have to overcome various types of obstacles like the lat-
tice itself (Peierls barrier), other dislocations (so called forest), solute atoms or precipitates and
subgrain boundaries, the plastic flow is a kinetic process. The kinetics of mobile dislocations is
controlled by thermal-mechanical characteristics of the obstacles, whereas the immobilization and
storage is controlled by its own kinetics. The formalism shows how to relate the physical para-
meters in the mathematical form. The formalism used here is reported in earlier publications.
Evolution of microstructure is characterised in the formalism by die two state variables, i.e. the
mean mobile dislocation density p m and the mean immobile dislocation density p{. In literature
different concepts of the internal state variables can be found. For example, (Klepaczko, 1975)
analyzed results of experiments on aluminium and copper and proposed a model based on the use
of the total dislocation density as the internal state variable with strain rate dependence of disloca-
tion accumulation. A similar approach, based on rate sensitive strain hardening, has been later
proposed by Kocks (1976). A more complete model of this kind has been discussed by Mecking
and Kocks (1981) and later generalized by Estrin and Mecking (1984). Recently, this approach
was extended into the high strain rate regime with the mechanical threshold stress as an internal
state variable (Follansbee and Kocks, 1988). The present formalism (Klepaczko, 1987, 1988)
differs of those discussed above (Mecking and Kocks, 1981 ; Estrin and Mecking, 1984). The
notion is adopted that plastic deformation in shear, defined as resolved shear stress xr and resol-
ved shear strain Tr, is the fundamental mode of deformation. The resolved quantities xr and Tr
can be related to the macroscopic flow stress in shear x or in tension/compression a by appropria-
te Taylor factors FT or F a . Thus,

T = Fx(r)Tr and a = F < j (r r )x r (1)

r =r/Ft(r) and e=r/Fa(r) (2)

An advantage of such formulation lies in the fact that for large strains a texture develops and the
Taylor factor is not a constant but depends on the state of stress and strain, for example (Canova,
1986).
Another fundamental assumption is partition of the flow stress xr into the effective stress x*r and
internal stress x . These two components are summed up giving the total stress

+ (3)
\ =\ \

Using (1) one can write

x = F ( 0 ( x +i*) or o = F (e)(x + x*) (4)

x m r a T\I
r

Finally, for the macroscopic quantities

x=x +x and G=G +G (5)

The assumption of additivness implies two different dislocation processes, or two sets of obsta-
 237
cles to dislocation motion. The internal stress x is associated with already accumulated immobile
dislocations and other athermal obstacles. The athermal obstacles are supposed to be strong, like
tangled dislocations, cell walls, grain walls, twins and so on. The secondary defects, while more
numerous, like forest dislocations, Peierls barriers, second phase particles, are supposed to be
weak obstacles and they can be overcome by mobile dislocations with assistance of thermal vi-
brations of the crystalline lattice and effective stress x*. Consequently, evolution of XL is associa-
ted with storage of immobile dislocations, whereas x* is related to the movements ofmobile dis-
locations. The kinetics of dislocation movements interrelates at constant microstructure, characte-
rized by j state variables Sj, the instantaneous value of the effective stress x* at the instantaneous
plastic strain rate t = dT/dt

T AG. (T,x*,s.)l
J
T = v. (T,Sj) exp L kT J (6)

or after inversion

x* = f * { S j [ h ( r , T ) ] , r , T } (7)

where Vj is the frequency factor, AGj is the free energy of activation, T is the absolute temperatu-
re and k is Boltzmann constant. The subscript i indicates the i-th, so far unspecified, thermally
activated micromechanism of plastic deformation. Generally, AGj depends on the effective stress
x* in a non-linear manner (Kocks et% al, 1975). Since the internal state variables Sj undergo an
evolution as a function of strain rate T and temperature T, the history of evolution is symbolically
introduced into eq. (7) as h (f ,T). As it has been discussed previously (Klepaczko, 1975 ; Kle-
paczko and Chiem, 1986), the internal stress % must also be rate and temperature dependent via
dynamic recovery processes, i.e. relaxation offiong range internal micro-stresses due to disloca-
tion annihilation and rearrangement of obstacles to dislocation motion. Consequently at constant
microstructure, the internal stress is also history dependent. Finally after (5)

x = f^ {s. [h (r,T)]} STR + f* {s. [h (r,T), r,T]} STR (8)

It is assumed here that recovery processes leading to structural evolution may be thermally activa-
ted. It is the source of an indirect strain rate and temperature dependence of x^. Both, strain rate
and temperature enter into eqs. (7) and (8) in the functional form, because f (f) and T(H are de-
fined deformation histories. It is important to note that the plastic shear strain f does not enter di-
rectly into es. (7), but via internal state variables Sj. Consequently, plastic response of a material
is divided into two logic steps : the flow stress x depends on the current microstructure, defined
by Sj internal state variables, and on the current values of f and T, next the microstructure evol-
ves with plastic strain T. This is the fundamental assumption of the formalism.

Both components of stress, eq. (8), are written for a current microstructural state characterized
by Sj state variables. Since the microstructure undergoes an evolution, and the state of micros-
tructure is defined by Sj variables, the evolution is completely described by a set of j differential
equations of the first order

ds.
- ± = Jf [ s k , r ( D , T ( r ) ] , k= 1 ... j (9)
dr
Solution of the set (9) provides current values of Sj to be introduced into eq. (8). In this way the
flow stress can be calculated for any deformation history f (T) and T (T).

IDENTIFICATION OF MICROSTRUCTURE

Flow stress or yield limit in polycrystalline metals and alloys can be related to characteristic spa-
238
cing of obstacles to dislocation motion associated with a particular microstructure. A range of
characteristic spacings is possible. The following four will be assumed as a satisfactory choice
for the internal state variables. The microstructure will be characterize by the mean distance L
between dislocations, the mean value of a dislocation cell d, the mean grain diameter D and the
mean distance between twins A. Each of those obstacles to dislocation motion will contribute to
the internal stress x . A general expression for x can be written

v m t «>Q;)S; k- 1...J (10)

where [i (T) is the temperature dependent shear modulus of elasticity, o^ are constants which
characterize obstacle strength, b is the modulus of Burgers vector, \ is the generalized characte-
ristic spacing (L, d, D, A) and 8 is an exponent which is equal 1 for one-dimensional spacing (L)
and d = 1/2 for two-dimensional spacings (d, D, A). The explicit form of eq. (10) for the four
variables is as follows

\=«i^T>b (r)+«2ncn Q) + cs^cr) (£) + «4^ro (!) (i i)

The mean spacing L between dislocations is related to the mean dislocation density p by p = L"2.
It is important to note that all characteristic spacings can be in principle determined by microsco-
pic observations. It is also obvious that L, d, D and A undergo an evolution during plastic de-
formation. It is natural, then, to assume p, d, D and A as the internal state variables Sj ; Sj = p
; S2 = d ; S3 = D ; s 4 = A. The first three terms in eq. (11) are related respectively to disloca-
tion/dislocation interaction, evolution of subgrain d(p), and the effect of grain diameter - so cal-
led Hall-Petch term. A more exact discussion of d(p) and the effect of D is provided elsewhere
(Klepaczko, 1987, 1988,1989). It is well known that at low temperatures and a very high strain
rates some metals and alloys produce deformation twins. There is a numerous experimental evi-
dence that begining of certain strain level, usually T * 0.08, dislocations form cells with linear
dimension & When deformation progresses d diminishes and the evolution of d(p) intensifies the
rate of strain hardening dx/dr with a larger effect at small strains, (Klepaczko, 1987, 1988,
1989). The exponent 8 in the second term of eq. (11) has a dual nature, 8 = 1 for cells and for a
small subgrains with large misorientations, and 8 = 1/2 for "ideal" subgrains in thermally recove-
red metals. Further improvents of the formalism have been pursued quite recently, namely the
total dislocation density p can be split into the mobile and immobile fractions

P = Pm + Pi (12)

In this case separate evolution equations for p m = s5 and p{ = s b as internal state variables, must
be formulated. For example, it is known that in FFC structures p does not change much, but in
BCC lattice an evolution of pm can play a dominant role (Klepaczko, 1984).

ONE PARAMETER FORMULATION

Common to all recent microstructure related models is that the set Sj of internal state variables is
reduced to a single structural parameter which can be identified with the mean dislocation density
p (Klepaczko, 1975, 1986, 1987, 1988 ; mecking and Kocks, 1981 ; Estrin and Mecking,
1984). Since in those references not very high strain rates are analysed generation and evolution
of twins is neglected.
A general form of the differential equation for structural evolution can be written as (Klepaczko,
1975 ; Klepaczko and Chiem, 1986)
 239

= M g (p,0-M a (p,r,T) (13)

dr
where the difference M^ff = Mg - Ma is the effective coefficient of dislocation multiplication (Gil -
man, 1969). Once Meff is known one can determine the current value of plastic strain T that will
be accumulated in any process of deformation by integrating eq. (13). At present there is no
agreement as to which equation for structural evolution, eq. (13), will provide the best quantitati-
ve results in constitutive modeling. Relatively complete description of strain hardening, dynamic
recovery and time dependent recovery has been so far proposed (Klepaczko and Chiem, 1986;
Klepaczko, 1988). Since the one internal state variable model with the mean dislocation density p
has been discussed in many publications cited above no attempt will be made to repeate its featu-
res.

One of many interesting consequences of application of this formalism is the analysis of the rate
sensitive mechanical threshold (Klepaczko, 1990). The mechanical threshold, i.e. the flow stress
back extrapolated to T = OK, has recently been studied and it was found that the mechanical
threshold is rate sensitive (Follansbee ex al, 1988 ; Tanimura et al.t 1985). This important ob-
servation, which demonstrates a definite rate dependence of the Mg (p,0 in eq. (13), leads to the
conclusion that at high strain rates, above ~ 10* s"1, an excessive generation of defegts (disloca-
tions) occurs. This effect causes an extremely enhanced rate sensitivity observed at T = constant
within the region of high strain rates, 10V 1 < f < 10V 1 . The experimental results of a rate sen -
sitive threshold stress x lead to the following derivation of x. Using the additivness rule, eq. (5),
one can write

x = x +x* ,T = 0 (14)

The component x„ of the threshold stress $ can be derived using the most simple relation for
structural evolution (Klepaczko, 1987)

^ = Mn(h-ko(p-po) , T=0 (15)

dr
where M n is the multiplication coefficient at T - 0, ICQ is the annihilation factor at T = 0 and p is
the initial dislocation density. Integration of eq. (15) with initial conditions T = 0, p = p0 yields

p=p o + - i _ [l-exp(-kT)], T=0 (16)

o

Neglecting the last three terms in eq. (11) the result for p can be introduced into the first term,
thus the x„ component is

$ = cc^ o b { p o + - S _ [1 - exp (- k o D] ) . T=0 (17)

H K
o

where |i(0) = \i . The thermally activated part of the threshold stress x* can be obtained directly
from the explicit form of the Arrhenius relation, eq. (6), (Klepaczko, 1988)

$*=2<K wi,
with p =fp
m
, T=0 (18)
b a*
240

where G0 is the activation energy for the overcoming of an obstacle by dislocations, a* is the
activation distance, a* « b, and f is the fraction determining the density of mobile dislocations
(for example, Klepaczko, 1975). Taking into account eqs. (11), (14) and (18) the threshold
stress can be written in the form

3-a l t i 0 b7^(l+ °°\ ) (19)

Introducing the solution for p, eq. (16), the final formula for x is obtained

1/2

(20)
OLU b a* o

The yield stress at T = 0, x is obtained from eq. (20) posing r = 0

^y = ^o b V^( 1 + -^T-)
v
(21)
cc^/a*7
It is important to note that the yield stress at T = 0, i.e. x , does not depend on strain rate f, whe-
reas the flow stress x does depend on strain rate via the rate sensitive multiplication of defects
(dislocations), i.e. M n (T). A more exact analysis of M n (f) has been attempted by Klepaczko
(1987, 1990) using experimental data for polycrystalline Al (Morrone et ai, 1986) and for Cu
(Dusek et a/., 1975). Numerical calculations of the mechanical threshold at different levels of
strain using eq. (20) (Klepaczko, 1990) have shown the same trends as found from experiments
(Follansbee et ai, 1988 ; Tanimura et al, 1985). Numerical calculations of the x = f (r>r f at dif-
ferent temperatures and strain rates, for both FCC and BCC metals, demonstrated capabilities of
the one parameter model, (Klepaczko, 1987,1988, 1989 and 1990). It appears that the one pa-
rameter approach provides a good description of the instantaneous rate sensitivity as well as the
long stress transients after abrupt changes of strain rate and temperature. The simplest evolution
of the mobile dislocation density, i.e. p = f p does not permit for a precise description of the
short stress transients, an important problem in stress wave propagation. The short transients can
be taken into account with a more exact description of the mobile dislocation evolution during
plastic deformation.

TWO PARAMETER FORMULATION

In the approach with the evolution of the total dislocation density p, many interesting features of
mechanical responses cannot be accounted for. A more advanced models should account for the
evolution of the mobile and immobile dislocation densities. When the mean distance between
immobile dislocations is Lj and related immobile dislocation density is p. = 1/L2j and the mean
distance between mobile dislocations is Ljn and related density of mobile dislocations is p m =
1/L2m, it can be assumed here that
1
1 +—
— =— 1 or p = p.+ p (22)
r l rjn
2 2 2
1 m

Since plastic deformation is the result of dislocation generation, movement and storage the rates
of p must be balanced, i.e.
 241

p,pi + p. a»d 4 . * U ^ (23,

dT dT dT

If p mremainsconstant, the frequent assumption in one parameter models, then p = p. or dp/dT

= dp/dT. For example, when evolution equations for p{ and p m are assumed in the following
form
d
Pm
— i = M m (r) - f (p, T, T) (24)
JT-, m ma x r ' v
'
dl
dp.
—L = M . ( n - f i a ( p , r , T ) (25)
dT
where M are multiplication factors and f are annihilation or immobilization functions, the balance
(23) of multiplication and storage leads to the relation

dp
M.(T) = M ( O - f (p,T,T) or M.=—2. (26)
dl

For this case the total multiplication rate is

% = M m ^ " tfma <P' *", D + fu (P, t T)] (27)

dT
where ^ + fia = L is the total annihilation rate of the dislocation population. Explicit forms for
dp/dr and dp/dT has been derived earlier (Klepaczko, 1990, 1991). Evolution equation for
pm, derived by Klepaczko (1990,1991), can be written in the form

^ = M n (H + (Pm- Pmo) Q - H2) sign f (28)

dT T
where T|, is constant characterizing sensitivity of dislocation sources to changes of strain rate, ru
is probability of slowing down of dislocation production or immobilization, p m o is the initial
mobile dislocation density. The explicit form of eq. (28) is discussed elsewhere (Klepaczko,
1991), the result is

- ^ = M n (T) h (T) + g (T,T) ( ^ 1 - TI 2 ) T11 exp (- r\2T) sign f (29)

dT T
General solution for eq. (28) or eq. (29) has the following form

Pm" Pmo = M n (T) f (O + g (T,H T11 exp (- i\JT) sign T (30)

where

h(n=[— (n,-n2n + i ] (3D

and f (T) and g (r,T) are unspecified function of T, f and T. In eq. (30) the second term with
242

g (r,T) describes "bursts" of the mobile dislocations when f is increased, or negative "bursts"
(i.e. reduction in production) when f is reduced.
The evolution and rate of storage of p. produce strain hardening. At present there is no agreement
for which form of evolution equation for pj provides the best results. At present the simplest rela-
tion by analogy to one parameter model is suggested
-2mT
^ i = M.(r,r,T)-k(il) (PfPio> (32)
dT °T
mo is the absolute rate sensitivity of strain hardening. The condition (26) leads to the relation

d d
Pi P,r
(33)
dT dr °v r ' l l0

where dp^dT is defined by eq. (28). Since the annihilation term in eqs. (32) and (33) is well es-
tablished in the one parameter models, it accounts here for the total rate of annihilation, i.e.
p + p:. The two parameter models give more flexibility in constitutive modeling, and in the first
place they can account for both short and long stress transients.

APPLICATION
Although analytical solutions in one parameter case are possible (for the simplest formulations
and for T = const, and T = const.), it .is necessary, in general, to apply numerical methods to de-
termine p^ and pj and next the x (r,r,T) curves. Usually the 4-th order Ruge Kutta procedure is
employed to integrate the set of equations (eq. (9)). Numerous result of numerical simulations
have been already reported for different variations of the formalism (Klepaczko, 1987, 1988,
1989, 1990), however the two parameter modeling has been explored recently (Klepaczko,
1990, 1991). One of those result for aluminium is shown in Fig. 1 where the shear stress x is
plotted as a function of strain at T = const, and T = const.

150

.05 .1 .15 .2 .05 .1 .15

SHERR STRRIN SHERR STRRIN

Fig. 1. xResults of numerical calculations for polycrystalline Al in the form

(Or.T with two parameter formalism; constant strain rate and
incremental simulations.
 243
In addition, the strain rate jumps at different temperatures were also simulated. The input parame-
ters in numerical simulations were the same as for experiments for polycrystalline Al (Senseny et
al, 1978). Also, similar calculations, but for one parameter model, Klepaczko (1987), have
shown the lack of the short transients. Those results are shown in Fig. 2 and Fig. 3. In Fig. 2
the constant strain rates and increments in strain rate is simulated at different temperatures (the
same input parameters as in Fig. 1). In Fig. 3 a similar simulations are presented but for the ca-
se of jump reduction in strain rate. Simulation of Fig. 3 has a special value since it is very diffi-
cult to perform experiments with abruptly reduced strain rates. All constants and parameters
which enter into equations are given in the papers cited above and they are not repeated here.

rr» 3«E2 s-1 rr- 3«E2 s-1

T i= 2«E-4s-l T i- 2*E-4s-l

1E-D01 1E-001

SHEAR STRAIN SHEAR STRAIN

Fig. 2. Numerical simulations of experiments on Al by Senseny et al. (1978)

with positive jumps in strain rate.

T i-3«E2 s-1 r s- 3«E;> s-i

fr-2»E-4 s-1 r 1" 2»E- 4 s-1

1E-001 1E-001
SHEAR STRAIN SHEAR STRAIN

Fig. 3. Numerical simulations of stress-strain curves for the same conditions

as in Fig. 2 but with jump reduction in strain rate.

Results of numerical calculations, those reported in the earlier publications as well as those
shown in Figs. 1, 2 and 3, indicate that the formalism enables for an exact modeling of transient
phenomena, during plastic deformation, including stress wave loadings.
244
REFERENCES

Canova, G. (1986). Relations Between Texture, Anisotropy, Constitutive Relations and Plastic
Instabilities in Polycrystals. D. Sc. Thesis, Metz University, Metz.
Dusek, F. (1975). Crystallographic Aspects of Plastic Deformation and Dislocation Mobility in
Cu Single Crystals. Reports IM-CAS, Brno.
Estrin, Y. and H. Mecking (1984). A unified phenomenological description of work hardening
and creep based on one-parameter models. Acta MetalL, 57.
Follansbee, P.S. and U.F. Kocks (1988). A constitutive description of the deformation of cop-
per based on the use of the mechanical threshold stress as an internal state variable. Acta Me-
talL, J6, 81.
Klepaczko, J.R. (1975). Thermally activated flow and strain rate history effects for some poly-
crystalline f.c.c. Metals. Mat. Sci. Engng., 18, 121.
Klepaczko, J.R. (1984). In : High Energy Rate Fabrication-1984, p. 45. ASME, New York.
Klepaczko, J.R. and C.Y. Chiem (1986). On rate sensitivity of f.c.c. metals, instantaneous rate
sensitivity and rate sensitivity of strain hardening. J. Mech. Phys. Solids, 34,29.
Klepaczko, J.R. (1987). In : Constitutive Relations and Their Physical Basis, p. 387. Riso Natl.
Laboratory, Roskilde.
Klepaczko, J.R. (1988). In : Impact, Effects of Fast Transient Loadings (W.J. Ammann et al.,
eds), p. 3. A.A. Balkema Rotterdam.
Klepaczko, J.R. (1989). In : Mechanical Properties of Materials at High Rates of Strain 1989 (J.
Harding, ed.) p. 283. Institute of Physics, Bristol.
Klepaczko, J.R. (1990). In : Inelastic Solids and Structures (M. Kleiber et al., eds.) p. 179. Pi-
neridge Press, Swansea.
Klepaczko, J.R. (1991). In : Proc. International Conference on High Strain-Rate Phenomena in
Materials, EXPLOMET, (M. A. Meyers et al., eds.), Marcel Dekker, New York; in print.
Kocks, U.F., A.S. Argon and M.F. Ashby (1975). Thermodynamics and Kinetics of Slip. Per-
gamon Press, Oxford.
Kocks, U.F. (1976). Laws for work-hardening and low temperature creep. J. Engng. Materials
and Technology, Trans. ASME, 98D, 76.
Mecking, H. and U.F. Kocks (1981). Kinetics of flow and strain hardening. Acta MetalL, 1865.
Morrone, A.A. and J. Duffy (1986). Strain Rate and Temperature Effects During Dynamic De-
formation of Polycrystalline and Monocrystalline High Purity Aluminum Including TEM Stu-
dies. MRL Brown University Report, Providence.
Senseny, P.E. and J. Duffy (1978). Experimentation strain rate history and temperature effects
during plastic deformation of close packed metals. J. Appl. Mech., 45,60.
Tanimura, S., T. Hayashi and K. Ishikawa (1985). In : Microstructure and Mechanical Beha-
viour of Materials (Gu Haicheng et al., eds.), Vol. II, p. 761. EMAS, Warley.
WS2a2

MODELLING 1HE UNIAXLAL VISCOFLASTIC BEHAVIOUR

OF AISI 316 STAINLESS STEEL AT IHE AMBIENT TEMPERATURE

A.M. ELEICHE (MM), C. ALBERTINI (M), M. S. ABDEL-KADER ( + ),

N. N. EL-HEFNAWY (x) and S. S. ALY-EL-DIN (#)

(MM) Dept. of Mechanical Design & Production, Faculty of

Engineering, Cairo University, Egypt
(M) Appl. Mech. Div. , CEC Joint Research Centre, Ispra, Italy
( + ) Dept. of Mechanical Engineering, M. T. C. , Cairo, Egypt
(x) Engineering Authority, R A . R , Cairo, Egypt
(#) Dept. of Mechanical Engineering, Zagazig University, Egypt

ABSTRACT

Newly acquired test data for AISI type 316 SS at the ambient temperature
under monotonic and jump tension, uniaxial complex strain-controlled cyclic
loading, and monotonic torsion are presented Differences in initial
yielding and in deformation-induced anisotropy between uniaxial tension and
torsional shear are exhibited On the other hand, Chaboche unified theory of
viscoplasticity is adopted to model the observed tensile response and predict
new more complicated ones. Modifying the von Mises criterion used in the
theory by means of a Hi 11-type anisotropic tensor allows the theory to
predict more accurately the torsional shear response as well.

KEYWORDS

316 stainless steel. Room-temperature properties. Monotonic tension Jump

tension Cyclic loading. Monotonic torsion. Modelling of material response
Chaboche unified viscoplasticity theory. Hill-anisotropy-modifier tensor

INTRODUCTION

AISI 316 stainless steel is used extensively in nuclear as well as non-

nuclear energy systems. Therefore, its deformation response to various
loading regimes, as determined by suitable tests, must be analysed, idealized
and cast into constitutive equations for use in the design, stress analysis
and life prediction of structural components.

In the present paper, test results obtained mainly under uniaxial monotonic,
jump and cyclic loading, at the ambient temperature, are presented Chaboche
(1977) viscoplasticity theory is used to model the observed responses and to
predict new ones. Calculated monotonic torsional shear behaviour does not
agree, however, with experimentally-generated results. An attempt to modify
the theory to account for this difference is also presented

EXPERIMENTAL WORK

AISI 316L SS was acquired in the form of solid bars. Chemical analysis

245
246
revealed the following composition (wtX): 0.082 C, 0.847 Si, 0.945 Mh, 18.03
Cr, 10. 36 Ni, 2. 19 Mo, 0. 018 P, 0. 01 S, 0. 14 Co, 0. 067 V. Average grain
size was found to be 40 p.m. Configurations of the used test specimens are
shown in Fig. 1. No post-machining heat treatment was applied.

Monotonic and jump tests were conducted under constant strain-rate controlled
tension on an Instron electrohydraulic universal testing machine, while
strain-control led tension/compression cycling was performed on a SchencR
HYDRO-PULSE machine. Farther details are given elsewhere (El-Hefnawy, 1989).

Monotonic and Incremental Tension Results. Engineering stress-strain curves

for monotonic tension up to 10/. strain at the strain rates of 4 E-5 and
4 E-3 /s are shown in Fig. 2. The curves are seen to be continuous and
smooth throughout, with quasi-linear strain-hardening inelastic portions.
Values of the yield and ultimate strengths obtained from these curves
indicate that the material exhibits viscoplastic behaviour, in agreement with
the response of the nuclear grade AISI 316H SS (Eleiche et al. , 1985).

Figure 3 (a) and (b) show the experimental and calculated stress-strain
responses, respectively, of a specimen which was firstly loaded at a strain
rate of 4 E-5 /s to 10/. strain, then subsequently loaded for 2/. strain at 4
E-3, then at 4 E-l, 4 E-5 and 4 E-l /s. The response is characterised by:
(i) initial nearly elastic response, (ii) ill-defined yielding, and finally
(iii) a worK-hardening phase, through which the transient response approaches
asymptotically the monotonic response obtained entirely at the new strain
rate. Limited sensitivity to strain-rate history is observed.

Cyclic Results. A series of cyclic tests has been performed over the strain
range of ±1.0 and at the strain rates of E-5, E-4, E-3, E-2, and E-l /s for
twenty cycles. Typical hysteresis loops obtained at £ = E-3 /s are shown in
Fig. 4, where the inset represents the strain-time stimulus. Large cyclic
hardening is seen to be induced The stress amplitudes of both tension and
compression sides of these tests are also plotted in Fig. 5, indicating that
the stabilised stress is hardly sensitive to strain rate. Moreover, the
stress amplitudes in both tension and compression sides are not equal,
particularly during the first few cycles, i. e. a compressive mean stress
develops and tends to vanish as stabilisation is approached

Figure 6 shows the strain-range history effect on the cyclic response at the
constant strain rate of 1. 2 E-2 /s. The strain range was set at ± 0. 6, ± 0. 8,
and ±1.0/., for three cycles each. This incremental increase of strain level
led to different cyclic hardening responses, which depended on the maximum
strain range imposed; more hardening was observed with increasing the strain
range. The results also indicate that the hardening depends essentially on
the largest inelastic strain range, irrespective of previous history.

Figure 7 shows the cyclic response of a test specimen sequentially cycled

under different mean strain ranges (zero, positive, negative, then zero), at
the constant rate of 1. 2 E-2 /s. Cyclic hardening is observed to be highly
affected by the strain range, mean strain, and loading history. The stress
level, during the course of hardening, is noticed to be higher when the mean
strain is positive. However, the hardening rate itself is nearly the same
irrespective of the mean strain.

MODELLING AND PREDICTIONS

Chaboche unified theory of viscoplasticity was chosen in the present work to

model the experimentally observed responses and to predict possible new ones.
 247

J 1r- r*—- T ~ J
1 h-
Zi_ J
^—9 -4- l
j
i
----J-i K-3
-l x
Stt
AISI 316 SS
28°C
_^==1=x=^±=i
(a)
1- y
35.8 35.6 „
tov 2
b

i—Jug-
e <"*c> PRED. fcXP.

IM 4 . 0 E-5

4 . 0 E-3

•
(b) S7RAIN. € OO

Fig. 2. Honotonic tension

Fig. 1. Test specimens response.
(a) t e n s i l e
(b) fatigue

500 . A I SI 316 SS
20 C

400

3C0
_ -j'"
'/ u
200 . //i i _, 1 , l
100 - / • « -4— 4.0 E-3 i M - ' ^ H • —- 4 . 0 E-5 i-1—1—4.0 E-l z -~
/ °v
L L
1 2 3 4 5 6 7 8 9
STRAIN. € « )
(a)
Fig. 3. Tensile jump response
(a) experimental
(b) calculated

Fig. 4. Experimental strain-controlled

cyclic response a t & = E-3 /s,
and £. = ± IX, for 20 cycles.
ENG. STRAIN 1X2

. . . 1
1
0 gg^jlL— ^
z ?5B. a
L-
— it-
w ■. a — n-
IC-
Fig. 5. Stress amplitude vs. number *
of cycles at £= E-5, E-4,
1
2
^rami.aa
E-3, £-^2, and E-l /s, at
6 = ± 1/.
5M. ■
is. • !
2a. •
NUMBER OF CYCLES
248
The theory is yield-based and assumes initial isotropy of the material; it
can model translation and expansion of yield surface in stress space during
the course of deformation via the use of a scalar variable to model isotropic
hardening, and a tensorial one to model kinematic hardening and associated
Bauschinger effects. Ihe main equations comprising the theory, as confined
to uniaxial loading, are:

6 = 6 + 6 (i) 6 = <JIE (2)

i = Vs r B) a)
" <Y> ro - o) s --^-*i- (t) (4)
,v
b -. C(OL&"_ IB-f) - ^|8l" S*vv(6) (5)

i> , b(^-D)j> (6a) » = <\ + ( D o - ^ ) e " ^ <6b>

tx |l&'Ut,
0
(7)
_ _ J _ N

where 6 , 6 , 6 are the total, elastic and inelastic strains, and a superim-
posed dot represents differentiation with respect to time, O" is the stress, E
is Young's modulus, $ is the yield function, B is the Kinematic hardening
stress, © is the isotropic hardening stress, ^ is the inelastic strain accu-
mulation, K, n, c, a, Y , m, b, q and D 0 are temperature-dependent parameters.
In its given form, the theory is incapable of modelling many important
physical phenomena. Thus, attempts have been made by the present authors to
modify the theory in order to account for the rate dependence of initial
yielding (Abdel-Kader et aL , 1986), dynamic strain ageing exhibited at
elevated temperatures (El-Hefnawy et al. , 1989), anisotropy and associated
yield surface distortion (Eleiche, 1991), phase transformations, etc.

Ihe material parameters of the theory have been evaluated employing uniaxial
test data Details involved in determining the initial values of these
parameters and their subsequent revision are given by El-Hefnawy (1989). The
final values of these parameters which were used in calculating various
predictions in the present paper are: K = 110 HPa^fs; n = 5. 80; b = 8. 80;
q = 270 MPa; ID0 = 160 MPa; c = 65. 0; a = 170. 0 MPa; m = 1. 3; Y = 8. 2 E-10 s
MPa""1*1 ; and E = 190000 MPa.

Together with the experimental monotonic and incremental stress-strain curves

shown in Figs. 2 and 3, respectively, corresponding predicted responses are
shown in the same figures. Experimental and predicted results compare
favourably, both qualitatively and quantitatively.

Hie predicted cyclic responses for the first twenty cycles at the strain
rates of E-5, E-4, E-3, E-2, and E-l /s over the strain range of ±1. OX have
been predicted and a representative output at the particular strain rate of
E-3 /s is shown in Fig. 8, whereas Fig. 9 exhibits the predicted peak stress
as function of the number of cycles for all five strain rates. Cyclic
characteristics exhibited by the material (cf. Figs. 4 and 5) are seen to be
predicted Thus, stress-strain hysteresis loops show progressive increase of
stress amplitude with corresponding decrease of inelastic strain amplitude.
Also, a relatively small compressive mean stress is seen to develop during
cycling, which tends to vanish as the number of cycles increases and the
response stabilizes, in consistence with the experimental response of Fig. 4.

The predicted strain-controlled cyclic response at the rate of 1. 2 E-2 /s and

successive strain ranges of ±(10. 6, 0.8, 1.0, 0.8, 0.6) X, each lasting for
three cycles, is shown in Fig. 10, whereas the response at the same strain
 ENG. STRESS CMPol
-'* A * - a «

' 1 J

230. ■
=^n/"7
/

300.0

ENG.STRAIN CX3
ENG. STRAIN C«
Fig. 6. ExperiEoental hysteresis loops, obtained Fig. 7. Experimental hysteresis loops, obtained
at strain ranges of ±0. 6X, ±0. 8X and at different mean strain ranges, and
ilZ; £>= 1.2 E-2 /s. £ = 1.2 E-2 /s.
STRESS, <r W o )
AISI 316 SS "•[
20°C «h 300

200
AISI 316 SS
| 100 20° C

- + - STUAW
STRAIN, €OQ 8f ° U/SIO
B-ioo 1.0 E-5
oi 1.0 E-4
-200 |- 1.0 E-3
. _ .1.0 E-2
1.0 E-l
-300

• 12
CYCLE NUMBER

Fig. 8. Predicted strain controlled cyclic Fig. 9. Predicted peak stress vs. number of
response at L = E-3 /s, and £ = ± IX cycles for t = E-5 to E-l /s;
249

for 20 cycles. £=±1X.

250
rate and a reversed succession of strain ranges, i. e. ±(1.0, 0. 8, 0. 6, 0. 8,
1.0) X, is shown in Fig. 11. The first nine cycles in Fig. 10 simulate
favourably the experimental response of Fig. 6; it is also noted that upon
decreasing the strain range from ±1. OX to ±0. 8X and then to ±0. 6X, no further
hardening takes place and the response seems to have stabilized However,
increasing the strain range from ±0. 6X to ±0. 8X and then to ±1. OX, as shown
in Fig. ll, induces further hardening, although at a decreasing rate.

The predicted cyclic response under the different mean strains of Fig. 7 is
depicted in Fig. 12, and also compares favourably with experimental results.
On the otJher hand, the Ghaboche theory can also model the dependence of tlie
unloading response on the rate of unloading. Figure 13 shows the monotonic
response at a strain rate of E-3 /s and the unloading responses at the three
unloading rates of E-5, E-3 and E-l /s for different prestrains of 0. 2, 0.4,
and 0.6 X. In all cases, the largest unloading rate (E-l /s) induces elastic
unloading, the intermediate rate (E-3 /s) results in limited inelasticity
followed by elastic unloading, while the lowest rate (E-5 /s) causes
considerable inelasticity (taking the form of stress relaxation) before
elastic unloading. Classical plasticity theories assume elastic unloading
and are not capable of predicting responses such as those of Fig. 13.

Finally, the calculated monotonic response at £ = 8. 1 E-4 /s is plotted in

Fig. 14, together with the experimental tensile data shown as filled circles.
Experimental torsional data have been recently collected on AISI 316H SS
(Eleiche, 1991) over a wide range of temperatures; those pertaining to i :
1.4 E-3 /s are represented by filled triangles also in Fig. 16. Definitions
used for the equivalent stress and strain are those based on the von Mises
criterion, i.e. cre = X (3, andfc>e= * / \f3. At equivalent conditions, the
material exhibits different responses when tested in uniaxial tension and
torsion; the initial yield being higher and subsequent strain hardening
smaller in torsion than in tension; this trend seems to persist also at 550
and 650 °C (Eleiche, 1991). Similar differences in behaviour between tension
and direct shear for 316H SS at the ambient temperature have been also
observed recently by Albertini et al. (1990). To account for such
differences, it is necessary that the yield function of von Mises used in
Ghaboche theory be modified by introducing a variable Hi 11-type anisotropy
tensor. In one-dimension, eq. (4) becomes:

i = H*~ B l - »(t> (8)

where H is the uniaxial anisotropy modifier, taken to depend on <*> , i. e.

M - H 0 +M d (t) , (9)

where 1M0 is a material parameter introduced to model initial anisotropy, if

any, whilst IM^(P) is intended to model deformation-induced anisotropy. The
form of IM<)L is chosen in accordance with the behaviour of the material
considered For AISI 316 SS, M^(p) is taken to have the form:

nt(t)-- ^(i-e-~t) , (10)

where IHi andcx are material parameters. Further details of the modification
can be found elsewhere (Eleiche, 1991). Final values of the additional three
material parameters involved are: M 0 = 0.65, M^ = -0.4, and<x = 1.75. Ttie
calculated stress-strain curve using this modified version of Chaboche theory
is also plotted in Fig. 16; it is seen that it provides better modelling of
the torsional data, thus accounting for initial as well as deformation-
induced anisotropies inherent in the tested material.
 AISI 316 SS
29 C

STRAIN, CO STRAIN, OO

Fig. 10. Predicted hysteresis loops at Fig. 11. Predicted hysteresis loops at
& = 1.2 E-2 /s, and successive strain & = 1. 2 E-2 /s, and successive strain
ranges ±(0.6, 0.8, 1.0, 0.8, 0. 6)Z, ranges ±(1.0, 0.8, 0.6, 0.8, 1.0) X,
each lasting for three cycles. each lasting for three cycles.

STRESS,, <r W o >

Fig. 12. Predicted hysteresis loops at STRAJH, OO

different mean strain ranges, and
t = 1. 2 E-2 /s. Fig. 13. Effect of unloading strain rate on
unloading response.
251
252

ill

a ji« MOORED CHABOCHE

§C ?0Oji'' ORIGINAL CHABOCHE
• TENSILE OATA
Fig. 14. Calculated equivalent stress-
▲ TORSIONAL DATA
strain curves using the
original and modified Chaboche
theories, and comparison with
experimental data.
EQUIVALENT STRAIN, e , ( V . )

CONCLUSIONS

The unified constitutive theory of Chaboche has been adopted to model the
ambient temperature viscoplastic behaviour of AISI 316 SS. Nine material
constants are needed to calculate the uniaxial response under monotonic,
jump, and strain-controlled cyclic loadings; predictions are in agreement
with test data available. More complicated behavioural aspects are also
predicted, but await experimental verifications. On the other hand, using a
Hill-type-anisotropy modifier with three additional material constants, the
theory can be improved to allow accurate prediction of torsional shear data.
Future improvements can be extended to multiaxial plasticity as well.

ACKNOWLEDGEMENTS

The cyclic tests reported herein have been conducted at the Appl. Mech. Div.
of the CBC JRC in Ispra, Italy. Special thanks are due to Dr. G. Verzeletti
and Mr. E. Gutierrez for permission to share their experimental results.

REFERENCES

Abdel-Kader, M. S. , J. Eftis and D. L. Jones (1986). An extension of the

Chaboche theory of viscoplasticity to account for rate-dependent initial
yield Proc. SBCTAH XIII, 863-269.
Albertini, C. , M. Montagnani, E. V. Pizzinato, A. Rodis, S. Berlenghi, G.
Berrini, G. Pazienza and A. Paluffi (1990). Mechanical properties in shear
at very high strain rate of AISI 316 stainless steel and of a pure iron.
Comparison with tensile properties. Proc. EXPLOMET '90.
Chaboche, J. L. (1977). Viscoplastic constitutive equations for the
description of cyclic and anisotropic behaviour of metals. Bulletin de
l'Academie Polonaise des Sciences, 25, 33-42.
Eleiche, A. M. , C. Albertini and M. Montagnani (1985). Ihe influence of
strain-rate history on the ambient tensile strength of AISI type 316
stainless steel. Nuclear Engineering and Design, 88, 131-141.
ELeiche, AM. (1991). Inelastic shear deformation of stainless steels under
quasi-static and impact sequential reverse torsion. Final report to CEC
JRC, EURATOM, Ispra, Italy.
El-Hefnawy, N. N. , M. S. Abdel-Kader and A. M. Eleiche (1989). Inclusion of
DSA modelling capability in unified viscoplasticity theories, with.
application to Inconel 718 at 1100 F. Proc. 19th Canadian Fracture
Conference on Constitutive Laws of Plastic Deformation and Fracture, pp. 8-
1 to 8-10.
El-Hefnawy, N. N. (1989). Constitutive theories of viscoplasticity: Theory
and experiment. Ph. D. Dissertation, M. T. C. , Cairo, Egypt.
WS2a3

CONSTITUTIVE RELATIONS OF ANNEALED COPPER

UNDER DYNAMIC LOADINGS

K. K1SHIDA, M. NAKANO and K. FUSE

Department of Precision Engineering, Faculty of Engineering,

Osaka University, 2-1 Yamadaoka, Suita, Osaka 565, Japan

ABSTRACT

Constitutive relation of annealed copper was investigated through the tests

under different loading histories, which consist of jump, dynamic and
dynamic reloading. The tests were performed on the stress bar method, where
the dynamic stress-strain behavior was measured precisely in small strain
range. A unique relationship was found between plastic strain rate and over
stress from the jump tests. On the other hand the relations were not unique
for dynamic and dynamic reloading tests that the curves were different from
that of the jump test in the initial stage of dynamic deformation, but it
became concurrent with the jump test. The behavior could be reasonably
explained by the model of varying density of mobile dislocations in the
thermal activation theory.

KEYWORDS

Annealed copper; stress bar method; strain rate; over stress; loading
history; mobile dislocation density.

INTRODUCTION

It is one of the fundamental subjects for the dynamic plasticity to reflect

effects of strain rate and strain rate history on the constitutive equation
of material. Strain rate sensitivity was confirmed for various metals by a
great number of experimental works (Harding, 1987). There exist, however,
limited works for the influence of strain rate jump on the stress-strain
curve using the split Hopkinson bar method.

In the present paper, dynamic stress-strain behaviors of annealed copper

were examined by the torsional stress bar method (Kishida et al.y 1968),
in which one dimensional stress wave propagation is strictly satisfied and
dynamic stress and strain are measured at a point of the specimen. Three
types of tests were executed; (i) jump (J) test in which a dynamic stress
was applied to a specimen during deformation at a static strain rate, (ii)
wholly dynamic (D) test and (iii) dynamic reloading (DR) test that a dynamic

253
254
stress applied to a specimen which had been statically strained and
unloaded.

EXPERIMENT

In Fig. 1 the fundamental of the stress bar method is shown. A tubular

specimen is joined to an elastic input tube of the same outside diameter and
thickness. An incident stress pulse n reaching the interface between the
input bar and the specimen a portion of the pulse is transmitted into the
specimen and the remainder is reflected. On the both side of the interface
equilibrium equation for stress r/v-r/p-rr always holds. The specimen
deforms plastically by ZT and it is gotten from n and r/? which are
measured by the strain gages A and B. Corresponding strain of the specimen
is measured by the gage C.

The experiments were executed with the apparatus shown schematically in Fig.
2. A torque is stored in the store bar between the twist end and the fixed
end where the bar is connected to the holding pins through a fracture plate.
When the plate is fractured by the torque stored and the fix is released a
torsional stress wave propagates along the input bar toward the specimen.
In the dynamic tests the specimen's end is kept free and the fracture plate
is set just contact with the holding pins as shown as (a) in the figure.
For the J test the specimen's end is clamped and the fracture plate is set
with a free angle as (b). In this case the stress wave loading is applied
on the specimen that has been statically strained during rotation of the
angle.

input bar $ specimen

A B C

f .x-l T
R — -*T I
fc
B

Fig. 1. Torsional stress bar method.

(a) (b)

Fig. 2. Schematic of apparatus.

 255
The specimen of thin-walled tubular section is high purity copper (99.99 %)
with outside diameter of 20.0 ram, wall thickness of 1.2 mm and length of 300
mm. The input tube is made of a Ni-Cr-Mo steel of the same diameter and
thickness. They are joined by brazing with a silver solder of 0.1 mm
thickness, and annealed at 550°C for 2 hours and furnace cooled.

EXPERIMENTAL RESULTS

In Fig. 3 stress-strain curves obtained from the J tests are shown. Rapid
changes of strain rate were given at 0.27, 0.60, 1.47 and 2.10 % strains.
In our experiments strain rate does not change step-like, we consider
accordingly the variation of strain rate through the dynamic deformation.

Following a treatment in the theory of viscoplasticity (Perzyna, 1966) we

intended to derive relations between plastic strain rate and over stress.
The over stress is defined as r-rs where r is the dynamic flow stress and is
the stress at static strain rate. The plastic strain rate is calculated
from ip = 7 - 7e = 7 - rjG where G is the shear modulus of the metal.

The over stress - plastic strain rate relation reproduced from Fig. 3 are
shown in Fig. 4. It is obvious that there exists a unique relationship for

& 60

Z 20

1.0 2.0 3.0 4.0

strain y (%)

Fig. 3. Stress-strain curves from J tests.

^ 20r

0 400 800 1200 1600

plastic strain rate Yp (1/s)

Fig. 4. Over stress - plastic strain rate curves

from J tests.
256
the results of the J tests. The relation can be expressed as

iP - C0(T - r,)m. (1)

The constants were determined as follows

C0 = 22 A [1 l{MPa)m s], m = 1.40.

It is shown by the dashed line in Fig. 4.

Next we describe the results from the D tests. Stress-strain curves for the
annealed copper obtained from four runs of the tests are shown in Fig. 5.
The rate of plastic strain is not expected to be constant in the D test,
then we derive the relation between over stress and plastic strain rate. An
example is shown in Fig. 6, where the arrows indicate the process of the
dynamic deformation in the test, and the dashed line is the result from the
J test. It is seen that the deformation in the D test proceeds differently
with that of the J test in the initial stage but becomes coincident.

In the last we refer to the DR test. A stress-strain behavior is presented

in Fig. 7, and the over stress - plastic strain rate relation in Fig. 8. It

20 s"
D14
'"''
15t
- ^
jr
101

( '/
1 -\\

4.0 ~0 400 800 1200 1600

plastic strain rate y-p (1/s)

Fig. 5. Stress-strain curves from Fig. 6. Over stress - plastic strain

D tests. rate curve from D test.

20
D98

15

10 / /
/s
3 20
I/* eauation (1)

v
\y
4.0 0 400 800 1200 1600
plastic strain rate -yp (1/s)

Fig. 7. Stress-strain curve from Fig. 8. Over stress - plastic strain

DR test. rate curve from DR test.
 257
is clear that the behavior is very similar to the result of the D test. It
should be pointed that the difference between the D or DR tests and the J
test lies in whether the dynamic loading is applied on the specimen of no
load or being strained at static strain rate.

DISCUSSIONS

Influence of strain rate on the flow stress of a metal has been studied on
the thermal activation theory of dislocations. Here we consider the
relation (1) according to the theory. The plastic strain rate iv is related
to the activation energy of dislocation AG as

iP = i0exp(-AG/kT), (2)

where k is the Boltzmann constant and T the temperature. y0 is a material

constant;

7o = P O ^ D / 2 . (3)

Po is the mobile dislocation density, b the Burgers vector and v& the Debye
frequency.

AG is a function of effective stress re and assumed to be as follows

A G = G0/n(r0/re). (4)

Go and ro are constants. The effective stress, which is concerned with the
dependence of strain rate, is given as re=r-n, where r is the applied
stress and n is the stress due to interaction of dislocation with long
range stress fields. n is assumed to be equal to the static flow stress
rs. Using (3) and (4) to (2), we get (1) putting C0 = p0b2vD/2T™ and
m = G0/kT.

It has been considered in (1) that Co is constant and thus the mobile
dislocation density does not vary. In order to explain the transient
behavior seen in Fig. 6 or 8, the factor will be assumed to be a variable
with the density of mobile dislocation as

C(p) = pb2vD/2r?. (5)

Using (1), (2), (3) and (5) we get

p/Po = C(p)/C0 = 7p/(r - rs)mC01 (6)

where Co and m have been determined. By the use of the data from the D and
DR tests we can estimate the ratio as a function of time, the origin of
which is taken at the start of plastic deformation, and it is shown in Fig.
9.

It is apparent that the mobile dislocation density for the D or DR tests

rises in the same manner with time to the value of Po in about 15
microseconds. The initial transient portions in Figs. 6 and 8 lie
correspondingly in the rising part of the curves in Fig. 9. It can be
considered that the mobile dislocation density is in a steady state at the
beginning of the dynamic deformation in the J test, while a certain time is
needed to get to the steady state when a dynamic load is applied on the
specimen unloaded.
258

2.0

1.5

1.01

0.5

10 20 30 40 50
time t (us)

Fig. 9. Time variations of mobile dislocation density

in D and DR tests.

CONCLUSIONS

Dynamic constitutive relationship for an annealed copper was investigated in

a comparatively small strain range through the tests under different loading
histories. The conclusions are as follows;
(1) A definite relation is found between the over stress and the plastic
strain rate for the dynamic deformation in the J test.
(2) The relations for the D and DR tests are different from the J test in
the initial stage of the deformation but tend to concur in the subsequent
stage in a definite time. The transient behavior is successfully explained
by the consideration of varying density of the mobile dislocations.

REFERENCES

Harding, J. (1987). The effect of high strain rate on material properties.

In: Materials at High Strain Rates (T.Z. Blazynski, ed.), pp. 133-186.
Elsevier Applied Science, London.
Kishida, K. and K. Senda (1968). New experimental method for determining
dynamic stress-strain relation of metals. Exper. Mech., 8-12, 567-571.
Perzyna, P. (1966). Fundamental problems in viscoplasticity. In: Advances
in Applied Mechanics, Vol. 9, pp. 243-377. Academic Press, New York.
WS2a4

CONSTITUTIVE MODEL OF SEVERAL MATERIALS AT HIGH RATES OF STRAIN

J.P.ANSART and O.NAULIN

Commissariat a l'Energie Atomique - Centre d'Etudes de Bruyeres le Chatel

B.P.12 - 91680 Bruyeres le Chatel. FRANCE

ABSTRACT

The influence of strain rate and temperature on yield stress and flow stress
of materials is introduced in a constitutive model. It is compared to
Steinberg Cochran and Guinan model. Several results are proposed on
different materials including beryllium and tantalum.

KEYWORDS

Elastoplasticity; strain rate effects; constitutive model.

INTRODUCTION

The increasing development of computer codes which calculate the impact res-
ponse of structures needs the use of elastic-plastic constitutive models.
These kinds of ir xiels must describe material properties at high strain rates
and should be as directly as possible introduced in computer codes.

First constitutive laws only took into account yield stress and its evo-
lution with strain rate and temperature. In the beginning of the eighties
Steinberg Cochran and Guinan (S.C.G.,1980) proposed a new model where a work
hardening function was introduced. This model is now used in many computer
codes.

In this paper, first we would like to discuss the formalism of this model
which is not, in its classical form, strain rate sensitive. Then, we will
modify S.C.G. model in order to take into account explicitly strain rate ef-
fects.

REQUIREMENT

In order to describe the mechanical properties of materials in a large range

of strain rates (lO'^s"1 <£< 10 s ) several approaches can be used to pro-
pose a relationship between stress, strain, strain rate and temperature
f (o,e,6,T)=0.
259
260
The first one is based on dislocation mechanisms and more generally on the
description of micro-mechanisms (for example Steinberg Lund approach 1989).
This can be considered as a theoretical approach. It needs many microscopic
data (mobile dislocation density, Burger's vector, Peierls stress . . . ) . We
think that it will be rather difficult to use it directly in computer codes.

On the other side, empirical relationships are proposed (Steinberg's ap-

proach) . This approach needs many tests and there are generally no tenden-
cies between different materials.

A mix of these both approaches can be used.

THE CONSTITUTIVE MODEL

The approach can be divided in two stages.

The first one is based on Steinberg model. Steinberg proposed two empirical
functions to describe shear modulus G and yield stress Y evolutions :

0 = O 0 [l + £(T) + g(P)]
n
Y = Y Q . (1 + M ) . [1 + f (T) + g(P)] P : pressure

As we said previously, e is not explicitly introduced.

We have recently proposed (Ansart Dormeval 1989) a function Y Q (6) which is

based on microscopic considerations : thermally activated processes. Viscous
drag mechanism which is often observed at large strain rates affects only
plasticity where large dislocation displacements are obtained. So we propose
to introduce a function YQ(£) which can be written as follow:

Y Q (e) = Y Q ' + a.log e .

This expression is valuable for most current temperatures T < T C where T c cor-
responds to the transition between thermally activated process and athermal
mechanisms. So we can write :

Y 0 (£,T) = Y Q '(T) + a(T).log 6 ; T < T C

Y Q (£,T) = Y Q ' (T) T>TC .

On the other side many experimental results show that work hardening parame-
ters p and n are really strain rate and temperature sensitive. One typical
example is tantalum behaviour which is reported fig. 1.

A semi-empirical approach is then used fitting 0-£ experimental curves for a

large scale of strain rates and temperatures. So the global formalism of the
model we propose is :

Y = (Y Q ' (T) + a(T).log i) . (1 + 0(6, T) .6) n <6' T > . [1 + g (P) ] .

 261
We can see that temperature sensitivity is directly introduced in the work
hardening function : f (T) doesn't exist any more. On the other side the
pressure sensitivity formalism is the one proposed by Steinberg.
G
MPa A
600
600 - £ = 103s"1 ^ - T=20°C
508(1+219.£)°
a= 508, ( 1 + 2 1 9 . £ ) ° - 0 3 3

400 400
|
—T=600 C
£ = 10
a= 149 (1+105. £ ) ° - 282
/ <y= i 9 i . ( i + 2 i . £ )

2004 200

T=20°C

, r**-
0 0.2 0.4 £ ° 0.2 0.4s
Fig.l. Tantalum 0-e curves.

OUR APPROACH

For every new material we have to develop a lot of experiments. First we

perform at several temperatures compressive tests from quasi static loading
conditions (classical universal machines) to high strain rates (Split Hop-
kinson pressure bar). This allows to propose some parameters of the model
and their evolutions with strain rate and temperature. Unfortunately unia-
xial compressive tests only lead to limited strains ( e<0.4 maximum) and to
limited strain rates (e < 3000 s"1 ) .

In order to extrapolate the values of parameters other experiments are ne-

cessary. We used Taylor test which allows to reach locally larger strains
(up to £=1) and larger strain rates (e = 1 0 5 s _ 1 ) . These experiments don't
give directly data but are only used to compare specimen profiles to predic-
tions of the model : this needs calculations.

RESULTS

In the following paragraphs we will show some results we have obtained on

two materials : beryllium and tantalum.

Beryllium

We can see on the table below a description of the material we used :

-beryllium S200F made by BRUSH-WELLMAN. Average grain size 15|im.
-composition (wt%)

element Be BeO Fe C Al Mg Si others

wt% 98,9 0,9 0,08 0,09 0,03 0,01 0,02 <0.04

262
Figure 2 summarize compressive experimental results. We can see that this
material is really strain rate sensitive. These results allow to propose a
model f (Y,e,e,T)=0 with the previous formalism where :
Y
0 - Yl+ V T
'* a<T) = a l
• b9
p(£,T) = b..£ , with bj and b 2 as exponential functions of T,
• n4
and n(£,T) = n1 + n2.loge + n3.e , where n i are functions of T
quasi static influence dynamic influence

MPa MPa
G= 336. (1+75.£)
G= 336.(1475.£)
^-T,20°C

T=300°C
0.210
G= 266.(1+910.£)

0 0.1 0.2 £ 0 0.1 0.2 £

Fig. 2. Beryllium 0-e curves.

Then we made some calculations of impact test sample profiles with a 2D code
using several models including elastic perfectly plastic, S.C.G. standard
and our model. We can see fig. 3 (Montoya and al. 1990) a comparison of cal-
culated and experimental profiles for a Taylor test sample impacted at
V = 150 m/s at room temperature. It is obvious that for this strongly harde-
ning metal, elastic perfectly plastic model doesn't work but we also show
that our model gives the best agreement with experimental profile.

— : experimental profile
•■•- : elastic perfectly plastic model Y = 330 MPa
o
il : Steinberg's model:
Y = 330 (1 + f(T) + g(P)).(l + 2 6 . 6 ) ),78 MPa
: our model:
Y = Y (£,T).(1 + g(P)).(l + 6 (£,T). I ) n(t,T)

la i> L(mm)

Fig. 3. Beryllium : comparison of calculated and experi-

mental profiles for a Taylor impacted sample.
 263
Tantalum
Description of the material : tantalum made by Thyssen.
composition wt% Ta : 99.8

average grain size : 70 um.

element C N O

wt (ppm) 20 15 20

We have seen fig. 1 how much this material is strain rate sensitive, so it
is natural to obtain a better agreement with our model (including strain
rate effects) than with S.C.G. model (fig. 4a : Taylor test profile
VQ = 145 m/s, T Q = 20 °C) . This agreement is again better at T Q = 400 °C
where even the specimen good final length is not obtained with S.C.G. model
(fig. 4b).

oerimental profile

elastic perfectly plastic model

Y-770 MPa

Steinberg's model:

(P)).(l + /J(£.T) £ ) n ( £ > T)

a.

b.

Fig. 4. Tantalum - Taylor test calculation results -

a : comparison of calculated and experimental
profiles
b : length evolution versus time
264
CONCLUSIONS

We have developed a new constitutive model. The formalism of this model is

perhaps more complex but our approach which is semi- empirical leads to good
results for large strains and strain rates limited to 10 5 s" 1 . Next we would
like to simulate plate impact experiments to reproduce experimental shock
and release wave profiles.

REFERENCES

Ansart J.P., Dormeval R. (1989) Advances in plasticity, Ed. A.S.Khan and

M.Tokuda p.371

Montoya D., Naulin G., Ansart J.P., International Conference on High Strain
Rate Phenomena in Materials (1990) to be published.

Steinberg D.J., Cochran S.G., and Guinan M.W. (1980). J. Appl. Phys. 51.
p.1498.

Steinberg D.J., Lund C M . (1989) J. Appl. Phys. ££,p.l528.

WS2b1

FURTHER DEVELOPMENT OF A UNIFIED ELASTIC-VISCOPLASTIC THEORY

S.R. BODNER
Department of Mechanical Engineering
Technion - Israel Institute of Technology
Haifa 32000, Israel.

ABSTRACT

Possible extensions and generalizations of the Bodner-Partom unified constitutive model for
elastic-viscoplastic behavior are described. These include incorporation of a phase angle effect
between plastic strain rate and deviatoric stress, consideration of strain rate and temperature
dependence of hardening, and generalization of the cyclic loading condition. Also the
particular treatment of directional hardening which is not based upon a back stress parameter is
discussed.

KEYWORDS

Constitutive equations, viscoplasticity, strain rate effects, hardening.

INTRODUCTION

The set of constitutive equations developed by the author and associates was intended to
represent the principal features of the small strainresponseof elastic-viscoplastic materials over
a wide range of temperatures, strain rates, and loading conditions. Their development was
motivated by the physics of inelastic deformation of polycrystalline media and placed in the
context of continuum mechanics. The main features of those equations, (B-P), given in
Table 1, are:

1. They do not require a prescribed yield criterion or loading/unloading conditions, i.e. both
elastic and inelastic strain rates are generally non-zero.
2. Plastic deformation is controlled by a flow law between plastic strain rate and deviatoric
stress and by a kinetic equation relating the second plastic strain rate invariant D£ to the
second stress invariant J2 and a scalar hardening variable Z.

3. Evolution equations for hardening consist of a scalar equation for isotropic hardening and a
tensor equation for directional hardening; a scalar effective value of the directional hardening
tensor Z D combines with the scalar isotropic value Z1 to give the total hardening parameter
Z; terms are included in both evolution equations for thermal recovery of hardening.

265
266

4. Strain rate dependence of plastic flow is controlled primarily by the parameter n which
varies with temperature; strain rate independent plasticity is realized as n becomes large
which should occur as the temperature approaches absolute zero; at absolute zero, the
effective (scalar) flow stress value referred to as the "mechanical threshold" becomes equal
to the hardening variable Z; the parameter Do represents the limiting plastic strain rate in
shear.

The set of equations given in Table 1 is relatively simple and appears to provide the main
characteristics of time dependent plastic flow for a number of materials subjected to a range of
temperatures and to various loading conditions, (Bodner, 1987). Restriction of the complexity
of the equations does, however, lead to exclusion of certain response characteristics, such as
transient effects, which may be of interest under some circumstances. Also, some aspects of
the equations are non-conventional according to present general practice. The purpose of this
paper is to outline methods to expand the applicability of the constitutive equations and to
discuss the somewhat controversial treatment of directional hardening.

TREATMENT OF DIRECTIONAL HARDENING

Important quantities in viscoplastic constitutive equations are history dependent hardening

variables which represent resistance to plastic flow. As such, they reflect an energy dissipation
mechanism and have the dimension of stress (work/unit volume) although they are not related
to an actual force per unit area; they could be scalar or tensorial. For the directional hardening
tensor pjj, the evolution equation (7) in Table 1 is similar in form to that used by a number of
investigators with the small difference that plastic work rate rather than plastic strain rate is
taken as the generating quantity. It is noted that this description enables separation of isotropic
and directional hardening effects under uniaxial monotonic loadings for many materials (Chan
et ai, 1988). For use in the kinetic equation, a scalar effective value of Py, namely, the
component of Pij in the direction of the current stress Ojj, Z D , is used as part of the total scalar
hardening parameter Z. The physical motivation for this procedure was the observations of
Halford (1966) on the stored energy of cold work (SECW) under cyclic loading. This is a
scalar quantity that exhibits rapid reduction upon stress reversal. It is well established that
SECW is related to the total dislocation density and to the hardening characteristics and thereby
serves as the physical counterpart for the total hardening parameter Z in the B-P constitutive
equations (Estrin and Mecking, 1986; Bodner, 1987). In this viewpoint, directional
hardening, which is the principal cause of the Bauschinger effect in terms of macroscopic
parameters, is interpreted as the potentially reversible portion of the total hardening that
becomes operational upon change in stress direction. The viewpoint also appears to be
consistent with Orowan's original explanation of the Bauschinger effect (Orowan, 1959), and
with more recent investigations on the subject (Sleeswyk et al, 1986; Stout and Rollett, 1990).

The "back stress" is also a phenomenological internal variable that is used to generate the
Bauschinger effect. It carries a "physical" name which implies a physical mechanism. The
term "back stress" appears to have its origin in the metallurgical literature in the graphical
representation of the difference between the forward (prior to unloading) and the reverse (after
unloading) portions of stress strain curves when superimposed with the same origin, e.g.
Lloyd (1977). It is also used for the localized self-equilibrating stress fields of dislocations
impeded by barriers. As pointed out by Orowan, (1959), and repeated in various texts, e.g.
McClintok and Argon (1966, pp. 185-6), physical back stresses, as a rule, are not the main
factor in the Bauschinger effect. It is also difficult to relate the phenomenological back stress
parameter to possible self-equilibrating stress fields in the material system except in the very
special case when the system can be modeled as a simple two bar structure with different
materials in each bar.
 267

TABLE 1

A Summary of the Elastic-Viscoplastic Constitutive Model

Decomposition of strain rate: c

ij c
ij T c
ij (1)

Flow law: eR = Xsy ; £^ = 0 (2)

with sij = o i j - ( l / 3 ) 8 i j o k k

,2Y>
Kinetic equation: D^ = D2, expl (3)
3J,
with D | = (l/2)e{je{j ; J 2 = ( l / 2 ) s i j s i j

from (2): A.2 = D^/J 2 (4)

Total hardening variable, Z= Z +Z (5)
Evolution equations of internal variables:

a. Isotropic hardening, Z1:

l
Z^m^-Z'JWp-A,^ Z - Z , (6)

with ZI(0) = Z 0 ; Wp = OijeP = o e f f eP f f ; Wp(0) = 0

b. Directional hardening, Pij,ZD:

1/21
pij = m 2 (Z3Ui j -p i j )w p -A 2 Z 1 (PuPu) (7)

\l/2
where uy = Oy / (o^c^)'^ , vy = py / (p u py) 1 ' 2 ;

andZ D = p ijUij ; ZD(0) = 0 , py(0) = 0 (8)

Material constants:

Do, n, Zo, Zi, Z2, Z3, mi, m2, Ai, A2, n, 1*2, and elastic constants; with n=n(T)

(In most cases can set Z2=Zo, Ai=A2, ri=T2)

268
The directional hardening parameter of the B-P constitutive model, Table 1, would be a load
history dependent material property that can be used directly in a formulation without a
prescribed or implied yield criterion. It can also identify with the residual stress state for the
two bar structural model but will not indicate the possibility of reverse inelastic deformations,
i.e. negative plastic flow for positive stress (force). With this parameter, the expression for the
dissipation rate takes on the standard form for the rate of plastic work. As a representation of
directional hardening for single and multi-phase materials, the procedure of the B-P equations
is generally satisfactory but would not indicate reverse plastic flow or a phase angle shift
between plastic strain rate and deviatoric stress. It is noted that although the back stress
parameter has the apparent potential to show those effects, additional back stress parameters are
generally needed for each of them implying that different physical mechanisms are operative.

ADDITIONAL HARDENING AND PHASE LAG EFFECTS

It has been observed that multiaxial non-proportional loadings can lead to additional hardening
and phase lag effects for various materials,e.g. Tanaka et al (1985). Limited tests indicate that
these are transient effects in the sense they would tend to diminish with resumed proportional
loading, e.g. Benallal and Marquis (1987). The physical mechanisms responsible for these
effects are complex and would be difficult to incorporate directly in a global type constitutive
theory. Alternatively, the effects can be introduced in a phenomenological manner through a
new internal variable that evolves with non-proportional loading history and diminishes with
maintained proportional loading. Possible measures of non-proportional loading have been
previously suggested, Bodner and Rubin (1986), Bodner (1987),

e^cos^VijVij) (9)

6 2 = cos-^UijUy) (10)

where

vl/2 . - a tin a \]/2

V;; Pij/(PkiPki)1/2 ; v = Pij/(pkIpkl) (ii)

Uij = V K i a k i ) 1 / 2 ; U
= V(*U6M)1/2 (12)

Equation (9) uses quantities which are load history dependent while eq. (10) uses current stress
and stress rate values. Another measure was adopted by Benallal and Marquis (1987) which
would reduced to eq. (10) for the basic form of the B-P equations but not for the Chaboche
type theory used by those investigators. Which measure is generally most appropriate has not
been decided.

With a measure of non-proportional loading, 9, an addition ai to the applicable saturation

value for hardening can be obtained by a suitable evolution equation for <xi,

a^m^Zjsinel-aJWp ; ax > 0 (13)

where rri4 is the rate and Z4 is the limiting value of ai. Upon return to proportional loading,
 269
sin0-»O so that <*i would become negative and oti would tend to zero. The limited test results
indicate that this hardening effect acts to increase isotropic hardening (Tanaka et al, 1985) so
that the saturation value would become Zj+oci with a maximum of Z1+Z4. An application of
this procedure for Hastelloy-X at room temperature is given by Bodner (1987).

Non-proportionality of loading can also lead to an angular deviation between ejj and sy which
would not be indicated by the basic flow law, eq. (2). Following the procedure of
phenomenological representation, the flow law could be modified to

e? = X[ss + b-f(e)wij] (14)

where X is the expression obtained from the basic form of the flow law (2,4) and the kinetic
equation (3), b is a new material constant, f(0) is a function of the non-proportional loading
parameter, and WJJ is the unit deviatoric tensor orthogonal to sy and having the same principal
directions. The tensor WJJ can be obtained mathematically from Sy at any stage in the loading
history, and f(0) should vanish for proportional loadings, e.g. f(0)=sin0. It seems preferable
to use 0=0i, eq. (9), because of its history dependent features. With an assumed form for
f(0), the constant b would be obtained from a non-proportional loading test.

It is noted that the term b • f(0)w^ does not contribute to the plastic work rate since Wy is
orthogonal to s^. The term does lead to a phase angle between e^ and s^ but will have
essentially no influence on the hardening variables, or on the stress levels for conditions of
strain control; it can have an influence on the direction of the stress tensor. The suggested
modification, eq. (14), therefore leaves the simple form of the basic equations intact for
proportional loadings and provides a means for incorporating the phase angle effect without the
introduction of a back stress variable.

As discussed previously, the B-P equations, Table 1, admit a procedure for obtaining the
material constants for both isotropic and directional hardening from monotonic stress-strain
curves at constant strain rates, Chan et ai, (1988). These derived constants have been shown
to be suitable for calculating cyclic stress-strain curves that agree well with test data for a
number of materials, Chan et at, (1988, 1989, 1990a,b). Within such a format, there would
be a relation between the monotonic stress-strain curves and the envelope of saturated cyclic
stress-strain curves at different strain amplitudes. In particular, the saturation values of the
hardening variables are the same for both cyclic and monotonic conditions. Although such a
relation does seem to exist for some materials, it is not sufficiendy general since the envelopes
of saturated cyclic curves can indicate wide variations with respect to the monotonic stress-
strain curves.
To enable the representation of cyclic stress-strain curves to have more generality and
flexibility, the measure of non-proportional loading 0i, eq. (9), can also be used for the cyclic
condition. Again, an additional hardening (or softening) variable has to be introduced which
depends on stress reversals, i.e. cyclic loading conditions, and which modifies the isotropic
hardening variable Z1 which controls the growth or contraction of cyclic stress-strain curves. A
suggestion of an evolution equation for a cyclic hardening parameter 0:2 that is added to the
saturation value of isotropic hardening is,

d 2 = m 5 [Z 5 - oc2](l - cos01)Wp (15)

270
where 1115 is the rate and Z5 is the limiting value of 0:2. Proportional loading without stress
reversal leads to cos9i=l or d 2 =0. For proportional cyclic loading, cosGj = - 1 over some
portion of the straining cycle for which eq. (15) takes on the standard form. This procedure
thereby includes the memory of the cyclic strain amplitude without introduction of an explicit
memory function. When both cycling and non-proportional loading are present, the saturation
value for isotropic hardening becomes Zi+oci+ot2 with the limit Z1+Z4+Z5. For materials that
cyclically soften, 0:2 and Z5 should have negative values.

It is noted that eq. (15) would give a non-zero contribution for non-proportional loading that is
not cyclic. There is therefore an interaction between the effects represented by eqs. (13) and
(15) for that loading condition. It would seem that the material constants 1115 and Z5 in eq. (15)
should be obtained initially from uniaxial cyclic tests prior to evaluation of the constants in eq.
(13) for the additional hardening due to non-proportional loading.

TEMPERATURE AND STRAIN RATE DEPENDENCE OF HARDENING

(STRUCTURE EVOLUTION)

In the basic form of the B-P equations, strain rate dependence of plastic flow is due to
nonlinear viscosity inherent in the thermal activation form of the kinetic equation (3). Primary
temperature (T) dependence is also a consequence of the kinetic equation (3) with the material
constant n=n(T). On that basis, the equation for the one dimensional stress condition can be
expressed as,

( a / Z ) = f(e p ,T) (16)

where f(e p ,T] —»1 as T —> 0°K. This simplified form does serve as a good approximation to
the behavior of a number of materials over ranges of strain rates and temperatures.

It is, however, fairly well established that the hardening variable Z does depend on temperature
and strain rate and especially at their higher values. In material modelling exercises, it is
common practice that some of the hardening parameters become empirical functions of
temperature. Alternatively, it may be useful in some cases to define Z as a specific function of
temperature. An exponential form is often used by material scientists while a linear form is
incorporated in the fairly simple Johnson-Cook equation for the flow stress, (Johnson and
Cook, 1985). These functions are explicit in the temperature and do not include temperature
history effects. It seems that these history effects are generally not important unless dynamic
strain aging or similar metallurgical mechanisms are active in the temperature range of interest.

Strain rate dependence of hardening has been noted by a number of investigators, e.g.
Klepaczko and Chiem (1986), and introduction of this effect into the B-P equations was
suggested by Estrin and Mecking (1986). Recent investigations at high rates of straining by
Follansbee (1988) and by Clifton (1990) have shown that the strain rate sensitivity of the
hardening rate is an important feature of the inelastic deformation of a number of metals. Such
a characteristic would lead to a strain rate history effect which has been observed for some
metals and loading conditions, e.g. Campbell and Briggs (1974), Hartley and Duffy (1984).

To incorporate strain rate dependence of the hardening rate into the evolution equations for
hardening of the B-P model is relatively simple as pointed out by Estrin and Mecking (1986).
That is, the saturation value of hardening should be made a function of plastic strain rate. This
procedure was also used by Clifton (1990) in the constitutive equations he developed to
represent his test results. Since the strain rate influence on hardening appears to influence the
 271

early time response of the material, it should probably be associated with directional hardening,
i.e. Z3 should be generalized to be a function of strain rate over a range of strain rates. A test at
a high strain rate with a rapidly imposed reduction in rate would exhibit a rapid stress reduction
due to the basic kinetic (viscosity) dependence while the stress reduction due to the influence of
strain rate on hardening would be gradual since it evolves with inelastic deformation. The
analysis of Clifton (1990) on the results he obtained for pure copper at varying high strain rates
indicated that strain rate dependence of the hardening rate was an important factor.

The kinetic equation (3) adopted in the B-P model does lead to a rapid increase of flow stress
as the limiting plastic strain rate Do is approached. Due to the strong strain rate dependence of
the hardening rate for some metals, it appears that the rapid increase of flow stress with stain
rate will commence at a lower strain rate than indicated by the kinetic equation (3) for a
reasonable physical value of DQ.

CONCLUSIONS

Various response characteristics not included in by the basic form of the B-P equations can be
incorporated by relatively simple modifications of those equations. These modifications leave
the structure of the formulation intact so that the original physical and thermodynamic
interpretation of the model is retained. Other response effects can probably be treated in a
similar manner.

ACKNOWLEDGEMENT

The author would like to thank his colleague, Prof. Miles Rubin, for many useful discussions
in the preparation on this paper.

REFERENCES

Benallal, A. and D. Marquis (1987). Constitutive equations for nonproportional cyclic elasto-
viscoplasticity. ASME J. Engng. Mat. Tech., 109, 326-336.

Bodner, S.R. and M.B. Rubin (1986). A unified elastic-viscoplastic theory with large
deformations. In: Large Deformations of Solids (J. Gittus, J. Zarka, S. Nemat-Nasser,
eds.), pp. 129-140. Elsevier Applied Science, London.

Bodner, S.R. (1987) Review of a unified elastic-viscoplastic theory. In: Unified Constitutive
Equations for Creep and Plasticity (A.K. Miller, ed.), pp. 273-301. Elsevier Applied
Science, London.

Campbell, J.D. and T.L. Briggs (1975). Strain rate history effects in polycrystalline
molybdenum and niobium. J. Less-Common Metals, 40, 235-250.

Chan, K.S., S.R. Bodner, and U.S. Lindholm (1988). Phenomenological modeling of
hardening and thermal recovery in metals. ASME J. Engng. Mat. Tech., 110, 1-8.

Chan, K.S., U.S. Lindholm, S.R. Bodner and K.P. Walker (1989). High temperature
inelastic deformation under uniaxial loading: theory and experiment. ASME J. Engng.
Mat. Tech., m , 345-353.
272
Chan, K.S., U.S. Lindholm, S.R. Bodner and A. Nagy (1990a). High temperature inelastic
deformation of the B1900+Hf alloy under multiaxial loading: theory and experiment.
ASME J. Engng. Mat. Tech., JJ2, 7-14.
Chan, K.S. and U.S. Lindholm (1990b). Inelastic deformation under nonisothermal loading.
ASMEJ. Engng. Mat. Tech.,U2, 15-25.

Clifton, R.J. (1990). High strain rate behavior of metals. Appl. Mech. Rev., 43, S9-S22.

Estrin, Y. and H. Mecking (1986). An extension of the Bodner-Partom model of plastic

deformation. Int. J. Plasticity, 2, 73-85.

Follansbee, P.S. (1988). The rate dependence of structure evolution in copper and its
influence on the stress-strain behavior at very high strain rates. In: Impact Loading and
Dynamic Behaviour of Materials (C.Y. Chiem, H.D. Kunze, L.W. Meyer, eds.), pp. 315-
322. Informationsgesellschaft, Verlag, Germany.

Halford, G.R. (1966). Stored energy of cold work changes induced by cyclic deformation.
Ph.D. thesis, Dept. Theoretical and Applied Mechanics, U. Illinois, Urbana, Illinois.

Hartley, K.A. and J. Duffy (1984). Strain rate and temperature history effects during
deformation of fee and bec metals. In: Mechanical Properties at High Rates of Strain,
1984 (J. Harding, ed.), pp. 21-39. Institute of Physics, Conference Series No. 70,
London.

Johnson, G.R. and W.H. Cook (1985). Fracture characteristics of three metals subjected to
various strains, strain rates. Engng. Fracture Mech., 21, 31-48.

Klepaczko, J.R. and C.Y. Chiem (1986). On rate sensitivity of fee metals, instantaneous rate
sensitivity and rate sensitivity of strain hardening. J. Mech. Phys. Solids, 34, 29-54.

Lloyd, D.J. (1977). The Bauschinger effect in polycrystalline aluminum containing course
particles. Acta Met., 25, 459-466.

McClintock, F.A. and Argon, A.S. (1966). Mechanical Behavior of Materials. Addison-
Wesley Pub., Reading, MA.

Orowan, E. (1959). Causes and effects of internal stresses. In: Internal Stresses and Fatigue
in Metals (G.M. Rassweiler, W.L. Grube, eds.), pp. 59-80. Elsevier Pub., Amsterdam.

Sleeswyk, A.W., M.E. Kassner and GJ. Kemerink (1986). The effect of partial reversibility
of dislocation motion. In: Large Deformation of Solids (J. Gittus, J. Zarka, S. Nemat-
Nasser, eds.), pp. 81-98. Elsevier Applied Science, London.

Stout, M.G. and A.D. Rollett (1990). Large strain Bauschinger effects in fee metals and
alloys, Report No. LA-UR-90-572, Los Alamos National Laboratory, Los Alamos, NM.

Tanaka, E., S. Murakami and M. Soka (1985). Effects of strain path shapes on non-
proportional cyclic plasticity. J. Mech. Phys. Solids, 33, 559-575.
WS2b2

VISCOPLASTICITY THEORY BASED ON OVERSTRESS AND ITS

APPLICATION TO THE MODELING OF METALS AND ALLOYS

Erhard Krempl

Mechanics of Materials Laboratory, Rensselaer Polytechnic Institute,

Troy, N.Y. 12180-3590, USA

ABSTRACT

The viscoplasticity theory based on overstress fVBO) is a "unified" theory and

has been formulated for isotropy (finite and infinitesimal deformations) and for
orthotropy (small deformation only). All inelastic deformation is considered
rate dependent and elastic and inelastic deformations are always present. In
the quasi-elastic regions inelasticity is vanishingly small. The inelastic rate of
deformation depends only on the overstress, the difference between the stress
and the equilibrium stress, a state variable. It is the path—dependent stress
which can be sustained in equilibrium. The equilibrium stress, the kinematic
stresss and the scalar isotropic stress are the state variables of the theory. It
has been applied to the modeling of cyclic hardening/softening, to high
temperature deformation of alloys and single crystals at slow rates. It is
shown that dynamic plasticity at high strain rates can also be reproduced by
the model which assumes that the stress increase with strain rate is viscous in
nature.

KEYWORDS

Viscoplasticity; dynamic plasticity; state variables; inelastic analysis; creep;

relaxation.

INTRODUCTION
During the last two decades, the modeling of inelastic deformation of metals
and alloys has progressed rapidly. Previously, rate—independent plasticity and
creep theory were used in stress analysis of components operating under severe
loading conditions and in the analysis of forming processes. New constitutive
models are now available which do not reproduce exactly linear elastic
behavior. Consequently, there is no boundary between linear elastic and
inelastic deformation. Inelasticity is present at all times but becomes
negligibly small in the quasi-elastic regions. Further, all inelastic deformation
is rate dependent and no separate equations for creep and plasticity are
introduced. Because of these features, these approaches have been labelled as
"unified" approaches. A review can be found in Walker (1980), Miller (1987)

273
274

and Ohno (1990).

The viscoplasticity theory based on overstress (VBO) is one of the unified
theories and has been developed over the last fifteen years in response to
experimental observations reported in the literature and made in the Mechanics
of Materials Laboratory at Rensselaer using a biaxial, servohydraulic,
computer-controlled MTS mechanical testing machine. These experiments
showed that inelastic deformation of ductile metals and alloys is rate—dependent
at room temperature. They also demonstrated that creep, relaxation and rate
sensitivity are interelated giving justification to a "unified" approach in which
no separate equations are postulated for rate—independent plasticity and creep
as is done in the conventional models. When the application temperature is
increased the rate dependence increases normally for metals and alloys. This
can easily be reproduced in the unified models by an increase in rate
dependence and the introduction of static recovery terms in the growth laws
for the state variables. In unified models, creep develops under constant stress
in homogeneous motions and relaxation ensues when the rate of deformation is
zero. In this way, creep and relaxation are nothing but manifestations of rate
dependence for stress and deformation rate equal to zero, respectively.
THE STRUCTURE OF THE VISCOPLASTICITY THEORY
BASED ON OVERSTRESS (VBO)
VBO is one of the "unified" constitutive models which has been developed for
small and for finite deformations. The current configuration is the reference
configuration and it is assumed that the rate of deformation D is the sum of
elastic and inelastic contributions
D = Del + D in (1)
with
Del = C ^ (2)
and
D in = H[* - g]. (3)
The elastic rate of deformation is given by the product of the elastic
compliance matrix C 1 and an objective Cauchy stress rate <r, see (2). The
inelastic rate of deformation is solely a function of the overstress, the
difference between the stress a and the equilibrium stress g, a state variable of
the theory. The function H is positive and increasing. (Square brackets
following a symbol denote "function of. All stress quantities are defined with
regard to the current configuration. For infinitesimal deformation, objective
rates become time rates and the rate of deformation is set equal to the strain
rate.) Substitution of (2) and (3) into (1) yields
D = C-1* + H[a - g], (4)
the flow law of VBO. No strain quantities appear in this flow law. Also,
the second term depends only on the overstress and does not contain a drag
stress dependence as in other theories. It has been pointed out by Krempl
(1987) that a drag stress term with growth law will result in a change of rate
dependence with deformation. Whether or not deformation induced changes
influence the rate dependence must be ascertained from experiments or from
microstructural consideration. However, such considerations are scarce.
Experiments on Type 304 Stainless Steel at room temperature showed
hardening to predominantly rate independent, Krempl and Lu (1984), Krempl
(1987). Because of the experimental observations and because of other
 275

desirable features of a pure overstress dependence is postulated in VBO.

The flow law is now augmented by the growth laws for the state variables.
VBO has three such variables, the equilibrium stress g, the kinematic stress f
and the isotropic, scalar variable A. Their growth laws are
g = G[&, a - g, f - g, A], (5)

f = F[a- g] (6)
and
A = B[A, effective strain rate, other variables] (7)

where G , F and B denote suitable functions. The modeling of quasi—elastic

regions and of a permanent set after loading to the inelastic region and
subsequent unloading to zero stress in an homogeneous motion rests with the
growth laws for the state variables. To reproduce quasi-elastic regions, the
growth law for the equilibrium stress depends on the objective stress rate. In
addition to a dependence on overstress and on the tensorial kinematic variable
f through the difference g — f, the growth law for the equilibrium stress rate
is a function of the scalar A which is the large time, asymptotic value of g —
f in a uniaxial test with constant rate of deformation. It is called the
isotropic stress or variable. When it is constant, VBO represents cyclic
neutral behavior akin to only kinematic hardening in rate—independent
plasticity. If an appropriate growth law is written for A then the theory can
represent cyclic hardening/softening and the effect of changing A is similar to
that of implementing isotropic hardening in rate—independent plasticity.

The identity a = (<r — g) + (g — f) + f helps to identify the contributions

to the current stress. They are the rate—dependent overstress a — g and the
"isotropic" contribution g — f. In actual implementations, the differential
equations are chosen such that the isotropic contribution is rate independent in
the asymptotic state. Further, in actual implementations the first order
differential equations appearing in (5) and (6) permit asymptotic solutions in a
uniaxial test with constant deformation rate for which a — g and g — f are
constant. If this is the case, the growth of a ultimately parallels that of f.
In the simplest case, we can postulate a growth of the kinematic variable f
with a constant modulus which can be positive, zero or negative. This choice
results ultimately in a hardening, perfectly plastic or softening stress—strain
diagram.

For the modeling of quasi-elastic regions, it is necessary for the equilibrium

stress to grow with nearly elastic modulus initially so that the overstress and
the inelastic rate of deformation are negligibly small. This is accomplished by
formulating the growth law (5) with two terms. The first one consists of a
variable modulus multiplied by the objective stress rate and dominates in the
initial, nearly elastic portion of the stress—strain diagram. The second term is
multiplied by the overstress and is largest in regions where the tangent
modulus is small compared to the elastic modulus. When the two terms are
comparable, the transition from nearly elastic to inelastic deformation occurs.

This structure of VBO is used in various applications in the small and finite
strain regime as indicated in Table 1. Of interest here is the incremental
theory which was developed after 1984. (The deformation theory of VBO, like
the deformation theory of rate—independent plasticity, is not applicable for
complex loading paths.) It can be seen that in addition to small and large
strain isotropic material behavior we have treated the orthotropic case which
276
includes cubic symmetry as a specialization. Also, several areas are labeled
"open" to indicate that insufficient research has been done to date.

Stress and strain control

Eqs. (1) — (6) are the constitutive equations of VBO applicable for stress or
strain control. It is not necessary to have separate stress and strain space
formulations. If a material is modeled which exhibits strain softening in the
inelastic range, then the computed stress—strain diagrams will ultimately have a
negative slope at every strain rate. For stress-controlled loading the solution
will become unstable after the maximum stress has been reached.

Modeling of permanent set

Within VBO the modeling of a permanent set is not a question of kinematics

but rather a question of the growth laws for the state variables, specifically
the equilibrium stress. The permanent set is found by performing numerically
what is done experimentally, loading to a strain in the inelastic region followed
by unloading to zero stress. Such a test has been performed with two
different growth laws for the equilibrium stress. In Fig. la, the incremental
growth law of Yao and Krempl (1985) with A = 0 has been used to perform
the loading and unloading experiment. The total growth law for the
equilibrium stress of Cernocky and Krempl (1979), which results in a unique
equilibrium curve for loading and unloading, forms the basis for Fig. lb. It is
seen that the loading and initial unloading portion are equal but much more
strain is recovered in Fig. lb at point B compared to Fig. la. For a long
time at zero stress all strain will be recovered in Fig. lb but only a small
strain reduction will be modeled in Fig. la. Equilibrium will be reached when
the equilibrium stress g intersects the strain axis which would at a strain
greater than 3% for Fig la but zero strain in the case of Fig. lb. This
strain constitutes the permanent set or plastic strain. It is defined as the
strain which remains in equilibrium at zero stress. The strain recovered at
zero stress is usually referred to as the anelastic strain which is found to be
small in experiments and this fact is reproduced by VBO with an incremental
growth law for the equilibrium stress. Kinematics does not play a significant
role in these definitions. The material model used to compute the results of
Fig. lb is a nonlinear viscoelastic solid. Its behavior may not be different
from that of a viscoplastic solid while under load (compare the stress-strain
curves in Figs, la and lb) but significant differences exist when unloading and
creep at zero stress (recovery) are being modeled.

Application to the modeling of high strain rate behavior

Most of the applications of VBO are in the region of small strain rates, see
Table 1. However, there is no reason why the theory could not be applied to
dynamic loading. Cernocky and Krempl (1979} have shown that the response
of the deformation theory of VBO is bracketed by the elastic response for
infinitely fast loading and by the equilibrium stress for infinitely slow loading.
These properties carry over to the incremental theory of VBO.

The pressure-shear impact experiments reported by Klopp, Clifton and Shawki

il985) is used to apply VBO. Their Fig. 5 shows a significant increase in

ow stress at 15% strain as the strain rate exceeds 105 1/s.

To show the capability of VBO, a simple version with A = 0 is adopted.

The shear stress is r and 7 denotes the engineering shear strain. Then
 277

7 = f1 + 7 in = r/G + 1—=^s (8)

G k[r]

gs = m*t - 16s -41WH - GOWA. (9)

U = Gt7 (10)
where k[r] and ifiT] are the positive viscosity and shape functions, respectively,
G is the shear modulus and Gt denotes the slope of the shear stress — shear
strain diagram at the maximum strain of interest, T = \r — g s | and
subscript s denotes the shear component. For constant positive strain rate
loading and large times, (8) — (10) admit the following asymptotic solutions
designated by { }
{r - gs} = (G - Gt)7k[{r - gs}] (11)
{gs - fs} = A s /(1 - G t /G). (12)
It can be seen from (11) that the asymptotic overs tress {r - g s } is non-
linearly related to the shear strain rate 7 via the viscosity function k[r]. If
k[r] becomes constant for T > r t h, where Tth is some value, the asymptotic
overstress will be linearly increasing with an increase in the shear strain rate.
For modeling of rate insensitive materials on the other hand, {r — g s } should.
change very little with rate and this requires that the function k has to
deacrease rapidly with increasing overstress. The overstress represents the
rate-dependent contribution to the stress, the rate independent contribution
being given by A s in (12). [Since usually Gt/G < < 1, the correction factor
in (12) is insignificant.)

In conformity with slow strain rate data, see Krempl and Kallianpur (1984),
no strain rate hardening is modeled. Such hardening has been observed in
dynamic tests on copper, Follansbee (1986). (The asymptotic solutions are
obtained irrespective of the initial conditions; whenever a constant strain rate
is acting long enough, they will be attained.) A possibility exists to model
strain rate hardening through an appropriately formulated growth law for A.
It may not be of the same format as indicated in (7).

For the modeling of the pressure—shear experiments on Polycrystalline

Aluminum reported by Klopp et al. (1985), the material constants listed in
Table 2 were used. Integration of (8) - (10) for various strain rates assuming
homogeneous strain controlled motions yields the stress—strain shown in Fig.
2a, taken from Choi (1990). The flow stress at 15% strain is then plotted vs
strain rate and compared with the experimental data of Klopp et al (1985) in
Fig. 2b. It should be noted that this was accomplished with one viscosity
function which becomes constant for Tth > 100 MPa, see Table 2. Details of
the development can be found in Choi (1990).

CONCLUSION
A brief overview of the status of the development of the viscoplasticity theory
based on overstress is given. This theory is of the "unified" type and
considers all inelastic deformation as rate dependent. Whereas most of the
applications to date have been in quasi-static application such as cyclic
hardening and ratchetting, the theory was also capable of simulating
pressure-shear, very high strain rate experiments. The theory assumes that
278

the observed increase in flow stress with strain rate is viscous in nature and
does not at present include strain rate hardening.

ACKNOWLEDGEMENT

This research was supported by the Department of Energy under Grant

DE-FG02-86ER13566 and by DARPA/ONR under Contract N00014-86-k0770
with Rensselaer Polytechnic Institute.

REFERENCES
Cernocky, E.P. and E. Krempl (1979). International Journal of Non—Linear
Mechanics. 14, 183-203.
Cernocky, E.P. and E. Krempl (1980). International Journal of Solids and
Structures. 16, 723-741.
Choi, S.H. (1990). Doctoral dissertation, Department of Mechanical
Engineering, Aeronautical Engineering and Mechanics, Rensselaer Polytechnic
Institute, Troy, NY.
Choi, S.H. and E. Krempl (1989). European Journal of Mechanics. A/Solids,
8, 219-233.
Follansbee, P.S. (1986). In: Metallurgical Applications of Shock—Wave and
High—Strain— Rate Phenomena (L.E. Murr, K.P. Staudhammer and M.A.
Meyers, eds.), pp. 451-479, Marcel Dekker, Inc., New York.
Hong, B.Z. (1989). Doctoral dissertation, Department of Mechanical
Engineering, Aeronautical Engineering and Mechanics, Rensselaer Polytechnic
Institute, Troy, NY.
Klopp, R.W., R.J. Clifton and T.G. Shawki (1985). Mechanics of Materials.
4, 375-385.
Krempl, E. (1987). Acta Mechanica. 69, 25-42.
Krempl, E. and S.H. Choi (1990). RPI Report MML 90-4, April 1990,
Mechanics of Materials Laboratory, Rensselaer Polytechnic Institute, Troy,
NY.
Krempl, E. and B.Z. Hong (1989). Composites Science and Technology. 35,
53-74.
Krempl, E. and V.V. Kallianpur (1984). Journal of the Mechanics and
Physics of Solids. 32, 301-314.
Krempl, E. and H. Lu (1984). Transactions of the American Society of
Mechanical Engineers. Journal of Engineering Materials and Technology, 106,
376-382.
Krempl, E. and P.S. Majors (1990). RPI Report MML 90-5, September 1990,
Mechanics of Materials Laboratory, Rensselaer Polytechnic Institute, Troy,
NY. To appear Proc. IUTAM Colloquium "Creep in Structures IV",
Krakow, Poland, September 1990.
Krempl, E., J.J. McMahon and D. Yao (1986). Mechanics of MaterialsT 5,
35^48.
Krempl, E. and M.B. Ruggles (1990). Journal of Mechanics and Physics of
Solids. 38, 587-597.
Krempl, E. and D. Yao (1987). In: Low Cycle Fatigue and Elasto-Plastic
Behavior of Materials (K.-T. Rie, Ed.), pp. 137-148, Elsevier Applied
Science Publishers.
Krempl, E. and N.-M. Yeh (1990). To appear in Proceedings IUTAM
Symposium on Inelastic Deformation of Composite Materials. Rensselaer
Polytechnic Institute, Troy, NY.
Lee, K.-D. and E. Krempl (1990). ASTM STP 1080, 40-55.
Lee, K.—D. and E. Krempl (1991a). To appear in International Journal of
Solids and Structures.
Lee, K.—D. and E. Krempl (1991b). To appear in European Journal of
 279
MechanicsT A/Solids.
Miller, A. K. (1987). Elsevier Applied Science Publishers Ltd, Essex, England.
Nishiguchi, I., T.-L. Sham and E. Krempi (1990a). Transactions of the
American Society of Mechanical Engineers. Journal of Applied Mechanics. 57,
548-552.
Nishiguchi, I., T.-L. Sham and E. Krempi (1990b). Transactions of the
American Society of Mechanical Engineers. Journal of Applied Mechanics. 57,
553-561.
Ohno, N. (1990). Applied Mechanics Reviews, 43, 283-295.
Ruggles, M.B. and E. Krempi (1990). Journal of Mechanics and Physics of
Solids, 35, 575-585. ~~
Siitgii, M. and E. Krempi (1990). International Journal of Plasticity. 6,
247-261.
Walker, K.P. (1981). NASA Report CR-165533.
Yao, D. and E. Krempi (1985). International Journal of Plasticity. 1,
259-274.

Table 1. Viscoplasticity theory based on orerstress (VBO) Table 2. Material constants for the Simulation of
pressure-shear experiments of Klopp et al. (1985)
DEVELOPMENTS
DEFORMATION THEORY <1980
G 27400.0 MPA
SMALL STRAIN
botropy, Cernoeky and Krempi (1979, 1980) G, 40.0 MPa
INCREMENTAL THEORY >1984
A, 14.0 MPa
SMALL STRAIN
Isotiopy, thermal and isothermal k(x] = lcexpflcexpHxI/k,)}
Cyclic Neutral, Yao and Krempi (198S), Krempi et al (1986)
Cyclic Hardening/Softening, Krempi and Yao (1987), Krempi and k, = 0.5-10-' s
Ruggles (1990), Ruggles and Krempi (1990),
Krempi and Choi (1990) k, = 0.4-10'
r of State (High Temperature Creep), Krempi and Majors
(1990, k, = 0.24-10' MPa
Application to Composites
Vanishing Fiber Diameter Model, Krempi and Yeh (1990)
*[x] = C.^C-Oexpf-Clxl)

Cyclic Neutral, Sutcu and Krempi (1990), Lee and Krempi Ci = 0.L10* MPa
(1991a, 1991b)
Cyclic Hardening/Softening (open) C, = 0.27-10* MPa
Recovery of State, Choi (1990)
Application to Ci = 0.5 MPa-'
Composite Laminates, Krempi and Hong (1989),
Lee and Krempi (1990)
Cubic Single Crystals, Choi and Krempi (1989)
FINITE STRAIN
Isotropy, isothermal
Cyclic Neutral, Nishiguchi et aL (1990a, 1990b)
Cyclic Hardening/Softening (open)
RecoTery of State (High Temperature Creep) (open)
Thermal (open)

I (open)
Deformation Induced (open)
280
100

Fig. la. Simulation of loading and unloading behavior using an

incremental growth law for the equilibrium stress. The
equilibrium stress unloads with the stress.

100

2 4
STRAIN, %
Fig. lb. Same as Fig. la except that the equilibrium stress is a
function of strain and is therefore unique (loading and
unloading follows the same curve).

120
7 = 2.0x10'
100 ~ / 7=1.0x10'
Cu

f 7=8^x10'
CO

I" 7=5.0x10^

x
CO 20
[r^ X
CO

' . . . . i . . . . i . .
LOO ( 5.00 10.0 15. 10 •» 10 -» 10 ' 10 • 10 ' 10 » 10 » 10 ' 10 '

SHEAR STRAIN (%) SHEAR STRAIN RATE (1/S)

Fig. 2a. Simulated stress-strain curves using eqs. (8) - (12) and Fig. 2b. Shear stress at 15% shear strain vs shear strain rate.
the material data of Table 2, from Choi (1900). Diamonds represent data from Fig. 5 of Klopp et al. (1985),
from Choi (1990).
WS2b3

DYNAMIC BEHAVIOR AND CONSTITUTIVE EQUATIONS OF MATERIALS SUBJECTED TO

IMPULSIVE LOADING

N. NAKAGAWA, T. IKEDA, Y. SEKIGUCHI, and T. YOSHIDA

Cluster 1, Faculty of Engineering, Hiroshima University

4.-1 Kagamiyama 1-chome, Higashi-Hiroshima 724. JAPAN

ABSTRACT

This paper deals with experimental analyses of dynamic properties of

SUS304-L, 2024. aluminum alloy, and S10C performed by the split Hopkinson
pressure bar method. Especially, dependence of dynamic properties of these
materials on strain rate is investigated and constitutive equations are
proposed.

KEYWORDS

Material testing; split Hopkinson pressure bar method; strain rate

dependency; constitutive equation; impulsive loading.

INTRODUCTION

Dynamic relationship between stress and strain of most materials is

influenced by strain rate, and the stress in a plastic region increases as
strain rate increases. Hence it is necessary to know both the dynamic
yielding stress of materials to design machines subjected to impulsive
loading and the dynamic relationship between stress and strain to work
materials plastically.

Impact tests have been performed to investigate dynamic properties of

materials (Nakagawa et_al., 1989) and some constitutive equations were
proposed (Malvern, 1951 » Symonds et al., 1964-> Nakagawa et_al., 1984-) •
However dynamic relationship between stress and strain of many materials has
not been fully investigated because of difficulties of experiments compared
with static experiments.

In this paper, dynamic properties of SUS304-L stainless steel, 2024. aluminum

alloy, and S10C steel are investigated by means of the split Hopkinson
pressure bar method (Lindholm, 1964.), and the influences of strain rates on
the dynamic properties are discussed, and further constitutive equations are
proposed.

281
282
Specimen
Incident Transmitted
Pressure Bar Pressure Bar
^ /

Fig. 1. Stress waves in pressure bars

EXPERIMENTAL ANALYSIS

Principle of Measurement

The stress waves in pressure bars are shown in Fig. 1. A specimen is

sandwiched between the incident pressure bar (i-bar) and the transmitted
pressure bar (t-bar). The one end of i-bar is impacted by a striker bar and
an impact wave propagates toward the specimen. The average strain £ g and
the average strain rate e in the specimen can be written as

where £. is the incident strain which propagates down the i-bar, e is the
reflected strain which is reflected at the surface between the i-bar and the
specimen, and1£+ is the transmitted strain which propagates into the t-bar;
CQ is an elastic wave velocity in the i- and t-bars and L is the length of a
specimen. The average stress in the specimen o can be obtained by

where A and A are the cross-sectional areas of the specimen and the i- and
t-bars, respectively, and E is dynamic Young's modulus of the i- and t-bars.
Hence the dynamic relationship between stress and strain can be obtained
from Eqs.O) and (3).

Test Apparatus and Specimen

The test apparatus consists of a striker bar, two pressure bars (i- and t-

Fig. 2. Experimental apparatus of split Hopkinson

pressure bar method
 283
bars), a strain measuring device, a striker-bar-velocity measuring device,
and a data analyzing system, as shown in Fig. 2. The i- and t-bars are 20 mm
in diameter, 1000 mm in length, and made of SNC22, while the striker bar is
20.7 mm in diameter and 200 mm in length, and made of SNC22. The specimens
are 19 mm in diameter and 8 mm in length.

A collision between the striker bar, accelerated by compressed air, and the
i-bar results in impulsive loading to a specimen. The velocity of the
striker bar is measured by the velocity measuring device composed of two
photoelectric sensors located at the end of a gun barrel.

Strain gauges are attached at the center of both i- and t-bars. Strain in
both bars are measured as voltage output from strain gauge bridges, stored
in transient memories, and sent to a microcomputer to obtain the
relationship between stress and strain under dynamic loading.

TEST RESULTS AND DISCUSSIONS

In this paper, compressive strain, strain rate, and stress are defined to be
positive for convenience.

To obtain dynamic Young's modulus E, of the i- and t-bars, an impact test

without sandwiching a specimen between two bars was performed. The obtained
value of C Q is 5085 m/s. Dynamic Young's modulus is then 203 GPa, calculated
by using the equation CQ= >/E/p, while static Young's modulus is 199 GPa.

Since the strain rate in the specimen differs among some materials at any
impact velocity (although the higher the velocity of the striker bar, the
higher the strain rate in the specimen), all test results in this paper are
discussed by use of average strain rates in the specimens.

Although so far an average strain rate is often used to discuss the

experimental results, its definition is not established, but depends on
investigators. In this paper, the average strain rate is defined by
averaging out the strain rate during the period of the yielding point and
the point at which stress begins to decrease. This definition enables to
compare experimental data among different materials.

Test Results of SUS304L Stainless Steel

The chemical compositions of SUS304-L is shown in Table 1.

Figures 3(a) to (c) show the relationships between strain rate-time, stress-
time, and stress-strain, respectively. The sampling time of measuring is 1 us
and stress-strain curves are obtained until stress begins to decrease.

At all tests, stress decreases gradually during the period from about 20 to
80 us. This period corresponds to the plastic regions of stress-strain
curves. Therefore the average value over this period is used to define the
average strain rate as shown in Fig. 3(a).

Table 1. Chemical compositions of SUS304L (weight %)

C Si Mn P S Cu Ni Cr Mo Al NQ 0,

0.012 0.57 1.030 0.028 0.003 0.230 10.38 18.^8 0.20 0.001 0.0^06 0.005
284
1200 600
cd

cd

u
-p
CO

100 100
Time ( y s) Time ( y s )
(a) Strain rate-time (b) Stress-time
600 i i i i
e=7.1xl02

400 \-
r ^^ ^ T e=5.0xl0 2 1
CQ

ra

U
w
IK\ V \ ~
£=2.7x10^
S t a t i c curve
J
200
=1 .1x10 2
/^

0.0 1.0 2.0 3.0 4.0 Strain rate (s~

Strain (%) Fig. 4.. Influence of average strain
(c) Stress-strain curves rate on over-stress
Fig. 3. Experimental results (SUS304X) (SUS304L)

No clear yielding point of SUS304.L was observed as it is known as one of the

dynamic properties of f.c.c. materials. As the average strain rates
increase, dynamic stress becomes higher than the static one. Dynamic stress-
strain curves in the plastic region are parallel to that of static region.
The difference between the dynamic stress and the static one is called over-
stress. The average over-stress of this material is proportional to a
logarithmic average-strain-rate as shown in Fig. 4-t where the straight line
in the figure is obtained by the least square method. The constitutive
equation of this material of average strain rates from 10 to 10-* s can be
expressed as
a(e,e) = f(e)-73+69-loge
U)
where f(e) indicates the static stress-strain relationship.

Test Results of 2024 Aluminum Alloy

The chemical compositions of 2024. aluminum alloy is shown in Table 2.

Table 2. Chemical compositions of 2024. aluminum alloy (weight %)

Cu Fe Si Mn Mg Zn Cr Zr+Ti

A.3 0.5 0.5 0.5 1.5 0.25 0.10 0.2

 285
500 1 1 1 1r™*™^"™^™"i

Static curve
-400 [•
a*
£&^*^
w
300 I s* - mC'
2
e=9 5x10 J
CO
e=4.7x10 2
\ 1"=1
CO

2 200

1/ ^
-p
co .5*10 2
100 H

0 I I I I » I
0.0 1.0
2.0 3.0 4.0 $.0
Strain (%)
Fig. 5. Stress-strain curves (2024 aluminum alloy)

It is found that the dynamic relationship between stress and strain of the
2024 aluminum alloy coincides with the static one under the average strain
rates from 140 to 880 s , as shown in Fig. 5«

Test Results of S10C Steel

Specimens of this material are 12 mm in diameter and 5 mm in length.

It is found that the upper yielding points of S10C which is classified into
b.c.c. material become clearer as the strain rates increase.

The relationships between strain rate-time, stress-time, and stress-strain

are shown in Figs. 6(a) to (c) for four kinds of strain rate, respectively.
Arrows in the Figs. 6(a) and (b) indicate the time of yielding points. When
the strain rate is low, the strain rate becomes maximum before the yielding
point and minimum at the yielding point. On the other hand, strain rate
increases after the yielding point when the strain rate becomes higher.
Dynamic stress-strain curves are parallel to the static one. The influence
of average strain rate on the over-stress is shown in Fig. 7. The
constitutive equation can be expressed as follows, under the average strain
rates of 10 2 to 10^ s .
<J(efe) = f(e)-60+76-loge (5)
where f(e) indicates the static stress-strain relationship.

CONCLUSIONS

1. The definition of the average strain rate proposed in this paper enables
to compare experimental results among different materials.
2. The dynamic stress-strain curves in the plastic region of SUS304L are
parallel to the static one under the strain rates from 10 to 10-* s ,
and the over-stress is proportional to the logarithmic strain-rate.
3. The dynamic stress-strain relationship of the 2024 aluminum alloy
coincides with the static one under the average strain-rate from 140 to
880 s"1.
4. The dynamic stress-strain curves in the plastic region of S10C steel are
parallel to the static one under the strain rates from 10 to 10-* s" ,
and the over-stress is also proportional to the logarithmic strain rate.
286
2600 800

-p

-P
CO

-400
100 100
Time ( u s ) Time ( u s )
(a) Strain rate-time (b) Stress-time
800 • ' I -" 1 r- » i i 1
250
3
E=2. 1x10

600 [ /\ ^ = 1 . 6x103 j
2
=7.2x10 ..- 0
u
co 400 V -p
E=*. 2x1 (A Static curve

200 >
o
£.0x103
0 i . i i 1 i ■ ■ ■ '
Strain rate (s )
0.0 5.0 10.0 15.0
Strain (%) Fig. 7. Influence of average strain
rate on over-stress
(c) Stress-strain curves
(S10C)
Fig. 6. Experimental results (S10C)

The yielding points of S10C become clearer as the average strain rates
increase.

REFERENCES

Lindholm, U. S. (1964.). Some Experiments with the Split Hopkinson Pressure

Bar. J. Mech. Solids, 12, 317-335.
Malvern, L. E. (1951). The Propagation of Longitudinal Waves of Plastic
Deformation in a Bar of Material Exhibiting a Strain Rate Effect. J. Appl.
Mech., Trans. ASME, 73, 203-208.
Nakagawa, K., K. Kishida, and S. Tanimura (1985). Constitutive Equations
of Materials Subjected to Rapid Deformation (in Japanese). Bull. The
Society of Materials Science, 384, 1115-1120.
Nakagawa, N., T. Ikeda, and T. Yoshida (1989). Measurement of Dynamic
Properties of Materials by using the Split Hopkinson Pressure Bar Method
(in Japanese). The third Symposium on Impact Problems of Materials, 17-20.
Symonds, P. S. and T. C. T. Ting (1964.). Longitudinal Impact on Viscoplastic
Rods — Approximate Methods and Comparisons. J. Appl. Mech., Trans. ASME,
31, 611-620.
WS2b4
ON THE CONSTITUTIVE EQUATIONS FOR NONPROPORTIONAL LOADING CONDITIONS

KOJI MBfURA1 and AKIO SHINDO:

Department of Mechanical Engineering, Faculty of Engineering

Kobe University, Nada, Kobe 657, Japan.

Department of Electro-Mechanical Engineering, Faculty of Engineering,

Osaka Electro-Communication University,
Neyagawa, Osaka 572, Japan.

ABSTRACT

The constitutive model with a modified anisotropic yield function and a

nonlinear kinematic hardening rule is proposed for the description of
inelastic behaviour of metallic materials under nonproportional loading.
The experimental verification by using bilinear plastic strain paths was
also carried out on S21C and A2017 aluminum alloy and the experimental
results were compared with the numerical simulation based on the proposed
model.

KEYWORDS

Constitutive equation; Anisotropic yield function; Nonproportional loading;

Strain history; Subsequent yield surface; Stress-strain relation;

INTRODUCTION

In recent years, so much attention has been given to inelastic behaviour of

materials under nonproportional loading that many constitutive models have
been proposed. For accurate prediction of inelastic response in
nonproportional loading, however, the change in the shape of subsequent
yield surfaces due to the deformation induced anisotropy as well as other
inelastic features should be taken into consideration in the constitutive
modeling. The earlier investigation in this field has been done by Baltov
and Sawczuk ( 1965 ) . Recently, Ishikawa and Sasaki ( 1988 ) have proposed
the quadratic yield function and applied their theory to the analysis of
cyclic plasticity. Furthermore, Imatani and Inoue ( 1989 ) can successfully
represent a rounded nose form in a subsequent yield surface by using the
extended Baltov-Sawczuk type plastic potential. This paper presents some
improvement in the representation of a subsequent yield surface and
inelastic stress - strain relation by using the modified anisotropic yield
function and the nonlinear kinematic hardening rules.

CONSTITUTIVE EQUATION

A brief summary of the mathematical structure of the proposed theory is

reproduced from the previous study (Shindo and Mimura,1989a).

287
288
ANISOTROPIC YIELD FUNCTION
Let us assume that the modified anisotropic yield function f with the
backstress and the isotropic hardening variable O is given by

f 3 N. .ln(S. .-a\ . X S ^ - a ' ) - a 2

= (1)
2 ijkl IJ ij kl kl' y
where, Nijkl is the anisotropic moduli tensor of forth order, Sij and <xfij
is the deviatoric stress and deviatoric backstress, respectively. If we can
assume that materials are initially von Mises body, the tensor Nijkl is
decomposed as follows
N.ljkl v 6.,6.x
M 1 = l/2(
ll jk + 6.lk
x6..)
jr - 1/3(6.
v
ij.6. ,) + M 1ljkl
kl'
2
. .. . + Mljkl
. .. n v (2)

Where, 6ij denotes Kronecker's delta. M 1 ijkl and M 2 ijkl are the anisotropic
parts of Nijkl due to the deformation induced anisotropy. Now, we define
the first anisotropic part M 1 ijkl as

(S
.. _ - -32 H P
M*.ijkl il" a , i1
—iJ X
)e
J klkl
+e
i1 (S
^ kl"kl
a,
kl
—
)
+ xQ s ij
£.s.£.
-
2 y kl . ] (3)

where, P and Q are the material constants. £ij is a second order symmetric
tensor which governs the development of the rounded nose form in the
subsequent yield surfaces. Its evolutional equation is given by

C. . = D ( C -4- E. . - C. . ) e p (4)

In equation (4), e^ denotes the Mises type equivalent inelastic strain

rate, Eij is the normalized inelastic strain rate, respectively. Namely,

E.. - e p . . / E p , Ep = ( - f e p . i p . . ) 1 / 2 (5)
ij ij 3 ij ij

M 2 ijkl is the tensor function to prescribe an elliptical form of a

subsequent yield surface. Perhaps it may be related to the long range
internal stress field due to the current deformation structure. Thus, it is
defined as
M 2 .. n - -4- C, p. ... (6)
v y
ijkl 2 I ijkl
where, C T is a constant. The forth order tensor pijkl in equation(6) is the
internal state variable which represents the development of the current
deformation structure. We define the evolutional equation of pijkl as

p. .. - = DT( 4 - E- • 4 " E. i - P- -1,1 ) £P (7)

K v
ijkl 1 3 ij 3 kl ijkl '
where, D T is a material constant. The equation (7) is the extended
representation of Nijkl=Aoepijepkl in Baltov and Sawczuk's original theory.
However, it has the dependence on the plastic strain path and also has the
fading memory.
 289

KINEMATIC AND ISOTROPIC HARDENING RULES

When bilinear loading path is given to a specimen ( it is the special case

of nonproportional loading. The subsequent loading direction is not
coincide with the previous one ) , increase of flow stresses due to cross
hardening is often observed. The reason of this may be that the
deformation structure formed during the previous deformation acts as a
certain resistance to dislocation movement in the new loading direction.
The general description of such effect under multiaxial loading condition
requires the reasonable definition of non-proportionality of the current
deformation process. From equation (7), we define it as follows
2 E 2 h
<t> = [(
v P - -|-
3 -IJ -P. .^P.,
ljkl klmn Emn ) / p ]
(8)
and

P = ( P ijkl Pijkl > 1 / 2

where, h is a material constant. The function <|> becomes zero if an applied
loading path is proportional. In other case, it takes a certain positive
value. By using the nonproportional function <|>, the modified evolutional
equations of nonlinear kinematic hardening rule ( Chaboche and Rousselier,
1983) are given by
m
' . . = Z .00 a ,v *'.. (9)
iJ k=1 xj
and
(k) (k) (k)
• no 2 (k) -D
a'}*'- ( 1 + x a <t. ) Da ( Ca O Q -§- E - <*'^ ; ) e P (10)

(k) (k) (k)

where, xa, Ca and Da are the material constants, o is the initial yield
radius of materials and Eij denotes normalized inelastic strain rate
defined_in equation(5). Similar way, we also define the isotropic hardening
radius a . We assume it as a function of effective plastic work ;

w = ( 0 i j - a ±j ) eP±j (11)
and temporary hardening parameter T ;

f = Dr ( Cr * - r ) lp (12)
By using W and T, o is written as
W
O =0 [ 1 + R ( --- ) n + T ] (13)
y
J o a
o

where, R and n are material constants. The second term in equation (13) is
the power formula of effective plastic work and the third term T denotes
the temporary hardening ( or softening ) due to the cross effect.

VERIFICATION AND DISCUSSION

To investigate the validity of the proposed constitutive model, the
290

Table 1 Chemical compositions of S21C and A2017

Material 0 St Mn P S Cu Ni Or Fe
S21C 0.21 0.20 0.45 0.017 0.024 0.01 0.01 0.03 Rest.
( WT* )
Material SI Fe Ou Mn Mg Or Zn TI Al
A20 17 0.38 0.36 4.2 0.48 0.40 0.02 0.05 0.02 Rest.
( WTX )

Table 2 Material constants used in calculation

S21C A2017 S21C A2017 S 2 1 0 A2017

P 1.44 0.0 Q 1.2 0.7
R 0.0 0.4 n 0.6 ForS21C.Ci»Dl»t8>ire
h 1.0 1.0 Go 160MPa 52MPa defined in the range of
Ci 1.85 0.6 Di 30.0 60.0 6>£ 0.014
Cr 0.55 Dr 55.0
Cg 1.0 1.0 Dg 800.0 600.0
Cft» 0.45 2.3 Dkn 60.0 30.0 0.4 1.0
Ck2) 0.72 0.5 DP 60.0 250.0 0.4 1.0
0.72 0.5 Dj?> 1000.0 1000.0 xk9) 0.8 1.0

experimental verification by means of bilinear plastic strain paths was

carried out. The materials employed in the experiments were S21C and A2017
aluminum alloy whose chemical compositions are shown in Table 1. The axial
and torsional combined loading was imposed on the thin walled tubular
specimen which has the gauge length of 90mm, the inner diameter of 20mm and
the outer diameter of 27mm, respectively. First, the tubes were subjected
to a certain amount of plastic strain by tension or torsion, then, the
subsequent plastic strain paths were bent to various directions within e p z-
yP//3 plain. The value of prestraining was YP/v/3 = 0.017 for S21C and £Pz =
0.015 for A2017. During the subsequent loading, subsequent yield surfaces
were measured at several points by using the small offset strain definition
for yielding ( 80ym/m for S21C, 200ym/m for A2017 ). Further details of the
experiments are discussed in the study ( Shindo and Mimura,1989b ).

Figures 1.(a),(b),(c) and figures 2.(a),(b),(c) show the subsequent yield

surfaces of S21C and A2017 obtained from the experiments. epsub and O in
the figures denote subsequent equivalent plastic strain measured pfrom
the preloading points and the value of stress at the preloading points,
respectively. To evaluate the validity of proposed model, the calculated
yield surfaces are superimposed on the experimental results. The material
constants and parameters used in the calculation are listed in Table 2.
 291

D
ANGLE OP BENT PLASTIC ANGLE OP BENT PLASTIC
STRAIN PATH 0-Q.Qifg U STRAIN PATH * - 1 8 0 t « « .

1.0 -

5^
u J
AT\ o\ X
p 2
\u t«
r •

-1.0 Va \ or
f / 4
j
\p AVD
—

( a ) ( b

ANGLE OF BENT PLASTIC

— CALCULATED SURFACE Oam STRAIN PATH 0-754«t.
STRESS PATH A 0.0
— :CALCULATED O 0.0005
¥- rBXPERIMBNTAL
• 0.0020

SURFACE a t PRELOADING
□ 0.0100
POINT

Fig. 1 Subsequent yield surfaces

of S21C

( C )

In the case of proportional loading i .e. the angle of bent plastic strain
path 6 is 0 or 180 deg., the ca lculated results well express the
development of rounded nose form of the experimental surfaces. In this
case, both experimental and calculated yield surfaces are symmetric to the
loading axis. While, in the case of 6 is near 90 deg. — Actually 6 = 75
and 101 deg. it is a typical nonpropor tional loading case — , experimental
surfaces show the remarkable rotation and distortion and sometimes their
shapes are not symmetric. Although the above situation, simulated surfaces
show fairly good approximation for the experimental results except for the
slight differences at small strain.

CONCLUSION

The mddified constitutive model for nonproportional loading is presented.

To, estimate the validity of the proposed model, the experimental
verification by means of bilinear plastic strain paths was performed.
Numerical simulations based on the proposed model show fairly good
approximation for the experimental results.
292

ANGLE OF BOrr PLASTIC

STRAIN PATH 0-18O4lfl.

CALCULATED SURFACE
STRESS PATH
:CALCULATED
rEXPERHMfTAL

SURFACE a t PRELOADING
roim-

Fig. 2 Subsequent yield

surfaces of A2017

( c )

REFERENCES

Baltov,A. and Sawczuk,A.(1965) A Rule of Anisotropic Hardening, Acta Mech.

1,81-92
Ishikawa.H. and Sasaki,K.(1988) Yield Surfaces of SUS304 under Cyclic
loading, Trans, of ASME, 110,364-371
Imatani,S. and Inoue,T.(1989) Effects of Induced Anisotropy on the
Plastic Behavior of Metals. In: Advances in Plasticity 1989, 227-230
Shindo,A. and Mimura,K.(1989a) On the Formulation of a Constitutive
Equation Using a Modified 4th Rank Anisotropic Moduli Tensor.
In: Advances in Plasticity 1989,107-110
Shindo,A. and Mimura,K.(1989b) The Experimental Investigation into the
Strain Rate and History Dependency of Metals. In: Proc. of 32nd Japan
Congress on Mat. Res. 45-51
Chaboche,J.L. and Rousselier,G.(1983) On the Plastic and Viscoplastic
Constitutive Equations - Parti and II, Trans, of ASME,105,153-164
WS2C1

MICROSCOPIC ASPECTS OF STRAIN RATE DEPENDENCY OF DYNAMIC FLOW STRESS

IN METALLIC MATERIALS

J. SHIOIRI, K. SAKINO, H. IMAIZUMI and T. MURAMATSU

College of Engineering, Hosei University

Koganei, Tokyo 184., Japan

ABSTRACT

In order to evaluate the effect of the strain rate history upon the dynamic
flow stress, two experiments (a) the test in which the strain rate is sud-
denly decreased and (b) the measurement of the ultrasonic attenuation under
dynamic plastic deformation are conducted for high purity polycrystalline
aluminium. The results indicate that the instantaneous strain rate plays
more important role than the strain rate history. Emphasis is put on the
microscopic aspects of the deformation at very high strain rates where the
steep increase in the strain rate sensitivity is observed.

KEYWORDS

Dynamic plasticity; flow stress; transition in rate sensitivity; dislocation;

rate change test; ultrasonic attenuation.

INTRODUCTION

A vast number of works have been done these decades for the macroscopic
behaviour and microscopic mechanism of the dynamic plastic deformation in
metallic materials. However, as pointed out in many review papers (Campbell,
1973, Lindholm, 1974, Harding, 1988, 1989), one of the problems not yet set-
tled is the mechanism of the steep increase in the strain rate sensitivity
(do/d loge: a is the flow stress and z is the strain rate) which appears at
strain rates above about 5000 /sec. At lower strain rates the flow stress o
increases linearly with increase in loge, while at higher strain rates o in-
creases linearly with increase in e. For this transition an explanation very
attractive for the dislocation theory was given by many authors; that is, the
above transition in the strain rate sensitivity is due to the transition in
the dominant rate controlling mechanism of the dislocation motion from the
thermally activated cutting of the point obstacles to the viscous phonon
drag. On the other hand, various questions have been also raised as to the
above explanation. Recently, Follansbee et al. (1985) pointed out that the
strain rate dependency of the flow stress is basically determined by the
internal structure reflecting the strain rate history and the contribution

293
294
of the instantaneous strain rate is small. They measured the "threshold
stress" (quasi-static yield stress at 0 K) after imposing a certain amount
of dynamic pre-deformation and showed that the dynamic flow stress can be
closely correlated with the threshold stress after the pre-deformation at
the same dynamic strain rate. Further, Follansbee and Kocks (1988) showed
that the dynamic flow stress at the state having the same threshold stress
depends upon the strain rate very little and the steep increase in the strain
rate sensitivity at very high strain rates is not observed.

At this stage of the problem, it seems important to confirm the effect of the
strain rate history upon the dynamic flow stress at very high strain rates by
using different methods. In the present paper, two experimental works done
by the present authors' group for this purpose are described briefly together
with discussion. The experimental works are (a) the decremental strain rate
test at very high strain rates and (b) the ultrasonic attenuation measurement
under deformation at very high strain rates. Both were conducted for high
purity polycrystalline aluminium.

DECREMENTAL STRAIN RATE TEST

In order to evaluate the effect of the strain rate history, many works have
been done for various materials using the various test techniques in which
the strain rate is suddenly changed. Since those works have been reviewed in
many papers (Campbell,1973, Duffy, 1979,1983, Harding, 1988, 1989) citation
of each work is omitted here. Usually, the strain rate changes in this type
of experiments were made from quasi-static to dynamic, dynamic to quasi-
static and dynamic to dynamic, and the deformation modes were mostly torsion
or compression since the dynamic loading were imposed with a torsional or
compressional split Hopkinson bar system. Further, in those tests, the
strain rates have been limited below about 2000 /sec. However, in order to
clarify the role of the strain rate history in the steep rise of the strain
rate sensitivity, the strain rate change test at very high strain rates,
higher than at least 10000 /sec, is required. Since it is difficult to
attain such a high strain rate by using the torsional apparatus, the present
authors' group tried at first a test by a compressional split Hopkinson bar
system with a stepped impact bar. However, owing to the dispersion of the
elastic wave in the incident and transmitter bars, sufficient time resolution
capability was not attained. Although the effect of the dispersion in the
transmitter bar can be corrected mathematically by using the dispersion
characteristics of the bar, but the dispersion in the incident bar make it
impossible to realise a sharp decrease in the strain rate, which is necessary
to separate the flow stress change due to the change in the instantaneous
strain rate from the flow stress change due to the change in the structural
state which occurs somewhat gradually in the form of the "fade-out of the
memory". Recently Sakino, one of the present authors, has devised a new
apparatus shown in Fig. 1. In this apparatus, the projectile hits the
specimen directly and then the velocity of the specimen side end of the
projectile is decreased sharply by the collision with the decelerator. The
flow stress of the specimen is measured with the strain gauges attached to
the pressure bar and recorded in the high speed digital memory. The data
are then transmitted to the computer and finally plotted in the form of the
true flow stress vs strain using the digital X-Y plotter.

Measurements were conducted for fully annealed 5N purity polycrystalline

aluminium at strain rates ranging up to 20000 /sec. The size of the speci-
men was 2 mm both in the diameter and length. The diameter of the pressure
bar was U mm, and in the used combination of the projectile and decelerator
 295

PROJECTILE DECELERATOR STRAIN

GAUGE

DIGITAL X-Y PLOTTER

Fig. 1. Devised apparatus for decremental strain rate test.

the drop of the strain rate was 4-1 %• An example of the detailed stress-
strain relationship around the strain rate reduction point is shown in
Fig. 2. In this figure the constant strain rate curves at the strain rates
before and after the strain rate reduction are also plotted. The constant
strain rate curves are drawn by an empirical formula determined from the
many constant strain rate tests at different strain rates. The drop of the
flow stress by the strain rate reduction is a little small compared with the
difference in the flow stress between the constant strain rate curves.
Further, the flow stress falls a little gradually compared with the steepness
of the strain rate reduction expected in the devised apparatus. This is not
likely due to the fade-out time of the memory of the strain rate history but
likely due to the elastic wave dispersion in the pressure bar for the stress
measurement. In fact, by assuming a stepwise drop of the flow stress and
taking account of the dispersion effect, computer simulation predicts the
broken curve shown in Fig. 2, which shows a fairly good agreement with the
experimental response of the flow stress. The dispersion characteristic used
in the simulation is experimental one obtained by impacting upon the end of
the pressure bar with a bar of the same material and diameter. This experi-
mental dispersion characteristic is very similar to the theoretical one given
in terms of Airy's integral except for a little smaller amplitude in the
oscillatory part.
296

STRAIN RATE REDUCTION

21338 TO 12589 /SEC

ASSUMED STEPWISE DROP

OF FLOW STRESS
COMPUTER SIMULATION __,„.,
90 EFFECT OF ELASTIC WAVE DISPERSION
IS TAKEN INTO ACCOUNT

80 .2
STRAIN

Fig. 2. An example of flow stress response to a sudden

reduction in strain rate. For comparison, re-
sponse predicted by computer simulation taking
account of wave dispersion in the pressure bar
for an assumed stepwise drop of "flow stress is
also shown.

STRAIN RATE BEFORE REDUCTION (sec-1)

Fig. 3. Ratio of observed flow stress fall to flow stress

difference between two constant strain rate
deformations respectively at strain rates before
and after strain rate reduction.
 297
Figure 3 shows the ratio of the observed flow stress fall to the flow stress
difference between the constant strain rate deformations at the strain rates
before and after the strain rate reduction. The ratio is between about 0.75
and 0.80. Discussion on the above experimental results is given later.

ULTRASONIC ATTENUATION UNDER DYNAMIC PLASTIC DEFORMATION

In order to obtain information on the behaviour of dislocations at high

strain rates, Shioiri and Satoh (1984-,1985) conducted the measurement of the
attenuation of the ultrasonic wave superimposed upon the dynamic plastic
deformation. As was given in the theoretical analysis presented in the above
works, the ultrasonic attenuation due to the moving dislocations can be
related to the derivative of the strain rate dependency of the flow stress
in the following way:

(Ax)m f = 2fiG (d£/do) Q=ao (1)

where (AA)m is the attenuation due to the moving dislocations, f the ultra-
sonic frequency, ft the orientation factor, G the shear modulus, subscript o
means the state of the basal dynamic deformation upon which the ultrasonic
wave is superimposed and accordingly oo i s the fl° w stress of the basal
deformation. Equation (1) indicates that the attenuation measurement of the
ultrasonic wave superimposed upon the basal dynamic deformation is a kind of
strain rate change test by a periodic perturbation of the strain rate with
a very high frequency and with a very small amplitude. Equation (1) can be
also written as

(da/de)o=a0 = 2ftG/[(AA)mf] . (2)

In the derivation of Eq.(l), since the stress and strain rate amplitudes of
the ultrasonic wave is very small, the ultrasonic components of the stress
and strain rate are regarded as the small perturbation superimposed upon the
basal dynamic deformation, and the linearised perturbation method is used.
The perturbation flow stress can be given in the following linear form:

(Aa) eiwt = a (A£) ei^t + b }(Ae) eiU)t dt (3)

where (Aa) and (Ae) are the amplitudes of the perturbation stress and strain
rate, respectively, and a and b are constants. The first term in the right
hand side of Eq.(3) is the term due to the instantaneous strain rate and the
second term represents the effect of the strain rate history. Since
jeiu)t dt = e^VCiui), the second term has a phase difference TT/2 between the
strain rate and further, at the ultrasonic frequency (£.10 MHz), its amplitude
should be very small compared with the amDlitude of the first term. There-
fore, the left hand side of Eq.(2), (da/de) a=a represents approximately the
dependency of the flow stress upon the instantSneous strain rate, and it
should be possible to evaluate the role of the strain rate history by
comparing the strain rate sensitivity obtained from the direct measurements
of the flow stress-with the rate sensitivity determined by using Eq.(2) from
the ultrasonic attenuation data.

In the previous works by Shioiri and Satoh cited above, the ultrasonic atten-
uation measurements under dynamic deformation were conducted at strain rates
up to 7000 /sec. The upper limit of the strain rate was limited mainly by
the time resolution capability of the ultrasonic apparatus. For the higher
strain rate range, discussion was made by an extrapolation based upon a
298

~ 3
1 5N ALUIMINIUM ^ • m _ • |
———-—^— ^
>-
o
#
P •
a
ex. ' • PRESENT WORK: 30 MHz

O /

L^
#
1 / ° PREVIOUS WOtfK: 10 MHz

< 0 -J I I I I 1, L 1 1 1
5000 10000
STRAIN RATE (sec-1)

Fig. 4.. Ultrasonic attenuation due to moving dislocations

against strain rate in the form of (AX)mxf vs e.
(AX)m is attenuation due to moving dislocations,
f ultrasonic frequency in MHz, e strain rate.

simple kinetic model of the behaviour of dislocations. However, for the

above mentioned purpose, especially to clarify the role of the strain rate
history in the steep increase in the strain rate sensitivity of the flow
stress the ultrasonic measurements at strain rates at least up to 10000 /sec
are required. For this purpose, recently a new ultrasonic apparatus has been
devised. The principle of the apparatus is the same as the apparatus used
in the previous works but a heterodyne circuit is adopted. It has a high
time resolution capability (0.7 jjsec) and a wide frequency range (5 to 200
MHz). Further, it has a pulse-controlled gain controller to measure accu-
rately the large and rapid change in the attenuation during the deformation
at very high strain rates. For measurements at very high strain rates, very
small specimens (3x3x4- mm), very small transducers (1.4x1.4. mm) and a higher
ultrasonic frequency (30 MHz) were used. The details of the apparatus and
experimental technique will be reported elsewhere.

Measurements were made again for fully annealed 5N purity polycrystalline

aluminium at strain rates up to 12000 /sec. The experimental procedure and
the method of separating the attenuation due to the moving dislocations from
the total attenuation are the same as in the cited previous works. The
results of the measurements are shown in Fig. 4- together with the results of
the previous works. A good agreement is seen between present and previous
results.

The strain rate sensitivity of the flow stress (do/d loge) calculated from
the ultrasonic data by using Eq.(2) are shown in Fig. 5 together with the
strain rate sensitivity obtained from the direct flow stress measurements.
 299

15 r
Q.
LL.
O z:
N—/

>- BASED UPON FLOW STRESS

1—
1 —1
MEASUREMENT
> »U
H H CT 10
t —1 o
1—
00
■o
z
00 ^«^
LU
D
TJ
LU
h-
< 00
G£ oo
LU
Z OH
i—i 1—
< 00
QZ
00 O BASED UPON ULTRASONIC
ATTENUATION MEASUREMENT

1000 5000 10000 20000

STRAIN RATE (sec-1)
Fig. 5. Strain rate sensitivities of flow stress calculated
from ultrasonic attenuation data and obtained by
direct flow stress measurements. Strain £=0.10.

The former is roughly 0.70 of the latter, and both curves rise in a similar
way with increase in the strain rate. Discussion on this result will be
given in the following.

DISCUSSION AND CONCLUDING REMARKS

As was pointed out as to Fig. 2, the stress drop observed in the decremental
strain rate test is not likely of structural origin reflecting the strain
rate history but likely due to the reduction in the instantaneous strain
rate. Accordingly, Fig. 3 indicates that, at very high strain rates where
the steep increase in the strain rate sensitivity is observed, in the flow
stress difference between at two different strain rates about 75 to 80 % is
the contribution of the difference in instantaneous strain rate and the
remaining rather small part is due to the effect of the strain rate history.

A similar conclusion can be obtained also from the ultrasonic attenuation

measurements. As was pointed out as to Eq.(3), the strain rate sensitivity
(da/d loge) calculated from the ultrasonic attenuation data by using Eq.(2)
represents the component due to the effect of the instantaneous strain rate.
As is seen in Fig. 5, the strain rate sensitivity calculated from the ultra-
sonic data is about 70 % of the rate sensitivity obtained from the direct
flow stress measurements.

The above discussion indicates that, in the strain rate dependency, the
instantaneous strain rate plays a more important role than the strain rate
300
history. This means that the instantaneous velocity of dislocations plays a
more important role than the dislocation structure formed during the defor-
mation depending upon the strain rate history. This conclusion drawn from
the results of the experiments at very high strain rates seems to have an
important meaning as to the cause of the steep rise of the strain rate
sensitivity in the very high strain rate range. However, it must be noted
that the above results have been obtained for aluminium. The decremental
strain rate test and the ultrasonic measurement for fee metals, especially
having different stacking fault energy, and for some of bec metals are in
preparation.

ACKNOWLEDGEMENT

The authors are grateful to The Mitsubishi Foundation for their financial
support to this work.

REFERENCES

Campbell, J.D. (1973). Dynamic plasticity: macroscopic and microscopic

aspects. Mat. Sci. Eng., 12, 3-21.
Duffy, J. (1979). Testing techniques and material behaviour at high rates of
strain. In: Mechanical Properties at High Rates of Strain (J. Harding,
Ed.), Con. Ser. 47, pp. 1-15. Inst. Phys., Bristol.
Duffy, J. (1983). Strain rate history effects and dislocation structure at
high strain rates. In: Materials Behavior under High Stress and Ultrahigh
Loading Rates (J. Mescall and V. Weiss, Eds.), pp. 21-37. Plenum
Publishing Corp., New York.
Follansbee, P.S., U.F. Kocks and G. Regazzoni (1985). The mechanical
threshold of dynamically deformed copper and NITRONIC 4-0. J. Phys., 4-6,
C5 25-35.
Follansbee, P.S. and U.F. Kocks (1988). A constitutive description of the
deformation of copper based on the use of the mechanical threshold stress
as an internal state variable. Acta Metall., 36, 81-93.
Harding, J. (1988). Material behaviour at high rates of strain. In: Impact
Loading and Dynamic Behaviour of Materials (C.Y. Chiem, H.-D. Kunze and
L.W. Meyer, Eds.), Vol. 1, pp. 23-4-2., DGM Informationsgesellschaft mbH,
Oberursel.
Harding, J. (1989). The development of constitutive relationships for
material behaviour at high rates of strain. In: Mechanical Properties at
High Rates of Strain (J. Harding, Ed.), Conf. Ser. 102, pp. 189-203.
Inst. Phys., Bristol.
Lindholm, U.S. (1974.). Review of dynamic testing techniques and material
behaviour. In: Mechanical Properties at High Rates of Strain (J. Harding,
Ed.). Conf. Ser. 21, pp. 3-21. Inst. Phys., Bristol.
Shioiri, J. and K. Satoh (1984.) • An ultrasonic study of the behaviour of
dislocations at very high rates of strain. In: Mechanical Properties at
High Rates of Strain (J. Harding, Ed.). Conf. Ser. 70, pp. 89-96. Inst.
Phys., Bristol.
Shioiri, J. and K. Satoh (1985). An ultrasonic study of the rate controlling
mechanism of dislocation motion at high rates of strain. J. Phys., 4.6, C5
3-10.
WS2c2

THE STRENGTH OF HARD STEELS AT HIGH STRAIN RATES

A. Chatani, A. Hojo and H. Tachiya

Department of Mechanical Systems Engineering,

Faculty of Technology , Kanazawa University,
Kodatsuno 2-40-20, Kanazawa, Japan

ABSTRACT

In order to know the dynamic strength of hard steels, a dynamic three-point

bending method based on Hopkinson pressure bar technique using long bars was
proposed. The stress applied to a specimen was determined by means of the
relation between bending moment and strain. The stress-strain relation of
hard steels with the Vickers hardness 3*^7.9 GPa at various strain rates up
to the order of 10^ 1/s was obtained. As a result, strain rate dependence
of the yield strength of hard steels having martensitic structure was found.

KEYWORDS

Dynamic stress-strain relation; three-point bending; strain rate dependence;

hard steels; high hardness; yield strength; impact test

INTRODUCTION

Many studies on the strength of various materials under dynamic loading have
been done. The strain rate dependence, however, of the strength of high
strength steels with Vickers hardness above about 5 GPa has been little re-
ported except for a few cases (Harding,1987). Therefore, from the practical
viewpoint of strength design data, the dynamic yield or fracture strength of
steels hardened by quenching was given in the present paper. And also
three-point bending test based on the Hopkinson pressure bar technique using
long bars was employed, since it could be performed without so many diffi-
culties in preparing specimens and setting up as compared with the case of
tension or compression.

On the other hand, to know the dynamic bending strength, the instrumented
Charpy impact test method has been very often used, but in the case it is
generally not so easy to evaluate the dynamic load applied to a specimen on
behalf of inertial load at high velocity (Venzi,.et al,1970) . Recently, to
evaluate the dynamic load and displacement for short period with ease, some
301
302

Hopkinson pressure bar techniques were applied to three-point bending test,

where how to determine the dynamic fracture toughness of metals (Yokoyama
et al,1989) and the dynamic strength of FRP (Higashida et al,1990) was de-
scribed. But in these studies stress-strain relations of metals including
plastic deformation are not referred and the dynamic test method by three-
point bending is not so well established. So the purposes of the present
study are to establish a three-point bending test method for obtaining
stress-strain relation at high strain rate and to offer some results of
aboye-mentioned hard steels by this method.

EXPERIMENTAL APPARATUS AND PROCEDURE

An outline of the experimental apparatus for three-point bending at high

strain rate above the order of 10 1/s and typical strains measured for de-
termining the stress-strain relation are schematically shown in Fig. 1. The
apparatus consists mainly of a three-point bending specimen ( L + 10 ) mm in
length, a striker bar 20 mm in diameter, an incident load bar 20 mm in di-
ameter and two support bars 13 mm in diameter. The length of the all bars
made of carbon steel is 1500 mm. Each end of them in contact with the
specimen has round surface with the radius of curvature 5 ~10 mm. The
striker bar dropped freely from the height of 0.5-1.5 m strikes the upper
end of the incident load bar at the velocity of V Q = 3.13~5.42 m/s. Owing
to the compressive stress wave propagation in the bar, the specimen is
loaded at its center and is subjected to dynamic bending. With the bend-
ing, stresses travelling in the specimen arrive at its both ends and are
transmitted to two support bars. It is for the slow rise of the incident
load that the lower end of the striker bar is truncated. From the incident

© Specimen
® Incident load bar
©Striker bar
© Support bar
© Rubber plate
© 0 ® Strain gage

E Strain of specimen
6| Incident strain
£R Reflected ••
6T Transmitted ••

0.2 0.4
Time ms

(a) Dynamic bending (b) Typical strains

Fig. 1. Experimental apparatus and strains measured

 303
strain ex ana< reflected strain £ R measured by the strain gage mounted on
the incident load bar, and transmitted strain 6"p measured by the same way
on the support bars, the load Pj at the center of the specimen and the load
P-p at its both ends are expressed as follows
Pp = ApE( £i - £ R ) (1)
PT = 2ATECT (2)
where Ap and A-p are the cross-sectional area of the incident load bar and
the support bars respectively, E is Young's modulus of the bars. Moreover,
by the Hopkinson pressure bar technique the loading velocity V at the center
of the specimen is written as
V = C ( sx + e R - e T ) (3)
where C is the velocity of elastic stress wave in bars. If necessary, the
deflection of the specimen can be obtained by the integration of V with re-
spect to time.

To know the characteristic of this method, for example, the variation of

the loading velocity V, the loads Pp and P-p at the same impact velocity V Q =
4.6 m/s is shown in Fig.2. From the figure it is found that the loads Pp
and P<p after a given initial period show a monotonous increase with increas-
ing time. And after the period which is short for the case of the short
span, the equality of the both loads can be seen. This means that the bend-
ing moment M applied to the center of the specimen will be expressed as
PpL/4 or P-pL/4 except for the initial short period. Hereby, for the con-
venience of computation, we consider
M = PTL/4 (4)
From the well-known Herbert's formula about plastic bending of a beam, the
stress a corresponding to the strain e measured by a strain gage at the
bottom surface of loaded portion of the specimen is expressed by M as
a = _2_ 2 ( 2 M + e f - ) (5)
where b and h denote the breadth and the height of cross-section of the
specimen respectively. The strain rate e is defined as the slope of e to
time.

S55C . HV=5.9 GPa.U>=4.6m/s

Fig. 2. Variation of loading velocity

and loads at different spans
304
The longer span L is desirable from an elementary beam theory. In contrast,
the shorter span L is desirable from the time when P T approaches to P-r. So
the meadium span L=60 mm was chosen here.

Experiments at low strain rate below the order of 1 1/s were conducted by
the constant speed type testing machine ( Shimazu Autograph 10T ) .

TEST SPECIMEN

The materials tested are carbon steels S55C , SK3 and alloy steel SCM3. The
latter SCM3 was used only for the measurement of yield strength. The chemi-
cal compositions of them are tabulated in Table 1.

The length of the specimen with rectangular cross-section ( b = h = 8 mm )

is 70 mm. After machining, specimens were heat-treated in salt bath.
Various Vickers hardness levels ( HV = 3-"8 GPa ) for test were prepared by
tempering at various temperature after quenching at 850°C. The structure of
them is martensite tempered.

Table 1. Chemical compositions ( weight % )

Materials C Si Mn P S Cr Mo
S55C 0.56 0.20 0.64 0.024 0.026 - -
SK3 1.07 0.32 0.92 0.021 0.021 0.15 -
SCM3 0.38 0.25 0.71 0.020 0.015 1.11 0.20

EXPERIMENTAL RESULTS AND CONSIDERATIONS

Stress-strain Relation

Fig.3 is an example of M, a, e versus e determined by eq. (4) and (5). It

is found that the smoothed slope for the initial range of curves M and G co-
incides with the slope by elastic beam theory, where the coordinate of M and
a is chosen so that the slope of them in elastic range may also coincide
with each other. Thus, since M corresponds to a, it will be seen in plastic

1.5

200 -
:
///_ 2- s. in
Q.
<0
2
b - 100UJ 1.0
. 0 / 0) (A
(A
/ _ Dynamic bending
U)

-rj^L-^*—
in <d (b ( 6 = 40 1/s)
Of
\- Static bending
c if)
0.5 Static tension
1«/5 - /
W S55C , HV= 5.29 GPa SK3 HV=4.4 GPa
1 i i i 0^ i I
1 0 0 1 2
Strain Strain %
Fig. 3. Bending moment, stress, strain Fig. 4. Stress versus strain (SK3)
rate versus strain (S55C)
 305
range that there is large difference between the stress by eq. (5) and the
apparent stress defined as bending moment divided by elastic section modu-
lus. Since e is not constant, the mean value of it was used in subsequent
results. Fig. 4 is another example of SK3. For comparison, the static re-
sult of bending and that of tension are shown in the figure. The coinci-
dence of them can be seen.

Hardness and Strain Rate Dependence of Strength

Stresses corresponding to a given plastic strain e p are determined from the

stress-strain relations. These stresses plotted to the Vickers hardness HV
are shown in Fig.5 and 6. The former is the static result of SK3 and the
latter is the dynamic one. In both cases, the stress increases with the
higher hardness. Moreover, stresses at the almost equal hardness are also
plotted to strain rate as shown in Fig.7 and 8. In all cases of HV == 7.9
GPa of SK3, completely brittle fracture occurred. As a whole, the strain

o2
Q.
O

_i_
4 5 6 7 8 4 5 6 7 8
Vickers hardness HV GPa Vickers hardness HV GPa
F i g . 5, S t a t i c s t r e n g t h v e r s u s F i g . 6. Dynamic s t r e n g t h v e r s u s
hardness (SK3) hardness (SK3)

• H V = 7 . 9 GPa m

o £
a
a.
o
a.
o

i/> ,

0 •/.
0.2 »
1.0 "

—i
-3 -2 -1 0 1
-3 -2 -1 0 1
Strain rate log 6 1/s
Strain rate log £ 1/s
F i g . 7. S t r a i n r a t e dependence F i g . 8. S t r a i n r a t e dependence
of s t r e n g t h (S55C) of s t r e n g t h (SK3)
306

Dynamic ■ • A
( E * 3 0 - 9 0 1/S)
J i i l i L
3 4 5 6 7 8
Vickers hardness HV GPa
Fig. 9. Relation between yield strength of
hard steels and Vickers hardness

rate dependence of the strength of steels seems to appear at high hardness

level above HV = 5 GPa as well as at low hardness level. To know the incli
nation of the strength to hardness, relations between the yield or fracture
strength a y corresponding to e p = 0 and the Vickers hardness of all
materials tested are shown in Fig.9. The dynamic strength at the strain
rate e = 30-90 1/s is higher than the static one at e = 0.0001-0.01 1/s
by the amount of about 10 % and is almost proportional to the Vickers hard-
ness. The value of the slope 0.282-0.297 slightly smaller than the value
0.3-0.5 for the usual case of the relation between the static tensile
strength and the Vickers hardness ( for example, Tabor,1951 ) .

CONCLUSIONS

Results obtained by the present study are summarized as follows

(1) A dynamic three-point bending test method using Hopkinson pressure bar
technique was established.
(2) Stress-strain relations of hard steels with the Vickers hardness 3-7.9
GPa at high strain rate up to the order of 10 2 1/s could be obtained by
the present method.
(3) Strain rate dependence of the yield strength of hard steels tested was
found, though it was within about 10 — 20 %.
(4) Yield strength ( 1-2.5 GPa ) in the both dynamic and static cases is
almost proportional to the Vickers hardness on the whole, though it is
scattered.

REFERENCES

Harding, J. (1987). The effect of high strain rate on material properties.

In: Materials at high strain rate ( T.Z. Blazynski, Ed.), pp.133-186.
Higashida, F. and K. Ogawa (1990). Impact three-point bending tests on FRP
by split-Hopkinson bar technique. J. Soc. Mat. Sci.,Jap., 39, 1462-1468.
Tabor, D. (1951). The hardness and strength of metals. J. Inst. Met.,
79, 1-18.
Venzi, S., A. H. Priest and M. J. May (1970). Influence of inertial load
in instrumented impact tests. ASTM STP, 466, 165-180.
Yokoyama, T. and K. Kishida (1989). A novel impact three-point bend test
method for determining dynamic fracture-initiation toughness. Exper.
Mech., 39, 188-194.
WS2c3

INFLUENCE OF TEMPERATURE ON STABILITY OF HIGH STRAIN RATE

DEFORMATION IN SOME COMMERCIAL ALUMINIUM ALLOYS

K Higashi, T. Mukai, K. Kaizu, S. Tsuchida+ and S. Tanimura

Department of Mechanical Engineering,
University of Osaka Prefecture, Mozu-umemachi, Sakai, Osaka 591,Japan;
+;Technical Research Laboratories, Sumitomo Light Metal Industries, Ltd,
Nagoya, Aichi, Japan;

ABSTRACT
The tensile properties of commercial aluminium alloys have been investigated at
strain rates between 4x102 to 4x103 s 1 over the temperature range from 77 to 723K
A decrease in the flow stress and an increase in fracture elongation with increasing
temperature was observed for all alloys. The ductility of the alloys is a function not
only of strain rate sensitivity exponent m but of depends on the relation between m
and the strain hardening coefficient y. In the high strain rate region an increase
in m with strain and maintaining a positive y with strain leads to high ductility.

KEYWARDS
Commercial aluminium alloys; deformation stability; temperature; high strain
rate; strain rate sensitivity; strain hardening coefficient

INTRODUCTION
It is well known that the flow stress of aluminium and aluminium alloys increases
rapidly with strain rate in the high strain rate range (> 103 s *) at room temperature
(Malvern, 1984). However, there is very little information available about the
ductility of aluminium alloys in the high strain rate region. It has been suggested
that the elongation to failure increases with an increase in strain rate for alumin-
ium ( Kawata et al.,1978) and aluminum alloys (Chiem et al.,1988).
For many models (Consider, 1885, Rossard, 1966, Hart, 1967, Campbell, 1967) the
amount of plastic deformation, in particular the amount of uniform elongation is
influenced by the strain hardening parameter and/or the strain rate sensitivity ex-
ponent. The ductility in rate-sensitive materials has been estimated as uniform
strain (eu) using Hart's criterion of stability for plastic deformation (1(e) =(l-y-m)/m
< 0), where y is the strain hardening coefficient (l/a)Qa/9e), and m is the strain rate
sensitivity exponent 91na/91ne. ettis defined as a strain when 1(e) = 0. The purpose
of this paper is to examine the instability parameter 1(e) at high strain rates as a
function of temperatures for several commercial aluminium alloys. And then, the
ductility of some commercial aluminium alloys( 1050, 3003,3004, 5182 and 7N01) has
been investigated as a function of temperatures in the range from 77K to 723K.
307
308
Table 1. Chemical compositions of the aluminium alloys.
ELEMENT (wt%)
ALLOY Zn Mq Cu Mn Cr Zr Ti Fe Si
1050 0.27 0.10
3003 0.15 1.20 0.61 0.27
3004 1.21 0.15 1.05 0.33 0.17
5182 4.52 0.35 0.03 0.25 0.10
7N01 4.50 1.71 0.15 0.35 0.16 0.15 0.05 0.21 0.12

EXPERIMENTAL PROCEDURE

The chemical composition of the commercial aluminium alloys used in this study
is given in Table 1. Tensile specimens machined from hot rolled plates, had their
tensile axes normal to the rolling direction. The gauge length of the specimen is 4.5
mm, and the diameter is 3 mm. All specimens were heated to 643 K with a heating
rate of 47 K / hour and then annealed for 2 hours in air. For the tensile tests, these
specimens were tested at strain rates between 4x10 2 to 4x10 3 s 1 at temperatures
over the range 77 to 723 K The dynamic tensile tests were performed using a split
Hopkinson pressure bar system where incorporates a specific attachment. The
specific attachment is shown in Fig.l. The test system is illustrated in Fig.2. The
use of this specific attachment allowed dynamic tensile tests to be performed by a
compression testing machine. compressor
Control box

Output bar

Output bar Specimen Input bar

Fig.1. Spesific attachment Fig.2. Split Hopkinson bar system

with measuring system

RESULTS
Typical engineering stress-engineering strain curves for 1050,3003,3004, 5182 and
7N01 alloys tested under three temperatures of 77K, 300K and 723K are shown in
Fig.3 respectively. The curves marked by * were drew up to the maximum strain
resulting from the measuring limit of machine. For all alloys, no significant
change is observed in the shape of the stress-strain curves at each temperature. The
slope of the curves is seem to decrease with increasing temperature. In addition,
it is observed that the maximum value of the stress increases with an increase in the
strain rate for all alloys at a given temperature.
The maximum flow stress and the fracture elongation values for all alloys at the
three testing temperatures are shown in Table 2. The maximum flow stress
corresponds to the ultimate tensile true stress. For any alloy, it is clear that the
maximum flow stress increases with increasing strain rate at a given temperature
and decreases with the increasing temperature at any strain rate except for the 5182
alloy.
 309

1050 3003

1570 s- 1

0.2 0.4 0.6 0.8 1.0

3004 ENGINEERING STRAIN

Fig.3. Typical engineering stress

-engineering strain curves
for 1050, 3003, 3004, 5182
and7N01 alloys respectively.

2150 S-1

0.4 0.6 0.8 0.0 0.2 0.4 0.6 0.8 1.0

ENGINEERING STRAIN

DISCUSSION
Fig.4 shows the relationship between the flow stress (at true strain levels,
e = 0.05, 0.1, ...0.3) and the strain rate for the 1050 and 7N01 alloys at 300K. Data
below 1x10 ^s 1 were observed using an INSTRON machine. In the shape of the
stress-strain rate curves of both alloys, no significant change with strain is
observed in the shape of the stress-strain curves over the strain rate range. In the
low strain rate range (< 1x10 's 1 ), the values of flow stress at given true strain is a
weak function of strain rate. As strain rate increases the flow stress increases with
strain rate. The slope of curves is strain rate sensitivity exponent. The values of flow
310
Table 2.
Thft maximum flow stress and the fracture elongations at three testing temperatures.
77 K 300 K 723 K
E 1040 1590 2130 990 1700 2250 850 1120 1840
1050 °m 268.67 - 276.12 124.49 138.79 142.11 44.53 70.18 81.39
E
f 67.56 65.66 70.83 69.88 70.46 73.51 86.19 88.96 95.15
e 1040 1570 2120 1100 1700 2250 990 1650 2100
3003 om _ 349.50 351.28 178.49 184.03 194.32 74.81 97.76 119.51
e
f 41.23 52.98 _ 56.00 57.34 58.60 82.67 74.60 69.93
p 1060 1550 2130 980 1700 2240 1060 2070 2230
3004 °» 441.52 437.87 442.76 240.90 _ 249.18 129.07 _ 143.74
Ef 35.95 37.12 39.34 50.05 48.08 50.19 56.98 47.60 54.03
e 1070 1600 2030 740 1600 2240 1100 1650 2140
5182 °m 475.4 503.16 575.7 328.54 338.6 340.34 168.20 194.09 203.12
Ef 33.71 31.50 30.85 46.77 44.9 45.78 33.37 34.27 39.14
£ 840 2070 2150 920 1700 2220 1060 1680 2160
7N01 °m 459.39 464.53 499.27 365.25 413.91 416.64 151.87 160.47 171.89
E
f 28.49 28.78 29.23 33.26 31.37 29.92 41.95 46.57 47.02
strain rate, maximum flow stress, MPa - f: fracture elongation, %

stress at given true strain levels in-

crease rapidly with increasing strain
rate in the range of this work. For these
alloys, the slopes of the stress-strain
rate curves, or the m values at a given
strain, reduce with increasing strain.
In the strain rate range of this work, the
flow stress of all alloys is sensitive to the
strain rate, therefore strain rate sensi-
tivity exponent m = 31na/31ne with in-
creasing strain is important to the sta-
bility for plastic deformation.
In many models about plastic instabil-
ity controlled by the mechanical proper-
ties of materials, the influence of the
strain hardening parameter and/or the
strain rate sensitivity exponent on the - 3 - 2 - 1 0 1 2 3
onset and growth of the necking has LOG( STRAIN RATE s"' )
been noted. In Hart's criterion of
stability (Hart,1967) the effect of strain Fig.4. The relationship betweep flow
rate sensitivity exponent with increas- stress and strain rate as a function of true
ing strain is considered, we have strain for the 1050 and 7N01 aluminium
adopted this criterion to investigate the alloys.
deformation stability. The ductility in
rate-sensitive materials has been esti-
mated as a uniform strain (eu)fromthe Hart's criterion of stability for plastic de-
formation. If in the course of "the deformation the magnitude of the cross section
difference does not increase, Hart calls the deformation stable [ (dA/dA)P£0,
where the subscript P means that the load P is constant, and dA is the variation
in area increment rate and dA is the variation in cross-section. ]. This condition
can be restated as, (dlnA/dlnA) P £ 0. The stability criterion can be stated as follows:
(dlnA/dlnA)P = (l-y-m)/m £ 0, which is expressed using the material parameters
y= strain hardening coefficient, y = (l/aXoo79e) and m = strain rate sensitivity
exponent, m = aina/dlne. The instability parameter 1(e) is given as 1(e) = (l-y-m)/m.
 311
Hart's criterion, the deformation is stable
if 1(e) = (l-y-m)/m < 0. Therefore, we
define the uniform straine as the strain
when 1(e) = 0. The material parameter y
which decreases with strain is com-
puted from the true stress-true strain
curves. The strain rate sensitivity expo-
nent at given true strain levels is com-
puted from the slope of the stress-strain
rate curves shown in Fig.4. The values of
y and m as a function of strain at 77K,
300K and 723K for 1050 alloy are shown in
Fig.5. In general, it was observed that
the maximum value of m increased
whereas, the maximum value of y was
observed at the lowest temperature. At
large strains e becomes negative. The
change of 1(e) value at a fixed strain rate
of 2x10 3 s 1 with strain for all alloys is
shown in Pig.6 at 77K, 300K and 723K re-
spectively. In general, 1(e) value is nega-
tive at small strain less than about 0.2,
however, above thatstrain whichincreases
to become positive with increasing strain.
The slope of I(e)-strain curve is getting
smaller with increasing temperature,
z./
but eu is getting smaller with increasing
temperature. For most of the present
STRAIN RATE =2" 10V
alloys, m values as a function of strain
increase with increasing temperature. o 77K

On the other hand, the y values as a Z 40^ A 300K

function of strain decrease with increas- a 723 K

ing temperature. Therefore, the large

ductility observed is not only a result of
STRAIN RATE = 2 * 1 0 V

1 .
o 77K
A 300 K

.^i
a 723K

STRAIN RATE =2*10V

_^
yy
o 77K
A 300K
□ 723K
0.2 0.3 /(/ 1
STRAIN

Fig.5. The typical change in y and m Fig.6. The typical change in l(e) with strain
with strain for the 1050 alloy. for the 1050, 3003, 3004, 5182 and
7N01 alloys at 77K, 300K and 723K.
312
high m value but the relation Table 3. Values of uniform strain at temperatures.
between the m and y values.
For example, in the 1050 alloy 77 K 300 K 723 K
m value with strain at 723K is E 2 4 . 5 5 1 9 . 7 2 12.04
greater than that at 77K, but «xp
1050
the y value becomes negative at *i-0 24.75 2 1 . 2 5 14.04
the smaller strains at 723K, as £
exp 21.11 17.06 19.14
shown in Fig.4. Then in 1050 3003
alloy e at 723K is smaller than ^-0 21.3 18.15 20.50
that at 77K. In present com- £
~P 18.73 16.55 16.38
mercial aluminium alloys, it 3004
is clear that one requirement h-0 1 9 . 4 7 1 8 . 2 5 1 7.30
to obtain high ductility in the £
ezp 18.65 16.47 15.27
high strain rate range is the re- 5182
lation between m and y. An in- *!-<> 19.71 18.00 17.36
crease in the value of m with 7N01
^ exp 12.22 12.22 9.44
strain while maintaining a posi- ^-0 13.90 12.90 9.60
tive y as a such strain leads to a
high ductility.
Table 3 shows the effect of temperature on the uniform strain for all the present al-
loys. In this table, e is the true strain where the load reaches the maximum value
in the load-displacement curve. In general, the uniform strain is seem to decrease
with increasing temperature. This change in uniform strain may be related to the
motions of dislocation at high strain rate for the testing temperature. The value of
e,^ is greater than that of e in the high strain rate range for all present alloys at
any temperature. The difference between these values corresponds to the magni-
tude of the m value.
CONCLUSIONS
The general conclusions can be established as follows:
(l)The strain rate dependence on both flow stress and ductility in commercial
aluminum alloys has been observed in high strain rate range at any testing
temperature. The values of flow stress at the ultimate tensile strength for all
the aluminium alloys decreases with the increasing temperature. The fracture
elongation for all alloys increases with increasing temperature.
(2) High ductility is not only a function of m but depends on the relation between m
and y. In order to obtain high ductility in the high strain rate range the relation
between m and y must be considered. Increasing the value of m with strain and
maintaining a positive y with strain leads to a high ductility.
(3) Uniform strain decreases with increasing temperature. This change in uni-
form strain might be related to the motions of dislocation. The uniform strain
defined by this method is larger than the uniform strain measured in the load-
displacement curve because of the strain rate sensitivity in this strain rate range.
REFERENCES
Campbell,J.D.(1967). Plastic instability in rate dependent materials. J.Mech.
Phys.Solids, 15,359.
Chiem,C.Y., ancTet al(1988). Dynamic response and microstructural aspects of
CP271 and CP274 aluminium-Hthium alloys, JOURNAL DE PHYSIQUE, C3-19.
Considere,A.(1885). Annales des Ponts et Chaussees, 9,579.
Hart,E.W.(1967). Theory of the tensile test. Ada Met., T8,351.
Kawata,K and et al(1978). In: High Velocity Deformation of Solids, (K. Kawata &
J.Shioiri, Ed.), Springer Verlag, New York, pp.1.
Malvern£i.E.(1984X I n: MechanicalPropertiesat high rates of strain, (J.Harding,Ed.)
The Institute of Physics, London, pp.1.
Rossard,C.(1966), Formation de la stnction dans la deformation a chaud par
traction, Rev. Met., 63,225.
WS2C4

STRENGTH OF ALUMINUM UNDER HIGH VELOCITY DEFORMATION

T. KUROKAWA and K. TANAKA*

Department of Aeronautical Engineering, Kyoto University,

Kyoto 606, Japan
^Current Address : Department of Mechanical Engineering,
Setsunan University, Neyagawa 572, Japan

ABSTRACT

The dependence of the stress-strain relation of aluminum 1050 on the strain

rate has been examined experimentally in a wide range of strain rate which
covers from 10~^s"^ up to l(T*s~ . Experiments were conducted by axial
compression tests at all rates of strain. A new technique was used for one
group of experiments at very high rates of strain, where flier plates of
steel struck specimens directly in order to avoid plastic deformation of the
input bar due to high velocity impact instead of ordinary split Hopkinson
pressure bar method. It appears that the rate sensitivity of aluminum 1050
begins to increase with the strain rate above the strain rate of 10 2 s - 1 and
becomes much more remarkable at the range of 10^s"~ .

KEYWORDS

Aluminum; high velocity deformation; impact; rate sensitivity.

INTRODUCTION

It has been recognized by some investigations for the dynamic deformations

of metals during the last decade that flow stresses of metals show the very
remarkable increase with the increase of strain rate at the ultra-high
strain rates instead of gradual increase under the ranges of the strain rate
of lO^s"" . Clifton, in his review paper (1983), presented his pressure-shear
impact method and measurement of flow stress at very high strain rate of
aluminum llOO-o by his Ph.D student C.H.Li. Their results showed that the
very rapid increase of flow stress occurs at the range of strain rate above
10's~ . This is explained to be the transition of deformation mechanism from
the thermal activation process to the dislocation drag control mechanism.

On the other hand, the upper limit of the strain rate by the conventional
split Hopkinson pressure bar method (SHPB) is several times lO-^s" . This is
because the maximum impact velocity for SHPB is restricted under about 20m/s
in order to prevent a plastic deformation in the elastic input bar. Some
experimental results by SHPB and other techniques intimated a possibility of

313
314
the abrupt change of flow stress at its upper limit regime of strain rate.
The ultrasonic attenuation experiment for pure aluminum (Shioiri et
al.,1983) showed an abrupt increase of flow stress in the range of strain
rate between lO^s"1 and lCrs -1 . Recently Higashi et al. (1990) conducted
dynamic tensile experiments up to the range of strain rate of 3xl0^s~^ by
SHPB for several kinds of aluminum alloy and presented that the flow stress
begins to rise steeply at the range of strain rate of lCHs" . In spite of
these experimental data, it has not been confirmed to narrow the gap of flow
stress between the strain rates under lCns"-*- and beyond 1(KS~ . Therefore
much more experimental data at this transition regime of the strain rate
between ICHs--1- and lO^s"1 are required.

In this paper, a new technique for dynamic compression test is proposed and
experimental results of compression tests for aluminum 1050 over wide ranges
of strain rate including the transition regime of strain rate between lO^s"1
and UxlO^s -1 is presented. This experimental technique, where a flier plate
instead of an input bar strikes a specimen directly, pushes up the upper
limit of impact velocity by one order higher than SHPB. It was converted to
the compression test from "one bar method" for tension test which was
developed and designated by Kawata et al.(l985).

EXPERIMENTAL DETAILS

Specimen

The specimens for the compression tests were machined from 12mm diameter
cold drawn bar of commercially pure aluminum 1050 to two types of geometry;
the thick type (l2mm in thickness x 8mm in diameter) and the thin type ( kmm
in thickness x 8mm inQ diameter). Some were used as drawn and some were used
after annealing ( U20 c, one hour). Only thin type specimens were used for
the high velocity test.

Quasi-Static and SHPB Test

Quasi-static compression tests at strain rates of lO^s'^-lCT-^s-1 were

conducted using Shimazu AG2000-A (Instron-type testing machine). Dynamic
compression tests at strain rates of 10 2 s _ 1 2xl(Hs -1- were carried out by
SHPB.

High Velocity Compression Test

As mentioned previously, an elastic input

bar cannot be used for high velocity tests
of more than 20m/s because of the elastic
limit of the input bar. The concept of the
new technique to carry out the high
velocity compression test beyond this ^Strain gage
limit proposed in this paper is shown in -Stopper
Fig. 1. A specimen attached in aid of SaboP
lubricant Molybdenum Sulphide to the end Fig.l Scheme of device for high
surface of the input bar was struck by a velocity compression test.
flier plate held by a plastic sabot. A projectile which consists of a flier
plate and a plastic sabot was projected by a compressed-air gun or an
explosive powder gun. The former is used for the velocity range of 30m/s-
 315
100m/s, and the latter for the velocity range above lOOm/s. The flier plates
were quenched carbon steel disks of 6mm thickness, and the masses of the
projectiles were about 92gr for the air-gun and about 35gr for the powder
gun. A specimen was set up to stick out a small amount of length, 6 , of a
quenched carbon steel stopper of 50mm thickness. The movement of the flier
plate is ceased by the stopper, therefore the specimen is deformed by the
amount of the indentation of the stopper and the flier plate in addition to
the sticking out length 6. The indentation of the stopper and the flier
plate was only elastic deformation for low velocity impact, however higher
velocity impact yielded the plastic indentation and it amounted to 0.5mm for
the impact velocity of l60m/s. The output bar is a steel bar of 15mm
diameter and U50mm length. The stress wave propagated along the output bar
was measured by the strain gages cemented on the surface of the bar at the
location of U5mm apart from the impact end. The history of the nominal
stress, o^(t), and the history of the velocity, Vjjtt), of the specimen at
the contact end to the output bar were derived on the assumption that the
stress wave is propagated without changing the shape.

a N (t) = ° T ( T )A T /A 0 (1)

V IZ (t) = aT(t)/pc0 (2)

where aip(t) is the stress history of the output bar measured by the strain
gages, and Arp, p, c Q are the cross sectional area, the density and the
longitudinal elastic wave velocity of the bar, respectively and A Q is the
initial cross sectional area of the specimen. On the other hand, the
velocity at the impact end of the specimen, Vj, is expressed as the
following equation,

Vj(t) = V 0 -l (AT/M)aT(t)dt (3)

where V Q and M are the impact velocity and the mass of the projectile. The
nominal strain rate of the specimen is expressed as follows,

eN = (VJ-VJJJ/IO (k)

where 1 Q is the initial length of the specimen. The nominal strain e N of the
specimen can be derived by integrating the equation (U), and the true
stress of the specimen is expressed by the equation (5).

a=aN(l_£N) (5)

RESULTS AND DISCUSSION

Some examples of the results of high velocity compression tests are shown in
Fig.2-Fig.6. Figure 2 shows the stress history of the output bar 0"T(t), when
an annealed specimen was subjected to impact of the initial velocity V0=32.5
m/s. The initial strain rate of the specimen was 8.1xl0^s_1. The decrease of
the strain rate of the specimen due to the deceleration of the projectile
during deformation was not so significant. The strain rate decreased to 7.8
xl 0 3 s -m± at the instant of 15Ps after impact when the nominal strain of the
specimen reached to 10%. The nominal stress-strain curve calculated from the
stress history in Fig.2 is shown in Fig.3, where the yield stress of the
specimen is assumed to be 30MPa in order to cut off the effect of the
precursor of the stress wave along the output bar.
316

300,
100i

GL

t> 50

10 20 30
10 20
Time ( | i s ) Strain 8N(o/o)

Fig.2. Stress history at z=l+5mm Fig.3. Nominal s t r e s s - s t r a i n

of output "bar. curve at the s t r a i n r a t e
(Annealed, VQ=32.5m/s) 8 x l 0 3 s - 1 . (Annealed)

100| 300

o
Q.
2
5(*
(A
(A
01

0 10 20 30
Time ( j i s ) Strain Cf/o/o)
Fig.U. Stress history at z=U5mm Fig.5. Nominal stress-strain
of output "bar. curve at the strain rate
(Drawn, VQ=36.1m/s) 9x103s"1. (Drawn)

Figure k shows the stress history of

the output bar, when a drawn specimen 1
was subjected to impact of the z=45mm
initial velocity VQ=36.1m/s. The q= 5mm/jzs
"=0.29
nominal stress-strain curve of the
specimen is represented in Fig.5. The *S
yield stress of the drawn specimens g
is assumed to be lOOMPa. Oscilations N/\/\J
of stress can be seen both in Fig.U t/>
and Fig. 5. The amplitudes of the <u Elementary
oscilations were larger if the impact fi 1 / theory
velocity was higher and the specimen
was drawn rather than annealed. This
oscilation is considered to be due to
0 10 20 30
the effect of the radial inertia of Time (|is)
the output bar. Skalak (1957) Fig.6 Stress history at z=U5mm of
obtained an analytical solution for output bar calculated by
the longitudinal impact of circular Skalak's solution.
elastic bar, taking the effect of the
 317
radial inertia into account. Figure 6 represents the calculated stress
history obtained by Skalak's solution using the condition of the output bar
of this experiment. The periods of the oscilations in Fig.U and Fig.6 show a
good agreement. Therefore the material characteristic is considered to be
represented not by the oscilating curve but by the central line between two
dashed lines in Fig.6.

The dependence of the flow stress on the strain rate is shown in Fig.7 and
Fig.8, where the true stresses at the strains £=0.05 and 0.1 are plotted for
various strain rates. Each of the variation ranges of flow stress
represented by vertical bars for the data points at high strain rates in the
figures corresponds to the amplitude of oscilation of stress-strain curve as
represented by two dashed lines in Fig.5. The increase of flow stress with
increasing strain rates is low at the low and medium strain rates, however
it is accelerated beyond the strain rate of lO^s"1 and it becomes more
remarkable at very high strain rates above 10^s~ . In Fig.9, the same data
of annealed specimens as in Fig.7 and Fig.8 are compared with the data of
aluminum llOO-o cited by Clifton (1983), where Clifton's data represented
originally by shear stress and shear strain rate are converted to equivalent
stress and equivalent strain rate using Mises criterion. Although the data
obtained in this experiment show a remarkable but more gradual increase
above the strain rate of 10 2 s" 1 than the abrupt change represented by dashed
line in Fig.9, they seem to follow Clifton's data smoothly.

CONCLUSIONS

(1) The one bar method using the impact flier can be used to obtain the
compressive stress-strain curve at the high strain rates of lO^s"1.
(2) The flow stress of aluminum 1050 begins to show a gradual increase
with increasing strain rate at the strain rate of about 10 2 s~ 1 and a more
remarkable increase at the strain rate of 10^s _1 rather than an abrupt and
sharp upturn at the strain rate of

ACKNOWLEDGEMENT

This work has been sponsored by Grant-in Aid for Scientific Research of The
Ministry of Education, Science and Culture of Japan ( Grant No.58U60077) and
by The Light Metal Educational Foundation Inc..

REFERENCES

Clifton,R.J. (1983). Dynamic Plasticity. J. Appl. Mech., 50, 9^1-952

Higashi,K., T.Mukai, K.Kaizu, S.Tsuchida and S.Tanimura (1990). High
Strain-Rate Deformation Characteristics in Commercial Aluminum Alloys. J.
of Soc. of Mat. Sci., Japan (in Japanese), 39, l6l9-l62U
Kawata,K., S.Hashimoto, S.Sekino and N.Takeda (1985). Macro- and Micro-
Mechanics of High-Velocity Brittleness and High-Velocity Ductility of
Solids. In: Macro- and Micro- Mechanics of High Velocity Deformation and
Fracture( K.Kawata and J.Shioiri, Eds.), Springer-Verlag, Berlin, 1-25
Shioiri,J., K.Sakino and K.Satoh (1985). A Constitutive Equation of FCC
Metals at High Strain Rates Based upon the Ultrasonic Study of Dislocation
Motion. In; Macro- and Micro-Mechanics of High Velocity Deformation and
Fracture( K.Kawata and J.Shioiri, Eds.), Springer-Verlag, Berlin, 179-188
Skalak,R. (1957). Longitudinal Impact of Semi-infinite Circular Elastic
Bar. J. Appl. Mech., 2k 9 59-64
318

300 300
Thick Thin
Thick Thin
Annealed o •
Annealed o •
Drawn O ©
Drawn o @

2 200 ± 200
D -t> O-

I 100 a
if) * •-
£=0.05 e=ai
_ i —i i i i i i

- 3 - 2 - 1 0 1 2 3 4 5 -3-2-1 0 1.2 3 4 5
iog£ log£

Fig.7- Dependence of flow stress Fig.8. Dependence of flow stress

at the strain e =0.05 at the strain e =0.1

300

- 2 - 1 0 1 2 3 4A 5
Equivalent strain rate log £

Fig.9. Dependence of flow stress of annealed pure aluminum.

WS2C5

DYNAMIC AND QUASI-STATIC TENSILE PROPERTIES

OF AL-LI ALLOY AT LOW TEMPERATURES
H. KOBAYASHI and M. DAIMARUYA

Department of Mechanical Engineering, Muroran Institute of Technology,

27-1, Mizumoto, Muroran, Hokkaido 050, JAPAN

ABSTRACT

In order to investigate the mechanical properties of Al-Li alloys at low temperatures, a series of
tensile tests was carried out at a quasi-static rate of 1.7 x 10"3 sec"1 and a dynamic rate of about
5.0 x 102 sec"1. Since tensile specimens were machined from a thick plate, the specimen with its
axis parallel to the short transverse direction was prepared as well as the longitudinal and
transverse directions. The effect of strain rate on the strength and elongation was observed in the
longitudinal and transverse directions. In the short transverse direction, however, remarkable
effect of strain rate was not observed.

KEYWORDS
Al-Li alloy, mechanical properties, low temperature, dynamic rate, specimen orientation

INTRODUCTION

Recently, Al-Li alloys are considered to be an important new material for stiff airframe structures
because the Al-Li alloys offer a combination of low density, high strength and high elastic
modulus(Nobel et ai, 1984, Miller et ai, 1986). Therefore, it is worth to investigate the
mechanical properties of Al-Li alloys not only at quasi-static rates but also at dynamic rates.
Mechanical properties at dynamic rates for various Al-Li alloys have been ascertained by a
number of researchers, in tension (Ohnishi and Ito, 1987, Kobayashi et ai, 1988) and in
torsion (Dodd and Kobayashi, 1990). However, these tests were carried out at room
temperature. In the present study, a series of dynamic and quasi-static tensile tests for an Al-Li-
Cu-Mg-Zr alloy was carried out at low temperatures. Since tensile specimens were machined
from a thick plate, the effect of specimen orientation was also investigated.

EXPERIMENT

Material and Specimen

The specimens used were machined from two plates (20 x 100 x 1000 mm) which provided by
Kobe Steel Ltd. The as-received plate was in the extrusion condition. Therefore, solution
treatment (793K, 90 min.) and aging(463K, 16 hours) were performed. The composition of
319
320

the alloy is given in Table 1. The tensile specimen used has a test section with diameter of 3 mm
and length of 6 mm as shown in Fig. 1(a). Three kinds of specimen were prepared with their
axes parallel to the longitudinal, transverse and short transverse directions, and referred to as
"L-", "T-" and "ST-" specimens, respectively (see Fig. 1(b)).

Table 1 Chemical composition (wt.*

Li Cu Mg Zr Fe Si Ti Na Al
2.53 0.95 1.15 0.11 0.05 0.04 0.04 0.004 Bal.

A/ 10 AJL
" / V
1 1
—
i r
j 1
1 11—1—7l

L6J
30 (20) Unit: mm
<* : »j

Fig.l Tensile specimen and specimen orientation in a plate.

Quasi-static and Dynamic Tensile Tests

The quasi-static tests were carried out by using a screw gear type testing machine. For the
dynamic tensile tests, Hopkinson bar type tensile testing apparatus, shown in Fig.2, was used.
A tensile specimen is located between input and output bars which are two long aluminium alloy
bars with diameter of 20 mm. To create the incident stress wave, an aluminium alloy pipe with
length of 750 mm and outer diameter of 32 mm, was dropped on the flange attached to the end
of the input bar. The dropping height adopted in the dynamic tests was 2.6 m. As shown in
Fig.2, the incident and reflected waves, o{ and ar, were measured by the strain gauge, G p
while the transmitted wave, o t , was caught by the gauge, G2. These wave data was then
processed by a microcomputer, after storage in a transient recorder, to obtain stress/strain
curves. The equations used to obtain stress/strain curves are:

1
o = —2-a, £ = - £(a i+ a r -a t )dt (1)
pc 0 L Jo

where, A0, p and c0 are the cross-sectional area, density and bar velocity of the input and output
bars and As and L are the cross-sectional area and the gauge length of the specimen. Both
dynamic and quasi-static tests were carried out at three different ambient temperatures, i.e. 77
K, 195 K and 293 K. These low temperatures, 77K and 195K, were accomplished by N2 liquid
and ethanol with dry ice, respectively. In the tests at low temperatures, specimens were retained
in the coolant for 5 minutes before testing.
 321

4m

4m

Fig.2 Arrangement of split Hopkinson bar apparatus for tensile version.

LB.; input bar, O.B.; output bar, F ; flange, S ; Striker pipe.

EXPERIMENTAL RESULTS AND DISCUSSIONS

Results of L-Specimen

The ultimate tensile strength, o B , the 0.2 % proof stress, o 0 2 , and the maximum strain, e ^ ^
obtained from quasi-static tests (e = 1.7 x 10"3 sec-1) and dynamic tests (e = 500 sec-1) of the L-
specimens are shown against the testing temperature in Fig.3(a) and (b), respectively. Where,
emax corresponds to the strain at which fracture occurred in the tests. The aB obtained quasi-
statically increases with the decrease of the testing temperature. The dynamic aB also increases,
however, the average of the dynamic aB is 20 - 30 MPa greater than that of the static aB at each
temperature. The dynamic emax increases from 5 to 7 % with decreasing temperature, while the
static £max are in the range of 4 to 5 %. As observed above, even at low temperatures, the
strength and elongation at dynamic rates are larger than those at static rates, therefore, the effect
of strain rate can be recognized at low temperatures as same as at room temperature. Both
averages of a() 2 obtained quasi-statically and dynamically at 293K are about 350 MPa. Whereas,
the quasi-static cQ2 at 195K is much larger than the dynamic one. In the c02 of 77K, the static
data seems to be slightly higher than the dynamic data. Therefore, it might be considered that at
low temperature, there is negative strain-rate dependence of stress in early stage of plastic
deformation, nevertheless the dynamic aB is larger than the static, as mentioned above.

Results of ST-Specimen

The results of ST-specimen tested at quasi-static rate of 1.7 x 10"3 sec'1 and dynamic rate of
about 450 sec"1 are shown in Fig.4(a) and (b), respectively. The distinctive feature here is that
322

the emax obtained are much smaller than those of L-specimens, about one third. The o B and the
8max obtained at 195K are lower than those obtained at other two testing temperatures, and this
can be seen in the both quasi-static and dynamic results. Similar temperature dependence of
strength was observed in a series of quasi-static tests for Al-Li-Cu-Mg-Zr alloy by Furushiro

600 600
D L-Dynamic ||
□ -.^ B .
500 h D
a
^ ^
400h
Q O
"—-Q^ o-"
300 Lh "—8- o

^ A
0
A -j
200 h r ^ "" ^ ^ A ^ A j

A^l
A
E
100 4 w

. i i 1 . 1 ]
100 200 300 100 200 300
Temperature (K) Temperature (K)
(a) (b)

Fig.3 Tensile strength, 0.2 % proof stress and maximum strain obtained from
(a) quasi-static tests and (b) dynamic tests for L-specimen.

500 500 i

400

e 300 h
PQ

200 h H 2

100 h 1 s
CO

100 200 300 100 200 300

Temperature (K) Temperature (K)
(a) (b)

Fig.4 Tensile strength, 0.2 % proof stress and maximum strain obtained from
(a) quasi-static tests and (b) dynamic tests for ST-specimen.
 323
et al. in 1986. It was said that this positive temperature dependence was caused by the ordered
5' precipitates (Al3Li) (Abe et al., 1990). In comparison with the static and dynamic data, the
GB, c02 and Emax, considerable differences can not be recognized, although the changing pattern
of a0 2 is slightly different in the quasi-static and dynamic data. In the ST-direction, therefore,
the effect of strain rate on the tensile characteristics appears not to be remarkable very much.

Results of T-Specimen

The quasi-static and dynamic tensile test results of T-specimen are shown in Fig.5(a) and (b),
respectively. The rates used are 1.7 x 10"3 sec"1 for the quasi-static tests and about 530 sec'1 for
the dynamic tests. In the results at room temperature(293K), the aB, G0 2 and emax obtained from
the both static and dynamic tests show quite similar values. In the aB at low temperatures,
however, relatively remarkable difference is observed. The dynamic oB increases with the
decrease of the testing temperature, as well as the aB of L-specimens. While, the static aB
changes in the similar way to that of ST-specimen. The emax obtained from quasi-static tests
scatters in the range of 3 to 7 % at every temperatures. The dynamic emax also scatters in the
same range as the static except for the result at 195K. To make sure the reason of this scatter,
therefore, more experiments are necessary.

500 500
T-Static|

400 h
^ E □'
B . Q-
^ □
300 h
CQ
□
10 8/
200 h L ^ § - ^— 8 - "8 -

A 6 A :

I A
100 h A
I _
A
I , I _J L i 1
100 200 300 100 200 300
Temperature (K) Temperature (K)
(a) (b)

Fig.5 Tensile strength, 0.2 % proof stress and maximum strain obtained from
(a) quasi-static tests and (b) dynamic tests for T-specimen.

Fracture Surface
The fracture surfaces of L-, ST- and T-specimens tested quasi-statically were observed using
scanning electron microscopy (SEM), as shown in Fig.6(a), (b) and (c), respectively. The
surface of L-specimen is very complicated, that of ST-specimen is relatively smooth and flat,
while, that of T-specimen shows zigzag ledges similar to 'sawtooth'. In an aged Al-Li alloy,
large grains elongated along the rolling direction and very thin in the ST-direction were observed
324
(Dodd and Kobayashi, 1990). From the observations above, the material used here seems to
have similar grains to that observed by Dodd and Kobayashi.

(a)i_ 500|im (b) 500UJTI

Top View

M
Specimen

v——-r——v
(c) I I 500pm

Fig.6 Fracture surface of (a) L-specimen, (b) ST-specimen and (c) T-specimen
tested quasi-statically at room temperature (293K).

ACKNOWLEDGEMENT

We have very grateful to Dr. Miyagi and Kobe Steel Ltd. for the provision of an Al-Li alloy.

REFERENCES

Abe, F., H. Araki, T. Noda and K. Kamada (1990). Precipitation hardening owing to 6' Al3Li
in low activation Al-3Li-12Si-3Mg alloy. Mater. Sci. Tech., 6, 829-837.
Dodd, B. and H. Kobayashi (1990). Dynamic fracture of binary Al-Li alloy in torsion. Mater.
Sci. Tech., 6, 447-452.
Furushiro, N., S. Ishihara, D. Zhang and S. Hori (1986). Temperature dependence of tensile
properties of an Al-Li-Cu-Mg-Zr alloy. J. Japan Inst. Light Metals, 36, 744-751.
Kobayashi, A., S. Hashimoto and A. Nakano (1988). Dynamic behavior of Al-Li alloys with
various microstructures. In: Impact Loading and Dynamic Behaviour of Materials (C. Y.
Chiem, H.D. Kunze and L.W. Meyer, Ed.), Nantes and Bremen, pp. 323-330.
Ohnishi, T. and T. Ito (1987). Effects of cathodic hydrogen charging on the mechanical
properties of an Al-Li-Cu-Mg-Zr alloy. 7. Japan Inst. Met., 5_L 1133-1138.
Miller, W.S., M.P. Thomas, D.J. Lloyd and D. Creber (1986). In: Aluminum-lithium alloys
HI (C. Baker, P.J. Gregson, S.J. Harris and C.J. Peel, Ed.), London, pp. 584-594.
Nobel, B., S.J. Harris and K. Harlow (1984). In: Aluminum-lithium alloys II (T.H. Sanders
and E.A. Starke, Ed.), Warrendale, pp. 65-77.
WS2c6

THE EFFECTS OF STATE-OF-STRESS AND STRAIN-RATE ON THE

DEFORMATION AND FRACTURE BEHAVIOUR OF REMKO IRON AND
PURE COPPER

J.L. STURGES+, D.C. BARTON*, G.H. MAJZOOBI* AND P. CHURCH$

+ Department of Construction, Leeds Polytechnic, Leeds, LS2 8BU, U.K.

* Department of Mechanical Engineering, University of Leeds, Leeds,
LS2 9JT, UK
$ Ministry of Defence, RARDE, Fort Hal stead, Sevenoaks, Kent,
TN14 7BP, U.K.

ABSTRACT

Notched specimens in pure copper and Remko iron were tested over a range of
stress-rate conditions and strain-rates. Copper showed reducing failure strains with
increased stress triaxiality, strain-rate having little effect. Remko iron, however,
exhibited a ductile-brittle transition at high states of stress intensity and at the higher
strain-rates.

KEYWORDS

State-of-stress, strain-rate, ductile-brittle transition, copper, Remko iron

INTRODUCTION

Previous work has shown that the state-of-stress within a deforming metal will have a
marked influence on its ductility - Bridgman (1952), Hancock and MacKenzie
(1976). Rate-of-strain will obviously be important too, particularly with body-
centred-cubic metals - Harding (1969). The present work has involved a programme
of dynamic and quasi-static testing on notched specimens in both pure copper and
Remko iron. A conventional machine was used for quasi-static testing and the
dynamic tests were performed using the 'Flying Wedge' impact test facility at the
University of Leeds. This device is capable of imposing simultaneous, symmetrical
impulsive loading at both ends of a tension specimen over a wide range of loading
speeds.

MATERIALS AND TEST-PIECE DETAILS

Notched test pieces were machined from BS1433 quality pure copper and from
Remko iron, five notch radii being produced: 0.5, 1.0, 2.0, 4.0 and 8.0 mm. All
specimens had a constant notch root diameter of 7.5 mm (r = 3.75 mm). The
copper specimens were annealed prior to testing, which produced a mean grain size
of 60 /xm. The Remko iron was tested in the as-received condition. Fig. 1 shows
details of the test-piece geometry used.
325
326

130

80

0 7-5

Profile M 20 Thread
015 rod. 1.5 Fine Pitch

Fig.l Specimen geometry

QUASI-STATIC TESTING

Quasi-static testing was performed on a Dartec machine at a rate of 10"3 s 1 . The

failure loads were recorded in each case.

IMPACT TESTING
One of the features of the 'Flying Wedge' device is that by interchanging the wedge
angles (semi-angles of 5°, 28° and 45° are available) a wide range of slider separation
speeds can be achieved. In the present work the 5° wedge was used to generate a
nominal separation velocity of 0.2 ms 1 and the 28° wedge to give velocities of 2.0
and 10 ms"\ The specimens were strain gauged to enable the times-to-fracture to be
experimentally determined. There were therefore two ways of determining the
strain-rate in the deforming material:

€ = slider separation velocity = ds/dt

effective specimen gauge length Lo

or
= failure strain
time-to-fracture
The 'Flying Wedge' device is equipped with velocity sensors to monitor the motion
of the wedge and of the two sliders to which the ends of the specimens are fastened.
Permanent records of tests were obtained using Datalab DL922 2-channel transient
event recorders. Latterly a Gould 1600 series 4-channel recorder was used. As a
further experimental confirmation of the time-to-fracture obtained using the strain-
gauge records, a HICAM moving prism camera was used on some of the tests. The
'Flying Wedge' was designed to allow the specimen to be easily observed during
testing. Before each test the specimen was very carefully centred in the machine so
that the striking faces of the wedges were equi-distant from the centre-line of the
notch. This was done to ensure simultaneity of loading as accurately as possible.
 327

TEST PROGRAMME
The main objective of the programme was to load the specimens to fracture and to
examine the micro- and macro-structural features of the deformed specimens after
fracture.

The test programme consisted of the following steps:

i) the influence of stress-triaxiality and strain-rate on the mechanical response of

pure copper and Remko iron was investigated at strain-rates ranging from
quasi-static to 104 s*1.
ii) the fracture radius and profile of the specimens were measured after fracture.

iii) metallographic examination of the deformed and fractured specimens was

carried out using optical and scanning electron microscopy.

iv) the experimental data were used for numerical modelling of deformation and
fracture at high strain rates.
v) times-to-fracture at the highest rate of loading were measured for a
representative range of specimen geometries for each material and compared
with numerically predicted times.
The present paper concentrates on steps (i) - (iii); the numerical studies will be
reported elsewhere.

RESULTS

Copper
A plot showing the failure strain 4 for copper against the triaxiality parameter P/Y
(as calculated using the Bridgman (1952) analysis for a naturally-necked tensile
specimen) is shown in Fig. 2. The trend of these results is very much as expected in
that the failure strain is reduced as the triaxiality factor P/Y is increased. However,
the ductility of copper was apparently strain-rate independent over the range of
conditions tested.

1.0-

tin

0-5mm profile rod.

10 mm profile rad
£0.5-
20mm profile rad.
4-0mm profile rad.
80mm profile rad.

Fitted curve

0-5 1-0
P/Y

Fig.2 Failure strain versus P/Y for pure copper

328
There are some unexpected variations in ductility observed between certain
geometries. In particular, the 2.0 mm notch profile specimens had lower average
ductility than the 1.0 mm profile specimens. This was attributed, in part, to the fact
that the specimens were not uniformly heat treated ie there were some temperature
gradients in the furnace. Further evidence for this was found in variation in grain
size between 0.5 mm and 2.0 mm profiles as well as variations in hardness:

PROFILE RADIUS HARDNESS

2.0 mm 100 Hv
0.5 mm 90 Hv

The finding that the ductility was apparently independent of strain-rate is in contrast
to the recent work by Dumont et al. (1989) where a slight increase in ductility at
rates of up to 2 x Mrs1 was reported.

Remko Iron

* ' ' *- »
^ 0-5 mm profile rad ♦
Y\ 10mm profile rad o
1.6* V\ 20mm profile rad m \
>lV\f 4-0mm profile rad A
u \ 80mm profile rad. X

\\ V Quasi-static fitted -
\ C "* 0.2m.s-l fitted
A \ 10m.s"1 fitted
1-2- I
\ \
\ X

0)
0-8- Transition "j ""V-*.

[ Brittle

0-A- [
\ /

°^ v ^ > ^^

0- 1 1 1 r 1 '
8 0-4 0-8 1-2 1-6 20
P/Y

Fig.3 Failure strain versus P/Y for Remko iron

The results for Remko iron in the as-received condition were more interesting. Fig.
3 shows plots of ef versus P/Y from which it is immediately apparent that there is a
 329
dramatic reduction in ductility for the small notch radius specimens at high strain-
rates. Obviously a ductile-brittle transition has occurred under certain conditions of
stress triaxiality and strain-rate. This ductile-brittle transition was confirmed by
metallography. The table below summarises the results for tests at 10 ms 1 :

Notch Nominal Strain Fracture Experimental

radius Velocity Time Strain-rate
(mm) (ms"1) (ms) (ST1)

Remkc 8 10 1.515 0.25 5943

iron 4 10 1.186 0.18 6671
2 10 0.331 0.05 6068

The results for the smaller notch radii specimens show lower hardness values at
higher strain-rates. This is quite consistent with the fact that the specimens
concerned have undergone much lower plastic strains that those tested at lower strain-
rates.

Examination of the fracture surfaces was also carried out by scanning electron
microscopy using a Cambridge CAMSCAN. The 0.5 mm profile specimens tested at
quasi-strain rates, 0.2 ms*1 and 10 ms 1 showed dimpled, mixed cleavage and
dimpled, and cleavage surfaces respectively (Figs. 4-6). The change from 100%
dimpled fracture surface at quasi-static rate to 100% cleavage fracture at 10 ms 1 for
this geometry confirms a transition from fully ductile behaviour to a completely
brittle behaviour.

The results for the 1.0 mm and 2.0 mm profile specimens at quasi-static rates show a
dimpled fracture surface and a cleavage fracture surface at 10 ms 1 for both radii.
Examination of other profiles (4 and 8 mm radii) showed ductile fracture throughout
the range of strain-rates developed. This confirms that the fracture mechanism is
dependent on notch radius and therefore on the stress triaxiality P/Y as well as on
strain-rate.

Fig.4 0.5 mm profile Remko iron tested Fig.5 0.5 mm profile Remko iron tested
quasi-statically at 0.2 ms*1
330

Fig.6 0.5 mm profile Remko iron tested

at 10 ms 1

Both optical and scanning electron microscopy confirmed that twinning had occurred
in all specimens of Remko iron tests at 10 ms 1 . This finding is in agreement with
the work of Nagata et al. (1970). In the present work it was found that the
specimens with larger notch profiles were more heavily twinned than those with
smaller profile radii. The 0.5 mm profile had the least number of twins. This
evidence is again consistent with the hardness data and further indicates that the
specimens with sharper notches have undergone less plastic strain prior to fracture.

REFERENCES

Bridgman, P.W. (1952). Studies in Large Plastic Flow and Fracture. McGraw-Hill,
New York
Dumont, C , Levaillant, C , Arminjon, M., Ansart, J.P. and Dormeval, R. (1989).
Ductile fracture of metals investigated by dynamic tests on smooth and notched
bars. lnst. Phys. Conf. Ser., No. 102, 65-72.
Hancock, J.W. and MacKenzie, A.C. (1976). On the mechanism of ductile failure in
high-strength steels subjected to multi-axial stress-states. / . Mech & Phys. Solids.,
Vol 24, 147-169.
Harding, J. (1969). The effect of grain size and strain-rate on the lower yield stress
of pure iron at 288°K. Acta Met., Vol. 17, 949-958.
Nagata, N., Yoshida, S. and Sekino, Y. (1970). Strain-rate, temperature and grain
size dependence of the lower yield stress of polycrystalline iron. Japan Iron and
Steel Institute, vol 10, 173-180.
WS2C7

IMPACT TENSILE PROPERTIES OF SUPER FIBER YARNS

T. KINARI. A. HOJO. S. SHINTAKU and N. IWAKI

Faculty of Technology, Kanazawa University

2-40-20, Kodatsuno, Kanazawa, Japan

ABSTRACT

A new i m p a c t t e n s i l e t e s t i n g a p p a r a t u s b a s e d on the o n e - d i m e n s i o n a l
e l a s t i c - s t r e s s - w a v e s theory has been d e v e l o p e d . It is m a i n l y composed
of an input bar to t r a n s m i t load to the s p e c i m e n and to m e a s u r e d y n a m i c
e l o n g a t i o n of the s p e c i m e n , a pair of load c e l l s to m e a s u r e the load of
the specimen and a striker energized by compressed air. It is designed to
i n v e s t i g a t e d y n a m i c m e c h a n i c a l p r o p e r t i e s of super fiber yarns, such as
aramid fiber and carbon fiber that have small breaking elongation compared
with most synthetic fibers. Using this apparatus and an universal testing
machine, s t r e s s - s t r a i n c u r v e s of several kinds of aramid fiber y a r n s and
a carbon fiber yarn are o b t a i n e d at the strain rates ranging from 1 0 " 8 / s
to lO'/s.

KEYWORDS

Impact test; super fiber yarn; stress-strain curve; stress waves; aramid
fiber; carbon fiber

INTRODUCTION

Super fibers typified by aramid fiber and carbon fiber have been known as
high s t r e n g t h and h i g h e l a s t i c m o d u l u s m a t e r i a l s . They are used in
various ways, such as reinforcement in composite m a t e r i a l s and are often
s u b j e c t e d to impact load. T h e r e f o r e it is important to c l a r i f y their
dynamic mechanical properties. Impact t e s t i n g a p p a r a t u s e s s u c h as
r o t a t i n g d i s c (Stone et al., 1955, S m i t h et al., 1 9 5 9 ) , f a l l i n g weight
(Lyons, 1963) and p n e u m a t i c a p p a r a t u s (Freestone et al.. 1972) were used
to o b t a i n the s t r e s s - s t r a i n c u r v e s of s e v e r a l k i n d s of y a r n s i n c l u d i n g
Nomex, g l a s s and m e t a l l i c y a r n s at the s t r a i n r a t e s up to 1 0 2 / s .
Relatively long specimen was used in these tests. Another technique would
be r e q u i r e d for impact t e s t i n g of the y a r n s w h i c h had s m a l l b r e a k i n g
e l o n g a t i o n such as super fiber yarn at further strain rates. An impact
t e n s i l e t e s t i n g a p p a r a t u s h a s b e e n d e v e l o p e d in o r d e r to o b t a i n the

331
332

W
BB ■
DM PA
££.
IB:Intput bar ST:Striker AG:Air gun GV,GL:Strain gauge
LC:Load cell YS:Yarn specimen SV:Solenoid Valve BB:Bridge Box
PA:Strain meter DM:Digital memory PCiPersonal computer

Fig.l Schematic diagram of testing apparatus.

d y n a m i c s t r e s s - s t r a i n c u r v e s of high s t r e n g t h and high e l a s t i c m o d u l u s

yarn (Kinari et al., 19 90). In this device the elongation of the specimen
is o b t a i n e d from the ai n a l y s i s of s t r e s s w a v e s in the bar and the load
induced in the specimen is measured by a cantilever type load cell. Using
this a p p a r a t u s , stress strain c u r v e s of K e v l a r 2 9 yarn were o b t a i n e d at
several strain rates up to 10*/s. However, it was hard for that apparatus
to o b t a i n an exact rec tangular incident p u l s e and to m e a s u r e large load
m o r e than 100N from it s s t r u c t u r a l limitation. In this i n v e s t i g a t i o n ,
therefore, a new appar atus which has simple c o n s t r u c t i o n and w h o s e load
cell has more rigidity is developed. Stress-strain curves of super fiber
yarns including aramid fiber yarns and a carbon fiber yarn are obtained at
the strain rates rangin g from K T ' / s to 10*/s.

IMPACT TESTING APPARATUS

Figure 1 shows the schematic diagram of the e x p e r i m e n t a l a p p a r a t u s . It

is composed of the input bar IB which transmits the load to specimen, two
load cells LC to measure the tensile load induced in the yarn specimen YS
and the striker ST which is accelerated by the air gun AG and hits IB to
generate the incident wave. IB consists of steel rod 20mm in diameter and
LiB=1000mm in length. ST consists of the same steel rod and its length is
chosen e i t h e r L 8 T = 3 0 0 m m or L S T = 1 0 0 0 m m a c c o r d i n g to the r e q u i r e d impact
velocity. The d e t a i l s and d i m e n s i o n s of LC and YS are shown in Fig. 2.

(a) Top-view (b)Side-view

Fig. 2 Details and dimensions of load cells and yarn

specimen. WG:Wedge-shaped gripping attachment
 333
The external corners of IB are slightly rounded to come in contact with YS
smoothly. LC has a tapered hole to grip YS. T h e yarn s p e c i m e n YS is
p l a c e d b e t w e e n a pair of load c e l l s t h r o u g h the right end of IB using
w e d g e - s h a p e d gripping a t t a c h m e n t s WG. YS makes an angle of 0 = 1 1 . 5 ' to
loading d i r e c t i o n , so the load induced in the s p e c i m e n is m e a s u r e d by a
pair of load cells LC. Gauge length of YS is 50mm at each side and its
elongation may be 0.980mm when IB moves 1mm rightward. Two semiconductor
s t r a i n g a u g e s GL a r e b o n d e d near the fixed end of LC. The natural
f r e q u e n c i e s of LC exceed 100kHz. It can be considered that there is no
effect of its natural frequencies on the load-time curves. The applied
load in this tests is so small that its o w n d i s p l a c e m e n t is n e g l i g i b l e .
The load cell is calibrated by static loads.

The stress waves in IB is measured by the wire strain gauge GV bonded at

the distance of X=600mm. Analyzing these stress waves on the basis of the
one-dimensional elastic-stress-waves theory, the elongation of specimen is
obtained as follows. A striker ST flies at the velocity 2V 0 and hits IB
as i l l u s t r a t e d s c h e m a t i c a l l y in F i g . 3 . As ST and IB have equal cross
s e c t i o n a l a r e a s a n d a r e t h e s a m e m a t e r i a l , t h e a m p l i t u d e of t h e
compressive stress generated in IB is

o o = E •V./ c (1)

and compressive stress of same amplitude is also generated in ST. Where c

is the velocity of the longitudinal waves and E is Young's m o d u l u s of IB
and ST. The compressive stress propagating in ST is reflected as tensile
stress - a o at its left end. This tensile stress propagates eliminating
the initial compressive stress in ST and transmits to IB. As a result, a
rectangular compressive pulse whose amplitude is o 0 and duration is 2 L S T /
c propagates in IB as an incident wave a i(t). This pulse is reflected
at the right end of IB as a t e n s i l e pulse of same a m p l i t u d e b e c a u s e the
load of yarn specimen is enough small. Consequently, the velocity of the
right end of IB Vi(t) and the elongation of specimen X (t) are obtained as
follows.

(Jo, Vo Cfc.Vo

0>,-Vo Ob.-V,
Fig.3 Stress waves p r o p a g a t i n g in input bar.
334
V i(t)= 2 a ,(t)-c/E (2)

X (t) - c o s ^ J V , ( t ) dt = c o s 0 «(2- c / E ) S o , (t) dt (3)

In the case of L S T = L I B = 1000mm, reflected waves in each bar just meet at

the contact face and both waves compensate each other. The right end of
IB, therefore, continuously moves at 2V 0 .

The resultant signals obtained from GV and GL are taken into a personal
computer PC (NEC PC9801) through bridge boxes BB, pre-amplifiers PA (Kyowa
E l e c t r o n i c Instruments Co.Ltd. C D V - 2 3 0 C ) and multi digital r e c o r d e r DM
(Iwatsu Co.Ltd. DM7100), and performed several kinds of operations. The
recorder used has a distortionless frequency response up to 250kHz.

200
TIME(HS) «»
(a)

100 150
TIME(HS)
(b)
Fig.4 Typical resuls at impact tests for Kevlar49 yarn.
(a):Measured stress waves (solid line) and calculated
result (broken line).
(b):Elongation-time curve (broken line) and load-time
curves at strain rate of 3 . 9 x l 0 2 / s . Loads are
measured by two load cells at one experiment, one
is shown by solid line and the other is shown by
dash-dotted line.
 335
Tabel 1. Yarns used in this investigation

Sample number Material

Linear Dens ity Sectional area
(tex) (mm 2 )
I Kevlar 29 166. 7 0. 1158
n Kevlar 49 127. 7 0.0881
in Kevlar 149 157. 8 0. 1073
IV Carbon fiber 211. 1 0. 1173
*: Calculated value assuming specific g r a v i t i e s o f I , n ,flland IV are
1. 44. 1.45. 1.47 and 1.80.

EXPERIMENTAL RESULTS AND DISCUSSION

In o r d e r to o b t a i n s t r e s s - s t r a i n c u r v e s , t e n s i l e tests were p e r f o r m e d .
Experiments were performed under 20*C, 65%RH. Yarn specimens investigated
are listed in Table 1. Curves at strain rates below 1/s are obtained by
the same load cells and an universal testing machine (Kinari et al., 1990).
In F i g . 4 ( a ) the o b s e r v e d and p r e d i c t e d s t r e s s w a v e s at the point G in
Fig. 3 are shown by solid and broken lines respectively for Kevlar49 yarn.
Both waves agree almost so it is proved that the right end of IB can be
regarded as free. In Fig.4(b) the X - time curve by means of eq. (3) for
F i g . 4 ( a ) is shown by a broken line. L o a d - t i m e c u r v e s m e a s u r e d by two
load cells are also shown by a solid line and a dash-dotted line. Both
curves almost agree. Plotting the load as a function of the elongation
at each time, stress-strain curve is obtained. Stress-strain curves at
strain rates r a n g i n g from 3 . 3 x l 0 ~ 3 / s to 3 . 9 x l 0 2 / s are shown in F i g . 5 .
Curves are almost straight and show little yielding phenomena. Comparing
these curves, it is o b v i o u s that the higher strain rate curve has higher
s t r e s s at the same s t r a i n . M e c h a n i c a l p r o p e r t i e s o b t a i n e d for o t h e r
investigated materials are also shown in Table 2. The elastic modulus M
increases with increasing strain rates. The breaking e l o n g a t i o n L
d e c r e a s e s with strain rates. T h e b r e a k i n g s t r e s s N d o e s not show
remarkable influence by strain rates. Stress-strain relations of super
fiber yarns tested in this i n v e s t i g a t i o n are almost linear and it can be
considered that they show viscoelastic behavior.

2.0 3.0
STRAIN (•/•)
Fig. 5 Stress-strain curves at strain rates ranging
from 3 . 3 x l O " V s to 3 . 9 x l 0 2 / s in Kevlar49 yarn.
336

Table 2. Mechanical properties obtained by experiments

Sample Strain rate (1/s)

Propert ies
number 3. 3 x 1 0 " ' 3. 3 x 1 0 " 2 3 . 3 X 1 0 ' 1 4 . 4 X 10 1 4. 0 X 1 0 2

M (N/tex) 40 40 43 58 58
I N (N/tex) 1. 6 1. 6 1. 6 2.0 1.8
L (%) 4. 1 4. 1 3.8 3. 4 3. 1
M (N/tex) 86 91 100 102 104
n N (N/tex) 2.0 2.0 1.9 2.3 1.8
L (%) 2. 3 2. 2 1. 9 2. 2 2.0
M (N/tex) 80 84 90 87 92
in N (N/tex) 1.4 1. 4 1. 3 2.0 1. 7
L (%) 1. 6 1. 6 1.5 2.4 2.0
M(N/tex) 64 67 73 89 78
IV N (N/tex) 0. 9 1.0 1.0 1.0 0. 9
L (%) 1.4 1. 4 1. 4 1. 1 1. 1

M:Elastic Modulus N:Breaking Stress L:Breaking Elongation

CONCLUSION

An i m p a c t t e n s i l e t e s t i n g a p p a r a t u s b a s e d o n t h e o n e - d i m e n s i o n a l
elastic-stress-waves theory has been developed. In this apparatus, the
e l o n g a t i o n of the s p e c i m e n is o b t a i n e d from a n a l y s i s of t h e i n c i d e n t
stress wave and the load induced in the specimen is measured by a pair of
load c e l l s . O b s e r v e d s t r e s s w a v e s in the input b a r a g r e e d w i t h the
one-dimensional waves theory prediction. Therefore the validity of this
technique was ascertained. Using this apparatus and an universal testing
machine, s t r e s s - s t r a i n curves at the strain rates ranging from 10"*/s to
10*/s were obtained for aramid fiber yarns and carbon fiber yarn. These
curves showed that there were consistent increase in the elastic modulus
with increasing strain rates, the breaking loads were almost constant at
any strain rate and the b r e a k i n g e l o n g a t i o n s d e c r e a s e d with i n c r e a s i n g
strain rates.

The authors wish to thank Prof.Chatani for his helpful advice.

REFERENCES

F r e e s t o n , W . D . , M . M . P l a t t and R . J . C o s k r e n ( 1 9 7 2 ) . The stress-strain

response of yarn at high rates of loading. J. Text. Inst., 63, T239-262
Kinari.T., A. Hojo, A.Chatani, S.Shintaku and I.Arai (1990). An impact
tensile testing apparatus for yarn and mechanical p r o p e r t i e s of aramid
fiber yarn at high strain rate. Proceedings of 33rd Japan congress on
Materials Research., 87-91.
Lyons,W.J. (1963). In:Impact phenomenon in textiles, M. I.T.press, Cambridge.
Smith. J.C., F. L. McCrackin, H. F. Schiefer, W. K. Stone and K.M.Towne (1956).
Stress-strain relationships in yarns subjected to rapid impact loading :
Part IV transverse impact tests. Text. Res. J. . 26., 821-828
Stone, W. K. , H.F.Schiefer and G. Fox (1955). Stress-strain relationships in
y a r n s s u b j e c t e d to r a p i d impact l o a d i n g : Part I e q u i p m e n t , t e s t i n g
procedure, and typical results. Text. Res. J., 25, 520-528
WS2c8
AN ANALYSIS OF EARLY TIME DEFORMATION RATE AND STRESS
IN THE TAYLOR IMPACT TEST

by

John D. Cinnamon, S. E. Jones

U.S. Air Force Academy, CO 80840

Joseph C. Foster, Jr.

AFATL, Eglin AFB, FL 32542

and

Peter P. Gillis
University of Kentucky, Lexington, KY 40506

ABSTRACT

The Taylor impact test is analyzed using ultra-high-speed photographic data to obtain stress vs. strain-rate results.

INTRODUCTION

Jones, et al. (1987), introduced a new equation of motion for the undeformed section of a Taylor Impact
Specimen.
fiv + B ( v - u ) = o / [ p ( 1 + e ) ] (1)

In this equation, elastic effects have been neglected entirely; & is the current undeformed section length, v is
the current velocity of the undeformed section, u is the particle velocity of the material on the plastic side of
the wave front, e is the engineering strain on the plastic side of the wave front, and P is the specimen density
(assumed constant) (see Figure 1). The presence of the relative velocity term in equation (1) has some far reaching
implications.
Jones, et al. (1990), divided the impact event into two
phases. The first phase was early-time mushrooming in which
<— C M the plastic wave front motion and resulting stress are nonlinear
with respect to time. The second phase was characterized by

I-.-I
A steady motion of the plastic wave front and comprised the
A considerable balance of the event. The elementary theory was
later applied by Cinnamon, etal. (1990), to construct dynamic
I yield stress curves for several materials. The strain-rates for
A the reported data ranged from 10 3 to 10 s per second. It
A I was noted that each two-phase analysis of a Taylor Test
H I produced a stress vs. strain-rate curve during early time
A deformation, rather than the single data point typically
reported by other techniques. The utility of this result is
A<
obvious. However, all the conclusions were based upon an
elementary assumption of a cylindrical volume representing
Figure 1. Impact Geometry of Deformed the geometry of the mushrooming region. Although all the
and Undeformed Specimen. conclusions agreed with data independently reported by
several researchers, the use of this geometry posed some questions. The purpose of this paper is to modify the
elementary cylindrical approximation to a conical frustrum and to note that there are only minor deviations from
the earlier results.

337
338
THEORY

As indicated by House (1989), the undeformed section of the specimen loses little or no speed during the initial
deformation phase. Hence, during this phase equation (1) becomes:

fi(v0 - u ) = o / [ p ( 1 + e ) ] (2)
This equation leads to an estimate for stress during phase one:

o = - p (u + h)(v 0 - u ) (3)

The time-dependent strain can be shown to have the form:

e = - ( v 0 - u ) / ( v 0 + h) (4)

where
e=(r02/r2)-1 (5)

and r is the radius of the plastic material behind the wave front while r 0 is the undeformed section radius.
These equations indicate that the dynamic stress, strain, and strain-rate behind the plastic wave front can be
found, provided that the particle velocity u , the plastic wave speed dh/dt , and the strain e behind the wave
front can be determined.
From Jones, et al. (1990), the position of the plastic wave front can be approximated by a power function:

h = h0 t n (6)

where h 0 is a constant and n is a constant exponent with 0 < n < 1. Conditions at impact allow n to be
estimated by:

n=(1-u0/v0j (7)

where u 0 is the initial particle velocity, estimated through elementary shock physics (see House (1989)). For
OFHC copper rods and aluminum rods impacting a 4340 steel anvil, n = 0.5 and n = 0.7 respectively.
Data from film records of the rod impact (see Wilson, et al. (1989)) indicate that the radial growth curve for
the mushroom r m = r m (t) can be well approximated by a power function of t with the same exponent
as h. See Figures 2 and 3. r m (t) = r 0 + b h(t)
 339
The volume in the plastic mushrooming region, V m can be estimated by assuming that the region is a conical
frustrum with base radius r m and upper radius r 0 (see Figure 4).

Vm = (1/3)^h(rm2+rmr0+r02 ) (8)

Since h, r m / and therefore, "m can all be approximated by power functions, it is reasonable to
assume that r in (5) is of a similiar form:

r=r(t) = r 0 + a t m (9)

where a is constant and m is a constant exponent. By substituting (9) into (5) and combining the result with
(4) and (6), we get the time-dependent particle velocity u.

u = v0 - ( 2 a r 0 t m + a2 t2 m
) (v0 + nh0 t " - » ) (r0 + at m )" 2 {10)

In order for the particle velocity to tend toward a finite non-zero value at impact (t = 0) , we require:
m + n=1 CM)

and

a = r0 (v0 - u 0 ) (2nh0 )"' = r0 v0 / (2h 0 ) (12)

This determines the power function r in terms of the

plastic wave front data in (6). The constant h0 is
determined by a "best fit" to the experimental film
data.
r
Because -> r o for t > 0, there is a
strain discontinuity across the plastic wave front. This
discontinuity is characteristic of rigid-plastic analysis,
on which this theory has been developed. Since the
strain does not proceed to zero as we cross the plastic
interface (because elastic effects are ignored), it
represents artifact of the analysis rather than a physical
variable to which some meaning is attached. However,
the rate at which this quantity is changing (i.e.
strain-rate) is a meaningful, physical variable.
Before examining the stress, strain rate results of this
modified theory, it is interesting to look at some
Figure 4. Idealized Mushroom Geometry:
kinematical results. The radial growth curve predicted
Phase I Deformation.
by the conical frustrum geometry can be used to force
the theoretical volume to match film data. However,
the corresponding »"m (t) is low in comparison to the film data. Theoretical volume is calculated
using (8) with r replacing r 0 . Because of the discontinuity between r andr 0 , r m ( t ) is forced
low to preserve the correct volume in the mushroom. However, agreement between r m (t) and
experimental data is much better than was achieved by the cylindrical geometry in Jones, et al.
(1990). (See Figures 5-8). It should be noted here that the analyses of JG-30 and JG-88 represent the
best and worst results of the modified theory respectively.
340

Time (*/« ) e <»"•

o F im
l - m(
V t) Fm,l v-m ( l, Q
Figur
e7 Volume of the Mushroo m v. Time . e8 Volum
e oFigur
f the Mushroo m v. Time
.
JG-0
3 ( O FCHCopper . A s - R e .c ) 8 ( 6 0 6 16- TAl ). JG-8

RESULTS AND CONCLUSIONS

Applying this conical frustrum analysis for the mushrooming region, slightly different stress versus strain-rate
results were obtained than from the cylindrical geometry in Cinnamon, et al. (1990).
The solution technique utilized to obtain the present results involved beginning with acurate film data
concerning the deformation event (see House (1989) and Wilson, et al. (1989)). In view of (7), h 0 can be
adjusted in equation (6) to obtain a best fit to the film data. At this point, the volume from the film data can be
calculated with (8). Using (7), (9), (11), and (12) allows the r (t) curve to be determined. Although not
crucial to the analysis here, the theoretical volume can be calculated and forced to fit the film data volume curve
by changing b and lowering the r m (t) curve accordingly. In any case, with r (t), the time-dependent
strain and particle velocity follow from (5) and (4) respectively. The stress and strain-rate over time can then
be generated through (3) and numerical differentiation of (5).
The strain, particle velocity, stress, and strain-rate curves versus time are of the same character as those
appearing in Jones, et al. (1990) and Cinnamon, et al. (1990). As noted there, the first two microseconds of the
event are not accurately predicted by this analysis. Therefore, this regime is ignored as a mathematical artifact
and the examination focuses on the data from 2 MS to the end of phase I (about 5 or 10 /us ). It is
for this reason that the inverted geometry in Figure 6 does not significantly impact our findings.
The yield stress versus strain-rate for four materials are presented in figures 9-12.
 341

L o g fo the Strai n Rat e

Log of the Strain Rat e
- T h e ovr Johnso n ( 1 9 8 3: ) • = . 1: +. • - 2 0:
- T h e oyr FoUansbee . et *J. ( 1 9 8 :8 ) e ' .06
: +. e = .16: O
FoUansbe e ( 1 9 8 6: ) ■ - . :1 A. • - 2: V
Figur e 10. Yiel
d Stress v. Log of the Strai n Rate .
Figure 9. Yiel
d Stres s v. Log of the Strai n Rat e
JG - 3 4. ( O FCH Cop
JG - 3 0. ( O F CH Copper . A s - R e.c )

These results do not differ dramatically from Cinnamon, et al. (1990), but do represent an improvement in
both the model of the deformation geometry and in the character of the yield stress vs. strain-rate curves.
The two-phase analysis presented in Jones, et al. (1990), Cinnamon, et al. (1990), and in this paper allows
the yield stress curve for high strain-rate deformation of the impacting material to be generated from one Taylor
Test. These curves compare favorably to previously published data points obtained by independent investigators
using other experimental techniques.

Log of the Strain-Rat e

- T h e ovr A F ALT I - . 0 10: . Sierakowski . et al. ( 1 9 8 0
: )i Log of the Strai
n -Rat e
Yield Stres s v. Log of the Strain Rate . - T h e oyr A F A T: Le= . 2. O
).
J G 8 .6 ( 2 0 2 4 - TI4 A Yield Stress v. Log of the Strain-Rate
.
J G - 8.8 ( 6 0 6 1 - T 6.A I )

REFERENCES

AFATL Data (Instron and Split Hopkinson Bar), unpublished.

Cinnamon, J. D.; Jones, S. E.; House, J. W.; and Wilson, L. L. (1990). "Dynamic Yield Strength Estimates
at High Strain-Rates Using the Taylor Impact Test" (submitted for publication).

FoUansbee, P.S. (1986). "High-Strain-Rate Deformation of FCC Metals and Alloys," in Metallurgical
Applications of Shock-Wave and High-Strain-Rate Phenomena, L.E. Murr et al. eds. (1986). Marcel
Dekker: New York.
342
Follansbee, P. S.; and Kocks, U. F. (1988). "A Constitutive Description of the Deformation of Copper Based
on the Use of Mechanical Threshold Stress as a Internal State Variable," Act MetalL, 36, 81.

House, J. W. (1989). "Taylor Impact Testing," AFATL-TR-89-41.

Johnson, G. R. (1983). "Development of Strength and Fracture Models for Computations Involving Severe
Dynamic Loading," AFATL-TR-83-05.

Jones, S. E.; Gillis, P. P.; Foster, J. C , Jr.; (1987). "On the Equation of Motion of the Undeformed Section
of a Taylor Impact Specimen," /. Appl. Phys., 61, 499.

Jones, S. E.; Gillis, P. P.; Foster, J. C , Jr.; and Wilson, L. L. (1990). "An Elementary Two-Phase Flow Model
for Taylor Impact Specimen," (to appear in the ASME J. Engng Materials Tbch.)

Sierakowski, R. L.; Malvem, L. E.; and Ross, C. E. (1980). "Compression Testing of Metals at Elevated
Temperatures," AFATL-TR-80-76.

Wilson, L. L.; House, J. W.; and Nixon, M. E. (1989). "Time Resolvable Deformation from the
Cylinder Impact Test," AFATL-TR-89-76.
WS2c9

HIGH STRAIN-RATE MATERIAL BEHAVIOR USING

TAYLOR ANVIL EXPERIMENTS

by

Joel W. House, Leonard L. Wilson and Michael E. Nixon

United States Air Force Armament Laboratory/MNW,
Eglin AFB, Florida, USA, 32542-5434

ABSTRACT

Taylor anvil tests are used to study the dynamic properties of materials. This paper reports the
application of high speed photography to record the deformation of OFHC copper during impact.
The film data was analyzed and compared with a numerical simulation. The comparison showed
good agreement between the experimental data and results obtained using the continuum model
EPIC-2.

KEYWORDS

Taylor anvil test; dynamic strength; OFHC copper, dynamic plasticity; continuum models.

INTRODUCTION

In the 1940,s, G.I. Taylor (1948) developed an experimental technique and analysis for char-
acterizing material behavior under high strain-rate conditions. This technique for characterizing
material behavior produced high strain-rate flow strength data, also called the "dynamic strength."
Taylor proposed to determine the dynamic strength by launching the material as a plane-ended
cylindrical projectile towards a rigid target. His analysis of the impact event was dependent on
several assumptions regarding material behavior and the use of postmortem specimen geometry.

To determine the dynamic strength, Taylor makes the following assumptions: (1) the material
behavior could be modeled as rigid-plastic, (2) radial inertia effects could be ignored, and (3)
the plastic wave front moved at a constant velocity. The latter allows the use of postmortem
measurements of the plastic wave front position to determine the entire wave front history. These
assumptions and the use of postmortem geometry classify the results as a first approximation
for characterizing high strain-rate material behavior.

In more recent years, investigators have used final geometry of Taylor anvil specimens to evaluate
the success of constitutive relationships embedded within continuum models (Johnson and Cook,
1983, Johnson and Holmquist, 1988). In this application of the Taylor test, the investigator is
seeking to test the capability of a material model under the conditions of high strain-rate and
multi-axial stress.

343
344
One example of a constitutive equation is the Johnson-Cook (1983) strength relationship.
This equation gives the following

CT = [A +Ben] [1 +C \ne] [1 -0>M] Equation (1)

where
c = Equivalent Flow Strength
e = Equivalent Strain
e = Dimensionless Strain-Rate
<J> = Temperature Factor
A, B, C, n, m = Material Constants

The first quantity in brackets on theright-handside of the equation represents parabolic work
hardening of a material. The second quantity adjusts the flow strength of the material for the
influence of strain-rate, and the third for temperature effects. The material constants embedded
within the algorithm are determined by laboratory experiments, such as, tensile tests, split
hopkinson bar tests and similar experiments carried out at elevated temperature, for more details
on this procedure see Johnson and Cook (1983).

The constitutive relationship is evaluated by simulating the deformation during the impact event.
The predicted geometry of the model can then be compared with that measured from an actual
specimen. The purpose of the comparison is to assess a particular material model in the regime
of strain, strain-rate, and stress produced during a Taylor test. Johnson and Holmquist (1988)
adopted this approach to evaluate material constants in the Johnson-Cook model.

Figure 1 shows the results of a calculation using the Johnson-Cook model in the program EPIC-2.
The material constants were chosen for Oxygen Free High Conductivity (OFHC) Copper in the
annealed condition. The specimen in the center of Fig. 1 was tested in the cold worked condition.
The specimen on the right was annealed one hour at 600 °C in a vacuum before testing. Both
specimens struck the target with equal kinetic energy.

In the one-dimensional analysis and in the comparison studies using the continuum models,
investigators have been limited by the use of only postmortem specimen geometry. One method
for improving the results of both types of analysis is by employing time resolvable data of the
material behavior, e.g., the motion of the plastic wave front with respect to time.

H h

(a) (b) (C)

Fig. 1. Comparison of final profile geometry of OFHC copper

specimens; (a) EPIC-2, (b) as received, (c) annealed.
 345
This type of experimental data was generated in a test matrix to study the behavior of OFHC
copper. The impact event was recorded using a Cordon 330A high speed framing camera. The
camera was operated at a frame rate of 300,000 and 1.0 million frames per second. These frame
rates produce a time resolution in the data of 3.3 and 1 |is, respectively.

Specimens used in this investigation were machined from drawn rods of OFHC copper. All of
the specimens were 7.595 mm (0.299 inch) in diameter. The specimen length was either 38.1mm
(1.5 inch) or 57.15 mm (2.25 inch) which produced an aspect ratio of 5 or 7.5, respectively.
Some of the specimens were annealed at 600° C for one hour in a vacuum.

This paper describes the experimental technique and data reduction. Results from the experiment
will be discussed and compared with an analysis using the continuum model program EPIC-2.

EXPERIMENTAL TECHNIQUE

A caliber 30 Mann barrel was used to launch the projectile toward a massive cylinder of hardened
4340 steel (Re 57). The gun tube was designed to accommodate the use of gun powder propellant.
Specific quantities of propellant can be used to launch a variety of projectiles with different
masses, over a range of velocities from 0.1 to 1 km/s. In this study the impact velocities ranged
from 176 to 227 m/s.

The test was instrumented with a series of laser beams which detect the position of the projectile.
By monitoring the output voltage of two laser beam detector circuits, a muzzle velocity can be
determined. In addition, the laser beam circuit was used as a synchronization device with the
high speed camera.

The record of the impact event was produced using shadow-graphic photography. The camera
and light source were placed on opposite sides of the projectile line of flight, see Fig. 2. The
silhouette of objects in the field of view, i.e, the target, specimen, fiducials, etc., were recorded
on Kodak's TMAX film (ASA 3200). Figure 3 shows a select sequence of images from test
JG-34. These images were generated at a frame rate of 1.0 million per second.

Fig. 2. Photographic configuration.

346

r =-10.0|as r = 5.0|xs

t = -5.0ns r = 10.0^s

r = -1.0|as r = 15.0^s

f = 0.0^s t = 20.0\is

Fig. 3. Selected sequence of images from test JG-34.

The Cordon 330A is classified as a continuous writing rotating mirror camera. This type of
camera requires that the test be conducted in a darkened room. Prior to triggering the firing
circuit, the mirror within the camera is brought up to the desired writing speed. The writing
speed of the camera is controlled by a gas turbine which shares a common axis with the rotating
mirror. Increasing the gas pressure to the turbine increases the writing speed of the camera. The
difficulty of operating a continuous access camera is synchronizing the event with the source of
illumination.

In these experiments, it was desirable to illuminate the field of view just before impact and to
terminate illumination before one full revolution of the rotating mirror had occurred. If the
illumination time of the light source exceeds the mirror period of the camera, the film record
will be double exposed. As stated above, the laser detector circuit also functions as a triggering
device for the light source. When the laser beam is interrupted by the projectile, the light source
provides the necessary illumination at the predetermined time and duration. The delay time,
between breaking the laser beam and illuminating the field of view, is determined by factors
such as camera writing speed, projectile velocities, and the number of pre-impact exposure
desired. Pre-impact data is necessary for verifying the projectile velocity and the precise moment
of impact, see Fig. 3.

The film images are analyzed by making spatial measurements. For example, the distance from
the leading edge of the projectile to the target provides information on the projectile velocity.
After impact, data is generated on the motion of the plastic wave front, and the diameter of the
specimen at the target and specimen interface.
 347
RESULTS

Data from the test matrix used in this investigation are given in Table 1. During test UK-145,
the camera was operated at a writing speed of 300,000 frames per second. This writing speed
provided a sufficient window of time to record the entire history of the deformation of the rod.
During the remaining tests, the camera was operated at a 1.0 million frames per second. For
these tests, only the first 20-25 |is of the event were analyzed.

Table 1. Test Matrix

Test # Impact Aspect Final Final Undeformed Frame Material
Velocity Ratio Length Diameter Length Rate Condition
m/s L/D mm mm mm million

UK-145 189 7.5 41.66 14.73 16.31 0.3 Half Hard

JG-30 176 7.5 42.9 13.72 25.15 1.0 Half Hard

JG-32 200 5.0 27.74 14.73 17.35 1.0 Half Hard

JG-34 204 7.5 37.01 11.68 1.0 Annealed

JG-38 227 5.0 22.48 14.48 1.0 Annealed

Figures 4-6 show the results of the plastic wave position and the mushroom diameter
measurements. The time between data points in Figs. 4 and 5 is 1 |is. In Fig. 6, the time resolution
is 3.3 |is.

These figures show a distinct similarity in the behavior of the copper rods. The results from
mushroom diameter measurements show that rapid radial motion occurs during the initial stage
of deformation, 0-10 us. This stage is followed by a period of deformation with a much lower
stain-rate. Figure 6 shows that for an as received specimen with an aspect ratio of 7.5, the growth
of the mushroom was completed by 40 (is into the event. The time resolved data cannot dis-
criminate any differences in the formation process of the mushroom for the two types of copper.
However, a postmortem analysis shows that cold worked copper generates a larger mushroom
diameter than does annealed copper for equal energy impacts, see Table 1 and Fig. 1. Similar
in character to the mushroom data, the plastic wave motion show no distinguishing differences
between annealed and cold worked copper material.

Test: J G - 3 0 . J G - 32
Material: OFHC Copper
Condition: As Received (Half Hard)
Position vs Time

Plastic Wave Front

» JG-30 Plastic Wove Front

• JG-30 Interface Diameter
" JG-32 Plastic Wove Front
• JG-32 Interface Diameter

Fig. 4. Experimental data for as received OFHC copper.

348

Test: J G - 3 4. J G - 38
Moteriol: OFHC Copper
Condition: Annealed
Position va Time

% 1.50 :
E

• ■»**

Plastic Wove Front

■ • « ■'

.....JG-34 Plastic Wave Front

.....JG-34 Interface Diameter
JG-38 Plastic Wove Front
■ ■■••JG-3B Interface Diameter

' io.bb 26.00 io.'ob 4

Time, (ju)

Fig. 5. Experimental data for annealed OFHC copper.

I Moteriol: OFHC Copper ( L / D - 7.5)

" ~ - ■ (Holf Hard)

■§3.0

Plastic Wave Front

. . . . U K - 1 4 5 Plastic Wove Front

• • • • U K - 1 4 5 Interface Diometer
Post Impact Measurement

100.00 150.00
Time.Qjs)

Fig. 6. Experimental data from test UK-145.

Both materials show an initial rapid wave which last 9-10 |xs into the event. This stage of
deformation is followed by a period of relatively constant wave motion. Figure 6 shows that for
the as received specimen in test UK-145, the plastic wave motion was completed at about 127p.s
after impact.

Figure 7 shows a comparison between the experimental data, shown in Figs. 4-6, and that pro-
duced by the program EPIC-2. The mushroom growth data was produced by storing the position
history of the free surface specimen node that is located at the specimen and target interface. In
this calculation a single slide line was used between the specimen and the target. The slide line
allows the projectile and target to exchange momentum and to have relative motion while
maintaining a distinct interface. No frictional effects were considered for this analysis.

The results of the comparison show aremarkablygood agreement between the data for cold
work copper and that produced by the continuum model. The comparison is not as favorable
with the annealed material, but is still reasonable considering that frictional effects have been
ignored.

The position of the plastic wave front motion was generated by an algorithm associated with
radial displacement of nodes along the free surface of the rod. When the current radial position
of the node at or near the plastic wave front exceeded a specific amount, then it is assumed that
the plastic wave hadreachedthat point on the free surface of the rod. This criteria was used to
establish a position history of the plastic wave as it moved towards thefree-endof the rod.
 349
4.00 -T 1

T j Test: U K - 1 4 5. J G - 3 0 . J G - 3 2 . J G - 3 4 . J G - 3 8
j i, j Material: OFHC Copper
H Position vs Time

% 3.00 H
E 1
■5 i Plastic Wave Front

Time.Ou)

Fig. 7. Comparison of time resolvable measurements with the

EPIC simulation.

The continuum model is in excellent agreement with the experimentally observed position of
the plastic wave front for the first 15-18 |is. The models then predicts an increase in the plastic
wave speed which is not observed experimentally. After this increase in velocity, the model
predicts that the wave speed decreases to a constant level. This velocity is maintained for the
remainder of the event. The predicted velocity of the plastic wave front in this later phase is in
good agreement with the experiment.

CONCLUSIONS

An experimental technique has been developed to make time resolvable measurements of the
deformation of material using Taylor anvil tests. Tests conducted using OFHC copper in both
cold worked and annealed conditions show no difference in the early time behavior of the
deforming rod material. A simulation using the Johnson-Cook strength relationship in the
continuum mechanics program EPIC-2 was in good agreement with the experiment. The ana-
lytical model did predict a period of increased plastic wave front velocity which was not observed
in the experimental data.
Taylor anvil experiments are well suited for analysis by continuum models because of the rel-
atively simple part geometry and boundary conditions. Time resolvable studies of the experiment
provides a unique opportunity to study material behavior under conditions of high strain-rate
and multi-axial states of stress. A comparison between the time resolvable data and continuum
model is useful for assessing the validity of constitutive relationships under the conditions
observed during the experiment.

REFERENCES
Johnson, G.R. and W. Cook (1983). In: Proceedings of the Seventh International Symposium
on Ballistics, The Hague, The Netherlands, 541-547.
Johnson, G.R. and T.J. Holmquist (1988). Evaluation of cylinder-impact test data for consti-
tutive model constants. J. Appl. Phys., 64, 3901-3910.
Taylor, G.I. (1948). The use of flat-ended projectiles for determining dynamic yield stress.
Proc. R. Soc. London, Series A, 194, 289-299.
WS2C10

COMPARISON OF MECHANICAL PROPERTIES IN TENSION AND SHEAR

AT HIGH STRAIN RATE FOR AISI 316 AND ARMCO IRON

C. ALBERTINI, M. MONTAGNANI, E.V. PIZZINATO and A. RODIS

Commission of the European Communities, Joint Research

Centre, Ispra Site, 21020 Ispra (VA), Italy

ABSTRACT

Stress-strain curves up to very high strain rate (3xl04s"1) determined by

shear testing of AISI 316 and ARMCO iron showed large strain at fracture and
saturation of flow stress (no strain hardening) at large strains.

The flow curves in tension showed strain hardening up to fracture.

The different macroscopic response in tension and shear are caused by dif-
ferences in the corresponding microscopic deformation mechanisms.
The flow curves in tension and the equivalent flow curves in shear (e.g. Von
Mises) were not coincident because the classical plasticity model assumes
the same microscopic deformation mechanism at each deformation mode.

KEYWORDS

Tension, shear test, strain rate, equivalent flow curves.

INTRODUCTION

Reliable calculations by finite element codes of rapid metal forming and

penetration of metal shields by missile impact require the knowledge of
material models which describe the response of the unit metal volume up to
large strains, at very high strain rate, under multiaxial loading, taking
into account the different deformation modes and straining paths.

Most of the viscoplastic material models used in the finite element codes
are generalized to multiaxial stress states by means of the yielding crite-
ria of classical plasticity (e.g. Von Mises).

351
352
Such yielding criteria are based on the concept of the unique equivalent
flow curve whatever the deformation mode, presuming that at microscopic
level the deformation mechanism is the same for each deformation mode.

Nevertheless few authors in the far, Ludwik (1925) and recent past, Hecker
et al. (1981), have shown that it is not possible to obtain a unique equiva-
lent flow curve by applying the Von Mises yielding criterion to the tensile
and shear flow curves of the same material (e.g aluminium, copper,
austenitic stainless steels, iron alloys).

Such demonstrations have mainly been performed by deforming the materials at

low strain rate while the present paper extends the comparison to the ten-
sile and shear tests of the austenitic stainless steel AISI 316 performed at
low, medium and high strain rate (e.g. from 10" 3 to 10 3 s " 1 ) .

EXPERIMENTAL PROCEDURE AND ANALYSIS

The tensile tests were performed using the specimen of Fig. 1 tested by
means of a Hounsfield Tensometer at low strain rate (10~3 s" x ), of a hydrop-
neumatic apparatus at medium strain rate (~1 s"1) and a modified Hopkinson
bar at high strain rate (~103 s"1) , described in Albertini et al. (1977).
The tensile specimens were filmed during testing by means of high speed cam-
eras, to record all the parameters needed to characterize the necking zone.

Fig. 1. Tension specimen. Fig. 2. Shear specimen.

The shear tests were performed using the specimens of Fig. 2, where the
gauge part consists of a thin circular crown built up by means of a slight
difference between the outer diameter of the smaller cylindrical part and
the inner diameter of the larger cylindrical part. The detailed development
of the shear specimen has been described by Albertini et al. (1990 a/b).
 353
The actual shear specimen was constructed with a short gauge length
a=0.25 mm, which allows a homogeneous stress distribution along the gauge
length even in the case of very high strain rate. In the case of shear test-
ing the strain rate was increased up to 3x10* s" 1 .

The apparatus for shear testing was the same as that used for the tensile
tests.

The stress-strain-strain rate curves in shear are shown in Fig. 3 and 4 for
AISI 316 and ARMCO iron respectively.

The comparison of the true stress strain curves in tension and of the equiv-
alent stress strain curves obtained from the shear test is shown in Fig. 5
for AISI 316.

In Fig. 5 the parts of the true stress strain curves in tension of AISI 316
traced with discrete points correspond to necking and have been recon-
structed following the analysis of Bridgman (1952) where true stress and
strain are given by (1) and (2):

(JAVO
(1)
(l+2R/a)[ln(l+a/2R)

a A vo = load divided by minimum cross section;

R = radius of curvature of the neck;
a = radius corresponding to the minimum cross section;

(2)
e = 2 in °2
2a

Do = initial diameter of the specimen.

The equivalent stress strain curves in shear of Fig. 5 have been obtained by
calculating the equivalent stress by (3) (Von Mises model),

CTEQV = V ^ T (3)

T = shear stress,

and by calculating the equivalent strain by (4) as suggested by Polakowski

and Ripling (1966),

= i ln[{f^?)+1]
e E Q v = - ^ ln| I V l + — ) + ^ I (4)

y = shear strain.
354
DISCUSSION OF THE RESULTS

The flow curves in shear at low and medium strain rate for AISI 316 and
ARMCO iron (Figs. 3 and 4) show strain hardening up to strain values of
about 2 after which there is saturation of flow stress (zero strain harden-
ing) ; at high strain rate the saturation of flow stress is reached much ear-
lier, at a strain of 1 for AISI 316 and immediately after initial yielding
for ARMCO iron, and is followed by a sharp strain softening.

800i
TEST TEMPERATURE: 22 oC TEST TEMPERATURE: 22 °C

*"-* - ^.-■ :r:r:r:7.r: r-

---=*£ > ^ — ^' - ~

CURVE STRAIN RATE (S 250 CURVE STRAIN RATE

(s1)
0.6x10-* ^ \ (s-1)
0.01
3.3 4.90

—
16
3.2x10«
\ 43
30000
0 1 2 3 4
ENG. SHEAR STRAIN ENG. SHEAR STRAIN

Fig. 3. Shear stress-strain curves Fig. 4. Shear stress-strain curves

at different strain rates at different strain rates
of AISI 316 stainless steel. of ARMCO iron.

The reason for these differences of the shear flow curves at low to medium
and very high strain rate is probably due to the presence of strain
concentrations at very high strain rate as reported by Albertini et al.
(1990 a) . Nevertheless the shear flow curves of both materials at low,
medium and high strain rate reach very high values of fracture strains com-
parable with those reached in metal forming operation and in penetration
problems.

The observation of the true stress strain curves in tension of AISI 316 and
ARMCO iron (Figs. 5 and 6) show that the necking instability arises very
early and gives rise to premature fracture strains. Therefore the tension
test is not appropriate for the study of large strain phenomena in metals.
However the necking phase of the tension test on AISI 316 has been studied
following the Bridgman (1952) analysis, utilizing the photographic records
and the whole true stress strain curves in tension have been compared with
the equivalent stress strain curves from shear testing (Fig. 5).

From this comparison it follows that:

- The tension curves by Bridgman (1952) analysis show strain hardening up to
fracture while the equivalent curves from shear test show saturation of
flow stress. This phenomenon is present at each strain rate.
- The fracture strain of the tension curves by Bridgman (1952) analysis and
of the equivalent curves from shear tests are comparable.
- The two precedent observations are valid also taking into account that
during necking the strain rate is about ten times higher than during uni-
form straining.
 355

GPCD A

° °«A

TENSION
TENSION
TENSION
SHEAR
SHEAR
SHEAR
0.4
EQUIVALENT STRAIN TRUE STRAIN

Fig. 5. Equivalent stress strain Fig. 6. True stress-strain curves

curves of AISI 316 stain- in tension at different
less steel from tension and strain rates, for ARMCO
shear tests at different pure iron.
strain rates.

The reasons for such discrepancies between the curves in tension and the
equivalent curves from shear test were ascribed by Jonas et al. (1981) to:
- yield criterion differences by microscopic anisotropy,
- different texture development at large strains in tension and shear,
- effect of strain path on the microscopic rate of strain hardening.

It follows that it is not possible to obtain a unique equivalent flow curve

from tension and shear tests as claimed in classical plasticity because the
physical phenomena are more complex than those included in the classical
material models.

CONCLUSIONS

Shear testing of AISI 316 and ARMCO iron allowed the obtaining of very large
fracture strains at low and high strain rate making such tests important for
studying large structural strains due to metal forming or accidental impact
loading.

Nevertheless shear tests showed saturation of flow stress at low and medium
strain rate together with strain concentration at very high strain rate.

Tension testing of the same materials showed strain hardening (except ARMCO
iron at high strain rate) up to the necking instability which arise very
early making this test inappropriate for the study of large strain capabil-
ity of structures and materials.

However the application of the Bridgman analysis to the necking phase of the
tension test shows strain hardening up to fracture (no saturation of flow
stress as in the shear test) and large values of plastic strain at fracture
comparable with those reached in the shear test.
356
The different phenomena shown by the flow curves in tension and shear are
caused by differences in yield criteria, texture development and straining
path dependence of microscopic strain hardening.

Comparison of the tension flow curves with the equivalent flow curves by
shear tests following the classical plasticity models (e.g. Von Mises)
showed unavoidable discrepancies from the concept of the unique flow curve
whatever the deformation mode because the model assumes a unique microscopic
deformation mechanism at each deformation mode.

Different material models are required to represent the material response in

tension and shear.

ACKNOWLEDGMENTS

Thanks are due to Messrs. M. Spampani and M. Rigutini of OTO-MELARA for high
speed camera records.

REFERENCES

Albertini, C. and Montagnani, M. (1977). Dynamic material properties of sev-

eral steels for fast breeder reactor safety analysis. EUR 5787 EN.
Albertini, C , Montagnani, M., Pizzinato, E.V., Rodis, A., Berlenghi, S.,
Gerini, G., Pazienza, G. and Paluffi, A. (1990 a ) . Mechanical properties
in shear at very high strain rate of AISI 316 stainless steel and of a
pure iron. Proc. of the Int. Conf. on shock-wave and high strain rate phe-
nomena in materials, University of California San Diego, under publication
by M. Dekker.
Albertini, C , Montagnani, M., Zyczkowski, M. and Laczek, S. (1990 b) . Opti-
mal design of a bicchierino specimen for double shear. Int. J. of mechani-
cal sciences, Vol. 32. No. 9. pp. 729-741.
Bridgman, P.W. (1952) . Studies in large plastic flow and fracture, Mac Graw-
Hill Company, New York, pp. 9-37.
Hecker, S.S., Stout, M.G. and Eash, D.T. (1981). Experiments on plastic
deformation at finite strains. Proc. of workshop on Plasticity of metals
at finite strains. Published by Div. of Applied Mechanics of Stanford Uni-
versity, pp. 162-205.
Jonas, J.J., Canova, G.R., Shrivastava, S.C. and Christodoulon, N. (1981).
Sources of the discrepancy between the flow curves determined in torsion
and axysimmetric tension and compression testing. Proc. of workshop Plas-
ticity of Metals at finite strain, Division of Applied Mechanics of
Stanford University, pp. 206-229.
Ludwik, P., and Scheu, R. (1925). Vergleichende Zug-Druck-Dreh-und Walzver-
suche, Stahl und Eisen, £5,, p. 373.
Polakowski, N.H. and Ripling, E.J. (1966) . Strength and Structure of Engi-
neering Materials, Prentice-Hall, Inc., Englewood Cliffs, pp. 382-383.
WS2C11

FRACTURE MODELLING OF CONCRETE UNDER LATERAL COMPRESSION AND

IMPACT TENSILE LOAD.

J. Weerheijm, H.W.Reinhardt* and S.Postma

TNO-Prins Maurits Laboratory, P.O.Box 45,2280 AA, Rijswijk,
The Netherlands.
♦Otto-Graf Institute, Stuttgart University, Pfaffenwaldring 4,
D-7000 Stuttgart 80 (Vaihingen), Germany.

ABSTRACT

Formerresearchshowed that the rate effect on concrete tensile strength can be modelled by the
description of crack extension in a fictitious fracture plane. The planerepresentsthe initial,
internal damage and the geometry of thefinalfracture plane. In the paper, the same approach
is applied to model the failure envelope for the biaxial loading condition of static lateral
compression and axial impact tensile load. The predicted failure envelope is compared with
data from the experimental programme.

KEYWORDS

Concrete; dynamic loading; biaxial loading; material properties; mathematical modelling;

experimental investigation; fracture.

INTRODUCTION

The rate effect on concrete properties was the subject of manyresearchprogrammes in the last
decade. Especially the tensile strength appeared to be sensitive for rate effects.
In cooperation with the Delft University of Technology (DUT), the TNO-PML studies the
material behaviour under the biaxial loading condition of static lateral compression and axial
impact tensile load. One of the objectives of theresearchprogramme, which consists of a
theoretical and experimental part, is to determine the shape of the failure envelope.The results
of the experimental programme show that the-rate effect on the residual impact tensile strength
decreases with increasing compression level (Weerheijm et al., 1991).
In the theoretical part of the programme, a model has been developed which describes the rate
effect on the uniaxial tensile strength for low and high loading rates very well. It was decided
to examine the possibility to apply the approach of the uniaxial model to the biaxial loading
condition of the test programme. The preliminary results are presented in this paper.

THE UNIAXIAL MODEL

The first and modified version of the model were described in (Weerheijm et al., 1985 and
1989). In summary the model is based on the following general features.
357
358

The tensile strength (ft) is determined by thefractureprocess at micro scale. The failure, or
fracture process starts with bond fracture, at about 0.6 ft, followed by matrixfractureat a load
level of 0.8 ft. Beyond this level, the microcracks in the mortar start to grow and bridging of
the bond cracks occurs; macro cracks are formed; crack propagation becomes unstable and the
final failure plane is formed.
In the model concrete is schematized as a material with penny-shaped cracks of single size 2a
and at equal intermediate distance 2b. A fictitious failure plane is considered containing the
flaws andrepresentingtherealfailure plane. Fig.l shows the planes of failure in concrete and
model. The initial damage is presented by cracks withradiusao. In the model two zones are
distinguished; one zone, A^, representing bondfractureand one zone, A m +A a , for mortar
and aggregate fracture.

tensile loading tensile loading 850223

c 0 n c r e te model

Fig.l. Thefractureplanes in concrete and model.

The geometry of the fictitiousfractureplane follows on one handfromthe demand that the
dissipatedfractureenergy in the real material corresponds with the dissipated energy in the
model. On the other hand crack extension in the fictitious plane is described by using the
stress- and displacement fields given by the Linear Elastic Fracture Mechanics (LEFM).
Application of the strength criterion of the LEFM yields that ao and 2^ are the critical crack
sizes at 0.6ft and 0.8ft respectively.
Using these criteria the geometry of the fictitious plane is known when the strength, Young's
modulus, Poisson's ratio, aggregate fraction, and the specific surface energies are known.
The crack extension is described by considering the balance of energies in theregionaround
the crack tip.
The model predicts a moderate strength increase for loading rates up to 15 GPa/s due to a
changing geometry of the fracture plane. Beyond the threshold of 15 GPa/s, the internal
inertia effects become dominantresultingin a steep strength increase. This predicted rate
dependency matches the available data from literature (Weerheijm et al., 1989 and 1990).
 359

THE BIAXIAL MODEL

From the results of the uniaxial model it was concluded that modelling the development of
internal damage by crack extension in a fictitious fracture plane results in a good prediction of
the rate dependent tensile strength. The biaxial loading condition of static lateral compression
and axial impact loading gives the sequence of increasing the internal damage and the internal
stresses followed by an impact test on the gradually damaged material. When it is possible to
determine the effect of lateral compression on the initial geometry of the fictitious fracture
plane, it should be possible to use the crack extension model to predict the rate effect on the
residual impact strength.

The initial conditions due to compression.

Qualitatively, the stress and failure development can be summarized as follows. Uniaxial
compression induces internal tensile stresses perpendicular to the load direction. Cones with a
three dimensional compression stress state are formed on the aggregates. The final failure, or
shear planes, are composed by bond fracture and matrix fracture along the surfaces of the
cones. To characterize the internal damage due to compression, a fictitious failure plane is
considered composed by the surfaces of bond and matrixfractureand loaded perpendicular by
induced tensile stresses.
Comparable with the fracture process under tension, the initial defects at the largest aggregates
start to grow at about 30% of the compression strength, fc. At 0.8fc the critical stress level for
microcracking in the matrix is reached.
Using the strength criteria from LEFM, the composed geometry of the failure plane and the
relevant parameters of the tensile schematization, the geometry of the fictitious failure plane
under compression can be determined without introducing new unknown parameters. Except
at the thresholds of 0.3fc and 0.8fc, the relation between the compression level and the degree
of internal damage is still unknown. The induced tension stresses, perpendicular to the
fictitious plane still have to be determined and related to the fracture process. This aspect is
described in the next section.

Iso-damage lines.

For biaxial loading only two failure modes are considered, i.e. the tensile failure mode and the
mode for compression. For low compression levels the compression cones on the aggregates
will just delay the development of bond failure under tension and the tensile failure mode will
occur. Only at high compression levels bond failure will be stopped and mortar failure will
occur along the surfaces of the cones.

To relate the bond failure processes under compression and tension the following procedure is
used. First the stresses along the surface of an elastic circular inclusion in an elastic matrix
were determined (Zielinski, 1985 and Mushelishvili, 1953) for uniaxial and biaxial loading.
These stresses are assumed to reflect the stress distribution at the aggregate surfaces. Further
it is assumed that each aggregate has just one single defect which orientation is randomly
distributed along the surfaces of the aggregates. Combination of both assumptions leads to a
sequence of initiated defects with increasing load level for each biaxial loading condition.
The load levels at which bond failure is initiated under uniaxial tension and compression are
used to construct Mohr's stress circles and derive a Mohr-Coulomb failure criterion with
tension cut-off for bond failure. This criterion and the sequence of initiated defects offers the
opportunity to construct lines with an equal amount of activated defects or, in other words,
with the same level of bond damage, see Fig.2.
In this way the damage and induced tensile stresses due to lateral compression are related to an
equivalent tensile load and crack size in the tensile model.
360

0 10 20 30 40 50 60 70 80 90 100
compression level (%)
bond failure

— — — 0 ■"■■■ ■ " failure envelope tension mode

37 % ■■■ ■ ~ ™ failure envelope compression mode

70 %

— 88%

100%

Fig.2. Iso-damage lines for bond failure and the predicted failure envelope for the
tested high quality concrete.

When bond failure has been established matrix fracture occurs whichresultsin an additional
residual strength of 0.2ft in the tensile mode. Therefore, the predicted failure envelope for
failure in the tensile mode is parallel with the equidamage line of 100%, see Fig.2.
The transition from the tensile mode to the compression mode is indicated by the work of
Kupfer (1973) and Nelissen (1972), i.e. at the ratio of tensile and compressive loading of -
1/30. Note that the models for the tensile and compressive failure mode offer the opportunity
to derive the transition by considering the energy demand for both options. At this stage the
empirical ratio is still used, see Fig.2.

As a first approximation it is assumed that the induced tensile stresses for compression levels
beyond 0.8fc are proportional with the compression level. Application of the crack extension
model in the fictitious failure plane under static compression loading, leads to the predicted
failure envelope as depicted in Fig.2 for high compression levels.
The predicted failure envelope for the tested high quality concrete is theresultof a rough
approach. But it matches the shape of empirical envelopes, e.g. Kupfer (1973), rather well
and it offers the opportunity to examine the rate effect on theresidualstrength.

THE RATE EFFECT ON THE RESIDUAL TENSILE STRENGTH

Following the procedure of the biaxial model, the initial damage and induced tensile stresses
due to lateral compression were determined and presented in Fig.2. Increasing the loading rate
for the subsequent impact load and calculate theresidualstrength,resultsin the curves of
Fig.3. In this figure the strength increase ratio under dynamic and static loading (PSI) is
related to the uniaxial condition of tensile loading for various levels of lateral compression.
These curves show that the rate effect decreases with increasing compression level. This result
is in contradiction with the, by Zielinski and Takeda claimed unique rate effect but
corresponds with the experimental data from the current programme, see Fig.4.
 361

+ 0% A 35% O 54% V 90%

1.20

1.00 H 1 1 1 1 1 1—H-

0.80
^fc:
0.60

0.40

0.20

mil i i i mill i i i mill i i i mill ■ ■ ■ "■■■' i i i mill i i i mill ■ » ■ "■"'

0.00
10"2 10"1 10° 10 1 102 103 104 10a 10e

loading rate [MPa/s]

Fig. 3. Ratio of Psi at x% compression and Psi at uniaxial loading.

A Exp.data o PML-model Kupfer

+ pol.fit + pol.fit empirical

<K Ov

1 4 -
(0

r: V s
3 N ^^_
c >>^-— *JL*A A
0
CO
2 -
7B
""°*~~A >^'"
~i
"O *"" ^ . X ' • •.
CO
CD
1 - "°-o"^ ^ * \ \ I
ex \
x
* \
n L 1 1 1 %

20 40 60 80 100

compression level [%]

Fig. 4. The predicted and experimentalresidualtensile strength at a loading rate of

15 [GPa/s] and the static failure envelope (Kupfer).
362

In thisfigure,the experimental data and the empirical failure envelope, proposed by Kupfer,
are presented Application of the predicted rate effect on this enveloperesultsin an almost
perfect fit to the experimental data. For static loading, however, the model predicts smaller
residual strength (see Fig.2.), which results in an underestimate of the dynamic residual
strength as shown in Fig.4. Note, that the predicted, static envelope is a preliminary result
from a straight forward approach based on the uniaxial strengths, Young's modulus and
aggregatefraction.Options for modification are present. At this stage of the study the main
result is that experiment and model show a definite decreasing rate effect with increasing
compression level.

CONCLUDING REMARKS

The theoretical and experimental programme on theresidualimpact strength of concrete as a

function of the lateral compression level showed that:
- rate effect on theresidualstrength depends on the compression level;
- rate effect on the uniaxial impact strength can be modelled by describing the crack
extension process in a fictitious fracture plane, which geometry follows from
concrete composition and static strength parameters;
- the internal damage and stresses due to lateral compression can be related to the
damage development under tensile loading as described in the biaxial model,
resulting in a level of internal damage and induced tensile stresses;
- the description of crack extension in the fictitious planes for the tension or
compression failure mode, leads to a prediction of the rate effect onresidualstrength
which corresonds with the available experimental data.

REFERENCES

Kupfer, H.B. (1973). Das Verhalten des Betons unter mehrachsiger

Kurzzeitsbelastung unter besonderer Beruecksichtigung der zweiachsigen
Beanspruchung. Deutscher Ausschuss fuer Stahlbeton. Heft 229, Berlin.
Nelissen, N.L.M. (1972). Biaxial testing of normal concrete, HERON Vol.18, 1972,
No.l.
Takeda, I. et al (1974) Mechanical Behaviour of Concrete under higher Rate of
Loading than in static Tests. Proc. Symposium: Mechanical Behaviour of Materials,
Kyoto 1974, Vol.11, 479-486.
Weerheijm, J., Karthaus, W. (1985). The tensile strength of concrete under dynamic
loading. Proc. Symposium: The interaction of non-nuclear munitions with structures.
Panama City Beach, Florida, April, 1985, 211-216.
Weerheijm, J. and Reinhardt, H.W. (1989) Modelling of Concrete Fracture under
Dynamic Tensile Loading. Proc. Symp. Recent Developments in the Fracture of
Concrete and Rock. Cardiff, Wales, September 1989, 721-729.
Weerheijm, J. (1990) Properties of Concrete under Dynamic Loading 3: Fracture
Model for Brittle Materials. PML report PML1990-65, October 1990.
Weerheijm, J., Reinhardt, H.W., Postma, S. (1991) Experiments on concrete under
lateral compression and tensile impact loading. Proc. Symp. on Fracture processes in
brittle disordered materials. Noordwijk, The Netherlands, June 1991.
Zielinski, A.J. (1982) Fracture of Concrete under uniaxial Impact Tensile Loading.
Delft University Press, Delft, 1982 (thesis).
Zielinski, A.J. (1985) Concrete under Biaxial Loading: static compression-impact
tension. Stevin report5-55-7, Delft, 1985.
WS2d1 STRESS WAVE PROPAGATION BEHAVIOR
IN
LAMINATED COMPOSITE HOLLOW CYLINDER

I.MAEKAWA,H.SHIBATA,M.NAKAYAMA

Department of Mechanical Engineering ll,Tohoku University,

Sendai,Aoba-ku,Aramaki,JAPAN.

and

A.KOBAYASHI

Tonen Co. Ltd.,Saitama,Iruma-gun,Ohi-Machi,Japan.

ABSTRACT

Elastic wave propagation behaviors in fourteen series of CFRP hollow cylin-

drical specimen subjected to an impact compression, impact torsion or
impact compression under a torsion are studied by Hopkionson bar method.
Every specimens are laminated by using two types of layer in which carbon
fibers are at angle of 0° and at angle of 45° to the axis. The wave veloci-
ty can be expressed by using an apparent elastic modulus derived from the
law of mixture. The ratio of strain pulse height at the output bar to that
of input bar, WTR, increased for impact compression but decreased for
impact torsion with increase of the number of 0°-layer. These reasons are
discussed based on a simple two layers model. The experimental results for
impact compression under a static torsion were quite different for differ-
ent configuration of lamination, and the influence of 0°-layer on the WTR
is described.

KEYWORDS

Hollow cylindrical specimen; CFRP; lamination; impact compression; impact

torsion; static torsion; velocity of elastic wave; ratio of wave transmis-
sion.

INTRODUCTION

When an impact force is applied to a machine element, stress waves propa-

gate in it. A stress pulse formed by the superposition of waves reflected
and transmitted at the boundaries gives an influence on the strength of a
finite body (Maekawa et al.,1988). Because of this complicated stress
state, dynamic fracture behavior is quite different from fracture caused by
a static loading. According to our previous studies, fatigue life of steel
specimens shows the size dependence, which is called mechanical size ef-
fect, under a pulsation of impact force (Maekawa et al., 1980,1982,1983,
1986). But graphite does not show clear size effect, because the attenua-
tion in the amplitude of a wave during the propagation is considerable in
the case of porous materials such as graphite (Maekawa et al.,1990). Thus,
the study on the wave propagation behavior provides one of important infor-
mation to understand the dynamic strength of materials. In general, funda-
mental study on the wave propagation is important whether we desire to
reduce wave propagation or, on the contrary to this, to attain effective
transmission.
363
364
By the way, recently, composite materials are expected to be useful materi-
al, especially for an air craft. However, it is considered that the proba-
bility of action of impact forces will be increased for such a high speed
vehicle. Since a composite material contains many discontinuities, wave
propagation behavior will be very complicated in it. Therefore, more funda-
mental investigation seems to be necessary to develop the study, although
many studies have been made on the strength of composite materials (For in-
stance; Bunsell,1988;Paul,1989jMallick and Newman,1990).

Thus, the purpose of this study is to make clear the effect of fiber orien-
tation and the configuration of lamination on the elastic wave propagation
behavior in a composite specimen subjected to an impact load.

MATERIAL, SPECIMEN AND EXPERIMENTAL METHODS

Material used was a carbon fiber reinforced epoxy resin, CFRP. Fourteen
series of hollow cylindrical specimen were prepared by a lamination with
ten layers by using two types of composite layer as shown in Table 1. In
each layer, the orientations of carbon fibers are parallel to the axis of a
specimen or at an angle of 4-5° to the axis, and these layers are concisely
called 0°-layer or 45°-layer hereafter, respectively. The mechanical
properties of each layer are shown in Table 2. The outer and the inner
diameters of these specimens were 25.4 and 22.1mm, and the length was
1100mm, respectively.

Impact compression experiments were carried out by Hopkinson bar method.

The set up is illustrated schematically in Fig.1(a). Impact torsion was
applied to a specimen by a striker, which strikes the nob of rotating input

Table 1. Configuration of lamination.

Orientation <of carbon fiber with regard to

the specimen axis (degree)
Series Inside Outside
A 0 0 0 0 0 0 0 0 0 0
B +45 -45 +45 -45 0 0 0 0 0 0
C 0 0 +45 -45 +45 -45 0 0 0 0
D 0 0 0 0 +45 -45 +45 -45 0 0
E 0 0 0 0 0 0 +45 -45 +45 -45
F 0 0 +45 -45 0 0 +45 -45 0 0
G 0 0 +45 -45 +45 -45 +45 -45 0 0
H +45 -45 +45 -45 +45 -45 0 0 0 0
I 0 0 0 0 +45 -45 +45 -45 +45 -45
J + 0 0 0 0
45 -45 +45 -45 +45 -45
K 0 0 +45 -45 +45 -45 +45 -45 +45 -45
L +45 -45 +45 -45 +45 -45 +45 -45 0 0
M +45 -45 +45 -45 0 0 +45 -45 +45 -45
N ...t.45., -45, +45 .-4.5,. __+4,5_.. -45 .145..,..-4.5 , +45, , -45
Table 2. Mechanical properties ( * calculated value )

Fiber Young's Shear Poisson's Density Wave velocity(m/s)

orientation modulus modulus ratio (kg/m ) CT CT
L
(degree) (GPa) (GPa)
0 127.40 4.508 0.30 1670 8734 1643
45 15.68 32.340 (0.73*) 1670 3064 4401
90 9.31 — 0.022*) 1670 2361
 365

J< ® ®
A?
1 I
©Striker
(D Input bar
(a) Impact compression *B
ft (3) Strain gage
© Specimen

D A?
(b) Impact torsion <D Output bar
(©Bridge box

t (c)€ x
©Amplifier

Impact compression
t # (§)Wave memory
(D Computer
under static torsion
©Nob

ran
4 r®i
©Ball bearing
©Joint
® H ® ©Weight

Fig.1 Experimental set up.

On input bar
On output bar

Fig.2 Typical example of

strain pulse profile.

0-025 msec

bar supported by two bearings to prevent a bending when an impact force is

applied as shown in Fig.1(b). Impact compression experiments were also car-
ried out under a static torsion which was loaded to a specimen by using a
couple of pulling wires with weights as shown in Fig.l(c). In these experi-
ments, a constant impact force was applied to the input bar, respectively,
by a striker flied by using an air gun. And both interfaces between a
specimen and two bars were lubricated by MoS ? . The propagation velocity of
a strain pulse and the attenuation in strain pulse height were measured by
strain gauges method. In order to reject the influence of the fiber orien-
tation of the outer layer, strain pulse profiles were measured on the input
and on the output bars. A typical example of a strain pulse profile, which
is a single wave without any superposition of reflected waves, is shown in
Fig.2.
366
EXPERIMENTAL RESULTS AND DISCUSSION

Impact Compression

Wave Velocity. It was presumed that the wave velocity in 0°-layer is more
faster than that of 45°-layer,because the Young's modulus of the former is
larger than that of the latter. In order to confirm this and to see the
effect of configuration of lamination, the wave velocity was measured for
each specimen. Wave velocity of these specimens were evaluated by measuring
the time a strain pulse needs to propagate the distance between two gages.
This results are shown in Fig.3(a). In this figure, wave velocity increased
with increase of the number of 0°-layer in the configuration and it does
not depend on configuration. This result can be explained by considering
that the velocity of elastic wave is given by eq.(l)

cL = JETTV (1)

E . = EoVo* E 4 5 ( 1 - V 0 )
where E is derived from the law of mixture for a composite material, and
E and £> are apparent Young's modulus and the density of a specimen. The
notation V Q means volume fraction of 0°-layer in a specimen and subscript 0
or 45 indicate that the quantity is Young's modulus of 0°-layer or 45°-
layer. Substituting the corresponding values used in this study, eq.(l)
gives a curve shown in Fig.3(a).

Ratio of Wave Transmission. A strain pulse height is attenuated during the

propagation. Then the wave propagation ratio, WTR, which is defined by the
ratio of the pulse height in the input bar to the pulse height in the
output bar, is investigated to see the characteristic property of composite
specimen. The relation between the WTR and the number of 0°-layer in a
configuration is shown in Fig.3(b). According to this figure, WTR value is
increased nearly linearly with increase of the number of 0°-layer. For
series K, I and J, the increase in WTR value with increase of 0°-layer is
smaller than that of other series. From these results, it is roughly summa-

0 20 40 60 80 100 0 20 40 60 o80 100

Lamination of 0°-layer(%) Lamination of 0°-layer
Fig.3 Influence of 0°-layer lamination on wave propagation behavior (°M
(Impact compression).
 367
rized, except for series E and M, that WTR takes comparatively large value
when 0°-layer is laminated in the outer layer and the number is many. Since
the rigorous analysis is troublesome for a specimen which has a complicated
many layers, the reason is considered qualitatively by using a two layers
model. When a compression wave propagates along the axial direction, a
radial deformation will be accompanied by it. For example, the deformation
at the inner face of outer layer is expressed as eq.(2) for the radius r.

Ar =
EoV0 + Ei(1-V0) (2)

where \) is the Poisson's ratio and subscript 0 or i indicate the outer

layer or the inner layer. The deformations in layers 1 and 2 are different
because their elastic moduli are different. This difference in deformation
yield an interaction at the interface between the inner and the outer lay-
ers. The interaction force Pm is given by eq.(3) in nondimensional form
with regard to the stress (J in a propagating wave.

N 1
_B» I 1-rWo .. 1 - rVioVj ~
* " Uo < *i + eH, X \ 2 + 9V0) ' W rE: (X a + 9Vi )(X 2 + eV, ) Fz(r)

(3)
E 0 V0 + E; (1 - V0 )

_ (XC+QVQ )r£n r3Xlfl - (XII+QVQ ) r f o rfo'1

F,(r)

_ . . _ (X22 + 9Vi )rfe 1 rfo - (X a + 9Vi )rfo"' rfo

^KQ = [ l - E k + ( - 1 ) Q { ( E k - 1 ) 2 - 4 E k f 2 ] / 2

Ek = rEk"eV|< + rEk -QEk'rVk/rEk

Ek = - 0 E k /rEk

k = 1 or 2 , Q = 1 or 2

and the left subscripts r and 9 show the direction of measurement in the
radial and the circumferential directions, and the right subscripts i and o
show the inner and outer layers. The radii of the inner surface, outer
surface and the interface are shown by r1,r_ and r^, respectively. If the
outer layer is 0°-layer, the interaction is tension. But the interaction is
compression if the inner layer is 0°-layer. The tensile interaction will
not prevent the radial deformation and so the influence on the WTR will be
little in this case. On the contrary, the compression will increase the
attenuation in pulse height when 0°-layer is in the inner layer. Thus, it
is considered that WTR values is reduced for series I,J and K.
Impact Torsion

Effect of 0°-layer on the Wave Velocity. The propagation velocity of

368
torsional pulse is reduced with increase of the number of 0°-layer as shown
in Fig.4(a). The velocity of torsional wave, C T , is expressed by using the
apparent rigidity modulus, G , which can be derived from the law of mixture
similar to eq.(l), as follows.

C T = JQ,*/ P W)
10
Gd = ( E Gi Ip. ) / IPa
where G and I are the apparent rigidity modulus and the apparent polar
moment of inertia for a specimen, and I . is the polar moment of inertia of
layer i. For typical two cases, that is, 0°-layer is in the outer layer and
in the inner layer, eq.(4) gives two curves as shown in Fig.4(a), substi-
tuting the corresponding value. It is seen that eq.U) can express experi-
mental results very well.

Ratio of Torsional Wave Propagation. The WTR is reduced slowly with in-
crease of 0°-layer as shown in Fig.3(b). This reason is also qualitatively
considered by two layers model. In general, the coefficient of transmission
for a torsional moment at the boundary between two different bars 1 and 2
is expressed as (Johnson,1972)

T2 = 2T, / ( 1 + Ip,Pi CT, / I P 2 P 2 C T 2 ) (5)

where T is a torsional moment and subscripts 1 or 2 indicate the bar 1 or

bar 2. Then the WTR is evaluated approximately by the ratio of the torsion-
al moment in the input bar, T., to the torsional moment int the output bar,

12
(a)
O
UD
TbTI
101 io-5
E
CO 0°- layer in k-

O 8 inner layer c 04 /M i
o < ,E
X
N( H^4
6 «/> 0 - 3 V*
^ T l \ G 1HT"-
£
s°- 2
V
o 4 H \B A
\
u
L-
> •4-^

2 * 01 -
> >
0-layer in outer layer a*
i i i1 i 11 1 i i 1
0 20 40 60 o80 100 0 20 40 60 o80 100
Lamination of 0°- layer Lamination of 0°- layer
(%)
Fig.U Influence of 0°-layer lamination on wave propagation
(Impact torsion).
 369
T , assuming a torsional wave can propagate without attenuation in a speci-
men, as follows.

4IPPCTIP2P2CT2
(6)
T, (Ip P CT ♦ I P ^ C T J )(I P P CT ♦ Ip, P, CT1)

In this equation, the propagation velocity of a torsional wave, C T , is

included, and the velocity depends on the number of 0°-layer as shown by
eq.(4). Therefore, the above ratio depends on the number of 0°-layer in the
configuration. Substituting the corresponding values used in this study
into eq.(6), two curves are obtained as shown in Fig.4(b) for the cases of
0°-layer in the outer and in the inner layers. These curves are also close
to the experimental results, although the attenuation is neglected. Then,
it is considered that the influence of transmission at both sides of a
specimen on the WTR can not be neglected.

Impact Compression under a Torsion

Wave Velocity. As described above, the velocity of P wave generated by an

impact compression was increased with increase of the number of 0°-layer
but the velocity of S wave generated by an impact torsion was reduced with
increase of the number of 0°-layer. And so, in the next place, the velocity
of P wave was investigated under static torsion to see the effect of tor-
sion on the propagation behavior of P wave. The results are different for
different configuration. And so typical cases are investigated.

The Effect of Configuration of Lamination on WTR. According to the above

investigations, it is considered that the interaction between two different
types of layer influence on the WTR each other. Then, the effect of sand-
wich lamination on the WTR was investigated. The experimental results are
shown in Figs.5(a) and (b). In Fig.5(a), the WTR is reduced considerably
for large torsional moment when all layers are in 0° orientation. However,
influence of torsional moment on WTR can not be seen when all layers are
4.5°-layer. And the WTR value is reduced to about one half of the value in

o (a)
o - o

I— r~
c (M
o
<fl
.52 0-3
E
c 0-2 rW +
V M
^ •
OJ
i_ • w
4_« • 0 6 /(±45) 2
<u 0-1 ° O10 o> 0-1 f- o(t45) 3 /0 4 ■ <yu45)3
> •(±45)5 ^ h M ± 4 5 V 0 2 A 0 2 /(*45) 4
* i 1 i i i _l_ J l _J L. _L.. J $ _i i_
0 0-5 10 1-5 20 25 3-0 0 a5 10 15 20 25 3-0
Torsional moment (Nm) Torsional moment(Nm)
Fig.5 Experimental results for impact compression under static torsion.
370
the case of 0°-layer. Thus, the wave propagation behavior is quite differ-
ent for different fiber orientation. Therefore, several series of specimens
are investigated as shown in Fig.5(b) to see the relation between the WTR
and the law of mixture.

According to Figs.$(a) and (b), it can be said that the WTR of a specimen
is more larger when more many 0°-layers are included in the outer layer and
the influence of static torsion on the WTR is not clear except for the case
of 0°-layers. From these results, it is considered that wave propagation
in 0°-layer is reduced by the presence of the inner 45°-layers for which
the WTR is smaller than that of 0°-layer as described in the previous
article concerned with Fig.3(b).

CONCLUSION

The velocity of compression wave was increased with increase of the number
of 0c-layer in the configuration of a specimen, and the velocity of tor-
sional wave was increased with increase of the number of 45°-layer, respec-
tively. These results were well explained by taking apparent Young's modu-
lus or rigidity modulus derived from the law of mixture.

Wave transmission ratio, WTR, for a compression wave is increased with in-
crease of the number of 0°-layer in the configuration. When a specimen
includes relatively few 0°-layers and includes them in the inner layer,
increase in the WTR with increase of the number of 0°-layer is small, and
this reason was discussed based on a two layers model qualitatively.

The WTR for a torsional wave is increased with increase of the number of
45°-layer. In these results, the influence of the transmission at both
sides of a specimen on the WTR can not be negligible.

When an impact compression is applied to a specimen under a static torsion,

the wave propagation velocity is not affected clearly by the torsional
moment in most cases and the WTR is quite different for different configu-
ration of layer in a specimen. On the whole, WTR value is large when a
specimen has many 0°-layers and has 0°-layers in the outer layer of a
specimen.

REFERENCES

Bunsell,A.R.,ed.,(1988).Fibre reinforcements for composite

materials. Elsevier. Amsterdam.pp.537.
Johnson,W.(1972).Impact strength of materials.Edward Arnold.London,p.4-6.
Maekawa,I.(1980).Damage produced by pulsating impact load.J.Soc.Mater.
Sci.,29,3,20,486-491.
Maekawa,I.(1982).Size effect in impact torsional fatigue strength. Proc.
21th Japan Cong, on Mater.Res.,124-127.
Maekawa,I.(1983).Size effect in impact tensile fatigue. Proc.ICF Inter.
Symp.on Fracture Mechanics,Beijing,China,757-762-
Maekawa,I.(1986).The influence of corrosive environment on impact fatigue
of structural steel. Proc.Int.Conf.on Engg.Mat.Strength.,2,347-352.
Maekawa,I.(1988).Impact strength in a finite rod.1,31,3,554-560.
Mallick,P.A. and Newman,S.,ed.,(1990).Composite materials
technology. Hanser Publishers.Munich.pp.400.
Paul,A.L.,ed.,(1989).Composite materials:Fatigue and fracture,
Second Volume.ASTM.STP,1012,Philadelphia,pp.422.
WS2d2

Dynamic Behavior of Axisymmetric Bodies

under Two-Dimensional Wave Propagation

S. Tanimura, K. Kaizu and K. Higashi

College of Engineering, University of Osaka Prefecture

Mozu-Umemachi, Sakai-City, Osaka 591, JAPAN

ABSTRACT

Stress focusing, local behavior and impact fracture initiation in a body

under stress wave propagation have attracted special interest recently. In
this paper, a brief survey of recent studies on these dynamic problems is
made. Such studies have been done mainly by analyzing two-dimensional
stress waves in elastic and elastic/viscoplastic bodies, using
bicharacteristic method. Newly analyzed results on dynamic behaviors of a
container which can be used for shock compaction of powder, obtained by
using bicharacteristic method, are presented. Influence of temperature
gradient in a cylindrical rod on two-dimensional stress wave propagation is
made clear.

KEY WORDS

Dynamic behavior; stress wave; impact fracture; two-dimensional wave; shock

compaction; numerical analysis; elastic/viscoplastic body.

1. INTRODUCTION

Finite difference method, based on integration along the bicharacteristics,

is the most suitable for analyzing two-dimensional stress wave propagation
in a body. The advantage of this method is attributed to the fact that
characteristic surfaces coincide with the wave fronts. Thus, by using this
method, the propagation, reflection and interaction of stress waves in a
body can be investigated in detail. This method was applied by Clifton
(1967) to the plane problem in dynamic elasticity. It was also applied by
Bejda (1968) to the plane problem in elastic/viscoplastic media. By the
same method, a two-dimensional stress wave in a circular cylinder was also
analyzed by Fukuoka and Toda (1978). Stress concentration associated with
two-dimensional stress waves in a circular cylinder was analyzed by
Tanimura et al. (1987). Mechanism of the impact fracture in a brittle body
for a circular cylinder was studied using the method by Liu et al. (1987).
Dynamic behavior of elastic/viscoplastic circular cylinders and tubes was
also analyzed by Liu et al. (1989b), and by Tanimura et al. (1989).

371
372
In this paper, by making a brief survey of such studies performed by the
authors and the colleagues, the mechanism of the impact fracture initiation
in a brittle body under two-dimensional stress wave propagation is made
clearer by showing numerical examples. Stress concentration associated
with two-dimensional wave propagation in circular tubes and a container is
demonstrated. Results obtained by analyzing variations in the maximum
tensile stresses generated in the circular tubes are presented. And,
influence of temperature gradient on the two-dimensional stress wave
propagation in a cylindrical rod is made clearer.

2. GOVERNING EQUATIONS

To deal with the dynamic problems of a circular cylinder and a tube, cylin-
drical coordinates (r,0,z) were used, where axis z coincides with the axis
of the cylinder and tube. Thus, the governing equations to the axisymmetric
problem becomes as follows (Liu et al., 1987; Tanimura et al., 1989):

L[W]=ATW +k\ +A^W -B=0 (1)

T n S
T n £
where the matrices A , A and A are square matrices of the sixth order
consisting of elements independent of unknown functions. W and B are
vectors as follows:
W^=[u,v,p,q,s,n],
Bt=[2q/n, n/n, u/n-2<D>(p-s)/3, -u/n-2<D>q, 2<D>(p-s)/3, -2<D>n]
where 2
T= Cl t/r 0 , n=r/rQ, C=z/rQ, u=v r /c 1 , v=v z /c 1 , p=(or+O0)/2pc1 ,
2 2 2
q=(0r-06)/2pc1 , s ^ / p c j , n=T rz /pc 1 .
0"r, 00, 0* and T r z denote each stress component, v and v denote each
particle velocity component, while Ci is the propagation velocity of the
dilatation wave, p denotes the density, t the time and T Q the
representative length. <D> is a function corresponding to the components of
the viscoplastic strain rate (Tanimura, 1979, 1982).

Accuracy of the computation is evaluated by comparing the energy applied

into the body with the total energy in the body. Relative errors are
analyzed within a 3% limit for all numerical examples.

3. NUMERICAL RESULTS AND DISCUSSIONS

. R(r.t)
3-1. Mechanism of the impact fracture initiation
in a brittle body
o|
(a) Circular cylinder 2fm
Two-dimensional stress waves in an elastic I
circular cylinder with a radius of T Q and a 2r.
length of L Q (Fig.l), were analyzed (Liu et
al.,1987) wnen an axisymmetric pressure pulse
was applied to the end surface of the circular
cylinder. The following load functions were
assumed:
tz
s=-f(x)F(n) (S=o, n < n ) (2)
where f| is the radius of themregion on which F i g . l Circular cylinder
the pressure pulse is applied, II^LQ/TQ, and f(x) and coordinate
and F(ri) were assumed as follows:
 373

f(T)- fmT/Tr (T^Tr) F(n)= [l+cos(7m/2r, m )]/2 (r,^i my)

T m
U, T Tw
, , <V« i>
fm( 2- )/^2-Tl) V T
f 2> 0 (nm<n)
k0 (T2ST),
where f m is the maximum pressure (non-dimension) and T is the rise-time.
In order to examine the effect of the shape of the pressure pulse on the
impact fracture patterns, the following values were chosen: T =0.05, Ti=
0.1 and To=0.5. Since the material was steel, the material constant were
chosen as follows: Ci=5.61xlO~Ws and the velocity of the shear wave
Co=3.24x10 m/s. In this analysis, only an elastic deformation was
considered, and it was assumed that <D>=0 in Eq.(l).

When the pulse length of an applied impulsive load was sufficiently short,
such as when a charge was detonated on the end surface of the circular
cylinder, local parts in the analyzed stress distribution were apt to be
formed where a tensile stress arises concentrically. When an impact load
is applied to a circular cylinder made of a brittle material, which is weak
in resisting a large tensile stress, it seems very likely that the position
of the fracture initiation will be closely related to the local part of the
highest tensile stress concentration. In connection with this presumption,
Tanimura et al. (1986, 1987) investigated the values of maximum tensile
stress °max/^m generated at various points in the cylinder: a denotes
the value or trie three principal stresses, {(s+p+q)/2+[(s-p-q) /4+n ] ' ,
p-q}. When a charge is detonated at the center of one of the end surfaces
of a cylinder, a number of different fracture regions are formed.
Originally, Kolsky and Shearman (1949) summarized these fracture patterns
from their experimental results, as shown in Fig.2. By comparing the
distribution of the maximum tensile stress arising in the cylinder as
shown in Fig.3 (Liu et al., 1987) with that for Fig.2, it can be recognized
that the large tensile stress along the axial of the cylinder, n=0, in
Fig.3 corresponds to the fracture PC (see Fig.2), and that the large
tensile stress at £=0 corresponds to the fracture ST and the large tensile
stress near the free boundary, £=1.0 in Fig.3(b), corresponds to the
fracture KH. It is evident that generation of the peculiar fracture
patterns under impulsive loading in a brittle cylinder can be explained
fairly well by the above analysis.

«/>=1.0 = 0.35 T=IA «//=i.o * L = i.o T=I.A

0.5 1

Fig.2 Diagram of
fracture region
in a cylinder F i g . 3 . Distribution of t h e maximum tensile stress

(b) Circular tube

Figure 4 shows an elastic circular tube with an outer diameter of 2Ro, an
inner diameter of 2R^ , and a length LQ=0.06III. The ratio of the wall
thickness of the tube to the outer radius is expressed as H^I^-R^)/!^.
374
The impact of a ramp-shaped rising velocity was assumed to be applied to

n
the end surface of this tube (Liu et a l . , 1 9 8 9 a ) . In this case the
following load function was assumed:
V(T)- f VmT/Tr STr),
(TS-i^. (3)
(T r ST)

where V denotes a constant velocity, which is dimensionless, after the

rise-time T . The material was steel and material constants were the same
as for the circular c y l i n d e r . Figure 5 (Liu et a l . , 1 9 8 9 a ) shows the
results of the maximum tensile s t r e s s , o* f in the t u b e s , w h i c h were
obtained by taking readings of the maximum values in the distribution
diagrams of the maximum tensile stresses arisen during the period up to
T=10 for respective calculation-conditions. While Figure 5 shows, together,
the results in the case of a circular cylinder (H=1.0). From Fig.5, it can
be seen that as the rise time, T , becomes shorter, the maximum tensile
stress CT*/V becomes higher. When H is greater than approximately 0.3, the
value of 0*/V increases suddenly a s shown in F i g . 5 , and the position
corresponding to 0*/V_ is located on the inner surface. It is also found
that the maximum value for the circular cylinder with no hole ( H = 1 . 0 )
corresponds approximately to that for the circular tube of H=0.3.

Figure 6 (Liu et al. , 1989b) shows the value of 0*/V in elastic/

viscoplastic tubes obtained in the same way as that for Fig.5. The impact
end conditions were chosen same as shown above in section 3.1(a) Circular
cylinder. That is, the condition (III)
shown in Fig.6 corresponds to the case
when only elastic deformation occurs.
From this figure, it is also found that
\y//////y//////\
even when the viscoplastic deformation Vo(t) 4— tf—cq
takes place,
occurrence of
the possibility of the
the impact fracture in
the cylinder containing a small co-
c4 CM|
Y/////A
VTZm
axial hole (0.4^H<1.0) becomes much
higher than that in a cylinder with
no hole (H=1.0). Fig.4 Circular tube and coordinate

r
r=1
^- - —
0.6

/ y
f/
>6<u gOA // -
"""""*
o
V
0.2 / — — ( F ) 1
■ ^>
— ■ — en

Fig.5 Fig.6
Variation in the maximum tensile stress generated in circular tubes

3-2. Dynamic Response of a circular container filled with liquid

Here, we consider two-dimensional stress waves in an elastic/viscoplastic

circular container filled with liquid. The container has an outer diameter
of 2R2=0.4m and a length of LQ=0.6m as shown in Fig.7. The impact of a
 375
ramp-shaped rising velocity was assumed to be applied to the end surface of
the container.

The governing equations are the same form as in Eq.(l). The material of the
container is steel and the values for the computation are the same as those
in section 3.1(a). The filled liquid is water and, values for the
computation in the liquid are chosen as: the density of water p1=1.0x10
kg/m and the propagation velocity of the pressure wave c=l.48x10 m/s.
Figure 8 shows the value of C m a x /V m obtained in the same way as that for
Fig.3. From Fig.8, it can be seen that a large tensile stress arises from
the solid-liquid interface.
;*l t * 8 H=025

V0(t)

B^ZZZZZZZM Z0 3D ^C 5 0
e°o

Fig.7 Circular container filled Fig.8 Distribution of the maximum

with liquid and coordinate tensile stress

3-3. Dynamic behavior of circular cylinder having a temperature gradient

Influence of temperature gradient in a circular cylinder on two-dimensional

stress wave propagation has been studied by numerically analyzing it, when
an axisymmetric impulsive load, of a ramp-shaped rising velocity, is
applied to the end surface of a semi-infinite cylinder which is heated to
produce a temperature distribution.
TblKl
D a 30[mm] -693
The governing equations are the A93
=20 [mm] 293
same form as in Eq.(l). Since the
material is 304 stainless steel,
the density p=8.057xl03kg/m3 and
the other material constants were
chosen from the experimental
results (Takeuchi et al., 1977).
In this case, the impact velocity W" -WT "2Kb
Vm=5.0m/s and the radius of the
cylinder rQ=10mm are used. The Fig.9 Temperature distributions
temperature distributions are
shown in Fig.9, where T is the
temperature and T Q is the tempera-
Tb[K]
ture at the impact end of the 693
cylinder. Figure 10 shows the
distribution of the axial stress
along the side surface of the
cylinder when the time T=20 and
the rising time Tr=10. From this
figure, it can be seen that stress
values at each temperature level,
at the impact end, are different
from each other. While the stress 2G0
value at room temperature is not
so different from that observed Fig.10 Stress distribution
at any other point apart from the along the outer surface
376
impact end. Therefore, when a temperature gradient in the cylinder becomes
more steeper, the more significant difference should occur between the
value of the stress at the impact end and that at any other point apart
from the impact end. These results have direct application in evaluating
the measuring error for an apparatus operating under a temperature
gradient, for example, a split Hopkinson bar. If one measures the stress at
£=6 as a gauge position of the Hopkinson bar, with a mean temperature
gradient of about 25°C/£ (=25°C/radius of the bar), which corresponds
to about 2.5°C/mm, the maximum difference between the stresses at the end
and at the gauge position reaches 3%.

CONCLUSION

Two-dimensional stress waves in a variety of axisymmetric bodies, which are

of elastic and of elastic/viscoplastic bodies, have been analyzed
numerically, when axisymmetric impulsive loads are applied to their end
surfaces. For the numerical analysis, the finite difference method based
on integration along bicharacteristics has been employed. By presenting
numerical results, stress focusing, local behavior and impact fracture
initiation in the bodies under stress wave propagation have been clarified,
quantitatively.

REFERENCES

Bejda, J.(1969). Propagation of two-dimensional stress waves in an elastic/

viscoplastic material. Proc. 12th Int. Congr. Appl. Mech., 121-134.
Clifton, R.J.(1967). A difference method for plane problems in dynamic
elasticity. Q. Appl. Math., 25, 97-116.
Fukuoka, H. and H. Toda (1978). High velocity impact of mild steel cylinder,
In: High velocity deformation of solids (K.Kawata and J. Shioiri, ed.),
IUTAM Symp., pp.397-402. Springer-Verlag, New York.
Kolsky, H. .and A.C. Shearman (1949). Investigation of fractures produced
by transient stress waves. Research, 2^, 384-389.
Liu, K., S. Tanimura and M.Daimaruya(1987). Dynamic behavior of a circular
cylinder under impulsive loads ( Mechanism of the impact fracture of a
brittle body). Bulletin of JSME (in Japanese), 53, 491, 1239-1245.
Liu, K., S. Tanimura, H. Igaki and K. Kaizu (1989a). The dynamic behavior
of an elastic circular tube due to longitudinal impact. J. JSME
international, 32, 4, 535-539.
Liu, K., S. Tanimura, K. Kaizu and M. Daimaruya (1989b). Dynamic behavior
of elastic/viscoplastic circular tubes due to longitudinal impact. J.
Soc. Mat. Sci. (in Japanese), 36., 411, 1309-1313.
Takeuchi,Y., N.Noda, S.Komori, H.Nyuko and T.Kitagawa (1977). Empirical
formulae of temperature dependency of elastic moduli of several steels
and aluminium alloys. J. Soc. Mat. Sci. (in Japanese), 26_* 282, 210-214.
Tanimura, S. (1979). A practical constitutive equation covering a wide
range of strain rates. Int. J. Engng. Sci., 17, 997-1004.
Tanimura, S. (1982). Practical constitutive equations for an elastic/
viscoplastic body covering a wide range of strain rates. Proc. 25th
Japan Cogr. Mat. Res., 25-30.
Tanimura, S., H. Igaki and K. Liu (1986). Dynamic behavior of a circular
cylinder under impulsive loads (Stress concentration associated with
stress waves). Bulletin of JSME (in Japanese), 52, 484, 2680-2684.
Tanimura, S. , K. Kaizu and K. Hatano (1989). Dynamic behavior of elastic/
viscoplastic circular tubes due to impulsive loads traveling on its
outer surface, ADVANCES in PLASTICITY (A. Khan and M. Tokuda, ed.),
pp.429-432, Pergamon.
WS2d3

DYNAMIC CRUSHING OF ELASTOPLASTIC CELLULAR SOLIDS

W.J. STRONGE

Department of Engineering, University of Cambridge

Cambridge CB2 1PZ, U.K.

ABSTRACT

Lightweight, open-celled foams and honeycombs are frequently used for

protective packaging because they mitigate impact damage by limiting
transmitted forces. These materials crush at a pressure that is very
insensitive to rate-of-deformation; this is a consequence of cellular
compliance that exhibits post-yield strain-softening. Crushing of cellular
solids is primarily due to buckling and plastic collapse of cell walls; at
any instant most of this deformation is localized in a thin band of cells.
As deformation proceeds, one layer of cells after another is crushed into the
densifled band of completely crushed cells.

Microinertia effects the shock mitigating properties of dynamically crushed

cellular solids because strain-rates are very high in the localized crushing
zone. This stabilizes some more compliant modes of deformation. Collision
tests on honeycombs reveal that rate effects depend on cell geometry; at
high strain-rates microinertia diffuses localization and amplifies the
intensity of transmitted shocks.

KEYWORDS

dynamic crushing, foam, honeycomb, microinertia, periodic structure, strain

localization, strain-rate

INTRODUCTION

Foam and honeycomb materials are frequently used as lightweight packaging

materials that protect fragile objects against collision damage. To guide
development of impact shock mitigating materials, this paper explains how
properties of cellular solids at high rates of loading depend on both
microstruetural and microinertia effects.

High void ratio, open celled metallic or polymeric cellular solids deform
first by flexure and ultimately buckling of cell walls. Static crushing of

377
378

Fig. 1. Strain localization in spruce wood

crushed by cross-grain compression.
Tubule width is ~ 0.05 mm.

both elastomeric and rigid-plastic foam or honeycomb exhibits a small strain

elastic phase, a large strain crushing phase at almost constant stress and a
final phase of densification due to mutual interference between highly
compacted cell walls. The major crushing phase is associated with a stress
plateau resulting from elastoplastic cell wall buckling. In rigid-plastic
cellular solids this buckling is localized in thin bands of strain-softening
cells (Stronge and Shim, 1988; Throne and Progelhof, 1984; Maiti et ai. ,
1984; Greene et al., 1969). A photograph of deformation localization in
dried spruce wood crushed across the grain (Fig. 1) illustrates that the mode
of quasistatic crushing is usually asymmetric. The yield stress and mode of
deformation for both regular and anisotropic foam and honeycomb cells have
been determined by Gibson et al. (1989). After initiation of crushing in a
single band of cells, static crushing proceeds by one layer after another
being compressed into the band of completely crushed cells; i.e. quasistatic
crushing consists of a highly nonhomogeneous, locally unstable deformation.
This behaviour is attractive for mitigation of collision damage since
quasistatic crushing occurs at an almost constant level of stress before
complete densification.

Following impact, the stress in an initial phase of crushing for an elasto-

plastic cellular solid is enhanced by two dynamic effects: (a) as impact
velocity increases the cells near the impact surface are more tightly
compressed during densification so crushing stress increases; and (b) the
highly localized nature of crushing results in very large strain-rates in the
crushing band and consequent stabilization of some modes of deformation by
microinertia. The first of these dynamic sources of stress enhancement has
been described as a 'shock' wave associated with the final strain-hardening
or densifying phase of cell deformation (Reid and Bell, 1984). For impact
speeds V(0) large enough to cause substantial densification, this results in
a nominal crushing stress that increases with V(0) (Shim et ai., 1990). The
second dynamic source of stress enhancement is microinertia from buckling of
cell walls. This tends to stabilize the more compliant unsymmetric modes
of cell deformation, thus diffusing crushing bands and increasing the
crushing stress plateau level (Klintworth, 1989). Microinertia plays a
 379

(a)
Al-alloy
Wall thick. h=0.92mm
Cell dissip. E=7.45J
E. intensity Q=3.04

(b)
Brass
Wall thick. h=0.71mm
Cell dissip. E=5.84J
E. intensity Q=5.1

(c)
Al-alloy
Wall thick. h=0.71mm
Cell dissip. E=3.87mm
E. intensity Q=7.9

Fig. 2. High speed photographs of crushing in metal

honeycombs for impact speeds V(0) = 27-32 m/s
and impact energy intensities Q = 3.04-7.9.
Final crushing x is proportional to Q.

(i) ~:

(ii)

0 0001 0002 0003

Tint (s)

0<A
(iii)
06 -
/__
0-4-
-j^Z* \\*' .
.--' /''♦ 14...-
..:---;
02- ■'\i'

km?\^££ -:*£:.:■£:"•"*$:
0 -
S!_j
0001 0-002
Timt Is)

(b) Brass, Q = 5.1 (c) Al-alloy, Q = 7.9

Fig. 3. Transient response of honeycombs b and c:

(i) deceleration of colliding body; (ii) force
transmitted at distal surface; (iii) deformation
of individual cells numbered from impact surface.
380
significant role in controlling distribution of crushing in lightweight
open-celled foams and honeycombs.

EXTENT AND DISTRIBUTION OF CRUSHING STRESS

In each cell, crushing initiates when the stress state equals the collapse
stress for a mode of deformation (Klintworth and Stronge, 1988). As a cell
begins to deform, large changes in geometry decrease the stress required to
continue deformation; at an intermediate phase of cell deformation there is
a reduction in the crushing stress by a factor as large as 1/2 (Stronge and
Shim, 1987). The extent of strain-softening during the intermediate phase is
largest for asymmetric modes and almost negligible for symmetric modes of
cell deformation. Hence if microinertia is sufficient to decrease the
compliance to the extent that deformation occurs in a symmetric rather than
an asymmetric mode, the transmitted forces are substantially increased. In
any case, if deformation continues in a layer of cells, interference between
cell surfaces and increasing constraint from neighbouring deformed cells
finally decreases mobility and causes strong strain-hardening during the last
phase of densification.

The distribution of crushing through the thickness of a cellular protective

barrier mainly depends on the impact energy intensity Q where Q = kinetic
energy of colliding body/energy absorbing capacity of impacted layer of
cells. Figure 2 depicts impact against 3 honeycombs composed of tightly
packed arrays of thin-walled metal tubes. A quasi-static pattern of crushing
develops if the impact intensity is small; in test (a) the crushed region
expands from the distal surface after an elastic stress wave is reflected
from this immobile end. Crushing at the distal surface is dependent on
accelerating most of the barrier to a critical speed v = a/pc. At a larger
impact intensity (c), cell collapse begins at the impact (proximal) surface
and it progresses into the array from this site. The barrier continues to
crush at the impact surface until the central core has been accelerated and
the colliding mass decelerated to almost the same speed. Whether the
intensity is large or small, strain-softening cell behaviour causes cell
collapse to steadily progress from one layer of cells into the next as
evidenced by the deformation of individual tubes in a column, Fig. 3.

The decelerating force is usually largest during an early phase of collision

before effects of large deflection (strain-softening) have reduced the
crushing force (Rosa and Fortes, 1988; Reid et al., 1989). For the
honeycombs in Fig. 2, forces at both the impact and distal surfaces show this
initial peak and subsequent decrease to a plateau level of crush force for
the honeycomb. Despite the initial peak, most deformation takes place at the
plateau level of stress so final crushing of the barrier is almost directly
proportional to impact energy intensity Q (Stronge and Shim, 1987).

CRUSHING STRESS ENHANCEMENT BY MICROINERTIA

Because of strain-softening, dynamic crushing is localized in a thin

deforming band where strain-rates are very large. In this band, buckling of
cell walls is the usual mechanism for plastic cell collapse; buckling motion
is resisted however, by inertia of the cell walls. Effects of microinertia
increase the crushing stress and diffuse the localized deforming region.
Diffusion of elastic waves is significant for wavelengths that are comparable
with the cell size L; a measure of this diffusion is the ratio of phase
 381
speed c in a regular hexagonal honeycomb with microinertia to phase speed
c for the same structure without microinertia:
o
C/CQ = 1 - (TTL/X) 2 .

Figure 4 shows small increases in the initial peak stress during 'plane
strain' crushing of aluminium honeycomb at 1.6m/s; in these high-rate tests,
the strain-rate in a layer of cells was on the order of 10 2 s -1 . A large
deflection analysis of cell collapse was used to calculate the enhancement of
peak stress due to microinertia in dynamic tests (Klintworth, 1988). For
this honeycomb, microinertial enhancement was increasingly important at
strain-rates above 10 s" . In Fig. 4 the data points represent measurements
of crushing stress for 'plane strain' compression in transverse principal
directions f and 17. Although this data contains considerable scatter it does
show the same trend as the theory. The analysis indicates that effects of
microinertia depend strongly on mode of deformation; they are largest for
asymmetric modes.

10 10 20
deflection (mm) deflection (mm)

001 0-1 1 10 100 1000 001 0-1 100 1000

strain rate (s~1) strain rate (s*

Fig. 4: Measurements of dynamic transverse crushing

force for 30 mm thick aluminium honeycomb
with cell size ~ 5 mm. Lower graphs compare
measurements of peak dynamic stress with
calculation of enhancement by microinertia.
382
DISCUSSION

Because of post-yield strain-softening and subsequent strain-hardening during

densification, impact forces transmitted through cellular materials exhibit
several stages depending on the impact intensity. If the impact energy
intensity Q is not much larger than unity, cells near the impact surface
experience small deformation in a symmetric mode that is relatively stiff.
Large crushing of individual layers of cells initiates only after an elastic
wave passes through the barrier and is reflected from the immobile rear
(distal) surface. Alternatively, larger values of Q have sufficient energy
absorbed by layers of cells at the surface so that these cells are driven
into the range of large deformations; then strain-softening in more
compliant asymmetric modes of deformation becomes prevalent. Hence if Q>6,
impact results in crushing that initiates at the impact surface and proceeds
sequentially through one layer of cells after another.

Two dynamic effects increase the crushing stress if impact energy intensity
is large. Microinertia stabilizes the more compliant symmetric modes so it
increases the crushing stress (particularly the initial peak) and diffuses
the crushing wavefront. At larger strain-rates there is also 'shock'
enhancement due to cell collapse that is overdriven during densification.

REFERENCES

Gibson, L.J., M.F. Ashby, J. Zhang and T.C. Triantafillou (1989). Failure
surfaces for cellular materials under multiaxial loads - I. Modelling.
Int. J. Afech. Sci. , 31, 635-663.
Greene, S.J., F.L. Schierloh, R.D. Perkins and S.G. Babcock (1969). High
velocity deformation of polyurethane foams. Exp. Mech. 9, 103-109.
Klintworth, J.W. (1988). Dynamic crushing of cellular solids. Ph.D.
Dissertation, University of Cambridge, U.K.
Klintworth, J.W. and W.J. Stronge (1988). Elastoplastic yield limits and
deformation laws for transversely crushed honeycombs. Int. J. Mech. Sci.
30, 273-292.
Maiti, S.K. L.J. Gibson and M.F. Ashby (1984). Deformation and energy
absorption diagrams for cellular solids. Acta Metallurgica 32, 1963-1975.
Reid, S.R. and W.W. Bell (1984). Response of one-dimensional metal ring
systems to end impact. In: Mech. Prop, of Mat. at High Rates of Strain
(J. Harding ed.) 471-478. Inst. Phys., London.
Reid, S.R., C. Peng and T.Y. Reddy (1989). Dynamic uniaxial crushing and
penetration of wood. In: Mech. Prop, of Mat. at High Rates of Strain
(J. Harding ed.) 535-542. Inst. Phys., London.
Rosa, M.E. and M.A. Fortes (1988). Rate effects on the compression and
recovery of dimensions of cork. J. Mat. Sci. 23, 879-885.
Shim, V.P.W., B.Y. Tay and W.J. Stronge (1990). Dynamic crushing of
strain-softening cellular structures - a one-dimensional analysis.
J. Engr. Mat. Tech. H 2 , 398-405.
Stronge, W.J. and V.P.W. Shim (1987). Dynamic crushing of a ductile
cellular array. Int. J. Mech. Sci. 29, 381-406.
Stronge, W.J. and V.P.W. Shim (1988). Microdynamics of crushing in cellular
solids. J. Engr. Mat. Tech. H O , 185-190.
Throne, J.L. and R.C. Progelhof (1984). Closed cell foam behaviour under
dynamic loading - I. Stress-strain behaviour of low density foams.
J. Cellular Plastics 20, 437-442.
WS2d4

ELASTIC WAVE PROPAGATION IN A METAL MATRIX COMPOSITE REINFORCED

BY PARTICLES WITH INTERFACIAL LAYERS

Y. SHINDO
Department of Mechanical Engineering E,
Faculty of Engineering, Tohoku University,
Aramaki-Aza-Aoba, Aoba-ku, Sendai 980, Japan

H. NOZAKI
Department of Mechanical Engineering,
Tokyo National College of Technology,
Kunugida-machi 1220-2, Hachioji 193, Japan

ABSTRACT

This study considers phase velocity and attenuation in an SiC-particle-

reinforced Al composite with interfacial layers. The effective complex
wave numbers follow from the coherent wave equations. Numerical results
are obtained and the effect of interface properties on phase velocities and
attenuations of coherent plane waves is discussed in detail.

KEYWORDS
Metal Matrix Composite; Particle-Reinforced Composite Material; Ultrasonic
Inspection; Stress Wave; Interface Layer; Phase Velocity; Attenuation

INTRODUCTION

The processing condition in the metal-matrix composites often induce the

interfaces surrounding inclusions(Datta and Ledbetter, 1986a, Datta and
Ledbetter, 1986b, Paskaramoorthy et al., 1988). In the present paper, we
study the scattering of time harmonic plane compressional and shear waves in
a metal-matrix composite with interface layers. The scattering of plane
elastic waves by a spherical inclusion with an interface is analized and the
results of the single scattering problem are applied to the composite
medium. Numerical results for SiC-particle-reinforced Al composite are
obtained and the effect of interface properties on phase velocities and
attenuations of coherent plane waves is discussed in detail.

STATEMENT OF THE PROBLEM AND SCATTERING FIELD

We consider a random distribution of identical spherical inclusions of

radius a 0 in an infinite matrix. Let A , fi , p , v be the Lame constants,
the mass density, the Poisson's ratio of the matrix, and A o , flo , Po» Vo
those of the inclusions. We assume that thick layers of uniform thickness
383
384
h with variable material properties are present at the interfaces
separating the matrix from each sphere.

In order to study the scattering of plane waves in a metal-matrix composite

with interface layers, we first consider the scattered field due to a single
spherical inclusion with an interface layer. The geometry is depicted in
Fig. 1 where (x, y, z) is the Cartesian coordinate system with origin at
the center of the sphere and (r, 6, (f> ) is the corresponding spherical
polar coordinate. The layer is subdivided into several thin shells and the
material properties within each shell of inner radius fly-i, outer radius
<2 / ( j = 1 — w ) and uniform thickness hj=aj—aj-i are A y , l± j , p / , Vj.
Let the components of the displacement vector u in the r -, 6, <t> -
directions be labeled by ur, u e, u * and the corresponding stress
components be <7 r r , ore , Or* .

We consider a plane longitudinal(P) wave propagating in the positive

£-direction or a plane shear (S) wave polarized in the x -direction and
propagating in the positive z -direction. Thus,

ul =w0exp[ i(kPz-(ot)]ez + u0exp[ i(ksz — <ot)]ex (1)

where a superscript i stands for the incident component, a) is the circular
frequency of the wave, t is the time, ex , ez are unit vectors in the x -,
Z -directions and w 0 , Uo are the amplitudes of the incident P and S
waves. kPf ks are the wave numbers of the P and S waves in the matrix,

ks = - a> (2)
Cp cs
C p, cs are the longitudinal and shear wave speeds in the matrix,

>-(¥*)'
rA+2/z\1/2 = / fi \ 1 / 2
c (3)

INCIDENT WAVES

Fig. 1. A spherical inclusion with an interface layer

and incident waves.
 385
In what follows, the time factor exp(— i co t ) will be omitted from all the
field quantities.

The boundary conditions for the scattered field are

Ur = Ur + Ur Orr = Orr + Orr

n S , i
U 8= U B+ U 6 (4)
n s , i n s i
U*= U + + U4 Or += Or + + Or *

J J J +1
Ur = ur Orr = Orr
J j y+i
( r = a/ f y =1— 72—1)
y+i
Ue = Ue Or e= Or e (5)
J j y+i
u+ Or *= Or *
u* =
t l

urt = Ur1 Orr

t
— Orr
1
Ue = Uo Or e— Or B ( r = a0) (6)
t I
Or *= Or *
u*=u*
where superscripts 5 , t and j , j + 1 ( j — 1 ~ n — 1) stand for the scattered
component within a matrix, the transmitted component within a spherical
inclusion and the field quantities within each layer.

It is easily shown that at a large distance from the sphere we have the
scattered field:

p
ur ~ e g(9, <t>)
r
ue ~ — eik*' hA9,<t>) (7)
r
u\ — eik*r hA9,<t>)
r
The function g (0 ,</>) is termed the far-field scattering amplitude for the
scattering P waves, and the functions hi(9,<f>) and h*(9,4>) the far-
field scattering amplitudes in the 9- and </> - directions, respectively, for
the scattered S waves.

The scattering cross sections for incident P and S waves are then (Barratt
and Collins, 1965)

(8)
kP
An
Zs= — — Im [cos0/*i(O, 0 ) - s i n 0 A«(0. <£)] (9)
ks
Once the scattered field due to a single inclusion is known, the phase
velocities and attenuations of the coherent waves through the composite can
be easily calculated. At low concentrations of inclusions we can use the
following dispersion relations(Foldy, 1945)
386

(10)
. k, . k p do
2
' Ks ' 3c
= 1 + ——^- {cos0/ii(O,
Icos <t> h 0)-sin0/i 2 (O, 0)} (11)
. fcs . ks do

where c is the volume concentration of randomly distributed inclusions in

the matrix and KPf Ks are the wave numbers of the effective P and S
waves.

NUMERICAL RESULTS AND DISCUSSIONS

To examine the effect of interface properties on the phase velocities and

attenuations of coherent plane waves through the composite medium, the far-
field scattering amplitudes have been computed numerically. The considered
composite was an SiC-Al composite. The constituent properties are given in
Table 1. We consider the case of the interfacial material through which the
elastic properties vary linearly from those of the inclusions to those of
the matrix. The material properties of the layer are calculated at the
midpoint of each layer.

In Figs. 2 and 3, the scattering cross sections £p/do, Zsldo of the P

and S waves are plotted as functions of the frequency a o 0) IC s for c = 0 . 0
and h I a o = 0 . 5 . Case (A) refers to the case in which the interface
material possesses the same properties as the inclusion. Case (B) refers to
the case in which the interface material possesses the same properties as
the matrix, that is the case of h I do = 0.0. The scattering cross sections
for constant interface properties are obtained by Paskaramoorthy et al.
(1988) using a finite element and eigenfunction expansion method.

Figures 4 and 5 show the variations of the phase velocities R e( k p IKP),

Re( k s /Ks) of the effective P and S waves with the frequency a o io IC s
for c = 0 . 1 , hi a0 = 0 . 5 . The phase velocities decrease with the frequency
and the interface effect increases the phase velocities. Figures 6 and 7
show the variations of the attenuations \m{KPlkP), lm(Ks/ks) of the
effective P and S waves with the frequency d o co IC s for c = 0 . 1 ,
h I d o = 0 . 5 . The attenuations increase with the frequency and the interface
effect on the attenuations is pronounced. The existence of the interface
layers produces greater values of the attenuations.

In conclusion, plane elastic wave propagation in a particle-reinforced

composite medium with interfaces has been analyzed theoretically and the
interface effects on scattering cross sections, phase velocities and

Table 1. Material properties of SiC-Al composite

SiC Al

Po(kg/m3) ^o(GPa) A0+2#0(GPa) p (kg/m 3 ) fi (GPa) A + 2 ^ (GPa)

3181 188.1 474.2 2706 26.7 110.5
 387
attenuations of the effective waves have been summarized in pertinent
drawings. Inspections of the numerical results show that the effects of
interface properties can increase them and depend on the frequency.

10 ' 10 :
( A^-H
( M ^
10 ° 10 '

- / / ( B ) " //

1//
/
/ / ( B )
10"' 10 °

10";
SiC-Al
c = 0.0
h/a o = 0 . 5
10'1 [/ SiC-Al
c = 0.0
h/ao = 0 . 5

lO'3 I . I . I i . i , lO2 , 1 \ ■ 1 i . i ,

0.00 0.40 0.80 1.20 1.60 2.00 0.00 0.40 0.80 1.20 1.60 2.00
aocj / Cs aocj / Cs

Fig. 2. Effect of interface Fig. 3. Effect of interface

on scattering cross on scattering cross
section versus frequency section versus frequency
for P wave scattering for S wave scattering

1.20 h 1 .40

\
1 . 15 1.30
" \ U )

"Z
^ \ ^ \ ( A )
1. 10 1 .20
SiC-Al SiC-Al
c = 0.1 c = 0. 1
h/ao = 0 . 5 D5
h/ao = 0 . 5
1 .05 1. 10
( B )
(B)

l . i . i i , i I . I .
1.00 1 .00
0.00 0.40 0.80 1.20 1.60 2.00 .00 0.40 0.80 1.20 1.6 2.00
BaCJ / C, aocj / c,

Fig. 4. Effect of interface Fig. 5. Effect of interface

on phase velocity versus on phase velocity versus
frequency for effective frequency for effective
P wave S" wave
388
lO"' 10 °

^3
(
10': \)// 10"
! (n.
\ / / /
10": 10":

SiC-Al SiC-Al
I /( B ) c=0. 1
h/ao = 0 . 5 1 /{B) c = 0. 1
h/ao = 0 . 5
10" 10":

10"; . i . i I . I .
10- 1 , 1 , 1 i . i .
0.00 0.40 0.80 1.20 1.60 2.00 0.00 0.40 0.80 1.20 1.60 2.00
aocj / Cs aocj / cs

Fig. 6. Effect of interface Fig. 7. Effect of interface

on attenuation versus on attenuation versus
frequency for effective frequency for effective
P wave S wave

REFERENCES

Barratt, P. J. and W. D. Collins(1965). The scattering cross-section of

an obstacle in an elastic solid for plane harmonic waves. Proc. Camb.
Phil. S o c , 6J_f 969-981.
Datta, S. K, and H. M. Ledbetter(1986a) . Ultrasonic characterization of
material properties of composite materials. In : Proceedings of the tenth
U. S. National Congress of Applied Mechanics (J. P. Lamb, e d . ) , pp. 377-
387.
Datta, S. K. and H. M. Ledbetter(1986b). Effect of interface properties on
wave propagation in a medium with inclusions. In : Mechanics of Material
Interfaces(A. P. S. Selvadurai and G. Z. Voyiadjis, e d s . ) , pp. 131-141,
Elsevier, Amsterdam.
Foldy, L. L.(1945). The multiple scattering of waves. Phys. Rev., 67, 107-
119.
Paskaramoorthy, R., S. K. Datta and A. H. Shah(1988). Effect of interface
layers on scattering of elastic waves. ASME J. Appl. Mech., 55, 871-878.
WS2d5

UNDERWATER EXPLODING WIRES

AND
PRESSURE WAVE GENERATION

Y.IMAIDA and T.HIRAI

Department of Mechanical Engineering, Doshisha University

Imadegawa Karasuma, Kamikyo-ku
Kyoto, JAPAN

ABSTRACT

The exploding wire phenomenon has become a matter of great scientific inter-
est and is being applied to a variety of industrial technology. The electro-
hydrauric forming method makes use of an electrically energy source across a
pair of electrode, which are usually bridged by an exploding wire. It is
necessary to consider various phenomena for the study of this process, par-
ticularly the wire explosion, and generation and propagation of an impulsive
pressure wave. The wave forms of the discharging current and the dischraging
voltage are measured on various spark conditions and image converter camera
is used to observe the wire explosion and its impulsive pressure wave. The
pressure wave is mainly generated during the vaporization stage and it is
observed by the Schlieren photography method.

KEYWARDS

High-energy rate forming, Exploding wire, Shock wave, Discharge.

INTRODUCTION

It is necessary to discuss the exploding wire phenomena, and generation and

propergation of the impulsive pressure wave generated by wire explosion. The
discharging current through the exploding wire and voltage across the spark
gap are measured by constituting a perfect symmetrical measuring circuit, and
a high speed camera is used to observe the electric and hydrauric phenomena
of the exploding wire. In the wave form of the current and the voltage,
discontinuity points appear as the phase of exploding wire changes from a
solid phase to a liquid phase, and then to a vapour phase. The discontinuity
points are closely affected by spark conditions. The electrical character-
istic of the spark gap and the behaviour of exploding wires are made clear.

389
390

EXPERIMENTAL EQUIPMENTS

The basic circuit of discharging equipment is shown in Fig.l. The equipment

used in this research consists of two main coponents, an electric powre sup-
ply unit and a forming unit. The electric power supply unit consists of a
heavy current impulse generator, whose main parts are a capacitor bank, a
charging devise, a switching apparatus and a control unit for carrying out
the required operations for processing. The maximum electric energy stored
in the capacitors is 45KJ; the maximum operating discharge voltage is 30KV,
and the total capacity is lOOyF. Specially designed heavy current coaxial
cables are used for all connections between the power supply unit and the
forming unit so as to decrease the dischargeing circuit inductance which
greatry influences the forming effect. The inductance of the discharge cir-
cuit is kept below 7yH. The wave form of the discharging current on a short
curcuited load is the damped oscillation type and its frequency is about 20
KHz. The power supply unit is designed so as to regulate the charging vol-
tage continuously from 0 to 30 KV. A change of the connection of coaxicial
cable in the power supply unit can select the capacity from 2yF to 100 yF.
The electric power supply unit is contained in a completely grounded steel
cabinet. To prevent the leakage of the magnetic flux, the coaxicial cables
and the coaxial type connecting parts are used in all discharging circuits.
Thus the magnetic induction generated in the discharging circuit by the im-
pulsive heavy current is reduced in significance. The inductance and the
resistance of the discharge circuit are 5.86 yH arid 0.068 ft respectively.
The discharge switch is mounted in series with the underwater spark gap.
The discharge begins between electrodes with an initiating wire in water
after a high voltage pulse is given to a gap switch. The aluminium, copper
and tungsten wire from 0.1 to 0.6 mm in diameter are employed as exploding
wires.

The Schlieren photograph method is used to observe the generation and prop-
agation of the impulsive pressure wave generated in the initiating wire by
the action of the rapidly expanding exploding wire. In this experiment, we
have used an image converter camera "IMACOM 790" in the framing mode.

The discharge current through the exploding wire and voltage across the
spark gap are observed with an oscilloscope of the rise time is 3.5 ns.

The pressure induced by the exploding wires is measured by a pressure trans-

ducer "KISTLER 6221" which is set in the horizontal position from the cen-
ter of the exploding wire at the distance
of 30 to 100 mm (shown Fig.2). The
tansducer is conneted with a low noise
and low capacity coaxicial cable to a O-
n Wire

charge amplifier and output is observed

with an oscilloscope. o'

9JL (V) Control device

V
600
Pressure
@ High voltage supply T __i-°- sencer
0 Condenser
1->"-"]
- 0

0 Switch 1/ -jAmprefire |
0 Work piece 0
0
0 Exploding wire CM j Oscilloscope|
0 Electrodes
F i g . l Experimental arrangement for Fig.2. Arrangement for pressure
electro-hydrauric forming. wave measurement.
 391

EXPERIMENTAL RESULTS AND DISCUSSION

An underwater discharge with an exploding wire causes following behaviours:

the start of discharge, the rise in temperature of the initiating wire, the
melting of the initiating wire, the evaporation of a wire, the formation of
a pressure wave and a gas bubble. It is considered that the generation of
a pressure wave by the underwater exploding wire is related to the rapid
evaporation of the initiating wire across electrodes.

In the wave forms of current and voltage, it is considered that the discon-
tinuity points will appear as the phase of exploding wire changes from a
solid phase to a liquid phase and to a vapour phase. The discontinuity
points are greatly affected by the spark conditions such as the material of
the initiating wire, the diameter and length of the initiating wire and the
charging voltage of a condenser bank. Fig.3 shows a wave forms of the
current through the exploding wire and the voltage across the spark gap.
The points, (a) (b) (c) (d) and (e) shows where phases change from a solid phase
to a vapour phase. The five points show the start of discharge, the end of
melting, the start of vaporization, the
end of vaporization and the start of the
arc discharge. The above current and
voltage waves suggest that the discon-
tinuity points are very much affected
by spark conditions. Fig.3 (A)(C) show
the points of phase change (b)(c)(d)(e)
have appeared in the first half-wave.
Fig.3 (B) shows that the point (b) has
appeared in the first half-wave of cur-
A TYPE, :700 A c'iv. 4320 V div. 5 us div. rent but the points (c)(d)(e) have ap-
Copper wire. Wire diame er 0.3 mm, Wire length 20 mm, peared in the second half wave of cur-
Charging voltage 14 KV, Charging capacitance 10 JJF.
rent wave.

Fig.4 shows the influence of charging

voltage on the current and voltage
across the spark gap. The initial rise
of the current and voltage wave increases
as the charging voltage increases. The
points of phase change appear clearly
as the charging voltage increases from
4 KV to 14 KV.
B TYPE, 38<40A/div. 2160V/div. lOps/div.
Tungsten wire. Wire diameter 0.4 mm, Wire length 20 m™,
Charging voltage 8 KV, Charging capacitance 10 uF.
25 25
4-mmk Voltage 1 14 1<v
> 20 10 1<v 20 <
15
n 1
1 15 -
0) 10 fi i- — n i
<v 10 .
o> 3*i»-\' A;"—- ^ •5 I
(0 b
- - ^ __
,, c S^-c.—
o 0 py£^ ^ 0 ±
> -5
\ V * * «. . --> p -5
-10 -10
10 20 30 uo 50
C TYPE 1540A/div. 4320V/div. 5 us/div. Time (ps)
Copper , Wire diameter 0.2 mm. Wire length 20 mm,
Charging voltage 4 KV Fig. 4. Influence of charging voltage
Charging capacitance 10 uF.

Fig.3.The wave forms of current and on the wave forms current and
voltage voltage.(Al 0.2mm in dia. 20mm
in length, 10 yF)
392
The wave form of the current and voltage allows us to caluculate the amount
of power through the discharging channel and the amount of resistance of the
spark gap. The results of the caluculation are shown in Fig.5 and Fig.6.
The maximum power through the discharging channel appears at the time when
vaporization ends. The position of the maximum in the power on a power-time
diagram moves toward the beginning of the discharge as the discharging volt-
age increases, and at the same time can be seen increase in absolute value.
The rise of the discharging energy increases with the increase in the
charging voltage.

Fig.6 shows the resistance of exploding wire. The resistance between elec-
trode keeps at a constant value (87mfi) for the first 13 microseconds after
break down, and then only slightly increases. When the point of the phase
change appears it increases rapidly.

1.5

Iii
Icharging voltage
O 1.6 kV
-•> 1.4 kV \l i
■<*■ 1.2 kV w 1
■•- 1.0 kV

(X 1.0
r I

20 30 40
Time (ps)
Fig.5. The influence of charging volt-
=a*±8 T*6&*
age on the power and the dis- 10 20 30 40
chraging energy.(Al,0.2 in dia. Time (ps)
20mm in length, lOuF) Fig.6.Relation between resis-
tance and time.(Al,0.3mm in
dia, 25mm in length, 120uF)
Fig. 7 shows a typical oscillogram of
the pressure transducer arranged 50mm
apart from the center of the exploding
wire. In this photograph, the first
peak means a shock wave induced by
exploding wire. The rise time of a
pressure wave is 3 ys and the pressure
value of the peak is about 50 MPa.
The oscillation after the first peak
of the pressure wave may be due to the
reflection frequency of the trans-
ducer.

Fig.7 The oscillogram of pres

Fig. 8 shows the influence of a stand sure wave. (wire:Al, 0.3mm in
off distance on the maximum pressure dia. 25 mm in length, charging
value. The maximum pressure values voltage:1.6 KV, condenser ca-
decrease exponentially with the pacity: 120 yF)
 393
increase in the stand off distance. 70
The velocity of the pressure wave
is measured to be about 1500 m/s. (0
\
Fig.9 shows the relation between 30 ^kN &
charging voltage and maximum pres- C h a r g i n g voltage N
sure value at the stand off dis- 1 —O— 1.6 kV
!20
tance 50 mm. The maximum pressure 1 —©— 1.1 kV
values increase as charging voltage —O— 1.2 k V
increases. # 1.0 k V
10
Fig.10 shows the influence of the r<\ 1—1 1
initiating wire length on the 10 20 30 40 60 80 100
maximum pressure value on the Stand-off (mm)

stand off distance 50 mm. In Fig.8 Influence of stand off distance

the wire diameter of 0.2 mm, the on the maximum pressure value, (wire:
optimum wire length which generates Al,0.2mm in dia,25mm in length, 120uF)
maximum pressure is 20 mm, but 60
Chargimg Wire
in the 0.3 mm diameter, the optimum 1 voltage diameter
length is 25 mm. - O 1. 6 k V 0 . 3 mm
50 -©- 1 . 4 k V 0.2 mm

A
-O- 1 2 k V X
Fig.9 and Fig.10 suggest that the 1. 0 k V
optimum wire length and diameter "*" r' ,®v '
which generate the maximum pressure -40 \?

A*\
value deped on the spark conditions. J* N T
D /<
w 3G
i s
—iTT-—-J \
20
•
\
0 10 20 30
Wire length (mm)
F i g 10 Inf l u e n c of t h e w i r e l e n g t h
on t h e maximum p r e s s u r e v a l u e .
(wire:Al, capacity:120uF)
•° 1.2 1.4 1.6
Charging voltage (kV) 60
Wire Wire
Fig.9 Relation between charging 50 h
length diamete r
voltage and maximum pressure
r
O 10mm 0.2mm
*m 40 h ® 10 0.3 •
volue.(wire:Cu,capacity:120uF) © 20 0.2
raffi

w L CD 20 0.3 .
30
©25 0.2
<u ©25 0.3
Fig. 11 shows the influence of the v. • 30 0. 3 m /
power during vaporization on the max- ^ 20
imum pressure value of the aluminium
wire plotted on a log scale. The re-
lation between the power during vapor-
ization and the maximum pressure value 10
lies almost on a straight line and 1 5 10 15 2 0 2 5
its exponent is 0.6. The experimental Power during vaporization (kW)

data suggest that the pressure gener- Fig.11 Influence of power during
ated by the exploding wire is deter- vaporization on the maximum pres-
mined by the discharging energy sure value.(wire:Al)
during its vaporization.
394
Fig.l2-(A),(B),(C) are show the photographs by Schlieren method to observe
the formation and propagation of the pressure wave generated by' the explod-
ing wire. Fig.l2-(D) shows the current wave through the spark gap and the
voltage across electrodes under the same condition as in the case of Fig.12
(A),(B),(C). As the vaporization starts, one [shown Fig.l2-(A)] or a few
[shown Fig.l2-(B)] spots of exploding begin to appear in the initiating
wire : then a spot (£r spots) rapidly expands in uniformity around its
center and generates a pressure wave. The pressure wave continues to
propagate and forms approximately a spherical front as shown Fig.12-(A),(C).
Many uniform spots do not appear in the initial stage : but when the first
spot appears, then second and third spots follow. Those spots are uniform-
ly produced along the wire and many pressure waves are observed in the ex-
ploding wire as shown in Fig.12-(B). Then we see the formation of the
pressure wave by the exploding wire, spreading over many small pressure
waves formed around each spot.

CONCLUSIONS
In the wave forms of the current and voltage, discontinuity points appear
as the phases of the exploding wire change : and discontinuity points are
greatly affected by the spark conditions. The pressure generated by the ex-
ploding wire very much depends on the discharging energy during its vapori-
zation. The formation of the pressure wave by the exploding wire is photo-
graphed, spreading over many small pressure waves formed around each spot
along the exploding wire.
REFERENCES
Isuzugawa, K.,M. Tsuji, Y. Okumura and M. Horiuchi,(1989). High-speed photo-
graphic study of spark-induced shock waves in water, ISEM-9. 289-292.
Robinson, J.W.,(1973) Finite-difference simulation of an electrical discharge
in water. J.Appl.Phys., 44-1, 76-81.
Skvortov, Y.V., V.S. Komel'kov and N.M. Kuznetsov (1961). Expansion of a
spark channel in a liquid. Sov.Phys. Tech.Phys.,5, 1100-1112.

24fis 27fis 30/xs 23/xs 30/xs 33/xs

(A) Front view (B) Front view (with 3 spots)
1 . v Q> *y Voltage 1
y^
7\ \ Current 1 <
s'

? to 1 / /
/ 7c \\
o
> o I/A/ \>
e 3
E X-
28/ts 33/xs 38/xs u
(C) Side view (D) Current and voltage T i m e <Ms)
Fig.12 Photograghs of the pressure waves generated by the exploding wire,
and the current and voltage wave. (wire:Al, 0.3 mm in dia. ,25 mm in length,
charging voltave:1KV,condenser capacity:120uF)
WS2e1
Shock compression of A1N ceramics

A. NAKAMURA and T. MASHIMO

Faculty of Engineering, Kumamoto University

Kumamoto 860, Japan

and

M. KODAMA

Kumamoto Institute of Technology

Kumamoto 860, Japan

Abstract

Hugoniot-measurement experiments of the aluminum nitride (A1N)

sintered ceramics were performed in order to study the shock
yielding property, phase transition, etc. Two type specimens
of the Y2O3 (6.2 wt%)-doped and pure polycrystal were used to
examine the doping effect. The Hugoniot parameters were
measured by means of the inclined-mirror method combined with
the keyed-powder gun. Although the Hugoniot-elastic limit
(HEL) stresses of both the specimens were almost same (7-10
GPa), it was pointed out that the Y20g-doped one maintains a
fairly shear strength, however, that the pure one loses a
comparatively large shear strength above the HEL.

KEYWORDS
Aluminum nitride; A1N ceramics; Shock compression; Hugoniot
compression curve; Hugoniot-elastic limit; Yielding property;
Powder gun; Inclined-mirror method; Doping.

INTRODUCTION
Mechanical properties or phase transitions of brittle materials
under shock compression depend strongly on the crystal-
chemical properties, thermophysical properties, fine structure,
etc.. However, the correlations of them and the mechanism have
not been so far well understood. Although so many fine
ceramics whose fine structure, such as crysttal particle shape
and size, doping, porosity, crystal domain, etc., have been
developed, the effects of their differences on the shock-wave
phenomena have not also been unknown. On the other hand, it
has been pointed out that the heat conductivity is strongly
related to the yielding property of brittle material through
the shear banding phenomena (Davison and Graham, 1979; Grady,

395
396
1980). However, we (Mashimo et al., 1988; Mashimo, 1988)
suggested that the chemical-crystal state should be included as
factors deciding shock yielding properties, rather than the
thermophysical properties, on the basis of the Hugoniot results
of A1 2 0 3 (Grady, 1980), Zr0 2 (Mashimo, 1988; Mashimo et al.,
1990a), Si 3 N 4 (Mashimo et al. , 1990b) etc. In order to clarify
the corelation and mechanism of the shock yielding of brittle
materials, the Hugoniot data should be measured for many
materials including ones with good conductivity.

Aluminum nitride (AIN) ceramics have been used for heat-

transfer materials and corrosion-resistant materials, and the
mechanical and thermal properties under static conditions have
been well investigated, so far. However, the dynamic
properties of this material has not been well investigated. In
the present study, the elasto-plastic properties of AIN under
shock compression up to 40 GPa were studied particularly
considering the effect of doping. For this purpose, the
Hugoniot compression curves of the Y2C>3-doped and pure AIN
sintered ceramics (polycrystal) with almost the same porosities
were measured by means of the inclined-mirror method.

EXPERIMENT

The plate-shaped ¥203(6.2 wt%)-doped and pure polycrystals of

approximately 5.5 mm in thickness and about 20X20 mm in width
were provided by the Sumuitomo Electric Industries Ltd.,. The
bulk densities of the Y203-doped and pure ones are measured to
be 3.314-3.318 g/cm3 and 3.198-3.201 g/cm3 by the Archimedean
method, respectively, whose porosities are about the same (1.3-
1.6 %). The ultrasonic measurement were performed by means of
the pulse-echo method (Kodama, 1985), using the specimen of
approximately 25 mm in length.

In the inclined-mirror method (Mashimo, 1989), shock waves were

produced by high-velocity parallel plate impact method using
the keyed-powder gun (Mashimo et al., 1984). Copper or tungsten
plates of about 1 mm in thickness, and tungsten, copper, or
aluminum plates of 1-3 mm in thickness were used as the driver
plate and the flyer plate, respectively. These plaxes and
specimens were ground parallel and polished to an accuracy of
2-3 jUm. A xenon-flash lamp was used as a light source. All
light from mirrors on the driver plate and the specimen is
routed to a mirror-rotating type streak camera. The particle
velocities of the elastic wave were analyzed by the free-
surface approximation method, and those of the plastic wave
were analyzed by the impedance-matching method. The Hugoniots
of the flyer plates and the driver plates (Al, Cu, W) used are
from Ref. (McQueen et al., 1970). The impact velocities of the
flyer plate were measured by the reflected-light method or
magneto-flyer method within an accuracy of 0.2 % (Mashimo,
1989). The shock velocities of the the plastic waves were
analyzed considering the interactions of shock waves and
rarefaction waves (Ahrens e t a l . , 1968).
 397

Fig. 1. Typical streak photograph by the inclined

-mirror method, when the specimen is the
pure polycrystal, and the impact velocity
is 1.362 km/s.

RESULTS AND DISCUSSION

Figure 1 shows a typical streak photograph by the inclined-
mirror method. In this figure, the copper flyer plate and the
tungsten driver plate are used, and the specimen is the pure
polycrystal at the impact velocity of 1.362 km/s. A slightly
dull kink is observed in the image of the inclined mirror.
This image is analyzed as a two wave structure in this study.
At points 1 and 2, the initial waves arrives at the rear
surfaces of the driver plate and the specimen, respectively,
and at point 3, the plastic wave arrives at the rear surface of
the specimen. In this case, the stresses of the elastic wave
and the plastic wave are analyzed to be 7.6 GPa and 18.7 GPa,
respectively.

Figure 2 shows the Hugoniot results between shock velocity

(Ug) and particle velocity (U ). The elastic wave velocities of
398

12
T ■
o Pare polycrjstil
11 nT 2 0,-doped polycrysta 1
CO
v . 10
m

' 9 L-

o 8

a>

*- 7
^d

o 6

4 J. JL
0 1.0 2.0
Particle v e l o c i t y — km/s
Fig. 2, Us-U Hugoniot results of the Y2C>3-doped
and the pure polyctystals

the Y2C>3-doped and pure polycrystals were consistent with the

longitudinal sound velocities, of 10.65 and 10.79 km/s,
respectively. In the plastic region, the shock wave velocities
of Y20g-doped one are higher than that of pure one. The Ug-U
relation can be closely described by the method of least
squares, as follows:

U =7. 04+1.29U_ (km/s): Y2C>3-doped polycrystal. (1)

23
L

U s = 5. 22 + 2. 11U (km/s): pure polycrystal. (2)

Figure 3 s hows the stress-density Hugoniot results which

calculated f rom the U s - U data. The Hugoniot-elastic limit
(HEL) stress es of th e Y203~doped and pure polycrysta Is are
determined to be 7.8-9 .8 GPa and 7.6-9 4 GPa, respectively. The
shapes of th e compres sion curves abov e the HEL's of the Y 2 0 3 -
doped and pu re ones a re different (li near and concave shapes,
respectively) This fact shows a difference in y ielding
property in the plas tic region betwe en these A1N ce ramies,
although the HEL st resses are almos t the same. Th e bulk
modulus ( K Q ) of the Y 2 03-doped and pur e ones were determ ined to
be 203.0 and 204.4 GPa , respectively, from the ultrasoni c data.

Figure 4 shows a model diagram of perfect elasto-plastic solid,

quasi-elasto-plastic solid and elasto-isotropic solid with
static compression curve to understand yielding properties of
solids under shock compression. In the figure, the elasto-
plastic solid behave as a rigid body even in plastic region and.
 399
50

40
o Pun poljcrystil
a T e0 3-Doptd poly crystal
30

20 h

10
HEL

3.0 3.5 4.0

Density - g/cm3
Fig.3. Hugoniot-compression curves of the
Y
2 0 3 - c * o P e c * a n c * t n e P u r e polycrystals.

maintain a considerable large offset from the static curve.

Metals have been usually included in this solid. On the other
hand, the elasto-isotropic solid catastrophically loses shear
strength above the HEL. Many brittle materials have been
included in this solid. Comparing the model diagram and the
measured ones (Fig. 3 ) , it is pointed out that the Y 2 03-doped
polycrystal behave as an elasto-plastic solid, however, that
the pure one may loses a comparatively large shear strength
above the HEL.

Generally speaking, the shock yielding properties are related

to the crystal-chemical properties, thermophysical properties,
fine structure, porosity, etc. In this case, the porosities and
heat conductivities of the Y 2 03~doped and pure polycrystals are
about the same. As a result, it is suggested that the doping
of Y2O3 strongly influences the shear strength of A1N ceramics
in the plastic region. Furthermore, the present result
suggests that the heat conductivity may not be ranked among the
big factors determining the shock yielding property of brittle
materials. Because the heat conductivities of A1N ceramics are
much greater than those of the other ceramics such as AI9O0,
Si3N4, Z r 0 2 , S i 0 2 , etc., and are as large as those of metals.
In order to clarify in detail the effects of the doping of
Y203, the recovery experiemnts shall be performed to observe
the fine structure of the starting and recovered specimens. In
addition, if the phase transition arise in the low stress
region, it may influence the yielding property. We are now
measuring the Hugoniot data of the denser pure A1N ceramics to
examine the phase transition.
400

Density
Fig. 4. Model diagram of the shock compression
curves of perfect elasto-plastic,
quasi-elasto-plastic and elasto-
isotropic solids, together with the
static compression curve.

ACKNOWLEDGMENTS

The authors would like to thank the Sumitomo Electric

Industries Ltd., for supplying the A1N ceramics.

REFERENCES
Ahrens, T.J., W.H. Gust and E.B. Royce (1968). J. Appl. Phys,
19, 4610.
Davison, L. and R.A. Graham (1979). Phys. Rep., 55, 255.
Grady, D.E. (1980). J. Geophys. Res., 85, 913.
Kodama, M. (1985). Phys. Chem. Glasses., 26, 105.
Mashimo, T., S. Ozaki and K. Nagayama (1984). Rev. Sci.
Instrum., 55, 226.
Mashimo, T. (1988). Shock Waves in Condensed Matter., 1987,
pp.285.
Mashimo, T., Y. Hanaoka and K. Nagayama (1988). J. Appl. Phys.,
63., 327.
Mashimo, T. (1989). Shock wave phenomena. Proc. 1988 Nat.
Symp. pp.105.
Mashimo, T., M. Kodama, K. Kusaba, K. Hukuoka and Y. Syono
(1990a). Shock Compression of Condensed Matter 1989,
pp.469.
Mashimo, T., A. Nakamura, K. Wakamori and M. Miyake (1990b). J.
Soc. Mat. Sci. Jpn.t 39, 1615.
McQueen R. G., S.P. Marsh, J.W. Taylor, J.N. Fritz, and W.J.
Carter (1970). In: High-Velocity Impact Phenomena (R. Kinslow,
ed.), Chap.7, pp.244-419. Academic, New York.
WS2e2

SHOCK MELTING OF SiC UNDER HYPERVELOCITY IMPACT

Zhang Ruoqi and Tang Wenhui

Department of Applied Physics,Changsha Institute of Technology,

Changsha,HunanyP. R. China

ABSTRACT
A three phase equation of state (EOS) for SiC is presented. Using a hydrocode simulation, the pro-
cess of solid-liquid transition under hypervelocity impact for SiC is investigated and the
pressure-temperature phase diagram of solid-liquid transition for SiC is obtained.

KEYWORDS

Hypervelocity impact; shock melting; SiC

INTRODUCTION

When a SiC target plate is striked by a hypervelocity flyer plate, it may be melted or vaporized, be-
cause of the high temperature caused by shock compress. This problem is very complex. The main
difficulty encountered with the computer simulation is that there is not reliable EOS for use in
hypervelocity impact.

This paper presents a three phase EOS for SiC (pg = 3.12? /cm , C a =* 8.13*m / s, S - 0.91) and
investigates the mechanical-physical process of solid-liquid transition under hypervelocity impact
for SiC, using a hydrocode simulation method.

EQUATION OF STATE

In general, the energy and pressure of matter can be written in the following form
E{T,p)~E9{p) + EB(T,p)+ Ef(T,p) (1)

401
402

where EQ and P are the cold energy and cold pressure, Em and P are the contribution of the atom
vibrations to the energy and pressure,while E and P are the electron thermal contributions.

The cold pressure was assumed to be expressed by

where a{ are six coefficients, p ^ ( « 1 / V9g) is the density of the matter at zero point (r « 0,P » 0
). Using the thermodynamic relation

we obtain the cold energy

based on Thomas-Fermi theory, the elctron thermal contributions are given by

i ...

where 0 is the electronic energy coefficient at zero point (r - 0,P * 0).

In order to describe the melting transition at high pressure, the following assumptions can be used
£}rover, 1971): (1) the entropy of melting is a constant ( » 1.16J?, where R represents the mole gas
constant); (2) the relation of the melting temperature Tm with volume V is given by Lindemann
law:

where y(V) is the GrQneisen coefficient; (3) the specific heat in the liquid state is given by

where a is a constant, T is the gaseous temperature, when T ^ T , that C « 3R / 2.

As a good approximation, we use the following GrQneisen coefficient

where p^ is initial density, and y# » y (/>,)■ Using (9) and (11), the melting temperature can be got

We define v as the progress variable for melting transition

 403

T ASo
26T-T-T=-Z—2 (15)
' \.2C\Fn
1 4- (45T— 1)(1 - l/<y), (c>\)
M (<r< 1)
where T and T are the temperatures on liquid us and solid us, \i is the average atom weight
permole, C # and S are the Hugoniot constants (D = C + Su). Then we obtain
Em = ORT+Em)/ n (17)
Pm = QyRpT + Pm)/ n (18)
(a) For T<Tm-dT (solid state)
tf.-^-O (19)
(b) For r w - &T < T < r^ + 3T (mixed-phase)
Em « v(r - var)(A5T - a) (20)
? B - kvpT mV±S - a) (21)
(c) For T +8T*T<T (liquid state)

*.-r.[A*-|(1 + ;r)] C2
>
^-ar.,p[A3f-|(i + ^-)] (23)
m

(d) For T > T (gas)

a
£ w = T B [A5f + | « - 1)] - C«r (24)

P B = A p I * B [ A 5 r 4 - | ( C 2 - 1)] -XptaT 05)

where £ = T / T .

RESULTS

In our calculations, the thickness of SiC flyer plate is 1mm, and the SiC target plate thickness is
6mm. Fig.l shows the pressure or temperature versus time at selected location which is 1.2mm from
the impact interface in target, the impact velocity is 11km / s. From Fig.l(b) one know, the target
material would remain solid state during shock loading. But during unloading, the target material re-
leases to a state in which there is partial melting, namely solid-liquid coexistance. Fig.2 shows the
time histories of the pressure and temperature at the same selected location in the target as before,
but the impact velocity is 12.5km / s. It may be found that the target material is in partial melting
state during shock compression, as release goes on, it would be turned into liquid gradually. After
full unloading, the mixed-phase region thickness of the target is about 4.3mm, and that in liquid
phase is about 2.3mm. It is notable that, at this time, the thickness of target had expanded into
6.7mm.

Changing impact velocity , we can get a series of melting temperatures and shock temperatures corre-
sponding to the various shock pressures (see Fig.3). For SiC material, the shock pressure which lead
404

to incipient melting or complete melting under shock loading is about 250GPa and 280GPa
respectively. The calculation also show that, upon release from a pressure about 200GPa on the
Hugoniot, the SiC material would begin to melt, and for release from a higher pressure (about
240GPa), SiC material would be totally liquid.

240

"i 1 1 1 r
1 1 1 T"^ r
0.0 0.1 0.2 0.3 0.4 0.5 0.0 0.I 0.2 0.3 0.4 0. 5
tQas)
t(ys)

(a) (b)
Fig.l Wave profiles in SiC target for SiC flyer plate impacting at
11km/s
(a) pressure vs time
(b) temperature vs time, the dashed curves represent phase bondaries.

-i 1 i r
-i 1 1 r~^ r
.0 0 . 1 0.2 0.3 0.4 0.5 0.0 0.1 0.2 0.3 0.4 0.5

t(JiS) Ujis.,

(a) (b)
Fig.2 Wave profiles in SiC target for SiC flyer plate impacting at
12.5km/$
(a) pressure vs time
(b) temperature vs time, the dashed curves represent phase bondaries.
 405

n 1 r
0 100 200 300
P(GPa)

Fig.3 The pressure-temperature phase diagram of solid-liquid transi-

tion for SiC

ACKNOWLEDGEMENT

We would like to thank professor Zhang Shize for assistance in presenting EOS of SiC.

REFERENCES

Orover, R. (1971). Liquid metal equation of state based on scaling. J. Chem. Phys.,
55. 3435-3448.
WS2e3

RATE EFFECTS ON CRACK PROPAGATION IN CONCRETE

AND BRITTLE FRACTURE OF CONCRETE STRUCTURES

J. TAKEDA and H. KOMOTO

Department of Architecture, Kumamoto Institute of Technology,
Kumamoto 860, Japan

ABSTRACT

The most difficult and important thing in dynamic design of structures

subjected to impulsive loadings is to take into consideration of rate effects,
especially unfavorable rate effects, for example brittlely rapid propagation
of cracks in concrete which is newly found in experimental study. This paper
deals with the rate effects on concrete and structural members and the study
on the prediction of unfavorable rate effects on concrete.

KEYWORDS

Rate effects; high rate loading test; brittle fracture of concrete; dynamic
fracture mechanics.

1. INTRODUCTION

It has been urgently required to develop the resistant impact and resistant
blast shock design method of structures, since the Chernobyl Nuclear accident.
The responses of structures under these impulsive loadings are governed by
the new constitutive equations which are changed by the loading rate, namely
rate effects. The rate effects, however, should be obtained in only high
rate loading tests which are carried out so as not make any disturbance and
any significant stress waves in specimens, because of the difficulty to
divide them from the effects.

The rate effects on concrete are divided into two effects, the first is on
the relation between stress and strain, and the second is on fracture crite-
rion and process of the fracture thereafter in which several unfavorable
rate effects for dynamic design of structures are eventually contained.

The above rate effects occur also in the tests in fracture mechanics on
concrete and make the changes not only on fracture toughness and various
constants in fracture mechanics, but also on the propagation speed of cracks
generated in the specimen during loading stage. This paper deals with the
rate effects on concrete based on the experiments of the authors by this time.
407
408
— i 1 1 1 1 1 \
10s 1 1 1 1—
concrete specimen concrete specimen
(W/C=0.55,15cm<J>x30cm) g (W/C=0. 55,15 e "0 X30 c ')
500 h cfb
£= 2000 ii /

w
o ° on
100

w 300

200

lOOh * £=250 n ° r
test -* 10
sile test-* 10"' 1 10 10* 103 10* 10s 10s
MEAN RATE OF STRAINING I (y/s)
10"' 1 10 10: 103 104 105 10G 107
STRAINING RATE e (y/s)

Fig. 1. Relation between rate Fig. 2. Relation between mean rate

of strain e and compressive of stressing 15 and mean rate of
stress a at the certain straining T.
values of strain.

2. RATE EFFECTS OBTAINED IN PRECEDING STUDIES

The rate effects on concrete have been already reported in ICM-1 based on
the experimental results carried out on various kinds of concrete and rein-
forced concrete structural members with the loading rate ranging up to about
10 times of that in static tests and various loading types, by the authors
(Takeda, 1971). These experiments were done under controlled applied load
so as not to make any disturbance and any significant stress waves, namely
by high rate loading tests. Summarizing the test results, the rate effects
on concrete are divided into two effects, the first is on the relation
between stress and strain in loading process before fracture begins and the
second is on fracture criterion and the fracture process thereafter.

By the first rate effect, the relation between the stress and strain of
concrete in loading process changes with the loading rate (or straining rate)
concern, as seen in Fig. 1 which shows an example and is indicating the ten-
dency that the stress a at a certain strain e increases gradually with the
increment of straining rate e, though there are considerably large deviations
between the data.

The stress and strain at the maximum stress point on the stress-strain curve
obtained in the test which is just the point at which the fracture of speci-
men begins, also change with loading rate by the second rate effect and the
relation indicated in Fig. 2, which is surprisingly neat, is obtained. The
similar relations to Fig. 2 have been found in all kinds of high rate load-
ing tests which have ever been done, not only on many kinds of concrete with
various mix proportions and with various types of loading (Fig. 3), but also
reinforced concrete structural members (Takeda,1971), wood, etc. Therefore,
it is considered that these relations must be quite fundamental relations
covering whole range of these high rate loading tests.
 409
The reason of the occurrence
of these rate effects is
explained by A.M.Freudenthal
by Statistical Physics in
terms of atomic structure
and derived next equation
on the rate of deformation
in the direction of the
applied load e,
kT
e = Cj—expC-q/nRT)
Sinh(&;/nRT) (1)
where C^ is a constant,k is
Boltzman's constant, h is
MO"5 10" lO'3 10" 10-' 1 10 10* Planck's constant, T is ab-
MEAN RATE OF DISPLACEMENT I (cm/s) solute temperature, q is
the energy level required
Fig. 3. Relation between mean rate of for activation, e^is the
stressing T and mean rate of dis- potential energy of applied
placement J in shear tests. load, R is gas constant and
n denotes a number of moles
(Freudenthal, 1950).
From this equation, Freudenthal has given explicit explanation on viscosity,
relaxation or the relation between straining rate and temperature, etc.

It is known that the straining rate e is proportional to the square of the

stress a at a certain strain e, from the equation (1), assuming that the
potential energy of applied load e$ is induced by elastic strain during the
test and using approximation of Sinh function. Accordingly, if the above
theory of Freudenthal is valid on the test data obtained in the compressive
test of concrete, shown in Fig. 1, the relation between £ and a at a certain
value of strain e must be expressed by a straight line in this figure, though
such tendency can be seen only within small range of both e and e. It might
be because the equation (1) is obtained in quasistatic equilibrium thermal
condition, and this shows that the responses of the specimens tested even
with high rate loading can not be explained by the equation (1). However,
it is entirely correct that the rate effects on concrete is based on thermal
effects.

3. SECOND RATE EFFECT AND BRITTLE FRACTURE OF CONCRETE

From the Fig.2, next equations of the mean stressing rate a and the mean
straining rate J,
S = o( I ) e , S/F = a m /e m - a( I ) 3 " 1 (2),(3)
are obtained, where a and 3 are both the constants which are influenced by
the kinds of the tests and specimens, and 3 is usually a bit larger than 1.00,
and crm,em are the stress and strain respectively at the maximum stress point
on the stress-strain curve obtained in the test. The equation (3) gives the
inclination of the secant line through the maximum stress point, which is de-
termined by the mean straining rate £ concern. Therefore it is considered
that the maximum stress point on stress-strain curve, namely the start of the
fracture of specimen, is determined by the equation (3).

The value of (3-1) in the equation (2) and (3) is usually positive, as men-
tioned above. Therefore, it is clear that the inclination of the above secant
410
mortar mean rate o( -
(15X15X50'" displacement d (cm/s)
/ M10(] ):4.66X10
- shear test
7 N15(H):1. 10
*\ M 1<S):1.76X10°

-Mioa yJ/
/ \

s~ 'f
1 / M 1(S)^
;MI5(DD\,'^^

1^"' /\^\

1000 2000 3000 4000 5000 0

1 ^^:
l^fe^^
<
0. 1
\! "1 "*~
!\!l.
0. 1
S T R A I N e (p) DISPLACEMENT 6 (cm)
(a) (b)
Fig. 4. The changes of stress-strain and stress-displacement
curves with the increment of mean rate of straining or
mean rate of displacement.

line increases gradually with the increment of the mean straining rate e
(Fig. 4 ) . There are two cases, however, as seen in (a) and (b) in the
figure, reflecting the both first and second effects stated above, which
work independently. In the case of the figure (a), the strain (or displace-
ment) at the maximum stress increases with the increment of the straining
rate (or displacement rate), and rather favorable rate effect for dynamic
design of reinforced concrete structures. In this case, comparatively small
value of (3-1), generally less than 0.02 is obtained in the tests (Takeda, 1
971). This was found in the high rate compressive, tensile and bending tests
on concrete and reinforced concrete structural members.

On the contrary, there is the case in which the strain (or displacement) at
the maximum stress decreases with the increment of mean straining rate (or
displacement rate) as seen in the figure (b), and in the highest rate of
loading, exceedingly brittle fracture is brought about on the specimens.
This is very dangerous and unfavorable rate effect for dynamic design of
structures. It was seen in shear tests on concrete, mortar, reinforced
concrete beam and even in the case of steel reinforcement only (Takeda, 1969)#

4. RATE EFFECTS IN DYNAMIC FRACTURE MECHANICS ON CONCRETE

The second rate effect, stated above, might be decidedly brought about by
the propagation of inner cracks in the specimen during the increment of
applied load, therefore, it is entirely natural that the same tendencies con-
cerning the rate effects are also seen in the tests of dynamic fracture
mechanics on concrete. Actually it has been found in the tests carried out
with the specimens of Mode I and II by the authors (Takeda, 1982, 1985).

Based on the data of Mode I test, the relation between the mean loading rate
P and the mean straining rate near the crack tip e a in the loading stage was
shown in Fig. 5. The mean straining rate e a is calculated from the measure-
ment of "strain gage G " which is stuck perpendicular to the initial crack
line at the distance of 8 mm from the crack tip. In the figure, the similar
tendency to Fig. 2 and Fig. 3 is also seen, except only a part in the high-
est loading rate of "specimen A", just in which curved propagation of cracks
was observed in the test as shown in the figure. It is already proved theo-
retically by Yoffe that at higher velocity the running crack in a media tends
to become curved. Therefore, it is inferred that the above tendency in the
highest loading rate on the "specimen A" was brought about by the large
 411
7
10 , , , , ,
acceleration, yielded in near part, r
to the cracks, rapidly propagating in
the specimen by the load application
in this test. The above inference,
HX 10s concerningJ:he bend of the line of
o log 7-log e a shown in Fig.5, is sup-
104 ported by many tests carried out with
high rate loading and especially by
the compressive test of sand layer,
in which the influences of acceler-
10' ation of sand particles may intrinsi-
^5" cally be intensified, reflecting that
specimen B the sand layer consists of independ-
<30 £ -x30 e "X5 e ") ent solid particles, and violent
specimen A-*10 10' 10 3 104 105 10G 107 liquefaction of sand layer is brought
spec imen B -» 1 10 10' 103 104 10s 10s 107 about in high rate loadings, for ex-
MEAN RATE OF STRAINING Ia ( y / s )
ample severe earthquakes (Takeda,196
9). It is considered that the rela-
tions deduced from the result of Fig.
Fig. 5. Relation_between mean 5, which are similar to that obtained
loading rate P and mean strain- from the equation (2) and (3)), may
ing rate £ in Mode I test. give the threshold value of applied
load namely fracture toughness influ-
enced by the loading rate concern, at
which the initial crack begins unstational propagation. Therefore, it is eas-
ily understood that the fracture toughness in fracture mechanics on concrete
also changes with the loading rate or the straining rate concern, as shown in
Fig. 6, and being governed by the similar to equation (2) and (3), and eventual-
ly violent brittle fracture of concrete may occur by high speed propagation
of cracks.

It has been already reported that the stress intensity factor, etc. also
change with the loading rate before fracture begins, and the propagation
speed of cracks in concrete under high rate loading is larger than that in
static loading and it is nearly 1000 m/s in the test of highest loading rate
(Takeda, 1988, 1988, 1989).

The change of the propagation speed of cracks is also one of the rate effects
200 r 1 T T 1 i

150 h * t
-s> 300mm
o /
100 [ - uS_J i 4 -
75mm
t h i c k n e s s iSO11™
* 500mm
O :mortar
» / /
D nR/ i
:concrete J2&8
rO— '~~~

i i i i i i i i 1
10"' 1 , 10 10s 103 10* 10s 10s 107 10'
MEAN LOADING RATE ? (kgf/s)
C a) ( b)
I » lOym
Fig. 6. Relation between fracture Phot. 1. Surfaces of propagated
toughness and mean loading rate cracks in Mode II test (xlOOO).
in Mode I test. (a)impact test,(b)static test
412
in the fracture mechanics on concrete and in Mode II test, the surfaces of
propagated cracks in impact test is completely different from that in static
loading test, as shown in Photo. 1 (Takeda, 1988).

5. CONCLUSIONS

(1) The rate effects are one of the thermodynamic effect, though the expla-
nation based on the Statistical Physics in thermal equilibrium state is
yet insufficient to the whole range of the rate effects caused in various
dynamic loadings (high rate loading and impact loading).
(2) The rate effects is divided into two effects, the first is on the
response before the fracture begins and the second is on the start of
fracture and thereafter. The second rate effect eventually work as the
unfavorable effect for the dynamic design of structures.
(3) The above unfavorable rate effect can be predicted by the relation be-
tween the mean stressing rate and mean straining rate. This is the same
as in the test of fracture mechanics.
(4) Not only the stress intensity factor, etc., but also the speed of crack
propagation are affected significantly by the loading rate concern.
(5) The propagation speed of cracks in concrete reaches nearly 1000 m/s in
high rate loading test and impact test, which is one of the second rate
effect.

REFERENCES

Freudenthal, A.M. (1950). The inelastic behavior of engineering materials

and structures. John Wiley and Sons. 109-140.
Takeda, J. (1969). Effect of Displacement rate of Horizontal Soil Reaction
in Sand. Soils and Foundation, 11, 15-34.
Takeda, J. (1971). Deformation and Fracture of Concrete Subjected to Dynamic
load. ICM-1, £, 267-277.
Takeda, J., Taehikawa, H. and Fujimoto, K. (1982). Basic Concept on the
Responses of Structural Members and Structures Under Impact or Impulsive
loading, and other paners. RILEM-CEB-IABSE-IASS Int. Sympo. (Berlin, BAM)
^1:13-18, S^:83-91,~S3:185-187, S4:289-295. ~
Takeda, J. (1985). Strain Rate Effects on Concrete and Reinforcements and
Their Contributions. MRS Sympo. (Boston), 64, 15-20.
Takeda, J., Komoto, K. (1988). Deteriorative Rate Effects on Brittle
Fracture of Reinforced Concrete Structures During Severe Earthquakes.
9WCEE, 1, 612-617.
Takeda, J. and Komoto, H. (1988). Rate Effects on Crack Extension in Mode II
Specimens of Mortar. Int. Workshop (Sendai). 386-392.
Takeda, J., Komoto, H. and Tanikawa, T. (1989). High Speed Propagation of
Cracks in Concrete or Reinforced Concrete Structural Members Under Impact
load (in Japanese). JSMS Sympo. on Impact Problems, 69-72.
Takeda, J. (1969). High rate shearing tests of reinforcement, bolt and the
thread of screw. Transactions of AIJ, extra, 1009.
WS2f1

EXPERIMENTAL ANALYSIS OF DYNAMIC CRACK PROPAGATION IN EPOXY

K. ARAKAWA and K. TAKAHASHI

Research Institute for Applied Mechanics, Kyushu University,
Kasuga-shi, 816 Japan.

ABSTRACT
Crack velocity a, acceleration a, stress intensity factor KID and crack extension
resistance R* for epoxy were measured in the course of crack propagation.
Effects of a and a on R* were analyzed using the R*-a diagram obtained.

KEYWORDS

Dynamic crack propagation; crack velocity; crack acceleration; stress intensity

factor; crack extension resistance; caustic method; high-speed photography.

INTRODUCTION

Dynamic fracture in brittle materials has been studied extensively for decades for
both experimental and theoretical viewpoints. Although significant progress has
been made through these studies, there are many aspects which are still beyond
our understanding. For instance, even with evaluation of the dynamic stress in-
tensity factor KID either by the photoelastic method or by the method of caustics,
there are still problems (as discussed by Dally et al.y 1985).

The purpose of this paper is to analyze the behavior of dynamic crack

propagation in epoxy specimens. Particular attention has been paid to the
correlation between fracture parameters and fracture velocity during crack
acceleration and deceleration. A parameter R*a> the product of specific crack
extension resistance R* and crack velocity a, is shown to play an important role
in understanding the behavior of dynamic crack propagation.

EXPERIMENTAL PROCEDURE

Experiments were performed on single-edge-cracked, tensile specimens of epoxy

(Araldite D). The specimen geometry is shown in Fig.l. Because of the specimen
geometry, cracks could experience both acceleration and deceleration stages in
one fracture process. The specimens were loaded at a cross head speed of lmm/min
on an Instron type tensile machine under room temperature.
413
414
Table 1. Material properties of epoxy
THICKNESS longitudinal wave speed: 2600 m/s
d=5
shear wave speed: 1170 m/s
Young's modulus: 4.39 GPa
Poisson's ratio: 0.37
density: 1170 kg/m3
stress-optical constant: 7x10-" m 2 /N
T\»K) (mm)

-150-

Fig. 1. Specimen geometry

Material properties of the epoxy specimen are listed in Table 1. The elastic
constants were evaluated under dynamic conditions by measuring velocities of
longitudinal and shear ultrasonic waves (400kHz). Dynamic stress-optical constant
was determined through experiment. We employed the method of caustics to
evaluate stress intensity factor KID during dynamic crack propagation. Caustic
patterns were successively photographed in a course of crack propagation using a
Cranz-Schardin type high-speed camera. The stress intensity factor KID was eval-
uated from the following equation:

Km =(2V2^/3z o ^ 3/2 )(0/3.17) 5y (1)

where 0 is the caustic diameter, z0 a distance between the specimen and the image
plane, d the specimen thickness, 77 a convergency factor for incident light and c
a dynamic stress-optical constant. The dynamic correction for Eq.(l) was consid-
ered to be unnecessary, because crack velocities in the present measurements did
not vary so widely and were appreciably lower than the elastic wave velocities.

To minimize data scattering of fracture parameters, we employed a data fitting

procedure; obtained values of K,D and a were expressed as ninth order polynomials
of t based on the least square method so that they might fit their observed vales
most closely. Values of a and a were obtained the first time and the second time
derivatives of the curve a(t), respectively. This procedure enable us to determine
crack velocity and acceleration quantitatively (Takahashi and Arakawa, 1987).

RELATION BETWEEN STRESS INTENSITY FACTOR AND CRACK VELOCITY

Figure 2 shows KID-a curves obtained from five epoxy specimens. The arrows indi-
cate the progressing direction of fracture. The open circles represent the position
of peak velocities obtained from eight specimens. The dotted curve of KID(a = 0)-a
was determined connecting these peak velocity points. Hence, this curve separates
the acceleration and deceleration areas in the KID~a diagram. It should be empha-
sized that KJD corresponding to a crack velocity was larger when the crack was
decelerated than it was accelerated. The curve KID('d=0)-a may be regarded as a
characteristic one for the material in the sense that no acceleration effect is
associated. Similar results have been obtained by the present authors for PMMA
specimens (Takahashi and Arakawa, 1987).

So far as we are aware, such experimental results on the KlD-a relationships as

shown in Fig.2 has never been reported. The results may appear unpredictable, be-
cause one may tend to presume that, if the dynamic stress intensity factor KID de-
pends on the crack acceleration, KID at a certain crack velocity should be larger in
 415

A.0
BRANCHING / \
4-OMN/m3'2 \

2-0 EPOXY
o (ARALDITED)

*i0(&=0)-a
1-5

1-0
2 ARREST
0.64MN/m3/2 ACCELERATION
/ AREA(a>0)
0-5 h

100 200 300 400

CRACK VELOCITY a. m/s

Fig.2. Relation between stress intensity factor KID

and crack velocity a for epoxy
the acceleration than in deceleration range. However, it is not certain yet wether
crack acceleration or deceleration plays a substantial role in yielding the relation
stated above, because there remains a question about the applicability of the
caustic method here employed. In order to get a clue to this question, we analyzed
the KlD-d relation from a dynamic fracture mechanics viewpoint based on the
fracture surface examinations.

EXAMINATIONS OF FRACTURE SURFACE ROUGHNESS

The roughness X was measured as a function of crack length a and correlated with
crack velocity a or stress intensity factor KID. The results showed that X cannot be
uniquely correlated with a or Kw \ X corresponding to a crack velocity was larger
when the crack was decelerated than it was accelerated. On the other hand, the
values of X for each stress intensity factor were slightly larger in the AT/D-increase
region than those in AT/D-decrease region (Arakawa and Takahashi, 1987).

To explain the discrepancies described above, the author have introduced a

parameter R*d which is the product of specific crack extension resistance R* and
crack velocity a. The specific crack extension resistance /?* is defined as follows:

R* = (K/}>-Kh)/Edy [N/m] (2)

where the Ku is the stress intensity factor for a crack arrest as shown in Fig.2.
Figure 3 shows how X changes as a function of R*a. No great discrepancy existed
between the two sets of data obtained in R*a-increase and fl*a-decrease regions.
The physical meaning of R*a is energy per unit crack width per unit time. A simi-
lar parameter has been used in theoretical analysis of dynamic crack propagation
for calculation of the flow rate of energy into the crack tip region (Sin, 1970). It
seems very likely that this parameter plays an influential role in changing the
fracture surface roughness.
416
008
E
*< EPOXY
in 0-06 (ARALDITE D)
in
tu
z
X
o
3 0-04
o
cr
UJ
u A , R * 6 INCREASE
^ 002 A,R*Q DECREASE
in

0 65 To 15 xlO5"
R*6, J/ms
Fig.3. Relation between fracture surface roughness X and R*d

I
x103

I 1-6 h
(ARALDITE D)
z A

a 1.4 2
■ ar-OBxK^m/s ^ | , ^ o a = 0
UJ
u
I1'2 R*a=278x10 3
//^Da=a5x106
/ J /r m/s2
12 io
0-8 [-
DC \ /¥
o
in
uj 0-6 R*a=146x103 III/ / ^ A a=1-0x106
UJ
I m/s 2

R*a=49x103 y//&y
g 0.2 R*a=20x103 ZS£z2£^~-
i I
100 200 300 400 500
CRACK VELOCITY a. m/s
Fig.4. Crack extension resistance R* for epoxy specimens
as functions of crack velocity a and acceleration a

ANALYSIS OF DYNAMIC CRACK PROPAGATION

Figure 4 shows the crack extension resistance R* as functions of crack velocity a

and acceleration a. These curves were formed by connecting the constant acceler-
ation points on KID-d data in Fig.2 and by transforming the KID to R* using Eq.(2).
All curves are described plainly. The larger the acceleration or the deceleration,
the further the corresponding curves lies from the a=0 curve. Five lines with
constant value of R*d are also represented for evaluation of a and a effects on R*.
As sated above, the roughness X is same value along a R*d=const line.

Schematic diagrams of an ideal crack propagation are shown in Figs.5(a) and (b)
for the convenience of analysis. In the diagram, state C represents a steady crack
propagation where a crack travels with constant velocity and with constant value
of R*. Hence the product of R*d is also a constant value with respect to time t.
 417

R?6c R:dA=RS60=Rcac
—?—

R?
—9—

6C

T
(S=A.D)

TIME t

Fig.5(a). Schematic diagram for an ideal crack propagation;

fracture parameters as a function of time t

Fig.5(b) Schematic diagram for an ideal crack propagation;

R*-a relation and R*a=const curve

In Fig.5(b), the two points of intersection of the R*a=const line and two constant
acceleration curves are indicated as State A for acceleration and as State D for
deceleration. Consider a crack propagation which changes from State C to State S
(5=i4,D), where the notation S designates State A or State D. The R*a=const line is
regarded as a reversible path for R * and a between two states since there is no
change in the energy dissipation at crack front along the line. In this case, the
R*-d relation between State C and the State S becomes as follows:

Re - ac = Rs - as = const, S =A, D
(3)

On the R*-a diagram in Fig.5(b), Eq.(3) describes a change in shape of rectangular

from region CC'OC" to region SS'OS" without change in the area. By use of the in-
crements of R* and a between the two states, Eq.(3) yields

Rc-ac = (Rc+ARZs)(ac + 4acs) = const., 5 =A, D (4)

418
where the two increments are shown in Fig.5(b) as Adcs = S'-C on a-axis and
A/?*CS=S"-C" on #*-axis, respectively. As shown in Fig.4, it should be noted that
there are positive increment AdCA and negative increment AR*CA for the accelerat-
ing crack; on the other hand for the decelerating crack, negative increment AdCD
and positive increment AR*CD. Figure 4 also suggests that the velocity increments
AdCA and AdCD have same absolute value for the constant acceleration and decelera-
tion curves; and their values are constant in the whole crack velocity region.
Equation (4) or comparison of the areas between two rectangular forms on R*-d di-
agram in Fig.5(b) yields the following relation:

RcAacs = -ARts (ac + Ahcs), S =A, D (5)

Equation (5) can be rewritten as follows:

ac
l+Aacs/ac (6)

where IA/?*CSI and \Aacs\ indicate the absolute values of A/?*csand Adcs, respectively.
Equation (6) shows that the value of IA/?*CSI is functions of R*c ydcznd Aacs\ and
that the value of IA/?*CSI increases with the ratio / ? * c / j c in the velocity region
\Aacslac\«\. Using Eq.(6), one can obtain:
\ARCD I = 1+AacA/ac
\ARCA\ 1+AacD/ac (7)

By assuming that Aac>i=-AaCD , following result can be obtained:

|^CD|>|^1/?CA| (8)

The result shows that the value of \AR*CD\ for the decelerating crack has larger
value than that of \AR*CA\ for the accelerating crack.

CONCLUSION

Dynamic crack propagation in epoxy specimens was studied using the relation
between crack extension resistance R* and crack velocity a during crack
acceleration and deceleration. It was found that a parameter R*d plays an
important role in understanding the behavior of dynamic crack propagation.

REFERENCES

K.Arakawa and K.Takahashi (1987). Effect of crack velocity on dynamic fracture

toughness and fracture surface morphology. Proc. 6th Int. Conf. on Photo-
mechanics and Speckle Metrology, SPIE Vol.814, pp.670-676.
J.W.Dally, W.L.Fouraey and G.R.Irwin (1985). On the uniqueness of the stress
intensity factor - crack velocity relationship. Int. J. Fracture, 27, 159-168.
G.C.Sih (1970). Dynamic aspects of crack propagation, in Inelastic Behavior of
Solids, M.F.Kanninen et al. (eds.), McGraw-Hill, pp.607-639.
K.Takahashi and K.Arakawa (1987). Dependence of crack acceleration on the
dynamic stress-intensity factor in polymers. Exp. Mech.27, 195-200.
WS2f2

MEASUREMENT OF FRACTURE TOUGHNESS AT HIGH LOADING

RATE AND LOW TEMPERATURE

M. NAKANO, K. KI SHIDA and K. YOSHIMOTO

Department of Precision Engineering, Faculty of Engineering,

Osaka University, 2-1 Yamadaoka, Suita, Osaka 565, Japan

ABSTRACT

The influences of loading rate and temperature on fracture initiation

properties of a carbon steel (JIS-S45C) and an aluminum alloy (Al 7075-T651)
were investigated at the rates of stress intensity factor from 4xl0_1 to
5xl06 MPa/m/s over a range of temperatures between 4.2 and 300 K. For high
rate fracture test, the dynamic fracture toughness was measured accurately
by using the elastic response analysis, where the dynamic stress intensity
factor and the transmitted stress through the precracked section of the
specimen were predicted by superposing the step response function under the
condition of no crack extension. For S45C, the fracture toughness decreased
with increasing loading rate and decreasing temperature. On the other hand,
for Al 7075-T651, the fracture toughness increased at extremely high loading
rate or low temperature.

KEYWORDS

Fracture toughness; high loading rate; low temperature; dynamic stress

intensity factor; carbon steel; aluminum alloy.

INTRODUCTION

The influences of strain rate and temperature on the flow stress have been
investigated from macro- and micro-scopic standpoints (Malvern, 1984).
Successful explanation of these influences on the yield stress has been
given by the thermal activation theory of dislocations (Dorn, 1968).

On the other hand, the micro-mechanism of fracture initiation has not been
made clear. It is very interesting and important to investigate the effects
of loading rate and temperature on fracture toughness. In the present paper,
the fracture toughnesses of a carbon steel (JIS-S45C) and an aluminum alloy
(Al 7075-T651) were measured accurately at the rates of stress intensity
factor from 4x10"1 to 5xl06 MPa/m/s over a range of temperatures between 4.2
and 300 K.
419
420

Transmitter gags Incident gage

Striker

Fig.l. Schematic diagram of impact fracture apparatus.

EXPERIMENTAL PROCEDURES

Figure 1 shows a schematic diagram of an impact apparatus for high rate

fracture test. The apparatus principally consists of a circumferentially
notched round bar (CNRB) specimen and a striker made of the same round bar,
25 mm in diameter. This apparatus is quite similar to the experimental
arrangement developed by Costin et al. (1977) except for the explosive
loading device. In the present test, a compressive pulse is generated by the
longitudinal impact of the striker and then a tensile pulse reflected at the
free end produces fracture of the specimen (Nakano and Kishida, 1990a). As
shown in Fig. 1, a circumferential notch was engraved on the specimen, the
size of which was 2 ram in width, 5 mm in depth in the outside and 0.1 mm in
width, 1 mm in depth in the inside. An annular fatigue precrack was grown
uniformly from the root of the narrow notch so that the remaining ligament
is less than 12 mm in diameter. Half collars were fitted into the wide notch
of the specimen. The initial compressive pulse almost entirely passes
through the notched portion with the aid of the inserted collars.

Two sets of strain gages were mounted on the specimen in order to measure
stress pulses, output signals of which were recorded by means of a digital
storage oscilloscope connected with a micro-computer. The tensile pulse
reflected at the free end of the specimen was measured by the incident gage.
The stress pulse transmitted through the precracked portion was measured by
the transmitter gage, which was located 25 mm apart from the notch.

For the impact fracture test at low temperature, the precracked portion of
the specimen was cooled by liquid nitrogen. The test temperature was
monitored by a thermocouple, which was placed on the specimen close to the
notch. The precracked portion was held at the test temperature over 6
minutes, until the ligament was cooled down to the same temperature as the
thermocouple indicated. It was confirmed in the experiments that the change
of mechanical impedance induced by the temperature gradient was negligible
for the measurement of dynamic fracture toughness.

Figure 2 shows typical outputs of the incident gage (the upper one) and
 421
2001

100|

M\ 7
0

\/r \r
V

\\r
»- 0
CO

-200J
100 200 300 400

Time
Fig.2. Typical outputs of incident and transmitter gages
in impact fracture test for S45C at 77 K.

transmitter gage (the lower one) in the high rate fracture test for S45C at
77 K. Both tensile and compressive pulses are recorded by the incident gage
and therefore they are occasionally overlapped. If the t e n s i l e pulse
overlaps with the compressive one, the incident t e n s i l e pulse at i s
estimated precisely from the compressive one using the analysis of
dispersion correction presented by Follansbee and Frantz (1983).

For the incident stress pulse cn> the dynamic stress intensity factor K(t)
and the corresponding static stress intensity factor Kstat are given by

K(t) = A / h(t-T)oi(r)dz (1)

Kstat(oi) = A 0 i ( t ) (2)

A = Jnb(l-e) O.dfe-^O.Se-^O. 375-0. 363e+0.731e2) ; e=b/R (3)

where h(t) is the step response function, R the outer radius of the specimen
and b the radius of the ligament (Nakano and Kishida, 1990b). The step
response function h(t) has been obtained from the dynamic and static finite
element analyses of the precracked round bar (Nakano and Kishida, 1990a).

The step response function g(t) for the transmitted stress at the position
of the transmitter gage has been also calculated by Nakano and Kishida
(1990a). So the transmitted stress at through the precracked section can be
estimated from the superposition integral

otPred(t) = j^ g(t-r)ai(r)dv (4)

pred
under the condition of no crack extension. The at (t) curve predicted by
eq. (4) must be separated from at(t) curve measured by the transmitter gage
when the fracture takes place and the stress wave is generated by the crack
extension.

Figure 3 represents the time variations of the incident stress at estimated

by using the analysis of dispersion correction and the transmitted stress at
measured with the transmitter gage. The transmitted stress atpred predicted
by eq. (4) is also shown in Fig. 3. Comparing the measured at (t) curve witft
th« predicted otpred(t) curve, the fracture initiation time tf can be;
422
determined as a separation point indicated in the figure. It is obvious that
the separation point appears before the peak of the measured ot(t) curve. It
should be denoted that the fracture initiation time tf cannot determined
precisely as the maximum point of the measured ot(t).

Fig.3. Typical time variations of Fig.4. Typical time variations of

incident and transmitted stress intensity factors
stresses for S45C at 77 K. for S45C at 77 K.

Figure 4 presents typical time variation of the dynamic stress intensity

factor K(t). The dynamic fracture toughness is determined as the critical
value of K(t) at t=tf. The stress intensity factor Kstat(ot) is also shown
in Fig. 4, which is obtained by the substitution of the incident stress oi
for the transmitted stress ot in eq. (2). Comparing the dynamic stress
intensity factor K(t) with Kstat(ot) calculated by the static formula, it
is seen a good similarity between those before the fracture initiation. It
can be said that the error is negligibly small in the evaluation of dynamic
fracture toughness by means of the critical value of Kstat(ot) at t=tf.

Low rate fracture tests were performed using a precracked round bar with the
same notch as the impact CNRB specimen and a standard three-point bend
specimen.

EXPERIMENTAL RESULTS AND DISCUSSIONS

Carbon steel (S45C)

Figure 5 shows the loading rate dependence of the fracture toughness for
S45C at 77 K. The fracture toughness decreased with increasing loading rate
at 77 K. Figure 6 presents the temperature dependence of the fracture
toughness for S45C at low loading rates. The brittle-to-ductile transition
was shifted to a higher temperature region by the increase of loading rate.
It is found that the fracture toughness has a tendency to decrease with
decreasing temperature and increasing loading rate for S45C. Such a tendency
was reported for some steels (e.g., Shoemaker and Rolfe, 1969).

The fracture toughness generally decreases with increasing the yield stress
for steels. This fact denotes that the plastic deformation around the crack
tip is tightly related to the fracture toughness. The influences of strain
rate and temperature on the yield stress have been explained successfully
by the thermal activation theory of dislocations (Dorn, 1968) and a
 423
functional relation has been obtained between the yield stress and the rate
parameter which is equivalent to the thermal activation energy. It has been
reported that the fracture toughness, as well as the yield stress, can be
indicated as a function of the rate parameter for steels (e.g., Shoemaker
and Rolfe, 1969). The results of the fracture toughness for S45C may be also
presented as an increasing function of the rate parameter. However, it has
not been clarified why the fracture toughness was correlated with the rate
parameter. To make it clear, some microscopic investigations are required
for wide discussions about the effects of loading rate and temperature on
the fracture toughness.

80

T- 77K If ° /C=0.7MP»,/in/s
| 60 I 601-
A #=400 MPa/m/s
v>
o CNRB
»
I 40 A Bend 40
3 <?
°
%
I 20 S 20k

10° 101 102 103 104 105 106 107 D 50 100 150 200 250 300
Loading rate K MPa/m/s Temperature T K
5. Loading rate dependence Fig.6. Temperature dependence
of fracture toughness of fracture toughness
for S45C. for S45C.

60i

f=300K O /<= 0.4 MPa/m/s

^50 50-
A A-=500MPaym/s
40J- 40 p o
°<5b fb>
M & ° Q)06 CD g o Cb 0 C
^3d-

~ 20L o CNRB ,20-

I ° Hat-shaped SEN
I iol-
LL.
A Bend
2 10V

0 5)1 ioo iSU Ztfl 2$if 3*0

"10" 10° 10' 102 103 104 10s 106
Loading rate K MPa/m/s Temperature T K
Fig. 7. Loading rate dependence Fig.8. Temperature dependence
of fracture toughness of fracture toughness
for Al 7075-T651. for Al 7075-T651.

Aluminum alloy (Al 7Q75-T651)

The loading rate dependence of the fracture toughness for Al 7075 at 300 K
is shown in Fig. 7. Results of impact fracture tests using a three-point
bend specimen (Yokoyama and Kishida, 1988) and a hat-shaped single-edge-
notched (SEN) specimen (Kishida et al, 1987) are also plotted in the figure.
424

The influence of loading rate on the fracture toughness for Al 7075-T651 was
not clearly seen below 7xl05 MPa/m/s. The rate dependence of the fracture
toughness shows an increasing trend in the range of very high loading rates
above 106 MPayrm/s. Figure 8 presents the temperature dependence of the
fracture toughness for Al 7075-T651 at low loading rates. The fracture
toughness has a tendency to increase with decreasing temperature, especially
below 50 K. It is found that the fracture toughness increased at extremely
high loading rate or low temperature for Al 7075-T651.

The loading rate dependence of the fracture toughness for S45C at 77 K below
2xl06 MPa/m/s is contrary to that for Al 7075-T651 at 300 K. However, it
should be noted that fracture toughnesses for not all steels decrease with
increasing loading rate. For example, Kalthoff (1986) has reported that the
data measured with high-strength-steel specimens indicate a sharp increase
of fracture toughness at loading rates exceeding 107 MPa/m/s. Therefore, it
is necessary to research whether the data for S45C at 77 K still show a
decrease of fracture toughness above 107 MPa/m/s. For this research, we are
developing an advanced experimental method for higher rate fracture tests at
low temperature.

Acknowledgments - The aluminum alloy was supplied from Kobe Steel, Ltd. The
analyses were carried out using an ACOS computer at Computation Center Osaka
University. The low rate fracture tests were performed using the mechanical
testing facilities of the Low Temperature Center, Osaka University.

REFERENCES

Costin, L. S., Duffy, J. and Freund, L. B. (1977). Fracture initiation in

metals under stress wave loading conditions. In: Fast Fracture & Crack
Arrest, ASTM STP 627, (G. T. Hahn et al. , eds.), pp.301-318, ASTM.
Dorn, J. E. (1968). Low-temperature dislocation mechanisms. In: Dislocation
dynamics (A. R. Rosenfield et al., eds.), pp.27-55. McGraw Hill, New York.
Follansbee, P. S. and Frantz, C. (1983). Wave propagation in the split-
Hopkinson pressure bar. Trans. ASME, J. Eng. Mat. Tech., 105, 61-66.
Kalthoff, J. F. (1986). Fracture behavior under high rates of loading. Eng.
Fract. Mech., 23-1, 289-298.
Kishida, K., Kataoka, T., Yokoyama, T. and Nakano, M. (1987). Behavior of
materials at high strain rates and cryogenic temperature. In: Macro- &
Micro-Mechanics of High Velocity & Fracture (K. Kawata et al., ed.),
pp.75-84. Springer-Verlag, Berlin.
Malvern, L. E. (1984). Experimental and theoretical approaches to
characterization of material behavior at high rates of deformation. In:
Mech. Prop, at High Rates of Strain, Inst. Phys. Conf. Ser. No. 70
(J. Harding ed.), pp.1-20, Inst. Phys., London.
Nakano, M. and Kishida, K. (1990a). Measurement of dynamic fracture
toughness by longitudinal impact of precracked round bar. Int. J. Pres.
Ves. & Piping, 44-1, 3-15.
Nakano, M. and Kishida, K. (1990b). Numerical computation of dynamic stress
intensity factor for impact fracture toughness test. Eng. Fract. Mech.,
36-3, 515-522.
Shoemaker, A. K. and Rolfe, S. T. (1969). Static and dynamic low-temperature
Aic behavior of steels. Trans. ASME, J. Basic Eng., 89-9» 512-524.
Yokoyama, T. and Kishida, K. (1988). Measurement of dynamic fracture
initiation toughness by a novel impact three-point bend test technique
using Hopkinson pressure bars. In: Impact Loading & Dynamic Behavior of
Materials (C. Y. Chiem et al., eds.), Vol.1, pp.273-280, DGM Verlag.
WS2f3

DYNAMIC FRACTURE OF PLATES DUE TO IMPULSIVE LOAD

Masashi DAIMARUYA, Hidetoshi KOBAYASHI and Mikio ODA

Department of Mechanical E n g i n e e r i n g ,
Muroran I n s t i t u t e of Technology
27-1 Mizumoto-cho, Muroran, Hokkaido 050, Japan

ABSTRACT

In t h e p r e s e n t paper, the dynamic f r a c t u r e s of plates s u b j e c t e d to an impulsive

load are i n v e s t i g a t e d by experiments and numerical simulations. The c e n t e r of
the f r e e e d g e of a s q u a r e or r e c t a n g u l a r plate with uniform t h i c k n e s s is
impacted b y a s t r i k e r while t h e o p p o s i t e e d g e and both s i d e e d g e s are free from
s t r e s s . The dynamic f r a c t u r e experiments are performed with plaster p l a t e s in
s e v e r a l dimensions and l e n g t h - w i d t h ratios. The f e a t u r e of f r a c t u r e p a t t e r n s is
d i s c u s s e d and then the numerical a n a l y s e s for a few f r a c t u r e p a t t e r n s are
carried out based on the dynamic finite element method. The s t u d y examined
q u a n t i t a t i v e l y that t h e o r i g i n s of f r a c t u r e are mainly c o r r e s p o n d i n g to t h e
r e g i o n s of dynamic tensile s t r e s s c o n c e n t r a t i o n due to s t r e s s wave reflection
and reinforcement from t h e back e d g e and both s i d e s of a plate.

KEYWORDS

Impact fracture; elastic w a v e s ; t e n s i l e stress concentration; plaster plate;

f r a c t u r e pattern; numerical simulation.

INTRODUCTION

It is well known that dynamic f r a c t u r e s p r o d u c e d by s t r e s s w a v e s differ from

t h o s e p r o d u c e d u n d e r c o n d i t i o n s of static loading for s e v e r a l different r e a s o n s .
Most of dynamic f r a c t u r e or damage might be c a u s e d b y c h a n g e o v e r of the initial
compression wave into a t e n s i l e w a v e at the f r e e b o u n d a r y of a body ( Kolsky,
1953). Not a few a c c i d e n t s or t r o u b l e s of machines and s t r u c t u r e s c a u s e d by
impact f r a c t u r e or impact f a t i g u e h a v e been r e p o r t e d u n d e r the situation of
i n c r e a s i n g s e v e r e requirement for their w o r k s . However, the mechanisms of
impact f r a c t u r e and impact f a t i g u e on machines and s t r u c t u r e s s u b j e c t e d to
impulsive loads have not b e e n clarified y e t . Some f r a c t u r e p a t t e r n s due to
impulsive loads in s u c h fundamental elements a s r e c t a n g u l a r s l a b s , w e d g e -
s h a p e d p l a t e s , cylindrical blocks and so on, are d e s c r i b e d in detail and widely in
the work of Johnson(1972). But, in g e n e r a l , the quantitative estimation of impact
fracture mechanisms may be not sufficient e x c e p t for s u c h a few c a s e s a s
425
426
s c a b b i n g a n d s p a l l i n g f r a c t u r e ( B r o b e r g , 1960, R i n e h a r t , i960, Gilath et al,,
1988). In t h i s s t u d y , t h e e l a s t i c wave b e h a v i o r a n d impact f r a c t u r e of a plate
s u b j e c t e d to an i m p u l s i v e load on i t s o n e e d g e a r e i n v e s t i g a t e d by e x p e r i m e n t s
a n d n u m e r i c a l s i m u l a t i o n s . The c e n t e r of o n e f r e e e d g e of a s q u a r e or
r e c t a n g u l a r p l a t e with an uniform t h i c k n e s s is impacted by a s t r i k e r in t h e
d i r e c t i o n p e r p e n d i c u l a r - to t h e front, erlge, while t h e back e d g e a n d b o t h s i d e
e d g e s a r e free from s t r e s s . The impact f r a c t u r e e x p e r i m e n t s a r e p e r f o r m e d with
p l a s t e r p l a t e s in s e v e r a l d i m e n s i o n s a n d l e n g t h - w i d t h r a t i o s . The f e a t u r e of
impart f r a c t u r e p a t t e r n s in e a c h p l a t e is d i s c u s s e d . Numerical a n a l y s e s for a few
f r a c t u r e p a t t e r n s a r e c a r r i e d o u t b a s e d on t h e d y n a m i c finite element method.

IMPACT FRACTURE EXPERIMENT YvITH PLASTER PLATES

E x pe i • i m e n t a 1 E g u i p m e r \ t

The s c h e m a t i c d i a g r a m of t h e e x p e r i m e n t a l s e t u p for impact f r a c t u r e is s h o w n in

Fig. 1. The e x p e r i m e n t a l a r r a n g e m e n t c o n s i s t s of a h i g h - p r e s s u r e a i r g u n (
omitted in t h e f i g u r e ) , a s t r i k i n g b a r a n d an i n p u t b a r t r a n s m i t t i n g an impact
force lo a s p e c i m e n . Both t h e s t r i k i n g b a r a n d i n p u t b a r a r e made of a c a r b o n
s t e e l . The i n p u t b a r h a s 20 mm d i a m e t e r a n d 2000 mm l e n g t h , while t h e s t r i k i n g
b a r h a s t h e same d i a m e t e r of 20 mm, but t h e l e n g t h of 500 mm. The s t r i k i n g b a r
s h o t o u t from t h e a i r g u n i m p a c t s axially a g a i n s t t h e i n p u t b a r which is set in
p e r p e n d i c u l a r c o n t a c t with t h e impact e d g e of a specimen p l a t e . The i n c i d e n t
p u l s e g i v e n at t h e impacted p o i n t of t h e e d g e of a p l a t e was o b s e r v e d from t h e
s t r a i n g a g e s mounted on t h e i n p u t b a r at a x i s y m m e t r i c l o c a t i o n s of 200 mm from
t h e e n d in c o n t a c t with a p l a t e . The s i g n a l from t h e g a g e s was amplified a n d
r e c o r d e d by a d i g i t a l oscilloscope (Nicolt, Model 410).

Specimen P l a t e s a n d F r a c t u r e P a t t e r n s

The p l a t e s u s e d in t h i s impact f r a c t u r e e x p e r i m e n t a r e made of a xilaster material.

The mechanical a n d a c o u s t i c a l p r o p e r t i e s of p l a s t e r p l a t e s a r e shown in Table 1.
Here, E is Y o u n g ' s m o d u l u s , p is t h e mass d e n s i t y , y is t h e P o i s s o n ' s r a t i o , <j .
a n d o" -.- is t h e t e n s i l e a n d c o m p r e s s i v e s t r e n g t h , r e s p e c t i v e l y , a n d CY, is t h e
velocity of l o n g i t u d i n a l e l a s t i c wave in a t h i n b a r . As s u g g e s t e d by Davids
(1960), Kida a n d Oda(1982), p l a s t e r could be u s e d a s a modeling material s t u d y i n g
for impact f r a c t u r e for o t h e r m a t e r i a l s . Fig. 2 s h o w s t h e d i m e n s i o n s of p l a s t e r
p l a t e s e m p l o \ e d in t h e impact f r a c t u r e t e s t a n d t h e c o o r d i n a t e s u s e d l a t e r for
numerical simulation. A s e r i e s of impact f r a c t u r e e x p e r i m e n t s w e r e p e r f o r m e d
with t h e plaster- p l a t e s shown in Fig. 2, u n d e r t h e c o n d i t i o n s of v a r i o u s i m p u l s i v e
loads.

500 2000
Striking bar Strain gages 200

Incident pulse Stress wave

Fig. 1. Schematic d i a g r a m of e x p e r i m e n t a l s e t u p
for impact f r a c t u r e of p l a s t e r p l a t e s .
 427
Table 1. Mechanical p r o p e r t i e s of a p l a s t e r specimen.

E P V (TT Co
GPa kg/m3 MPa MPa m/s

12.1 1.52 X 1 0 3 0.20 3.11 30.0 2820

Plate L x W (mm)
A 360 x 40
B 240 x 120

C 240 x 240

Fig. 2. Dimensions of p l a s t e r p l a t e s u s e d in experiment

Typical p a t t e r n s of impact f r a c t u r e for each plate are shown in Fig. 3(A), (B) and
(C). In the c a s e of t h e plate with comparatively narrow width a s shown in Fig.
3(A), s c a b b i n g or spalling f r a c t u r e t e n d s to o c c u r due to the reflected t e n s i o n
w a v e s from another f r e e e n d , likewise a long thin bar s u b j e c t e d to detonation on

(B)

(C)
(A)

Fig. 3. F r a c t u r e s in each plate impulsively loaded

at t h e c e n t e r of t h e u p p e r e d g e .
428
o n e e n d ( J o h n s o n , 1972). On t h e o t h e r h a n d , in t h e c a s e of t h e s q u a r e or
r e c t a n g u l a r p l a t e a s s h o w n in Fig. 3(B) a n d (C), t h e r e f l e c t e d t e n s i o n w a v e s from
t h e s i d e e d g e s t e n d to g i v e r i s e to t h e c e n t r a l f r a c t u r e p a r a l l e l to t h e s i d e s .
M o r e o v e r , s u c h r e f l e c t e d w a v e s , t o g e t h e r with t h e r e f l e c t e d w a v e s from t h e back
a n d also f r o n t e d g e , may i n t e r f e r e a n d r e i n f o r c e e a c h o t h e r a n d p r o d u c e v e r y
complicated s t r e s s d i s t r i b u t i o n s c a u s i n g o t h e r t y p e of f r a c t u r e s s u c h a s c o n e r
c r a c k s . In t h i s s t u d y , in o r d e r to u n d e r s t a n d t h e impact f r a c t u r e mechanism
q u a n t i t a t i v e l y , a numerical simulation was c a r r i e d o u t to examine t h e p r o p a g a t i o n
of e l a s t i c w a v e s in p l a s t e r p l a t e s , p r o v i d i n g t h a t no f r a c t u r e o c c u r s e v e n if t h e
s t r e s s e s exceed t h e f r a c t u r e s t r e s s .

NUMERICAL CONSIDERATION

A n u m e r i c a l a n a l y s i s was p e r f o r m e d u s i n g t h e d y n a m i c finite e l e m e n t m e t h o d .
For siin|)licity, a p l a t e c o n s i d e r e d h e r e is a s s u m e d in p l a n e - s t r e s s s t a t e a n d its
c o o r d i n a t e s y s t e m is s h o w n in Fig. 2. The impact is r e p r e s e n t e d by a d i s t r i b u t e d
force with 2a w i d t h a c t i n g on t h e c e n t e r of f r o n t e d g e of t h e p l a t e . The s i d e
e d g e s a n d also t h e f r o n t a n d back e d g e s of t h e p l a t e a r e s u p p o s e d f r e e from
s t r e s s e x c e p t at t h e impacted a r e a on t h e f r o n t e d g e . The e q u a t i o n of motion for
t h e finite element formulation is g i v e n by ( Nakano a n d Kishida, 1990)

[K]{AU} + [M]{AU} = {AF} (1)

w h e r e [ A/] is t h e mass matrix, [ K] t h e s t i f f n e s s matrix. { Ju } a n d { jii }

a r e t h e i n c r e m e n t v e c t o r s of nodal d i s p l a c e m e n t a n d nodal d i s p l a c e m e n t
a c c e l e r a t i o n , r e s p e c t i v e l y , which a r e d u e to t h e i n c r e m e n t v e c t o r of nodal force
v e c t o r { J F } . The time i n t e g r a t i o n of Eq. (1) is c a r r i e d o u t by t h e N e w m a r k - /3
a l g o r i t h m in which t h e disj^lacement un a n d t h e v e l o c i t y u r , a r e g i v e n a s follows,

(2)
"* = "„-/+('-r)4f •*„_, + yAt-uH
w h e r e t h e s u b s c r i p t n d e n o t e s t h e n - t h time i n t e r v a l a n d t h e p a r a m e t e r s /3 a n d
y c o n t r o l s t h e s t a b i l i t y a n d a c c u r a c y of t h e a l g o r i t h m . By making u s e of Eq. (2),
Eq. (1) may be w r i t t e n in t h e form

I n o r d e r to i n s u r e s t a b i l i t y of t h e s o l u t i o n s , t h e c o m p u t a t i o n s a r e c a r r i e d out
with /3 - 1 / 4 , y = 1 / 2 , a n d t h e i n c r e m e n t of time It l e s s t h a n i / C , t h a t
c o r r e s p o n d s to t h e time for t h e e x t e n s i o n a l wave C, in a p l a t e to p r o p a g a t e t h e
minimum n o d e d i s t a n c e / . The half s p a c e of a p l a t e is d i v i d e d i n t o a n u m b e r of
f o u r - n o d e d i s o p a r a m e t r i c e l e m e n t s . The nodal f o r c e was g i v e n by t h e i m p u l s i v e
f o r c e m e a s u r e d in t h e impact f r a c t u r e e x p e r i m e n t of p l a s t e r p l a t e s . U n d e r t h e
c o n d i t i o n s mentioned a b o v e , n u m e r i c a l c o m p u t a t i o n s c o r r e s p o n d i n g to t h e
e x p e r i m e n t s shown in Fig. 3(A), (B) a n d (C) w e r e c a r r i e d o u t . On a c c o u n t of
limited s p a c e , t h e n u m e r i c a l r e s u l t s will b e s h o w n only for t h e r e c t a n g u l a r p l a t e .
Fig. 4 show's t h e s t r e s s d i s t r i b u t i o n s of t h e r e c t a n g u l a r p l a t e a t e a c h i n s t a n t of
t h e d i m e n s i o n l e s s time T - W / C , , w h e r e W = 120 mm a n d C, = 2880 m / s for t h i s
r e c t a n g u l a r p l a t e . T h e n , for example, a t T = 1.0, an e x t e n s i o n a l w a v e f r o n t
g e n e r a t e d a t t h e c e n t e r of t h e impact location m a k e s j u s t o n e r e t u r n t r a v e l a l o n g
t h e f r o n t e d g e of t h e p l a t e . In t h e f i g u r e s o"x» <TV a n d <y , d e n o t e t h e s t r e s s e s in
t h e x a n d y d i r e c t i o n a n d t h e maximum p r i n c i p a l s t r e s s , normalized by <y a ,
 429

Fig. 4. Stress distributions of rectangular plate

at each instant T = 1.25, 1.75 and 4.0.
430
r e s p e c t i v e l y . <y0 i s t h e maximum s t r e s s of t h e i n c i d e n t c o m p r e s s i v e p u l s e into
t h e plate. In each f i g u r e t e n s i l e s t r e s s r e g i o n s are s h a d e d . In comparison with
Fig. 3, a number of different f r a c t u r e p a t t e r n s are p o s s i b l e to be r e c o g n i z e d ;
that i s , (a) central line f r a c t u r e e x t e n d i n g downwards in the x direction from the
impact location, (b) multiple s c a b b i n g or spalling f r a c t u r e in the y direction, and
(c) corner f r a c t u r e . T h e s e are shown diagrammatically in Fig. 5(A). Fig. 5(B)-(D)
p r e s e n t s the variations of s t r e s s e s with dimensionless time at the s t a t i o n s a, b
and c shown in Fig. 5(A). It can be s e e n from t h e a b o v e f i g u r e s that the o r i g i n s
of impact fracture are c o r r e s p o n d i n g to the r e g i o n s of dynamic tensile s t r e s s
concentration due to s t r e s s wave reflection and i n t e r f e r e n c e from the back and
also front e d g e s and both s i d e s of a plate.

Fig. 5. Fracture p a t t e r n s and variations of s t r e s s e s v s .

dimensionless time at station a, b and c.

REFERENCES

Kolsky, H. (1953). Stress Waves in Solids. Clarendon P r e s s , Oxford.

Johnson, W. (1972). Impact Strength of Materials. Edward Arnold, London.
Broberg, K.B. (1960). Some a s p e c t s of the mechanism of s c a b b i n g .
In: International Symposium on Stress Wave Propagation in Materials
( N. Davids, Ed.), I n t e r s c i e n c e , New York, pp.229-246.
Rinehart, J.S. (1960). The role of s t r e s s w a v e s in the comminution of brittle,
rocklike materials. In: International Symposium on Stress Wave Propagation in
Materials ( N. Davids, Ed.), I n t e r s c i e n c e , New York, pp.247-270.
Gilath, I., S. Eliezer, M.P. Dariel and L. Kornblit. (1988). High strain rate ductility
of aluminum in uniaxial tension a s an effect of laser induced shock w a v e s . In:
Impact Loading and Dynamic Behaviour of Materials ( C.Y. Chiem, H.-D. Kunze
and L.W. Meyer, Ed.), Vol.2, DGM Informationsgesellschaft, Verlag, p p . 669-676.
Davids, N. (1960). Some problems of t r a n s i e n t a n a l y s i s of w a v e s in plates. In:
International Symposium on Stress Wave Propagation in Materials( N. Davids,
Ed.), I n t e r s c i e n c e , New York, pp.271-288.
Kida, S. and J. Oda (1982). On f r a c t u r e behavior of brittle c a n t i l e v e r beam
s u b j e c t e d to lateral impact load. Experimental Mechanics, 22, 69-74.
Nakano, M. and K. Kishida (1990). Numerical computation of dynamic s t r e s s
i n t e n s i t y factor for impact f r a c t u r e t o u g h n e s s t e s t . Engineering Fracture
Mechanics, 36, 515-522.
WS2f4

TRANSIENT MODE-III STRESS INTENSITY FACTOR OF A

SUBSURFACE CRACK DUE TO CRACK-FACES POINT FORCES

M. K. Kuo
Institute of Applied Mechanics
National Taiwan University
Taipei, Taiwan 10764
R. O. C.

ABSTRACT
The transient elastodynamic stress intensity factors (SIF) of a sub-surface semi-infinite
crack in an elastic half plane are analyzed. The crack is parallel to the surface of the half
plane where a pair of anti-plane force are acting at a fixed position on the crack faces.
Exact expressions are obtained for the mode-Ill SIF as functions of time. The results are
exact for the time interval from initial loading until the first wave scattered at the crack
tip is reflected three times at the surface of half plane and returns to the crack tip.

KEYWORDS
Dynamic fracture mechanics; transient stress intensity factor; anti-plane motion; sub-
surface crack; concentrated impact forces.

INTRODUCTION
Only few papers deal with the transient interaction between the crack and the outer
boundaries of the body. For the sub-surface crack geometry with point impact loading,
the fixed characteristic lengths arise not only in loading but also in geometry. The crucial
steps in the analysis are the integral transforms together with the Wiener-Hopf technique
and Cagniard-de Hoop method as if there were no fixed characteristic length.

PROBLEM STATEMENT
Consider anti-plane deformations of a sub-surface semi-infinite crack in a isotropic half
plane which is characterized by the shear modulus fi, and mass density p. The crack is
assumed to be parallel to the surface of the half plane. A Cartesian coordinate system
(x,y) is defined in such a way that the only nonzero displacement w(x,y,t) is normal
to the xy-plane, the half plane locates at — oo < y < a, and the crack lies in the line
y = 0, x < 0. The crack geometry, the half plane and the coordinate system are shown
in Fig. 1. Anti-plane wave motions of solids are governed, in terms of w(x,y,t), by

d2w d2w «d2w / / xi/o

431
432
The relevant stress component is ayM = /x dw/dy.

Fig. 1. Loading, coordinate and cracked half-plane geometry.

The elastic half plane is at rest initially. For time t > 0, a pair of anti-symmetric
concentrated anti-plane shear forces in the ^-direction of magnitudes ±F are acting on
the crack faces y = 0 ± at x = — I

crVM(x,y,t) = -FH{t)6(x + l), x < 0, _ n0±

y = (2)

where H and 6 are the Heaviside and Dirac delta functions, respectively. The surface of
the half plane are assumed to be free of tractions; while the material are perfectly welded
ahead of the crack tip . Of the particular interest the mode-Ill SIF i* defined as

KUJ{t)= lim.[27rx] 1 / 2 a l/ ,(x,0,0 (3)

x-»0+

METHODS OF SOLUTION
Apply one-sided Laplace transform over t, with kernel exp(—p£), and two-sided Laplace
transform over x, with kernel exp(—p£x), to (1). Transformed general solution, which
satisfy the traction free condition on the surface of the half plane, can be written as

"tf.y.Pj - I (4)
B eXp(p7y), -oo < y < 0

where 7 = (s2 — f 2 ) 1 / 2 , and A and B are arbitrary functions of £ and p. The branch
cuts of 7 have been taken as from £ —► —00 to —s and from s to 00, such that Re (7) > 0
in the entire cut complex £-plane, where 'Re' denotes the real part. The one-sided and
two-sided Laplace transforms are denoted by superposed bar and tilde, respectively.

From (4) the transformed displacement and shear stress along the whole crack line are

j A cosh(p7a), y = 0+ , .
W- + W+

A «:«v,f \
f -/xp7Asinh(p7a), y 0+n+
exp(p££)+a+ (6)
P \ UPlB y = 0

In (5) «;_({,0 ± ,p) is the transformed unknown crack-face-displacements w-(x,0±it) of

the upper and lower crack faces. By virtue of the theory of Laplace transform, iy_ is
 433
analytic and goes to zero as |£| —► oo in the half complex £-planes Re(£) < s. Likewise, 5+
and u)+ are analytic and go to zero as |£| —► oo in the half complex £-plane Re(£) > —s,
where a+ and u>+ are transformed unknown stress field and displacement, respectively,
ahead of the crack tip. The one-sided Laplace transformed SIF can be obtained from
a+(£,0,p) by using the Abelian theorem (Noble, 1958, p. 36 ) as

A>//(p)=2 1/ *lim(p0 , ' , * + (£,O,p) . (7)

p£-»oo

In relating transformed crack line stress to displacement through (5)-(6) by eliminating

A, B and tD+, one has

-/iP7L(e,p)«r- = * + - ( F / p ) e x p ( p ^ ) ; L(£,p) = (1 - e-**")/2 (8)

where W_ = u)_(£,0 + ,p) — t/)_(£,0~,p), which denotes the transformed crack opening
displacement. Notice that L(£,p) depends only on the geometry of the cracked half
plane. By (8) the problem has now been reduced into a form suitable for the Wiener-
Hopf technique, and its solution then depends upon being able to write related functions
as the product and the sum, respectively, of regular functions.

WIENER-HOPF TECHNIQUE
Instead of performing the quotient splitting directly to L, let us construct series for the
crack opening displacement W _ and the crack-line stress a+ as

w.{i,P) = w(0J(i,p)+w™{z,p)+w™(i,P) + --- (9)

*+(e,p) = ^ 0) (e,p)+^ l) (e,p)+^ , (e,p) + --- (10)
with W _ and 5+ being solutions of the following problems

-(l/2) W T7-^ ( _ 0 ) = b[?h+-{Flp)D{i) (11)

1) l) 2pio r )
-(l/2)/»P7-*- = ^ /'T+-(l/2)/iP7-«- « - (12)
-(1/2)MP7-^ ( _ J) = h{?h+ - ( 1 / 2 ) W H _ e-^'W^ (13)

where D(£) = exp(p^)/7 + . It is easy to verify that the infinite series of (9) and (10)
constructed in this manner certainly satisfies (8). By using the definition of Kin given
as (3), it is apparent that the series corresponding to (9) and (10) is

K>i/ = K $ + A $ + * £ } + ••• • (14)

Equation (11) is exactly the corresponding Wiener-Hopf equation for a cracked infinite
plane with concentrated point forces acting on the crack faces. It, as one would ex-
pect, implies that in the short time approximation the Mode-Ill elastodynamic SIF for
a cracked half-plane can be computed for a crack in an infinite plane, provided that the
applied loads are the ones corresponding to the original half-plane problem. Since D(£)
434
is analytic and goes to zero as |£| —► oo in the strip —s < Re(£) < s, the formula of
sum splitting (Noble, 1958) directly applies. By deforming the integration path to warp
around both the upper and lower faces of the appropriate branch cut, one has

,i5
*«> - ir^c^-™-^ 1
»
D_(e) = (p/x) " exp(ptl) f'n-V'expl-pit + sWdr, . (16)
Jo

Equation (11) now becomes

- (l/2)/ip7- W^ + (F/p) D.(t,a) = b(?h+ - (F/p) Z>+(£) (17)

The left- and right-hand sides of (17) are regular in the overlapping half-planes Re(£) < s
and > — 5, respectively. By analytic continuation each side is the analytic continuation
of the other into the complementary half plane, and both sides represent the same entire
function. By the use of the Liouville's theorem and the fact that the near-tip stress and
the crack-opening-displacement exhibit inverse square root and square root behaviors,
respectively, with the result that the entire function vanishes completely, hence,

9l?(t,0,p) = (f/p) 7+ £>+(£) (18)

z (o)
(l/2)/iPTf-W- (i,0,p) = (F/p)D-(t) . (19)

By inverting the two-sided Laplace transform to (18), changing the order of integration
between the integral over £ and the integral in D+(£,a), and then using the Cagniard-
de Hoop method, after some manipulations one has the zeroth order SIF as

Kfkt) = {^)lliFH(t-st) . (20)

Equation (20) is exactly the appropriate static result for crack in the infinite plane.

From (12) and (19), the equation governing W _ and a+ is obtained as

- (\l2)Mn-WW = 5< 1) /7 + - (F/p) G(£, 2a) (21)

where G(£, a) = exp(—jricc) £>-(£)• As in the zeroth order problem, the uses of the sum
splitting, the analytic continuation and the Liouville's theorem conclude

%\t,0,p) = (F/p)-r + G + (e,2a) (22)

= (i)
(1/2)M-W_(t,0,p) = (F/p)G_(£,2o) . (23)

By using the Abelian theorem and the Cagniard-de Hoop method, the one-sided Laplace
transform of SIF can be inverted by inspection, after some manipulation, one has

(t — SUQ)NI(U0)
K^t,a) = H(t-tl)ir[jr4t_si)]1/tKe (24)
[u0f (Ua-Uo)1/2 J
 435
where tt{a) = s(£2 + a2)1!2, u 0 = l+ia, ua = [t2 - s2(l2 + a2)]/[2s(t - si)], the expression
of AT,(u) is denned for s(l2 + a 2 ) 1 / 2 < t < s{l + a) as TT, and for t > s{l + a) as

»r/X -l -{2M«a-«)(Ua-«)]1/2 + («a-2u)£+Uau}

^(.) = .log-l ^ - ^ - i . (25)

It is of interest that for the case of s(t2 + a 2 ) 1 / 2 < * < $ ( £ + a)the result of (24) with
Ni = n can be obtained easily by a contour integration in the complex plane as
1/2 ,
Km(t,a) = F sin - ; 0 = TT - tan _ 1 (a/£) . (26)
TT(£2 + a 2 )V2j 2

Equation (26) is exactly the appropriate static and also the transient Km for semi-infinite
cracks in an infinite plane loaded by a point force of 2F at (x,y) = (—t, a).

t^'and^'
- (2) ~(2)
From (13), (19) and (23), the Wiener-Hopf equation for W _ and o+ is obtained as

- (1/2) WT-*- ) = *?Vl + " (F/P) G& 4<0 + (*7P) « ( 0 (27)

where Q(£) = exp(-2|rya) G+(£,2a). In (27), the relation G_(£,a) = G(£,a) -<7+(£,a)
has been used. As in the first order problem, the uses of the sum splitting, the analytic
continuation, the Liouville's theorem, the Abelian theorem, and the Cagniard-de Hoop
method conclude

MBM -«iii(M.)->-■.)IT™M,- J-tt-wd° <28>

where
2
fAjW^fa)
Nl{v) = 2Re{E^r^L\
£1 uj/2(uc - Uy)1/2 • ■*• (»)
2 2 2 2
( * - 0 v ) - , s ( £ + 4a ) , , , r , w / , , ,
Uc = t t
2s(t-2av-sl) ' ^ W = i - ( - ^ ( ^ ) ( 3 °)
j , , = [s2(T2-4s2a2-«lR2)+2rJ2+T2}(l-u)
V , ;
(T 2 -45 2 a 2 -r/ 2 . J R 2 ) 2 + 4 r 7 2 r 2 ( £ - u ) 2 v ]

t2 = 2sa + s{l2 + 4a 2 ) 1 / 2 , and Ui and u 2 are the zeros of the denominator of J with
positive imaginary parts. The expression of N\(u) is defined as n for ue < I and as (25)
for uc> I with u 0 being replaced by u c .

RESULTS
The elastodynamic Mode-Ill SIF of a sub-surface semi-infinite crack in the half plane, as
in (14), is the sum of (20), (24) (with a = 2a) and (28). Fig. 2 shows the dimensionless
SIF Kju/Kfjj versus the dimensionless time t/[(sl)2 + s 2 (6a) 2 ] 1 / 2 for various values of
l/a. The Km actually jumps first from zero to Km = [2/(7r£)]1/2F, which corresponds
to the appropriate static stress intensity factor of a cracked infinite plane, at time t = si,
as (20), for any values of l/a and then retains the constant value until t = s(l2 + 4a 2 ) 1 / 2 .
436

The discrepancies in the magnitudes and the positions of the first discontinuities for
various values of t/a in the Figure are the consequences of the normalization. At time
t = s(l2 + 4a 2 ) 1 / 2 , the Kni jumps again to another constant values with the amount
of discontinuities 2(2/TT) 1 / 2 (£ 2 + 4a 2 )" 1 / 2 Fsin(^/2) until t = s(l + 2a), where 0 = n -
tan _1 (2a/£).

KJJJ

Fig. 2. Mode III stress intensity factors versus time.

CONCLUSION
In this paper the mode-Ill transient elastodynamic stress intensity factors (SIF) of a
stationary sub-surface semi-infinite crack in a half plane has been determined for a par-
ticular case of anti-plane point loadings. The characteristic lengths of the problem arise
not only from the loading but also from the geometry. The exact solution has been
obtained by integral transforms together with the direct application of the Wiener-Hopf
technique and the Cagniard-de Hoop method, which was believed not to be appropriate
even for problems with only the characteristic length in loading presented. Instead of
performing the quotient factorization directly in the resulting Wiener-Hopf equation, the
solution has constructed in a series form. The first term in the solution series is exactly
the solution of the crack in an infinite plane and hence the waves have not yet reflected
against the surface of half-plane. With each further term in the solution series, it cor-
responds to the solution that the waves has reflected more times against the surface of
half-plane. The first three terms in the series for the SIF history have been computed
numerically. The results are exact for the time interval from initial loading until the first
wave scattered at the crack tip is reflected three times at the surface of half-plane and
returns to the crack tip. It has been shown that the smaller the depth of sub-surface
crack is, the larger is the maximum of the transient SIF.

REFERENCE
Noble, B. (1958). Methods based on the Wiener-Hopf Technique, Pergamon Press, New
York.
WS2f5

MECHANICAL CHARACTERIZATION OF ADHESIVE JOINTS,

INFLUENCE OF THE RATE OF LOADING.

D. GRAPOTTE * and J-L LATAILLADE *>**

* Laboratoire de M6canique Physique, URA CNRS 867, 351 crs de la Liberation,

33405 Talence Cedex, France.
** Professor, Ecole Nationale Supgrieure des Arts et Metiers, Esplanade des
Arts et Metiers, 33405 Talence Cedex, France

ABSTRACT

This research paper deals with the application of fracture mechanics to the
characterization of adhesive joints subjected to different rates of loading and
tested according to different stress configurations ( mode I, mode II and mixed
mode I+II ).

KEYWORDS

Epoxy resin; adhesive joint; fracture mechanics; fracture energy; mode I;

mode II; mode I+II; rate of loading.

INTRODUCTION

Adhesives, such as epoxy resins, are increasingly being used in all forms of
transport where the adhesive joints are subjected to vibrations and shocks. It is
therefore necessary to evaluate their mechanical behaviour at impact rate
loadings. Our contribution deals with the influence of the rate of loading on the
adherence of a sheet-steel / epoxy resin / sheet-steel bond. A linear-elastic
fracture-mechanics approach was used to determine the fracture energy of
adhesive joints, with an initial interfacial defect, under different stress
configurations ( mode I, mode II and mixed mode I+II ).
437
438

EXPERIMENTAL

The materials

The structural adhesive used was a one-part rubber-toughened epoxy resin.

The hardening of the adhesive was obtained by curing ( the temperature was
raised from 20 °C to 150 °C in 30 min., maintained at 150 °C for 60 min. and
then brought down to 20 °C in 120 min ). The substrate used was 0.67 mm thick
sheet-steel, simply degreased using trichloroethylene.

Preparation of adhesive joints

To make these specimens, a guiding apparatus was used ( Fig. 1 ). The lower
part of a clamp was placed in the apparatus. A square of sheet-steel ( 40*40
mm 2 ) was put into place and a PTFE-covered adhesive film was stick on to
create a defect of known initial length. Two PTFE wedges were used to calibrate
the thickness ( 1 mm ) and the width ( 10 mm ) of the joint. A strip of epoxy
resin was added before putting the upper square of sheet-steel in place. The
upper part of the clamp was tightened to obtain a slight pressure to fix the
specimen, which was then removed from the apparatus to undergo the
reticulation cycle. The specimen was then fixed onto the supports to be
subjected to different modes ( Fig. 2). Fixation was obtained by bonding with a
cyanoacrylate adhesive applied to the entire surface of the square of sheet-steel.

Fig. 1. Different stages in the making of the adhesive joint.

 439

Sheet-steel
Adhesive
Defect

Mode I
IT
^
Mode II Mode I+II

Fig. 2. Specimens and the three different modes.

Experimental devices

For the lower rate of loading ( 5 mm/min and 500 mm/min ) an Instron 1186
conventional tensile machine was used. The dynamic tests were carried out on
a Hopkinson bar tensile apparatus, whose principle is based on the
propagation of transitory tensile waves in a mechanical line : elastic input bar -
specimen - elastic output bar. The presence of the specimen induces an
impedance variation, such that the incident wave is transformed into a
reflected wave and a transmitted wave. The force F(t) in the specimen was
deduced from the transmitted wave £x(t) :

F(t) = A B E B &&) A B bar section , E B bar modulus

The waves were received by two strain gauge bridges and recorded on a DRAM
numerical oscilloscope ( Lecroy 9400 ). A Zimmer OHG optical extensometer
was used to follow the relative displacement of the two plates of sheet-steel.

Specimen

Output bar [ ■ ^ Input bar"

Air gun I
Fig. 4 Schema of the loading principle using Hopkinson bars.
440

To determine the critical energy release rate

From the curves F(t) and A(t), it is possible to measure the energy U absorbed by
the specimen up to the crack initiation,

rt R
U= F(t)A(t)dt
Jo
But only a part of this energy is used to initiate a crack. The idea then was to
plot U against B(D-a) while varying the length of the initial flaw ( B width of
joint = 10 mm, D length of joint = 40 mm ). The slope of the linear part of this
curve corresponds to the energy release rate Gc ( Williams, 1984; Kinloch et
aZ.,1987).

RESULTS AND DISCUSSIONS

During these tests mainly interfacial failures were noted, i.e. propagation was
on the interface and a very thin film of adhesive remained on the the surface of
the sheet-steel. There were one or two cases where the crack branched towards
the other interface. Depending on the stress configuration, different failure
times were obtained ( Table 1 ). For each configuration and for each rate of
loading the curve U = f [B(D-a)] was plotted with different values of a: 5, 7.5,10,
12.5, 15 and 20 mm ( Fig. 4 ). Each plot corresponds to the average obtained out
of 5 tests. The values Gc obtained are grouped together in Table 1.

Table 1. Results of the energy release rates in kJ/m2

and failure times.

Mode I Mode II Mode I+II

Gc Tf Gc Tf Gc Tf
Static 5 mm/min 0.39 1.5 s 3.2 10.5 s 0.36 8.8 s
0.5 m/min 0.45 0.14 s 5.6 0.22 s 0.79 0.18 s
Dynamic 6 m/s 4.9 41 us 7.6 41 us 2.8 43 us
8 m/s 5.9 33 us 10.6 33 us 4.0 35 us
 441

o 5 mm/min o 6 m/s
U i n mJ • 500 mm/min U in mJ • 8 m/s
60
50
40
30
20
10 4

l5o 25o 3&T 400 "2S0 axf 400

B(D-a) in mm 2 B(D-a)in mm 2

o 5 mm/min o 6 m/s
• 500 mm/min U i n mJ • 8 m/s
2000

100 "25o" 300 400 100 "255 355"

B(D-a) in mm 2 B(D-a)inmm 2

U in mJ o 5 mm/min U in mJ o 6 m/s
• 500 mm/min • 8 m/s
120 600

15o~ 200 300 400 i5o~ 400

B(D-a) in mm2 B(D-a) in mm 2

Fig. 4. Curves U versus B(D-a) for mode I (a, b), mode II (c, d) and
mode I+II (e, f).
442

These results show that for the three modes, Gc increases with the rate of
loading. The energy absorbed U follows this trend up to rates of 6 m/s and then
decreases for a rate of 8 m/s. For the latter rate, a rapid fall in the performance
of the assembly was noted when a increased. A comparison of the three modes
shows that mode II by far requires the most energy. The mixed mode I+II
gives the lowest values of Gc : a phenomenon already observed by other authors
(Kinloch 87 ).

CONCLUSIONS

The method used to determine the energy release rate Gc requires several tests
but give good results. In particular the technique of Hopkinson tensile bars,
adapted to fracture mechanics of bonded joints is satisfactory for the high
values of loading rates ( Gc/Tf « 300 kJ.m-2. s-l ). These results show that Gc is
highly sensitive to the failure mode and that in the case of the mixed mode the
constitutive law of the resin determines the predominant mode. Moreover, the
mixed mode presents lower values of Gc. It is therefore necessary to show
extreme care because in the reality failure modes are indeed highly complex.
In our research Gc increases with the rate of loading but the energy U
absorbed decreases as from 6 m/s.

ACKNOWLEDGEMENTS

The authors would like to thank the Centre National de la Recherche

Scientifique, the Regional Council of Aquitaine, and the CECA company, a
branch of Elf-Aquitaine for having funded this research study for the doctorate
thesis of D. Grapotte.

REFERENCES

Kinloch A.J. and Kodokian G.A. (1987). The Impact Resistance of Structural
Adhesive Joints. J. Adhesion, 24, 109-126.
Williams J.G. (1984). Fracture Mechanics of Polymers. Ellis Horwood Limited,
Chichester.
Kinloch A.J. (1987) Adhesion and Adhesive. Chapman and Hall, London.
WS2g1

NUMERICAL STUDY ON SHADOW SPOT METHOD FOR

MEASURING DYNAMIC FRACTURE TOUGHNESS

S.AOKI and T.KIMURA

Department of Mechanical Engineering Science,

Tokyo Institute of Technology
O-okayama, Meguro-ku, Tokyo 152, JAPAN

ABSTRACT

The shadow spot (caustics) method as applied to the measurement of the

dynamic fracture toughness K I d is studied by using a finite element
method. A cracked plate subject to a ramp or step load is considered
and the crack is assumed to begin to propagate when the theoretically
exact value of dynamic stress intensity factor Kj(t) reaches a critical
value K c r i t . The shadow spots by reflection are generated by making
assumption of plane stress condition. It is found that there exists a
delay time to detect crack initiation due to the slowness of the
development of the stress high enough to have an apparent effect on
shadow spots, and that the delay time explains the dependence of the
measured K j d on the input wave form and loading rates for a short time-
to-fracture.

KEYWORDS

Shadow s p o t m e t h o d ; f i n i t e e l e m e n t s i m u l a t i o n ; dynamic f r a c t u r e
toughness; s h o r t t i m e - t o - f r a c t u r e ; delay to d e t e c t crack i n i t i a t i o n .

INTRODUCTION

I t has been r e p o r t e d r e c e n t l y t h a t in the short t i m e - t o - f r a c t u r e , the

v a l u e s of dynamic f r a c t u r e t o u g h n e s s K I d i n d i c a t e an enormously sharp
i n c r e a s e or depend on t h e i n c i d e n t s t r e s s wave form (Kalthoff, 1986,
Shockey et al., 1983, Homma et al., 1983). These p e c u l i a r behaviors of
K I( j r a i s e a s e r i o u s q u e s t i o n a b o u t t h e e x t e n t t o which t h e b a s i c
c r i t e r i o n , K j ( t ) = K I d , can be v a l i d l y used ( A o k i , 1 9 8 8 ) . These
p e c u l i a r b e h a v i o r s can be explained by assuming a f r a c t u r e incubation
time ( K a l t h o f f , 1986, Shockey et al. , 1983, Homma et al., 1983), but
i t s p h y s i c a l b a c k g r o u n d remains u n c e r t a i n . In the p r e s e n t s t u d y , a

443
444
f i n i t e element simulation of an impact fracture t e s t using shadow spot
( c a u s t i c s ) method, which i s usually used for measuring K Id under high
l o a d i n g r a t e s , i s performed in an attempt to e x p l a i n the p e c u l i a r
behaviors of K Id .

SHADOW SPOT METHOD

Let us c o n s i d e r a f l a t p l a t e with a through-crack. One surface of the

p l a t e i s assumed to be r e f l e c t i v e . When loads are applied to the p l a t e ,
due to the r e s u l t i n g change in t h i c k n e s s a small depression near the
crack t i p i s made on the surface of the p l a t e , as shown in F i g . l . A
family of i n c i d e n t l i g h t rays i s r e f l e c t e d on t h i s deformed surface.
The v i r t u a l e x t e n s i o n s of the r e f l e c t e d rays form a shadow s p o t
surrounded by a bright curve ( c a u s t i c curve) on the v i r t u a l screen.

The maximum t r a n s v e r s e diameter D(t) of the shadow spot (width of the

shadow s p o t in the d i r e c t i o n p e r p e n d i c u l a r t o the crack l i n e ) i s
r e l a t e d to the dynamic s t r e s s i n t e n s i t y factor K j ( t ) . The r e l a t i o n for
a stationary crack i s given as (Kalthoff, 1986, Rosakis et al., 1988)

Kj(t) =
10.7 Z Q vB
{D ( t ) J 52 (1)

where E i s the Young's modulus, v the Poisson's r a t i o , B the thickness

of the p l a t e . In usual dynamic f r a c t u r e toughness t e s t s under high
l o a d i n g r a t e s , the photographs of shadow s p o t s are taken by a high
speed camera, then the Kj(t) i s obtained by using e q . ( l ) .

PARALLEL
CAUSTIC LIGHT

SHADOW
SPOT

VIRTUAL SPECIMEN
SCREEN

Fig. 1. Shadow spot method

 445
FINITE ELEMENT SIMULATION

Let us consider an elastic 6 0 m m x 6 0 m m x 5 m m rectangular steel pannel

with a central crack (30mm in length), and apply a ramp or step
pressure o*0(t) on the crack surfaces. The spacial distribution of the
pressure c 0 ( t ) is assumed to be uniform over the crack surfaces. In
order to avoid the effect of the edge of the plate on the stress and
strain fields near the crack tip, we restrict our attention to the
period of time in which the stress waves due to cr0(t) travel through
the plate, reflect at the edge and come back again near the crack tip.

The 4-node isoparametric elements are used. The finite element mesh is
shown in Fig.2. Analyses are carried out with the assumption of the
plane stress condition by using the finite element program "ABAQUS" .
The material constants are assumed as E = 210 Gpa, v = 0.29 and
density = 7.86 g/cm . The crack node release technique (Kanninen, 1974,
Mulluck et al.j 1980) is employed for modeling crack propagation.

The shadow spots by reflection are constructed numerically by using the

law of reflection with the out-of-plane displacement w, which are
obtained by the finite element plane stress analysis, and Kj(t) is
determined from D(t) of the numerically obtained shadow spot by using
eq.(l). It is necessary to make a little correction in eq.(l) for a
rapidly propagating crack (Nishioka and Kittaka, 1987). However, we
will use eq.(l) without correction even for a rapidly propagating
crack, because we will focus on the KI(j (i, e., the value of Kj(t) at
the onset of crack propagation) in the present investigation.

RESULTS

A ramp pressure i s a p p l i e d on the crack surfaces from time t = 0. The

crack i s s t a t i o n a r y for t < t 0 (t Q = 7/zs) and i t begins to propagate at

Fig. 2. F i n i t e element mesh

446
t = tQ. The amplitude of the ramp pressure is chosen in such a way that
the theoretical value of Kj(t) reaches K c r it at time t = tQ, i.e.,
Kj(t 0 ) = K c r i t ( K c r i t =68.5 MPa-Am). The crack velocity v is assumed to
be 0.1 C 1 .

Let S n and S r denote the maximum and minimum values of X-^coordinate of

caustics as shown in the inlet in Fig.3. The time variations of S n ,
S r and (S h +S r )/2 are shown in Fig.3, where Z 0 / ( C 1 t Q ) = 12.5. It is
found that the apparent change of caustics due to crack initiation is

-0.20
0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
t / t0

Fig. 3. Detection of crack initiation

1.6 -i 1 1 1 1 1 1 1 1 1 1 1 rprj-

Theoretica
1.2 • •• v=o.ict
ooo V = 0. 5C6
0.8

+- 0.4

_i I i I i I i I i L
0 0.2 0.4 0.6 0.8 1.0 1.2 1.4

t / tn

Fig. 4. Time variation of measured Kj(t)

 447
observed at t / t Q = 1.16. This means that the crack initiation is
detected a little later than the actual one in case where the loading
rate is high and the time-to-fracture is less than 10 jus.

The time variations of Kj(t) obtained from D(t) of the numerical shadow
spots by using eq.(l) (which will be referred to as K m (t)) and the
t h e o r e t i c a l v a l u e of K j ( t ) (which will be r e f e r r e d to as
Kj (t)) are shown in Fig.4. The results for v = 0.5C^ are also plotted
in the same figure for comparison. The K j ( t ) has a peak at t/tQ= 1.0,
while K m (t) has a peak at t/t Q = 1.16.

Since the time (t/t Q = 1.16) at which K m (t) has a peak coincides with
the time at which the crack initiation is detected (Fig.3), the value
of K m (t) at the peak gives the measured K I d . It follows from this that
the measured K I d is greater than K cr it for the case where the time-to-
fracture is short. It is also found in Fig.4 that the measured K I d is
i n d e p e n d e n t of the crack speed v and that K m ( t ) < K j n ( t ) for
t/t o <1.0.

Figure 5 compares the results for a ramp pressure and a step pressure.
The result for a ramp pressure is the same as in Fig.4 for v =
O.IC-L- The amplitude of the step pressure is chosen in such a way that
Kj (t Q ) = K c r j ^ (tQ= 7>us). Other test conditions for the step pressure
are identical with those for the ramp pressure. It is observed that
there exists a difference between the K I d value obtained under a ramp
load and that under a step load. This means that the K I d values
measured by shadow spots depend on input stress wave form. Note that
the delay time of detection of crack initiation coincides with each
other.

1.6 i ■ I ' r
■H

: Theo re t i c a
1.2 ooo step
• • • Ramp

~ 0.4

_i I i I i I i I i I i I i L
-0.4-
0 0.2 0.4 0.6 0.8 1.0 1.2 1.4
t / t0

Fig. 5. Effect of input stress wave form on

measured K I d
448
The effect of loading rate on K I d is shown in Fig.6. The solid circles
indicate the same result in Fig.5 for a ramp pressure or in Fig.4 for v
= 0.1C1, while the hollow circles are the result for a more rapid ramp
pressure, under which Kj n (t) reaches K c r i t at t = 4 u s. Other test
conditions are identical with each other. It is found that K T d is
overestimated more under higher loading rate, and also that there is
not a significant difference in delay time of detection of crack
initiation. It is suggested from these results that the correct KTri
value (i. e. K c r i t ) would be obtained in case where the time-to-
fracture is large (at least more than 15 jus) under low loading rate.

DISCUSSIONS

Figure 7 compares the exact (Ma et a i . , 1 9 8 6 ) , numerical and

approximate (by the singular term) solutions of the stress a 2 2 ahead
of the crack tip (x 2 =0, x 1 > 0 ) for a step pressure. The amplitude of
the step load <r a is identical with that in Fig. 5. The numerical
solution is found to agree well with the exact solution. It is found
that a flat stress field spreads widely behind the wave front, i, e.,
x 1 /(C 1 t) = 1.0, and also that the radius R of the K^h(t)-field may be
represented by R = 0.02C1t.

Since R increases slowly, the Kjh(t)-field is not developed enough to

cover the initial curve even at the crack initiation time. This
e x p l a i n s the r e s u l t in F i g . 5 that K m (t) < K^ h (t) for t < t . Simil ar
e x p l a n a t i o n may be a p p l i c a b l e t o t h e r e s u l t s t h a t ° K m ( t ) <
Kj ( t ) for t < t 0 under the ramp load (Figs.4 and 6 ) .

The s t r e s s f i e l d s after crack i n i t i a t i o n can be described as the sum of

-Theoiet ical
ooo High
St lain rate
• •• Low
St tain iate
-0.4- J_ J i L J i 1 i I i L
0 0.2 0.4 0.6 0.8 1.0 1.2 1.4-

t / t0

Fig. 6. Effect of loading rate on measured K

 449
(A)those of a statonary crack subjected to the pressure o" 0 (t) on i t s
s u r f a c e s and (B)those of a propagating crack subjected to the pressure
<* Q ( 1 ) + P ( t ) o n t n e newly created surfaces. The pressure p ( t ) denotes
the pressure which i s equal to the n e g a t i v e value of t e n s i l e s t r e s s
a c t i n g on the plane ahead of the crack t i p . The s t r e s s f i e l d s ( B ) i s
equal t o the change of s t r e s s due to crack e x t e n s i o n . Although the
f r o n t of the s t r e s s wave g e n e r a t e d by crack e x t e n s i o n from t = t 0
extends at time t to the d i s t a n c e C 1 (t - t Q ) from the o r i g i n a l crack
t i p , the f l a t s t r e s s f i e l d i s thought to spread widely j u s t behind the
wave front for v = 0.1 C - ^ 0 . 5 Ci.

Because the s t r e s s in t h i s f i e l d i s small, i t does not have an apparent

e f f e c t on the shadow s p o t . The s t r e s s which has an apparent e f f e c t on
the shadow s p o t s p r e a d s so s l o w l y ( 0 . 2 - ^ 0 . 3 C^ ) t h a t i t takes a
c o n s i d e r a b l e time for t h i s s t r e s s to reach the i n i t i a l curve which has
a l r e a d y d e v e l o p e d l a r g e a t t = t Q . U n t i l t h i s s t r e s s reaches the
i n i t i a l c u r v e , the shadow s p o t s c o i n c i d e with those for the s t r e s s
f i e l d s ( A ) and c o n t i n u e s t o d e v e l o p . This e x p l a i n s the d e l a y of
d e t e c t i o n of crack i n i t i a t i o n shown in Fig.3 and the overestimation of
K
c r i t s n o w n i n Figs.4—6.

Since the increment in K m (t) during the delay of d e t e c t i o n of crack

i n i t i a t i o n i s equal t o t h a t in the s t r e s s f i e l d s ( A ) , the measured
K Id depends on the incident s t r e s s wave and loading rate. This explains
the r e s u l t s in F i g . 5 and 6. Therefore, The delay time may explain to
some e x t e n t the meaning of the incubation time. Further study would be
necessary to e x p l a i n f u l l y the physical meaning of the incubation time
which might e x i s t in the microscopic fracture behaviors.

3.0
Exac t
o o o F . E.M.
2.0 App r ox i ma t e
(by Ki ( t )

1.0 h

0 h ^-o-o._
~D cr o

0.2 0.4 0.6 0.8 1.0

Fig. 7. Stress distribution ahead of the tip of a

crack subjected to a step pressure o"0(t)
on its surfaces
450

For l o n g t i m e - t o - f r a c t u r e ( a t l e a s t l o n g e r than 15 jus f o r s t e e l ) , the

e f f e c t of d e l a y time t o d e t e c t c r a c k i n i t i a t i o n i s not s i g n i f i c a n t , and
h e n c e t h e b a s i c c r i t e r i o n K j ( t ) = K I d i s u s e f u l . In c a s e where a crack
i n i t i a t e s near t h e m i d - t h i c k n e s s of t h e s p e c i m e n , i t t a k e s a
c o n s i d e r a b l e t i m e f o r the s t r e s s wave due t o c r a c k i n i t i a t i o n t o r e a c h
t h e s p e c i m e n s u r f a c e . The d e l a y t i m e t o d e t e c t c r a c k i n i t i a t i o n i s ,
t h e r e f o r e , more s i g n i f i c a n t t h a n t h a t o b t a i n e d i n t h e t w o - d i m e n s i o n a l
simulation.

CONCLUSIONS

A f i n i t e e l e m e n t s i m u l a t i o n o f m e a s u r i n g K I d by t h e s h a d o w s p o t
( c a u s t i c s ) method i n t h e r a n g e o f s h o r t t i m e - t o - f r a c t u r e i s performed
i n t h i s s t u d y . I t i s found t h a t t h e r e e x i s t s a d e l a y time t o d e t e c t
c r a c k i n i t i a t i o n b e c a u s e of t h e s l o w n e s s o f t h e d e v e l o p m e n t o f t h e
s t r e s s h i g h e n o u g h t o have an a p p a r e n t e f f e c t on shadow s p o t s . The
p e c u l i a r e x p e r i m e n t a l d a t a t h a t K I d d e p e n d s on i n p u t wave form and
l o a d i n g r a t e a r e q u a l i t a t i v e l y e x p l a i n e d by t a k i n g t h e d e l a y time of
d e t e c t i o n o f c r a c k e x t e n s i o n by t h e s h a d o w s p o t m e t h o d i n t o
consideration.

REFERENCES

Aoki, S. ( 1 9 8 8 ) . On t h e m e c h a n i c s o f dynamic f r a c t u r e . JSME Int. J. ,

Ser.I, 31, 487-499.
Homma, H . , D . A . S h o c k e y and Y.Murayama ( 1 9 8 3 ) . R e s p o n s e of c r a c k i n
s t r u c t u r a l m a t e r i a l s to short p u l s e l o a d s . J. Mech. Phys. Solids, 31,
261-279.
Kanninen, M.F. ( 1 9 7 4 ) . A dynamic a n a l y s i s of u n s t a b l e c r a c k p r o p a g a t i o n
i n t h e DCB s p e c i m e n . Int. J. Fract., 10-3. 415-431.
K a l t h o f f , J . F . ( 1 9 8 6 ) . F r a c t u r e b e h a v i o r under h i g h r a t e s of l o a d i n g .
Eng. Fract. Mech., 23., 2 8 9 - 2 9 7 .
Ma, C . C . and L . B . F r e u n d ( 1 9 8 6 ) . The e x t e n t of t h e s t r e s s i n t e n s i t y
f a c t o r f i e l d d u r i n g c r a c k growth under dynamic l o a d i n g c o n d i t i o n s .
J. Appl. Mech., 108., 3 0 3 - 3 1 0 .
M a l l u c k , J . F . a n d W . W . K i n g ( 1 9 8 0 ) . F a s t f r a c t u r e s i m u l a t e d by
c o n v e n t i o n a l f i n i t e e l e m e n t s : A c o m p a r i s o n of two e n e r g y r e l e a s e
a l g o l i t h m . I n : Crack arrest methodology and applidations (G.T.Hahn
and M.F.Kanninen, E d . ) , ASTM-STP 7 1 1 . 3 8 - 5 3 .
N i s h i o k a , T . and H . K i t t a k a ( 1 9 8 7 ) . A t h e o r y of c a u s t i c s f o r mixed mode
f a s t r u n n i n g c r a c k s . Trans. JSME, Ser.A, ( i n J a p a n e s e ) , 54., 1 0 6 1 -
1068.
R o s a k i s , A . J . , A . T . Z e h n d e r and R . N a r a s i m h a n ( 1 9 8 8 ) . C a u s t i c s by
r e f l e c t i o n and t h e i r a p p l i c a t i o n t o e l a s t i c - p l a s t i c and dynamic
f r a c t u r e m e c h a n i c s . Optical Eng., 21_, 5 9 6 - 6 1 0 .
S h o c k e y , D . A . , J . F . K a l t h o f f and D . C . E r l i c h ( 1 9 8 3 ) . E v a l u a t i o n of
dynamic crack i n s t a l i b i t y c r i t e r i a . Int. J. Fract., 22_, 2 1 7 - 2 3 1 .
WS2g2

ESTIMATION OF TRUE FRACTURE ENERGY FOR DYNAMIC FRACTURE TOUGHNESS

EVALUATION BY COMPUTER AIDED INSTRUMENTED IMPACT TESTING (CAI) SYSTEM

Isamu YAMAMOTO and Toshiro KOBAYASHI

Department of Production Systems Engineering,

Toyohashi University of Technology
Tempaku-cho, Toyohashi, 441, Japan

ABSTRACT

In CAI system, the real absorbed energy can be obtained by subtracting the
energy consumed by the elastic deformation of the Charpy impact testing
machine from the measured absorbed energy by the compliance correction
method. It is very important to use accurate total compliance (Ct) and
specimen compliance (Cs) in this method. At first, therefore, Ct and Cs
were measured under the various impact velocities. However, its method can
not be corrected for the brinelling deformation of the specimen.Therefore,
the energy consumed by the brinelling deformation was investigated under
the dynamic loading condition. From these results, the energy consumed by
only the deformation and fracture of specimen itself were estimated.

KEYWORDS

F r a c t u r e t o u g h n e s s , Charpy t e s t , c o m p l i a n c e c o r r e c t i o n , brinelling
d e f o r m a t i o n , d e f l e c t i o n , s t r a i n gauge

INTRODUCTION

I n o r d e r t o e v a l u a t e p r e c i s e l y t h e f r a c t u r e t o u g h n e s s of m a t e r i a l s , i t i s
needed t o measure t h e energy consumed by only a d e f o r m a t i o n and a f r a c t u r e
of specimen i t s e l f . In JSME S001(JSME, 1 9 8 1 ) , i t i s recommended t o c o r r e c t
t h e e r r o r s caused by an e l a s t i c d e f o r m a t i o n of a j i g and a b r i n e l l i n g
d e f o r m a t i o n of a t h r e e p o i n t b e n d i n g s p e c i m e n . I n c o m p u t e r a i d e d
i n s t r u m e n t e d Charpy impact t e s t i n g system (CAI s y s t e m ) ( T . K o b a y a s h i e t a l ,
1 9 8 9 ) , t h e a b s o r b e d e n e r g y i n t h e s p e c i m e n i t s e l f c a n be o b t a i n e d by
s u b t r a c t i n g t h e energy consumed by t h e e l a s t i c d e f o r m a t i o n of t h e m a c h i n e
f r o m t h e m e a s u r e d a b s o r b e d e n e r g y by t h e c o m p l i a n c e c o r r e c t i o n
method(T.Kobayashi, 1 9 8 3 ) . I t i s v e r y i m p o r t a n t t o u s e a c c u r a t e t o t a l
compliance ( C t ) and specimen compliance (Cs) i n t h i s method. T h e r e f o r e , a t
f i r s t , t h e impact v e l o c i t y dependency of Ct and Cs w e r e i n v e s t i g a t e d and
t h e r a t i o of Cs t o Ct ( C s / C t ) was d i s c u s s e d f o r four k i n d s of m a t e r i a l s .

By t h e way, a b r i n e l l i n g d e f o r m a t i o n i s g e n e r a t e d a t t h e impact p o i n t of

451
452
t h e s p e c i m e n and i t w i l l g i v e an e r r o r t o a l o a d - d e f l e c t i o n c u r v e .
However, i t c a n n o t be c o r r e c t e d by t h e c o m p l i a n c e c o r r e c t i o n method.
T h e r e f o r e , t h e r e l a t i o n s h i p b e t w e e n t h e b r i n e l l i n g d e f o r m a t i o n and t h e
d e f l e c t i o n was i n v e s t i g a t e d u n d e r t h e dynamic l o a d i n g c o n d i t i o n and t h e
energy consumed by t h e forming of t h e b r i n e l l i n g d e f o r m a t i o n was e s t i m a t e d
from t h i s r e l a t i o n s h i p f o r t h r e e k i n d s of m a t e r i a l s . F i n a l l y , t h e t r u e
a b s o r b e d energy i n only t h e specimen i t s e l f was e s t i m a t e d from t h e a b o v e
results.
EXPERIMENTAL

M a t e r i a l s and specimen g e o m e t r i e s

The m a t e r i a l s used in t h i s study a r e p a r t i a l l y s t a b i l i z e d z i r c o n i a ceramic

(PSZ), SS41 s t e e l , d u c t i l e c a s t i r o n (DCI) and 6061-T6 aluminum a l l o y . The
specimen g e o m e t r i e s used a r e summarized i n T a b l e 1.

Table 1. Materials and specimen geometries used.

Specimen Geometries (mm) j

Materials
Thickness Width Length a/W Notch
Partially Stabilized Zirconia (PSZ) 4 8 40 —
SS41 steel 10 10 55 0.6 Slit
Ductile Cast Iron (DCI) 10 10 55 0.6 Slit
6061-T6AI alloy 10 10 55 0.6 Slit
a/W:notch to width ratio

Measurement of the t o t a l compliance (Ct) and specimen compliance (Cs)

The s t r a i n gauge was attached onto the specimen s u r f a c e (T.Kobayashi e t

a l . , 1989). The gauge attached position i s 2mm transversely from the s l i t
t i p . In an unnotched specimen, the s t r a i n gauge was put on the e q u i v a l e n t
p o s i t i o n to the notched specimen. At f i r s t , the l o a d - s t r a i n gauge output
r e l a t i o n was recorded in the e l a s t i c r e g i o n under t h e s t a t i c l o a d i n g
c o n d i t i o n . The r e l a t i o n s h i p between the deflection of the specimen i t s e l f
and the s t r a i n gauge o u t p u t i s a b l e t o be o b t a i n e d from t h e o r e t i c a l
d e f l e c t i o n e q u a t i o n of beam and t h e recorded l o a d - s t r a i n gauge output
r e l a t i o n . Next, the hammer l o a d - d e f l e c t i o n curve and t h e hammer l o a d -
s t r a i n gauge o u t p u t were recorded simultaneously by using the 1.47J or
490J c a p a c i t y i n s t r u m e n t e d Charpy impact t e s t i n g machine a t i m p a c t
v e l o c i t y range from O.lm/s to 4.0m/s. Since the deflection in the hammer
load-deflection curve i s that of t h e whole measuring system, Ct i s the
r e c i p r o c a l of the s l o p e of the i n i t i a l e l a s t i c region on t h i s curve. On
the other hand, Cs i s obtained from the l o a d - s t r a i n gauge output curve and
the r e l a t i o n s h i p between the d e f l e c t i o n of the specimen i t s e l f and the
s t r a i n gauge output.

Study on t h e r e l a t i o n s h i p between t h e b r i n e l l i n g deformation and

deflection

The r e l a t i o n s h i p between the d e f l e c t i o n and the b r i n e l l i n g deformation

under the impact loading c o n d i t i o n was i n v e s t i g a t e d by the s t o p block
t e s t ( T . K o b a y a s h i , 1983) for SS41 s t e e l , DCI and 6061-T6 aluminum a l l o y .
After the stop block t e s t , the b r i n e l l i n g deformation at the 1/2 p o s i t i o n
of t h i c k n e s s d i r e c t i o n was measured by the t o o l microscope of 20
magnifications.

RESULTS AND DISCUSSION

 453
Impact velocity dependency of the total compliance (Ct) and the specimen
compliance (Cs)

Figure 1 shows the changes of Ct with changing impact velocity for

materials used. Fig.2 shows the changes of Cs with changing impact
velocity for materials used. For PSZ and SS41 steel, both of Ct and Cs are
decreased with increasing impact velocity. Especially, its variation is
remarkable below about l.Om/s. For 6061-T6 aluminum alloy, both of Ct and
Cs are not dependent the impact velocity for the whole impact velocity
range. Th.Macke et al.(Th.Macke et al., 1990) have reported the reason of
changes of Ct and Cs as the following phenomena involved in the tup-
specimen interaction: (l)the change in the contact stiffness during the
impact due to an increase in the contact surface, (2)the significance of
the brinelling effect, and (3)a plastic hardening of the material in the
2 5
iO 6 0 6 1-T6Alalk>y|
•
A
PSZ
S S 4 1 steel
2 0 ▲ DCI 1
z o
E
E 15

1 0

ii^W.ni Z# "■■■■-A,,

1 .0 2.0 3.0 4.0 5.0

Impact velocity (m/s)
Flg.1 Variation of Ct with the impact velocity.

1 0 I T 'T ^—1
l O : 6 0 6 1 T6AI alloy • : PSZ
| A : S S 4 1 steel A : DCI

D o
O
•—. o o - O- -
E O
▲
E ▲ H
A A-A
A A

to
O

— • • •
i i i 1
1.0 2.0 3.0 4.0 5.0
Impact velocity (m/s)
Fig.2 Variation of Cs with the impact velocity.
454

v i c i n i t y of the impact area. However, there was no b r i n e l l i n g deformation

traces in PSZ specimen. Moreover, the impact velocity dependency of Ct and
Cs could not be observed in 6061-T6 aluminum a l l o y . T h e r e f o r e , i t i s
assumed t h a t they were caused by the s t r a i n r a t e dependency of t h e
d e f o r m a b i l i t y . I t have been thought t h a t an e l a s t i c modulus under the
dynamic loading condition i s larger than the one under the s t a t i c l o a d i n g
c o n d i t i o n . From a view point of the h e a t - e l a s t i c theory, heat generation
by a s t r a i n i s diffused i s o t h e r m a l l y in the s t a t i c l o a d i n g c o n d i t i o n .
S i n c e t h e r e i s n o t enough t i m e t o d i f f u s e in the dynamic l o a d i n g
condition, a h e a t t r a n s f e r i s a d i a b a t i c . Then, if the s t a t i c e l a s t i c
modulus i s e q u i v a l e n t to the isothermal e l a s t i c modulus and the dynamic
one i s e q u i v a l e n t t o the a d i a b a t i c o n e , t h e r e l a t i o n s h i p between
isothermal e l a s t i c modulus and adiabatic e l a s t i c modulus i s represented by
the eq.(l)(JSME, 1980).

1/E.i s o -1/E ad.: = ( T 0 n / ( / C p ) (1)

where T is an absolute temperature,^ is a coefficient of thermal

expansion, f is a specific gravity and Cp is a specific heat at constant
pressure. It is found by calculating eq.(l) for SS41 steel that a
difference between the dynamical elastic modulus and the statical elastic
one is only 0.15%. This dose not explain the rapid changes of Ct and Cs
below 1 m/s. Consequently, it may be assumed that the impact velocity
dependency of Ct and Cs are caused by the effect of the change of hammer-
specimen interaction in addition to the strain rate dependency of a
deformability.

Figure 3 shows the changes of Cs/Ct with impact velocity. For materials
used, Cs/Ct are held at the constant values for whole impact velocity
range. It is found from these results that Cs/Ct is determined from only
the specimen geometry, specimen material and testing machine. The
relationships between Ct, Cs or Cs/Ct and the static elastic modulus for
SS41 steel, DCI and 6061-T6 aluminum alloy are shown in Fig.4. Both of Ct
and Cs are non-linear for the static elastic modulus assumed from the
theoretical deflection equation of the beam. It is found from Fig.4 that
the ratio of Cs to Ct (Cs/Ct) and the static elastic modulus hold a good
correlation. Therefore, there is a possibility that Cs/Ct is presumed from
the static elastic modulus.
1 o o 1 1 1 1 1

A
*
A

O 5 0
O «-r>--« •

IO: 6 0 6 1 -T 6 Al alloy
• : PSZ
A : S S 4 1 steel
|A : DCI
L i i i i
1.0 2.0 3.0 4.0 5.1
Impact velocity (m/s)
Fig .3 Variation of Cs/Ct with the impact velocity.
 455
T 1 11 0 0
<*
\\
s-^
2

E \ V A

n
E \ 3?
O \ N
s>' '
J2*
r- 1 0 5 0
o
■ ** "

o *C!
(6061-T6)
X o

o
to
1°
•
C t
C s
(DCI) —•
(SS41 steel)
1A C s/C t
i . j
10 0 2 0 0 30 0
Statical elastic modulus ( GPa )
Fig.4 Relationships Cs, Ct and Cs/Ct and
static elastic modulus.

Discussion about the true deformation and fracture energy in the specimen

According to the compliance correction method, the absorbed energy in the

specimen itself is estimated by eq.(2)(T.Kobayashi, 1984).

Ei=Eifx(Cs/Ct) (2)
where Ei ' i s t h e a p p a r e n t absorbed energy measured from t h e l o a d -
deflection curve, Ei i s the true deformation and f r a c t u r e energy in the
specimen i t s e l f . Therefore, i t can be considered that 1-Cs/Ct c o r r e l a t e s
with the energy (Ew) consumed by the e l a s t i c deformation of Charpy machine
to E i ' . Energy consumed by the e l a s t i c deformation of the Charpy machine
for a/W=0.6 type specimen are shown in Table 2.
M o r e o v e r , t h e e r r o r of l o a d - d e f l e c t i o n curve i s a l s o given by the
b r i n e l l i n g deformation formed a t the impact p o i n t . F i g . 5 shows t h e
r e l a t i o n s h i p between the d e f l e c t i o n and the b r i n e l l i n g deformation for
SS41 s t e e l , DCI and 6061-T6 aluminum a l l o y . The r a t i o of the energy (E R )
consumed by the the forming of t h e b r i n e l l i n g deformation t o Ei' are
summarized in Table 2. The true deformation and f r a c t u r e energy in the
s p e c i m e n i t s e l f can be o b t a i n e d from t h e s e a n a l y s i s and a r e a l s o
summarized in Table 2.

Table 2. Analysis of the absorbed energy.

Materials EM (%) EB (%) Ei(%)
SS41 steel 26.9 5.0 68.1
Ductile Cast Iron (DCI) 53.3 14.7 32.0
6061-T6AI alloy 64.5 6.4 29.1
EM : consumed by tne elastic deformation of the machine
EB : consumed by the brinelling deformation
E i : true defromation and fracture energy in the specimen itself
456
U. i ■ -~t 1 "i I

O : ss4isteel
• : 6 0 6 1-T6AI alloy
^ A:DCI

E
E o
^C_^0.2 /
/ A
.2
o /
//
CO
E
o /
/^—- " •
o>
^%-^t
"5 0.1
c •j
CO

4> i 1
2.0 3.0
Deflection ( m m )
Fig.5 Rleationship between deflection and
brinelling deformation.

CONCLUSION

(l)It is found that Ct and Cs in PSZ and SS41 are dependent on the impact
velocity and the ones in 6061-T6 aluminum alloy are not dependent on the
impact velocity. It has been suggested that the impact velocity dependency
of Ct and Cs are caused by the effects of the deceleration of the hammer
at impact and the change of hammer-specimen interaction in addition to the
strain rate dependency of a deformability.
(2)The ratio of Cs to Ct (Cs/Ct) and the static elastic modulus have a
good correlation. Therefore, there is a possibility that Cs/Ct is presumed
from the static elastic modulus.
(3)It was found for SS41 steel, DCI and 6061-T6 aluminum alloy that the
true deformation and fracture energy in the specimen itself was about
68.1%, 32.0 % and 29.1% of the apparent absorbed energy until the maximum
loading point.

REFERENCES

The Japan Society of Mechanical Engineers( 1981).Standard Method of Test

for Elastic-Plastic Fracture Toughness J,C.JSME S 001-1981.
The Japan S o c i e t y of M e c h a n i c a l E n g i n e e r s (1980).
Kinzokuzairyou-no-danseikeisuu ( in Japanese ), pp.20-21.
Th.Macke, E.Martin, J.J.Balette and J.M.Quenisset (1990).Compliance
calibration during instrumented Charpy impact testing. Eng.Frac.Mech. ,
37, 831-838.
T.Kobayashi and M.Niinomi(1989). Evaluation of dynamic crack initiation
and growth toughness by computer aided Charpy impact testing system.
Nuclear Engineering and Design, 111, 27-33.
T.Kobayashi (1984). Analysis of impact properties of A533 steel for
nuclear reactor pressure vessel by instrumented Charpy test.
Eng.Frac.Mech., 2£, 49-65.
T.Kobayashi (1983). Measurement of dynamic fracture toughness J JH by
instrumented Charpy test.Int.J.of.Fracture, 23, R105-R109.
WS2g4

MIXED-MODE IMPACT FRACTURE TESTS AND THEIR NUMERICAL SIMULATION

Toshihisa Nishioka, Tatsuyuki M u r a k a m i / Y u t a k a T a k e m o t o and K e i g o Sakakura

D e p a r t m e n t of O c e a n M e c h a n i c a l E n g i n e e r i n g
K o b e U n i v e r s i t y of M e r c a n t i l e M a r i n e
5-1-1 F u k a e M i n a m i m a c h i / Hi g a s h i n a d a - k u / K o b e / Japan

ABSTRACT

In the p r e s e n t study/ using t h r e e - p o i n t bend s p e c i m e n s of PMMA s u b j e c t e d to

the impact load by a d r o p p i n g rod at o f f - c e n t e r line/ a s e r i e s of m i x e d - m o d e
impact f r a c t u r e t e s t s w e r e c a r r i e d out . T h e e c c e n t r i c i t y of loading point
w a s s y s t e m a t i c a l l y c h a n g e d . T h e r e l a t i o n s a m o n g the i n i t i a t i o n a n g l e / global
p r o p a g a t i o n a n g l e and the loading eccentricity were obtained. Generation
phase simulation was performed for the m i x e d - m o d e impact f r a c t u r e t e s t s ,
u s i n g m i x e d - m o d e s i n g u l a r e l e m e n t s that can d i r e c t l y c o m p u t e K and K . It

was found from the s i m u l a t i o n r e s u l t s that/ for the c a s e s of larger loading

e c c e n t r i c i t y / the c r a c k s u r f a c e s in the vicinity of the crack-tip make
contact each other/ and s u b j e c t to only m o d e II d e f o r m a t i o n . T h e f r a c t u r e
i n i t i a t i o n a n g l e s in t h e s e c a s e s a g r e e w i t h the m a x i m u m e n e r g y r e l e a s e rate
criterion. This kind of p h e n o m e n o n is e x t r e m e l y d i f f i c u l t to find by the
experiment alone.

KEYWORDS

M i x e d - M o d e ; Impact F r a c t u r e ; S i n g u l a r E l e m e n t ; Finite Element Simulation;

High-Speed Photography; Dynamic Crack Closure;

I N T R O D U C T I ON

Stress waves in s o l i d s are usually induced by the c o l l i s i o n w i t h o t h e r

o b j e c t s . On the o t h e r hand/ initial c r a c k s are u s u a l l y c a u s e d by f a t i g u e or
by stress corrosion cracking under q u a s i - s t a t i c l o a d i n g s . T h u s , in m a n y
actual c a s e s , impact s t r e s s w a v e s o b l i q u e l y impinge to the crack-tips, and
produce unsymmetricaI m i x e d - m o d e s t a t e s a r o u n d the c r a c k - t i p s . In s p i t e of
the i m p o r t a n c e of m i x e d - m o d e impact f r a c t u r e in actual s i t u a t i o n s / fracture
mechanics in t h i s c o n t e x t has not been well e s t a b l i s h e d . T h i s is due to the
following difficulties arising in m i x e d - m o d e fracture problems. For
instance/ (i) Impact fracture cannot be inferred from s t a t i c f r a c t u r e
m e c h a n i c s / s i n c e the impact s t r e s s w a v e p r o p a g a t e s w i t h h i g h - s p e e d in very
complex manners. (ii) T h e m o d e I and m o d e II s t r e s s i n t e n s i t y f a c t o r s are
s o m e t i m e s d i f f i c u l t to s e p a r a t e , (iii) T h e boundary conditions vary with

457
458
t i me # and c o n t a c t / n o - c o n t a c t c o n d i t i o n s may o c c u r at the loading point and
at s u p p o r t e d p o i n t s of the s p e c i m e n .

In the p r e s e n t paper/ e x p e r i m e n t a l r e s u l t s for m i x e d - m o d e f r a c t u r e t e s t s are

s h o w n f i r s t . T h r e e - p o i n t bend s p e c i m e n s s u b j e c t to u n s y m m e t r i c a I impact load
w e r e u s e d . Next/ in order to s i m u l a t e these e x p e r i m e n t s / a m i x e d - m o d e
singular finite element method is d e v e l o p e d . N u m e r i c a l r e s u l t s for the
generation p h a s e s i m u l a t i o n of the m i x e d - m o d e impact t e s t s are also s h o w n .
The mixed-mode dynamic stress intensity f a c t o r s are e v a l u a t e d by the
s i n g u l a r e l e m e n t m e t h o d . D y n a m i c c r a c k c l o s u r e p h e n o m e n a prior to the impact
f r a c t u r e are m a n i f e s t e d by the n u m e r i c a l s i m u l a t i o n .

MIXED-MODE IMPACT F R A C T U R E TESTS

T h e g e o m e t r y of a t h r e e - p o i n t bend s p e c i m e n is s h o w n in F i g . 1 . Polymethyl
m e t h a c r y l a t e w a s used in the p r e s e n t e x p e r i m e n t . T h e initial c r a c k c o n s i s t s
of a m a c h i n e n o t c h (35 m m ) and a f a t i g u e c r a c k (15 m m ) . T h e s p e c i m e n was
collided by a d r o p p i n g rod (5.05 K g ) at the o f f - c e n t e r line. To induce
v a r i o u s m a g n i t u d e of m i x e d - m o d e s t a t e in the s p e c i m e n / the e c c e n t r i c i t y of
loading ( e = A / ( s / 2 ) ) w a s s y s t e m a t i c a l l y c h a n g e d . T h e initial impact v e l o c i t y
of the rod w a s set as 5 m / s e c .

High-speed p h o t o g r a p h s of the m i x e d - m o d e f r a c t u r e test s p e c i m e n s w e r e taken

w i t h a laser light w h i c h can be p r o m p t l y s y n c h r o n i z e d to the initiation of
impact loading by the h a m m e r . F i g u r e 2 i l l u s t r a t e s the t r i g g e r s y s t e m of the
laser light s o u r c e for the h i g h - s p e e d c a m e r a used in the p r e s e n t e x p e r i m e n t .
A H e - N e laser of 5 mW and a laser d e t e c t o r w e r e used for the t r i g g e r s y s t e m .
W h e n the head of the d r o p p i n g rod i n t e r c e p t s the laser beam/ the photo-cell
in the laser d e t e c t o r in c o n j u n c t i o n w i t h the t r i g g e r c i r c u i t (see F i g . 3)
p r o d u c e s a t r i g g e r s i g n a l . The o p t i c a l s e t u p for the t r a n s m i t t e d caustic
m e t h o d is s h o w n in F i g . 3 . A n o t h e r H e - N e laser of 5 0 mW w a s used as the light
s o u r c e of the h i g h - s p e e d p h o t o g r a p h y . The t r i g g e r c i r c u i t s e n d s the trigger
signal to the a c o u s t i c optical m o d u l a t o r . T h e n / the d i r e c t i o n of the laser
beam is c h a n g e d in an e x t r e m e l y s h o r t time/ for a few m i l l i s e c o n d . T h e laser
beam r e a c h e s the h i g h - s p e e d c a m e r a ( C o r d i n D y n a f a x 3 5 0 / 3 5 0 0 0 f r a m e s / s e c )
being t r a n s m i t t e d t h r o u g h the s p e c i m e n .

T h e h i g h - s p e e d p h o t o g r a p h s of the m i x e d - m o d e impact f r a c t u r e test for e = 0 . 5

are s h o w n in F i g . 4 . In the p r e s e n t e x p e r i m e n t / the p h o t o g r a p h s w e r e taken at
the time i n t e r v a l s of a b o u t 30 P s e c . F i g u r e 5 s h o w s the p h o t o c o p y of the
f r a c t u r e d s p e c i m e n for e = 0 . 5 / and also i n d i c a t e s the d e f i n i t i o n s of various
a n g l e . T h e c r a c k s t a r t s p r o p a g a t i n g w i t h the i n i t i a t i o n a n g l e 8 / then
c
p r o p a g a t e s s t r a i g h t w i t h the global a n g l e 8 for a large a m o u n t of d i s t a n c e
g
until the c r a c k r e a c h e s the v i c i n i t y of the loading p o i n t . However/ the
c r a c k c h a n g e s its d i r e c t i o n a b r u p t l y near the loading point/ as s h o w n in
Fig.5.
T h e i n i t i a t i o n a n g l e 8 and the global p r o p a g a t i o n angle 8 against the
c g
loading a n g l e 8 Q w e r e p l o t t e d in F i g . 6 . It is noted that the o r d e r s of the
m a g n i t u d e s of the a n g l e s are consistently/ 8 f t / 8 / and 8 /for all the
x g c
eccentric loading c a s e s . T h e v a r i a t i o n of the i n i t i a t i o n angle 6w i t h the
c
loading e c c e n t r i c i t y e is s h o w n in F i g . 7 . It is seen in the f i g u r e that the
initiation angle 8 s a t u r a t e s even for i n c r e a s i n g loading e c c e n t r i c i t y
c
( e > 0 . 2 ) . T h e p h o t o g r a p h of the f r a c t u r e d s p e c i m e n s is shown in F i g . 8 .
 459
MIXED-MODE SINGULAR ELEMENT

N i s h i o k a and A t l u r i ( 1 9 8 0 ) h a v e d e v e l o p e d the m o v i n g s i n g u l a r e l e m e n t m e t h o d
in w h i c h the mode-l general solutions for a p r o p a g a t i n g c r a c k - t i p w e r e
i n c o r p o r a t e d as the d i s p l a c e m e n t f u n c t i o n s . This moving singular element
method m a d e it p o s s i b l e to p r e c i s e l y s i m u l a t e the p r o b l e m s of d y n a m i c c r a c k
p r o p a g a t i o n and a r r e s t u n d e r m o d e - l c o n d i t i o n s .

In the present paper/ the m o v i n g s i n g u l a r e l e m e n t m e t h o d w a s e x t e n d e d to

m i x e d - m o d e p r o b l e m s . T h e d i s p l a c e m e n t f u n c t i o n s in the s i n g u l a r e l e m e n t can
be e x p r e s s e d by the f o l l o w i n g e q u a t i o n ( N i s h i o k a and A t l u r i / 1 9 8 0 ) :

where (x/y) is the m o v i n g c o o r d i n a t e s y s t e m c e n t e r e d at the c r a c k - t i P / and

m o v e s w i t h the c r a c k v e l o c i t y C. U. can be e x p r e s s e d by using the general
solutions for a dynamically propagating crack-tip under mixed-mode
c o n d i t i o n . W h e n the c r a c k speed is zero, the general solutions reduce to
those for a s t a t i o n a r y c r a c k . T h e f u n c t i o n s U. i n c l u d e the z e r o s t r e s s e s
and rigid body motions (n=0)/ the singular stresses and corresponding
displacements (n=1)/ the c o n s t a n t s t r e s s e s and linear d i s p l a c e m e n t s ( n = 2 ) ,
and the higher-order terms (n>3) . Thus/ coefficients ocA and or are
equivalent to the dynamic stress intensity factors K. and K. . The

compatibility of displacements/ velocities/ and accelerations at the

boundary between the s i n g u l a r e l e m e n t and r e g u l a r e l e m e n t s (see F i g . 9 ) can
be s a t i s f i e d t h r o u g h a l e a s t - s q u a r e a p p r o a c h ( N i s h i o k a and Atluri/ 1980).
The m o s t a t t r a c t i v e f e a t u r e of the m i x e d - m o d e s i n g u l a r e l e m e n t p r o c e d u r e is
that the s t r e s s i n t e n s i t y f a c t o r s at each time step can be determined
d i r e c t l y as K.-oc. and K = a by s o l v i n g the f i n i t e e l e m e n t e q u a t i o n s .

NUMERICAL RESULTS

Figure 9 shows the f i n i t e e l e m e n t b r e a k d o w n w i t h the s i n g u l a r e l e m e n t and

the r e g u l a r 8 - n o d e i s o p a r a m e t r i c e l e m e n t s . D u e to the eccentric load/ the
entire region w a s used for the a n a l y s e s . In o r d e r to c h e c k the a c c u r a c y of
the p r e s e n t s i n g u l a r e l e m e n t m e t h o d / a s t a t i c p r o b l e m w i t h the a p p l i e d load
at the c e n t e r - l i n e ( e = 0 . 0 ) w a s a n a l y z e d by using the m e s h p a t t e r n s h o w n in
F i g . 9 . N u m e r i c a l r e s u l t s for K and the c r a c k o p e n i n g displacement at the
notch mouth 6 are shown in T a b l e 1. B o t h K and 6 v a l u e s o b t a i n e d by the
present method agree with other solutions within IX e r r o r s .

F o r the a n a l y s e s of the impact f r a c t u r e t e s t s / d i s p l a c e m e n t - c o n t r o l l e d loads

w i t h the loading p o i n t v e l o c i t y of 5 m / s e c were applied at the distances
A=es/2 (e=0.0/ 0 . 1 ^ 0 . 5 ) from the c e n t e r line. T h e d y n a m i c s t r e s s i n t e n s i t y
f a c t o r s K. and K.. d u r i n g the impact loading are s h o w n in F i g . 1 0 / for the
cases of e = 0 . 0 , 0.1/ and 0 . 2 . In the c a s e of e = 0 . 0 / K. v a l u e s are positive/
w h i l e K. v a l u e s are a l w a y s z e r o . T in the f i g u r e s indicate the fracture
initiation time obtained in the experiments. In the c a s e s of e = 0 . K K
v a l u e s are n e a r l y z e r o U P to 8 5 M s e c . T h e m o d e II d e f o r m a t i o n is domainant
comparing the mode I deformation. F u r t h e r m o r e / in the c a s e of e = 0 . 2 , K.
values become negative. The negative K values cannot be occurred in the
real situation. This is due to the a s s u m p t i o n in the a n a l y s i s that allows
460
the o v e r l a p p i n g of the c r a c k - f a c e s . T h e r e f o r e / in the c a s e s of e>0.2, the
c r a c k s are s u b j e c t e d to inplane s l i d i n g under the compression.

In o r d e r to f u r t h e r i n v e s t i g a t e the d e f o r m a t i o n p r o c e s s of the s p e c i m e n / the

same problems were a n a l y z e d by the r e g u l a r 8 - n o d e d i s o p a r a m e t r i c e l e m e n t s
o n l y . T h e d e f o r m e d s h a p e s of the s p e c i m e n s for e=0.1 and 0.2 are shown in
Figs. 11 and 12/ r e s p e c t i v e l y . In the c a s e of e = 0 . 1 / it is s e e n in F i g . 11
that only m o d e II s l i d i n g d e f o r m a t i o n o c c u r s until a b o u t 100 M s e c . In the
c a s e s of e = 0 . 2 / the o v e r l a p p i n g of the c r a c k - f a c e s is seen at 100 M s e c . T h i s
a l s o c o n f i r m s that/ p r i o r to the impact fracture initiation/ the dynamic
c r a c k c l o s u r e t o g e t h e r w i t h the c r a c k s l i d i n g o c c u r s for the c a s e s of e > 0 . 2 .
The saturated v a l u e of the f r a c t u r e initiation angle is
=75.6°6 (see
c
Fig.7). T h i s a n g l e is very c l o s e to the p r e d i c t e d a n g l e of 7 5 . 8 * for a pure
m o d e II c a s e (Hayashi and N e m a t - N a s s e r / 1 9 8 1 ) / based on the m a x i m u m energy-
release-rate c r i t e r i o n / but is at v a r i a n c e w i t h 7 0 . 5 ° by the m a x i m u m s t r e s s
c r i t e r i o n ( E r d o g a n and S i h / 1 9 6 3 ) / and with 85.8° by the strain energy
d e n s i t y c r i t e r i s o n (Sih/ 1 9 7 2 ) .

CONCLUSIONS

T h e f o l l o w i n g p o i n t s w e r e found from the e x p e r i m e n t a l and n u m e r i c a l r e s u l t s .

(1) E v e n for small e c c e n t r i c i t y of the impact loading/ the c a u s t i c patterns
were greatly u n s y m m e t r i c a I w i t h r e s p e c t to the c r a c k - a x i s . T h i s r e s u l t s in
domainant K v a l u e s in this type of m i x e d - m o d e impact f r a c t u r e t e s t .
(2) F o r d y n a m i c a l l y p r o p a g a t i n g c r a c k s , the c a u s t i c p a t t e r n s w e r e s l i g h t l y
u n s y m m e t r i c a I w i t h r e s p e c t to the c r a c k - d i r e c t i o n . T h u s / the m o d e I stress
i n t e n s i t y f a c t o r s w e r e d o m i n a n t w i t h small f r u c t u a t i n g K values.

(3) W h e n the loading e c c e n t r i c i t y e is equal to or greater than 0.2/ the

fracture initiation occurs under only inp I a n e - s I iding mode (mode II)
together with dynamic crack-face contact.
(4) T h e fracture initiation a n g l e s in the c a s e s of e > 0 . 2 a g r e e w i t h the
p r e d i c t e d a n g l e based on the m a x i m u m e n e r g y r e l e a s e rate c r i t e r i o n for the
P U re m o d e I I c a s e .
(5) W h e n the loading e c c e n t r i c i t y is large ( e > 0 . 2 ) / dynamic crack closure
o c c u r s prior to the f r a c t u r e i n i t i a t i o n . T h e r e f o r e / d e v e l o p m e n t s of both new
e x p e r i m e n t a l and s i m u l a t i o n t e c h n i q u e s taking a c c o u n t of d y n a m i c crack-face
c o n t a c t are r e g u i r e d for f u r t h e r i n v e s t i g a t i o n . T h e s e are p a r t l y u n d e r w a y .
A c k n o w l e d g e m e n t : The authors gratefully acknowledge the support of the
S c i e n c e and T e c h n o l o g y G r a n t from T o r a y S c i e n c e F o u n d a t i o n .

REFERENCES

Erdogan/F and G.C.Sih (1963). On crack e x t e n s i o n in p l a t e s u n d e r p l a n e

loading and t r a n s v e r s e s h e a r . J. B a s i c Eng./ £ 5 / 5 1 9 - 5 2 7 .
Hayashi/K. and S . N e m a t - N a s s e r ( 1 9 8 1 ) . E n e r g y - r e l e a s e rate and c r a c k k i n k i n g
u n d e r c o m b i n e d l o a d i n g . J. A P P I . M e c h . / 4 £ / 5 2 0 - 5 2 4 .
Nishioka/T. and S.N.Atluri (1980). Numerical modeling of d y n a m i c c r a c k
p r o p a g a t i o n in finite bodies/ by moving singular elements/ Part I:
f o r m u l a t i o n . J. A P P I . M e c h . / 4 1 / 5 7 0 - 5 7 6 .
Nishioka/T. and S.N.Atruli (1983). Path-independent integrals/ energy
release rates/ and general solutions of n e a r - t i p f i e l d s in m i x e d - m o d e
d y n a m i c f r a c t u r e m e c h a n i c s . E n g . F r a c t . M e c h . / J_&/ 1-22.
Sih/G.C. (1972). Introductory chapter: a special theory of crack
p r o p a g a t i o n / M e c h a n i c s of F r a c t u r e / V o I . 1 , 2 1 - 4 5 .
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S = 400 i 10 mm

1- * »l
TfT

—if

CD CD
k s =4
Fig.1 T h r e e - p o i n t bend specimen
Fig.5 Definitions of v a r i o u s angles
s u b j e c t to an e c c e n t r i c impact load

-^@_-)l-aser
Detector

F i g . 2 T r i g g e r system for
high-speed photography Fig.6 V a r i a t i o n s of t h e f r a c t u r e
i n i t i a t i o n and t h e g l o b a l c r a c k
p r o p a g a t i o n angle/ with the loading angle
| H«-N« LASER t>

TRIGGER
LASER
.3
Fig.3 E x p e r i m e n t a l setup for e
the laser c a u s t i c m e t h o d Fig.7 R e l a t i o n between the fracture
i n i t i a t i o n a n g l e and t h e l o a d i n g e c c e n t r i c i t y
462

_k
CRACK

Fig.9 Finite element breakdown with a singular

e l e m e n t and 8 n o d e d i s o p a r a m e t r i c e l e m e n t s

T a b l e 1 C o m p a r i s o n of s t r e s s i n t e n s i t y factors
and c r a c k o p e n i n g d i s p l a c e m e n t
u n d e r a s y m m e t r i c a l s t a t i c load
P= 4 9 . 4 9 C N 1
Fig.8 Fractured specimens Ki [ M P a B , / z] 6 [..]
S i n g u l a r E l e i e n t Method 0.1649 0.5986
B o u n d a r y C o l l o c a t i o n Method 0.1660
Body F o r c e Method 0.5951
Error -0.66% +0.59%

KI O Ki
A Ki
I o Ki e = 0. O KI
TP
A KI

o°°°

* M 8 A ' A A A A A A A A A A A AA
AAAA
<*^ t
—4
t Usec] t^sec] t [tfsec]
Fig.10 Variations of s t r e s s intensity factors

tu, : 2 0 — u• x 5 0 tu,x20 •- t

100M s e c 1 0 0 ix s e c

rMl
—YutrrT
\ \

i 111"*=
1 5 0 ix s e c

F i g . 1 1 D e f o r m e d s h a p e of F i g . 1 2 D e f o r m e d s h a p e of
the impact s p e c i m e n ( e = 0 . 1 ) the impact s p e c i m e n ( e = 0 . 2 )
WS2g5

AN EXPERIMENTAL STUDY ON SURFACE SINGULARITY OF

FAST PROPAGATING CRACKS IN PMMA

S. SUZUKI
Department of Energy Engineering,
Toyohashi University of Technology
Tempaku-cho, Toyohashi, 441 Japan

ABSTRACT
An optical system of pulsed holography is developed and applied to take
instantaneous photographs of both the opening and the front edge of a crack
which is propagating through a PMMA plate specimen at a speed of several
hundred meters per second. Crack opening displacement (COD) on a specimen
surface is measured along the crack in the vicinity of the tip where the stress
field has three-dimensional (3-d) structure. The COD is proportional to the
squared root of the distance r from the crack tip. It means that the stress
field on a specimen surface has the singularity of l//r, even in the 3-d stress
field. The singularity is unchangeable even though the crack speed changes.
Crack front edge angles are also measured, and they are obtuse. In the case
of lower crack speed, the measured angles agree with the numerical result
of a slowly propagating crack given by Bazant and Estenssoro. As the crack
speed increases, the angles decrease and seem to approach a right angle.

KEYWORDS
Fracture mechanics; brittle fracture; fast propagating crack; surface singularity;
crack front edge angle; optical engineering; pulsed holography.

INTRODUCTION
When a through-crack of the opening mode exists in a elastic plate specimen
of thickness t, a singular stress field appears around the crack tip (Yoffe,
1951). In the case the specimen is infinitesimally thin (t+0), the singular stress
field satisfies the plane stress condition and has the singularity of l//r, where
r is the distance from the crack tip. On the other hand, if the specimen
is infinitely thick (t-*») and if the crack front edge is straight, the singular
stress field satisfies the plane strain condition and has the singularity of l//r
again. But in the case of a specimen of finite thickness there appears three
dimensional (3-d) stress field in the near tip region, because of existence of
free corners at which a crack front edge is terminated by specimen surfaces
(Benthem, 1977; BaYant and Estenssoro, 1979, 1980; Suzuki, 1990). It is an

463
464
important and interesting problem that the 3-d stress field has the same
singularity as that of the two dimensional stress field, or not.

Some studies have been carried out to know the singularity of the 3-d stress
field. Benthem (1977) theoretically studied the singularity around a free corner,
which is called surface singularity, of a stationary crack. He showed that
the singularity differs from l//r if the crack front edge is straight and makes
a right angle with a surface of a specimen. Bazant and Estenssoro (1988)
studied the same problem numerically and, obtained the same result as Benthem's
one. They furthermore showed that the 3-d stress field of a propagating crack
must have the singularity of l//r on a surface of a specimen, and, consequently,
the crack front edge doesn't meet the surface at a right angle. The above
studies indicate that the crack front edge angle, which is the angle between
a crack front edge and a specimen surface, is an important quantity to
understand the surface singularity of the three-dimensional stress field in the
vicinity of a crack tip.

In the present study, we experimentally study the surface singularity of the

3-d stress field and crack front edge angle of fast propagating cracks in PMMA.

PHOTOGRAPHING METHOD

Pulsed holographic microscopy (Suzuki et al., 1988, 1990) is applied to take

an instantaneous microscopic photograph of the opening of a fast propagating
crack in PMMA. And pulsed holography is simultaneously applied to take an
instantaneous photograph of the front edge of the crack.

Holographic recording
Figure 1 shows the optical system for holographic recording of the opening
and the front edge of a crack. A crack propagates in the PMMA specimen
S perpendicularly to the paper plane at a speed of several hundred m/s. When
the crack is propagating, the Q-switched ruby laser PL oscillates once and,
emits an pulsed light beam. The light beam is divided into two parts by
the beam splitter BS1. The reflected beam from BS1 is collimated and impinges
on the holographic plate HP1; this is the reference beam for holographic
recording of the crack opening. The light beam transmitted through BS1 is
divided again into two parts by the beam splitter BS2. The transmitted beam
is collimated and is divided again by the beam splitter BS3. The beam
transmitted through BS3 falls onto the specimen surface perpendicularly. Part
of the beam is reflected by the specimen's surface. The reflected beam is
half reflected by BS3, passes through the lens L6 and falls onto the holographic
plate HP1. This is the object beam for holographic recording of the crack
opening. Behind HP1, the object beam makes the real image RI of the crack.
The real image is recorded as a hologram.

The reflected beam from the beam splitter BS3 falls onto the holographic
plate HP2; this is the reference beam for holographic recording of the crack
front edge. The reflected beam from the beam splitter BS2 is incident upon
the side boundary A of the specimen. After the passage of the side boundary
A, the light beam becomes diffusive one and illuminates the crack surface
uniformly. The illumination beam is weakly scattered by the crack surfaces.
The scattered light passes through the side boundary B and falls onto the
holographic plate HP2; this is the object beam in holography. The front edge
of the fast propagating crack is recorded as a hologram in this manner.
 465

Fig. 1 The optical system for holographic recording.

Reconstruction and photographing

After development, illuminated with the He-Ne laser beam, the hologram HP1
reconstructs the real image of the crack opening. The real image is magnified
and photographed through a conventional microscope, which is focused on the
specimen surface illuminated at the holographic recording (Suzuki, 1988).
Similarly, the hologram HP2 reconstructs the virtual image of the crack front
edge observed through the side boundary B of the specimen. The virtual image
of the crack front edge is photographed through a common camera (Suzuki.
1990)

RESULTS
Figure 2 shows an example of fast propagating cracks which are photographed
with the method described above. The crack was propagating at a speed of
233m/sec. The figure shows that pulsed holography and pulsed holographic
microscopy can simultaneously take photographs of the opening and the front
edge of a fast propagating crack.
466

No. 29
v=233m/s
JOOh No.29
e V=233m/s
100pm 3_

COD=1-38ra503
% ■ 'VI
1 ■ ■ ■ ■■■■■■ ' "■ ■ ' ■ '■""

10 100 1000 . 10000

r(pm)

COD
(b)

«=95.7°
Crack tip
/3=104.3

(c)
(a)
Fig.2 An example of fast propagating cracks in PMMA.

Surface singularity

Shown in Fig. 2(a) is the microscopic photograph of the crack opening, which
is the dark region on the photograph. Crack opening displacement (COD) can
be measured as a function of distance r from the crack tip. The measured
COD is shown in Fig. 2(b). The specimen is 20mm in thickness and the COD
was measured as far as 8mm from the crack tip. Consequently, the COD
 467

200 220 240 260

Crack speed ( m / s )

Fig. 3 Exponent X versus crack speed.

~ 110i
Numerical result on a slowly
01 I /— propagating crack

H
iooh

s
90h
U J_ _L _L
0 200 220 2A0 260

Crack speed ( m / s )

Fig. 4 Crack front edge angle versus crack speed.

measurement might be carried out in the three dimensional stress field whiGh
appears around a crack tip. Assuming that the COD is proportional to r ,
we obtain the exponent X by means of the least square method.

The exponent X is obtained for each crack through the above procedure, and
is shown in Fig. 3 as a function of crack speed. The figure indicates that
the exponent X is independent of crack speed and, is equal to 0.5 within the
range of measurement errors. In other words, COD is proportional to / r even
in the 3-d stress field. The fact means that the 3-d stress field of a
propagating crack has the surface singularity of l//r, which is independent
of crack speed.
468

Crack front edge angle

Figure 2(c) shows the crack front edge of the crack shown in (a). The crack
front edge angles a and 3 are measured from the photograph. As shown in
Fig. 2, as an example, crack front edges are not straight but curved, and
crack front edge angles are obtuse. The front edge of the crack in Fig. 2
is a bit asymmetric. Front edges of some cracks were symmetric but some
were asymmetric, in the present study. The asymmetry may be due to out-
of-plane bending of specimens, which bending is very small but appears when
a tensile force is applied to the specimen like compact tension one. In the
case of an asymmetric front edge, the two front edge angles, a and 3, have
different values. But, if a is large then 3 is small, and vice versa. This
fact means that the two angles, a and 3, is not independent each other.

Figure 4 shows the mean value of a and 3, that is (a+3)/2. The dark circles
• indicate the crack front edge angles obtained from the experiments for
simultaneous measurement of COD and crack front edge angles. The open
circles o indicate the crack front edge angles obtained from the experiments
for measurement of crack front edge angles only. There is the tendency that
the crack front edge angle decreases as crack speed increases. Bazant and
Estenssoro numerically obtained the crack front edge angle of a slowly
propagating crack. According to their results, the crack front edge angle
is at 104 in the present study. The numerical result is in agreement with
the measured values of crack front edge angle at lower crack speed in the
present study.

From the above mentioned results, it can be said that the crack front edge
angle changes with crack speed in order to conserve the surface singularity
of the crack to be l//r.

ACKNOWLEDGEMENT
The present study was performed during the tenure of Grant-in-Aid for General
Scientific Research (01550071) of The Ministry of Education, Science and Culture.
The author expresses his gratitude for the grant. The author also wishes to
acknowledge I. Yoshiyama, who were students in our university and worked
together in a part of the study.

REFERENCES
Yoffe, E. H. (1951). The moving Griffith crack. Phil. Mag., 42, 739-750.
Benthem, J. P. (1977). State of stress at the vertex of a quarter-infinite crack
in a half-space. Int. J. Solids Structures, 13, 479-492.
Bazant, Z. P. and Estenssoro, L. F. (1979). Surface singularity and crack
propagation, Int. J. Solids Structures, 15, 405-426, and (1980). Addendum
to the paper, Int. J. Solids Structures, 16, 479-481.
Suzuki, S., Homma, H. and Kusaka, R. (1988). Pulsed holographic microscopy
as a measurement method of dynamic fracture toughness for fast
propagating cracks, J. Mech. Phys. Solids, 36, 631-653.
Suzuki, S. (1990). Three-dimensional measurement of opening displacement of
rapidly propagating cracks in PMMA, Applied Stress Analysis (Ed. by
Hyde, T. H. and Ollerton, E.), Elsevier Applied Science, London, 26-35.
WS2g6

MEASUREMENT OF IMPACT LOAD IN CHARPY IMPACT TEST

USING DECONVOLUTION TECHNIQUE

H. INOUE, K. KISHIMOTO and T. SHIBUYA

Department of Mechanical E n g i n e e r i n g for Production,

Tokyo I n s t i t u t e of Technology,
2 - 1 2 - 1 , O-okayama, M e g u r o - k u , Tokyo 152, Japan

ABSTRACT

The e f f e c t of w a v e propagation in impactor h a s b e e n one of t h e most s e r i o u s

problem in measurement of impact load. The a u t h o r s d e v e l o p e d a method u s i n g
deconvolution t e c h n i q u e to s o l v e t h i s problem. In t h i s paper, t h e method i s
applied to measurement of impact load in t h e i n s t r u m e n t e d Charpy impact t e s t . It
i s shown that t h e e f f e c t of w a v e propagation i s s u c c e s s f u l l y c o r r e c t e d and
c o n s e q u e n t l y that t h e impact load i s a c c u r a t e l y measured.

KEYWORDS

Impact; deconvolution; material t e s t i n g ; Charpy impact t e s t ; f r a c t u r e t o u g h n e s s .

INTRODUCTION

Instrumented impact t e s t i n g i s widely applied for e v a l u a t i n g mechanical

p r o p e r t i e s of materials u n d e r impulsive loading. Impact load a c t i n g on a
specimen is one of t h e most important measure in t h e t e s t i n g . However, it is
r a t h e r difficult to measure t h e impact load d i r e c t l y s i n c e t h e load is transmitted
into impactor in t h e form of s t r e s s w a v e which p r o p a g a t e s in a complex manner.
For t h i s r e a s o n , q u a s i - s t a t i c loading i s often assumed for measuring t h e impact
load. Based on s u c h assumption, t h e e f f e c t of w a v e propagation must d i s t o r t t h e
time h i s t o r y of impact load. Therefore, it should be c o r r e c t e d for a c c u r a t e
evaluation of material p r o p e r t i e s .

The a u t h o r s (Inoue et ai., 1988a, b) h a v e d e v e l o p e d a method for measuring an

impact load a c t i n g on a body of a r b i t r a r y s h a p e . The method i s based on t h e fact
that impact r e s p o n s e of impactor i s related to t h e impact load b y time
convolution. The impact load i s estimated from r e s p o n s e of t h e impactor b y
deconvolution. In t h e method, t h e e f f e c t of t h e wave propagation is taken into
a c c o u n t a s far a s it i s linear. Therefore, application of t h i s method to t h e impact
t e s t i n g of materials will g i v e a solution for t h e problem mentioned a b o v e . In t h i s
paper, we apply t h e method to measurement of impact load in Charpy impact t e s t
and demonstrate i t s validity.
469
470

DECONVOLUTION TECHNIQUE FOR IMPACT LOAD

Consider a body of arbitrary s h a p e s u b j e c t e d to an impact load, f(t), at one

point. If strain r e s p o n s e , e ( £ ) , at any point of t h e body is linear, it can be
e x p r e s s e d by t h e following convolution integral:

e(t)= P h(t-T)- f(r)dr, (1)

w h e r e h(t) is t h e impulse r e s p o n s e and f(t)=e(t) = h(t)=0 at £ < 0 . In
general, it is relatively e a s i e r to measure t h e strain r e s p o n s e than to measure
t h e impact load directly. If t h e impulse r e s p o n s e is g i v e n , t h e impact load can be
obtained from t h e strain r e s p o n s e by s o l v i n g E q . ( l ) , i.e. by deconvolution.
Fourier transformation of E q . ( l ) g i v e s
E(o)) = H(a))- F(a))t (2)
where E{a)), F{a)) and H{co) are Fourier transforms of e ( £ ) , f(t) and h( t)
r e s p e c t i v e l y . H(co) is called t r a n s f e r function. After t h e Fourier transformation,
t h e impact load is obtained by simply d i v i d i n g E{co) by H(co).

Since e(t) is an experimental data, numerical treatment i s r e q u i r e d for t h e

deconvolution. For t h e numerical treatment, f u n c t i o n s are d i s c r e t i z e d and
t r u n c a t e d according to t h e sampling theorem. In practice, windowing is often
r e q u i r e d for r e d u c i n g e r r o r s a s s o c i a t e d with discretization and truncation. We
adopt t h e following window function in t h e p r e s e n t s t u d y :
w(t)=exp(-at), (3)
where a is a p o s i t i v e c o n s t a n t . The Fourier transformation with exponential
window is equivalent to t h e Laplace transformation. The d i s c r e t e Laplace
transformation and i n v e r s i o n are calculated b y t h e following equations:
N-l
F(n- Aoj) = At JC f(k-At)-exp(-a- k- A £ ) - e x p ( - 2 ^ i • n- k/N), (4)

* e x p ( a - k- At) N-l *
f (k- At)= 2 F (n- Aoj)-exp(-2 7Ti- n- k/N), (5)
T n=0
where T=N*At and * d e n o t e s complex c o n j u g a t e . It is known that an
appropriate value of a g i v e s good r e s u l t (Wilcox, 1978; Krings and Waller, 1979).
In t h e following, we s e t a = 5 / T . Equations (4) and (5) can be computed
efficiently by t h e u s e of t h e f a s t Fourier transform (FFT) algorithm.

INSTRUMENTATION OF CHARPY TESTING MACHINE

According to t h e scheme d e s c r i b e d a b o v e , we measured impact load in Charpy

impact t e s t . Pendulum of t e s t i n g machine is r e g a r d e d a s a body s u b j e c t e d to an
impact load. Therefore, t h e impact load can be estimated from t h e strain r e s p o n s e
of t h e pendulum by deconvolution t e c h n i q u e .

Since t h e t r a n s f e r function is initially unknown, we h a v e to determine it first by

c o n d u c t i n g a calibration. The calibration i s performed by s t r i k i n g a s l e n d e r long
rod with t h e pendulum a s shown in F i g . l . a . In t h i s c a s e , t h e impact load can be
measured u s i n g a strain g a g e a d h e r e d to t h e rod on t h e b a s i s of t h e
one-dimensional wave propagation t h e o r y . The p r o c e s s of calibration is
summarized a s follows:
1. Attach a strain g a g e to t h e pendulum to measure t h e strain r e s p o n s e .
2. Prepare a s l e n d e r long rod and attach a strain g a g e to i t s end to measure t h e
 471

Strain gage

u
Circular rod
3 e(t)\

(a) Calibration - Impact of rod (b) Testing - Impact of specimen

Fig.l Charpy pendulum subjected impact.

impact load.
3. Strike the rod with the pendulum in a similar manner as in the testing
(Fig.l.a).
4.Obtain data of the impact load, f( t), and strain response, e( £).
5. Determine the transfer function from the Laplace transforms of these data.
H{a>) = E{a))/F{o>). (6)

Once the transfer function has been determined, every impact load applied to the
specimen can be estimated from the strain response of the pendulum. The
procedures are as follows:
6. Conduct a testing of specimen and measure the strain response of the
pendulum (Fig.l.b).
7. Estimate the impact load applied to the specimen.
F{QJ) = E{CO)/H{O)). (7)

Since deformation of the pendulum and that of the anvil are considered to be
much smaller than the deflection of the specimen, energy absorbed by the
specimen is approximately equal to the work done by the pendulum. The
deflection of the specimen can be obtained from the impact load by considering
the motion of the pendulum as follows:
u(£) = Pv(r)cf7-, (8)
D ft
v(t)=v(0)- (9)
W-L JO
where:
u{t) deflection of the specimen at the point of impact,
v(t) velocity of the point of impact,
t time originated at the beginning of the impact,
D distance from the axis of support to the center of gravity of the
pendulum,
L distance from the axis of support to the point of impact,
W mass of the pendulum.
472

Experimental devices Measuring devices Data processing device

Charpy testing machine Strain gage Personal computer

JIS B 7722, 294 J (30 kgm) gage length 2mm NEC, PC-9801VM
gage factor 127
Circular rod
mild steel, 01Ommxlm D.C. bridge

D.C. amplifier

Digital memory
Kawasaki electronica,
HRV-220
Fig.2 Experimental setup.

Thus, the energy absorbed by the specimen, i2Le> is obtained as follows:

Ec= j * ^ f(t)d{u(t)} , (10)
where t o d is the time when the impact terminates.

Experimental setup is shown in Fig.2. Sampling rate of the data was 2 /zs/word
and length of the data was 1024 words. Two kinds of polymeric materials, PMMA
and epoxy resin (Araldite-B), were tested. The specimen was the type of No.4
specimen of JIS Z 2202.

RESULTS AND DISCUSSIONS

First, we conducted calibration for determining the transfer function. Figure 3

shows typical signals measured. The transfer function was determined from
these data. The impact load is a rectangular pulse. The strain response is similar
in shape to the impact load, but a sinusoidal oscillation is superposed. The
sinusoidal component corresponds to the vibration caused by wave propagation
in the pendulum. As mentioned above, the impact load is often measured by
multiplying the strain response by a constant factor on t h e assumption of
quasi-static loading. It is obvious that such a method will give inaccurate
evaluation of the impact load. Therefore, it is understood that the effect of wave
propagation needs to be corrected.

After the transfer function was determined, testing of the specimen was
conducted. Figure 4 shows strain responses of the pendulum when PMMA
specimens were tested under several impact velocities. Similar results were
obtained when epoxy resin specimens were tested. The impact loads were
estimated from these strain responses as shown in Fig.5. Both the strain
response and the impact load are sawtooth-like pulses. Two important facts can
be pointed out from these results.
l.The strain response contains sinusoidal oscillation which is identical with that
shown in Fig.3. As mentioned above, this component corresponds to the
vibration of the pendulum. On the other hand, the impact load does not contain
such component. Therefore, the effect of wave propagation seems to be
successfully corrected by the deconvolution technique.
 473

—i n -i 1 1
T

fN, Impact Velocity Impact Velocity

Q
2.08 m/s J 2.08 m/s
2; 1.40 m/s
1.40 m/s .* 4
r 1 1
1
3 2i
1/ -w>-

—J 1 ±_ . . i
0.5 1.0 1.5 2.0 0.5 1.0 1.5 2.0
time [ms] time [ms]
(a) Strain response (b) Impact load
Fig.3 Results of the calibration.

Vbf*w<^^

0 0.5 1.0 1.5 0.5 1.0 1.5

time [ms] time [ms]
Fig.4 Strain response of the pendulum. Fig.5 Impact load obtained
by deconvolution.
474
2. Another oscillation is seen in the rising portion of the pulse. This oscillation is
due to the vibration of the specimen. The strain response takes negative value
at some points during the rising portion where the impact load remains
positive. Therefore, the method based on the assumption of quasi-static
loading will give negative load during the impact, that is impossible in reality.

The energy absorbed by the specimen is

plotted in Fig.6. Results of static 0.5 i i i
bending test are also plotted together.
The energy approaches to the value of
static case as the impact velocity 0.4
decreases. In usual, the energy is
evaluated by measuring the angle of the n ~
pendulum. In the present case, however, 2
the energy could not evaluated in a j»
usual manner because it was much ^ Q ^
smaller than the capacity of the testing
machine used. Nevertheless, the energy
was successfully evaluated by the 0.1
present method. Moreover, the energy
obtained by the present method does
not contain energy absorbed by the ° I 1 1 i 1
0 1 2 3 4
pendulum. Impact velocity [m/s]
Fig.6 Energy absorbed by the specimen.

CONCLUSIONS

A method for measuring impact load acting on a body of a r b i t r a r y shape was

applied to the instrumented Charpy impact test. In the method, the impact load is
obtained inversely from the strain response of impactor by deconvolution
technique. The validity of the method was thoroughly demonstrated.

The present method can be also applied to various type of impact testing
methods. If impact load has already measured on the assumption of quasi-static
loading, the accuracy of the data can be examined by conducting a calibration as
shown in the present paper.

REFERENCES

Inoue,H., T.Shibuya, T.Koizumi and R.Watanabe (1988a). Measurement of impact

force history by deconvolution method. Proceedings of the 6th International
Congress on Experimental Mechanics, 463-468.
Inoue,H., T.Shibuya, T.Koizumi and J.Fukuchi (1988b). Measurement of impact
force applied to a plate by the deconvolution method. Journal of JSNDI
(Hihakai Kensa), 37, 874-878.
Krings,W and H.Waller (1979). Contribution to the numerical treatment of partial
differential equations with the Laplace transformation. International Journal
for Numerical Methods in Engineering, 14, 1183-1196.
Wilcox,D.J. (1978). Numerical Laplace transformation and inversion. International
Journal of Electrical Engineering Education, 15, 247-265.
WS2g7

EXPERIMENTAL ANALYSIS OF DYNAMIC PROPERTIES OF HOLLOW

ELASTIC CYLINDER WITH A CIRCULAR CRACK IN INNER SURFACE

GUO MAOLIN , CHEN ZENGTAO , WANG DUO

Department of Mechanics , Harbin Institute of Technology,

Harbin Institute of Technology , Box 344

Harbin , P. R. China (150006)

ABSTRACT

In this paper, a hollow elastic cylinder with an inner-surface circular crack under an im-
pacting tensile load has been analysed by experimental method , the varying curve of dynamic
SIF with time has been put forward . This results is helpful in theoretical research of the
near-tip field of symmetric three-dimensional problem.

KEY WORDS
Hollow elastic cylinder , Dynamic SIF ; near - tip field.
INTRODUCTION
Since Chess , (Chess , 1886) many researchers have discussed the dynamic properties of the
transimission of elastic wave in hollow cylinder , especially in the effection of it on the dynamic
stress or strain field . (Heimann et. al 1966) But nearly all the previous work are concentrated
on theoretical analysis to draw an integral equation and solve it by integral -transfering meth-
od . (Zhang, 1989) Then a series method to expand the transfering equation to an
approxiamate equation which can be solved by computer method . In a recent paper (Kong ,
et. al . 1989) the authors present the SIF of surface a flaw in an elastic hollow cylinder under
remote steady tensile load with the assumption of infinite length of the cylinder , even though
all the results were drawn from an experimental method . However , theoretical solution of fi-
nite-length cylinder under impacting or other dynamic load has not been seen so far for its dif-
ficulty in mathematics , especially the echo wave's influence is complicated . In this paper , a
set of experimental equipment has been used to analyse the strain field of a point in the
near-tip field of an inner-surface circular crack and the dynamic SIF has been determined
approxiamately.

EXPERIMENTAL METHOD
The experimental system is shown in Fig. 1
475
476

W-

Fig. 1 The experimental system Fig. 2 The dimmensions of the specimen

where in Fig. 1 1 is specimen; 2 is strain gage; 3 is super-dynamic strain recorder; 4 the

force sensor ; 5 is electro-magnetic loading device, the impacting load is created by the de-
vice; 6 is electric charge amplifier, 7 is a transient wave form memory (with two channels); 8
is X - Y ploter.

As the force suddenly impacts on the radial surface of the specimen , the strain gage gives a va-
rying strain and amplified by super-dynamic strain recorder , it is transfered to one channel of
device 7 . Meanwhile , the impacting load recorded by the force sensor and amplified by de-
vice 6 is also put into the other channel of device 7 . So the varying strain and impacting
load with time has been obtained.

The dimmensions of the specimen is shown in Fig. 2

In our experiment herein in this paper, L is llOOmmm . 1 is 100mm, dx is 20mm , d2 is

16mm , the depth of the crack is a = 1.5mm , 1.0mm respectively .

DETERMINATION OF DYNAMIC SIF [IC S I F

The position of the gage in polar coordinate with crack tip as origin is showing in Fig. 3

k?(N/mml)

t(*«)
0 400 800 1200 1600

Fig. 3 The position of the gage Fig. 4 Dynamic SIF with time as
independent variable
 477

The cylinder is under single tension , so ,

<7y = E d e y (1)

Where ay is the axial stress component, ey is the strainrecordedby the strain gage , Ed is the
dynamic modulus of the material.

From Fig. 3 , we get

* — cos-y
mc I 1 4 - cir» — sin-^-
(1+sm cm ) (2)
2nr

where K? is the dynamic SIF.

Inverse eq. 2 , substituting eq . 1 into eq. 2.

KJ = Edeyyf^ I <£s-| (1+sin-l s i n ^ - )] (3)

Define:
E
* = d V ^ 7 / [ o o s - | ( l + r i n - | s i n - | - )] (4)

Hence,
K? = ^£y (5)

So just amplifying the curve of ey with t by 5 , the dynamic SIF can be determined eventual-
ly.
CONCLUSION
From Fig. 4 , we can see the varying trend of the dynamic SIF; As time increases , DSIF
shows an increasing trend at the beginning , and then undulates cycling a constant value . The
variation period of DSIF is concerned with the echo period of stress wave in the cylinder . As-
suming the velocity of longitudinal stress wave in elastic cylinder 300m / s, considering the
length of the cylinder 1100mm , the above two periods coincide each other .

REFERENCES
Chess . C . (1886). Longitudinal Vibrations of a Circular Bar . Quart. J. Pure & Appl.
maths. , 21 , 287-298
478

EXPERIMENTAL METHOD
The experimental system is shown in Fig. 1
Heimann. J. H & Kolsky . H. (1966), The Propagation of Elastic waves in Thin Cylinderical
Shells. J. Mech. Phys. Solids . 14, 121-130
Zhang Zimao (1989). Ph. D. Dissertation . Harbin Institute of Technology. Harbin Kong
Xian-ming (1989) Engng. Fract Mech, 33 , 105-111
WS2h1

A STRAIN-LOCALIZATION ANALYSIS FOR ADIABATIC SHEAR

BAND AT DIFFERENT ENVIRONMENTAL TEMPERATURE

LiLi WANG and Hesheng BAO

Mechanics and Materials Science Research Center

Ningbo University
Ningbo, Zhejiang 315211, P.R.C.

ABSTRACT

A strain-localization model based on material imperfection and taken

into accout both heat generation and dissipation is suggested. By means
of computer numerical simulation, the development of strain, strain-rate
and temperature in both defective and non-defective regions can be
calculated with the increase of average strain, and an analysis for the
critical condition of adiabatic shearing is given. A strain-, strain
rate- and temperature- dependent criterion of thermo-viscoplastic
instability for adiabatic shearing is obtained.

KEYWORDS

Strain-localization; adiabatic shearing; thermo-viscoplastic instability;

temperature-dependent; high strain rate.

INTRODUCTION

The adiabatic shearing as a special phenomenon and one of the main

failure forms of materials at high strain-rates has been studied for
some decades. Similar to the situation in researches on other failure
forms, the criterion for adiabatic shearing is a key problem received
greater attention by many investigators.

Beginning from Zener and Hoi 1 onion (1944), who explained the above
phenomenon as thermo-plastic instability, a number of criteria have been
suggested, based on the concept of instability of macroscopic mechanical

479
480

behaviour of materials. Among those, the critical strain-rate criterion

(e.g. Recht, 1964) and the critical strain criterion (e.g. Culver, 1973)
are well-known in engineering application. However, as pointed out by
the authors, both the strain and strain-rate, and furthermore the
environmental temperature should be considered as un-negligible control-
variables for adiabatic shearing, and then a multi-variables criterion
based on the thermo-viscoplastic instability was suggested (Wang et al.,
1985; Wang, 1986; Wang et al., 1988, Bao et al., 1989).

On the other hand, from the microscopic point of view, the adiabatic
shearing is a strain-localization phenomenon. Correspondingly, some
analyses of strain-localization, similar to that in the micro-mechanics
approach, have been developed (Semiatin et al., 1983,1984; Batra et al.,
1989). However, most of them concentrated the main attention upon how
the non-uniform strain distribution develops with time in a specific
space, rather than the criterion and its control factors.

In the present paper, a strain-localization model based on the material

imperfection and taken into account both heat generation and dissipation
is suggested and used to analyse the critical condition for adiabatic
shearing, in connection with the authors' multi-variables thermo-visco-
plastic instability criterion mentioned above.

STRAIN-LOCALIZATION MODEL FOR ADIABATIC SHEARING

It is recognized that some initial imperfections or heterogeneity, such

as of material, geometry or temperature etc., always exist in a real
material. So a deformed body is assumed here to consist of two regions,
a small "defective" region with volume percentage of V., and the non-
defective region with volume percentage of V surrounding the former.
Obviously, at any time, there should be
vn+ vd=i (i)

The material considered here, both for defective and non-defective, is

rate- and temperature- dependent, i.e. thermo-viscoplastic. Its general
form of constitutive equation, for a simple shear state, is
x = f(Y, Y,T) (2)
where T , Y , Y and T are shear stress, shear strain, shear strain-rate
and temperature, respectively.

The temperature rise dT, due to converting from non-elastic work T dv

into heat, is generally described by
p c dT = p x dY (3)
where p is the density, c the specific heat, and p the fraction of
 481
non-elastic work converted to heat. Although Eq.(3) is mainly used for
an adiabatic or quasi-adiabatic process, it can be generalized to a non-
adiabatic process, which may exist in the defective and particularly in
the non-defective region, by taking the heat dissipation into account
(Bao and Wang, 1990). In fact, for a perfect adiabatic process at very
high strain-rate, the non-elastic work is completely converted into heat,
i.e. p =1, while for a perfect isothermal process at very low strain-
rate, the heat is totally dissipated without any temperature rise, i.e.
p =0. The real deformation processes at different strain-rates must be
between such two extreme cases, and correspondingly should depend on
strain-rate, i.e.
OO-MvXl, (4)
Furthermore, in addition to taking into accout the possible influence of
environmental temperature, considering that the temperature difference
between the defective and non-defective regions may be quite large, the
specific heat c should be regarded as a function of temperature, i.e.
c=c(T) (5)
Thus, for a more general process, Eq.(2) should be modified to
PC(T) dT = p ( Y ) T ( Y , Y,T)dY (6)
Obviously, the solution of T from Eq.(6) can generally be expressed by
T-T(Y,Y) (7)
which means that the temperature during the deformation process is
determined by both strain and strain-rate.

Notice that Eq.(2)-(7) should be satisfied in both defective and non-

defective regions, although the material parameters in the two regions
may be different. From now on, the subscripts d and n will be used to
denote the quantities in the defective and non-defective region,
respectively, whenever it needs. For the simple shear state discussed
here, the quantities in each region have been assumed to be uniform.

Moreover, it should be noticed that although the strains, strain-rates

and temperatures in the defective and nondefective regions are generally
different whenever strain-localization exists, the stresses and
temperatures should always keep continuity, respectively, along the
boundary between two regions, that is to say
n d
or, from Eq.(2)>
T
< Y n ' Y „ ' V k i n > -*<V v d' T d' k id> <8>
where k.(i = l,2,3,....) denote the material parameters. Substitute Eq. (7)
into Eq.(8)/ we obtain
T
< Y n' Y n'T< Y .' Y .»kin>> kin> "T < Y d' Y d'T <v d' Y d» kid>> k id>' <9>
Notice that the relation betweren Y and Y , Y . and Y . are known
n n a a
482
from the definition of strain-rate, i.e.

*.-yp <10a)
yA-^f> dob)
However, what can be measured or controlled is neither Y or Y ., nor
Y or Y ., but the apparent (average) strain Y and strain-rate Y ,
i.e.
Y a = VnY n+ V,Y
a «u

Y
a =Vn+VdYd <»>
where V and V, should satisfy Eq.(1).

Thus, if p ( Y ) and c(T) are known (so that T ( Y , Y ) can be solved), and
if the constitutive equation of material (including all material
parameters) is known then for a given initial condition, e.g.
Y =Y =0 T for t=0 (12)
„ d ' W e
where T is the environmental or initial temperature, and for a given
process of apparant deformation, e.g. for a constant apparent strain-
rate process
Y a = Y .(const.), (13)
we can calculate the four unknown quanlities Y , Y , Y . and Y , from
the four equations (9)-(ll) and subsequently the temperatures T and T.
from Eq.(7). The critical condition for instable strain-localization can
then be studied by means of computational simulation.

COMPUTING RESULTS AND DISCUSSION

Since the p -titanium alloy TB2 (Ti-8Cr-5Mo-5V-3Al) is a typical

material susceptible not only to strain-rate and temperature but also to
adiabatic shearing (Wang, et al., 1985; Bao, et al., 1989), as an
example, the strain-localization process was numerically analysed for it.

The calculation conditions are as follows. Firstly, its thermo-visco-

plastic constitutive equation has been given by the authors as

T=(T +EX Y)(l+g ln^- )(l-at- ) (14)

0
o o
where x , E., g, Y , a, and T are material parameters given in
previous paper (Wang, et al., 1986). Next, the P ( Y ) is assumed to
described by the following function
 483

p(Y)=J*rctg(itg-|^ lgv)+J, (15)

3
since it satisfies not only the high strain-rate condition 0 (10 /s)=0.9
and l.imp(Y) = l, but also the quasi-static condition p (10~3/s)=0.1 and
Y —*oo
U m p ( Y ) = 0. Thirdly, the c(T), according to the Einstein's theory, is
Y -*0
taken as
9P exp(8 R /T)
c=3kN(-y-^) 2 ^— (16)
[exp(9 E /T)-l] 2
where k is Boltzmann constant, N is Avogadro constant and 0 p is Einstein
characteristic temperature which is 242.9K for titanium and its alloys.
Fourthly, assume that V.=0. 1X>estimated from the microscopic observation
for adiabatic shear band in TB2 (Lu, et al.,1986)> And at last, a small
difference in the material strength parameter x between the two
regions, i.e. A T = T - T O ( J ( > 0 ) ' is considered as the only initial
imperfection for simplification.

For Y =10 3 /s and A T =40MPa ( A T / T ^ 5 X ) / the calculation results

are shown in Fig.1, showing how the (a) strain, (b) strain-rate and (c)
temperature in both regions develop with the increase of apparent strain
Y . It can be seen that basically there are three stages. In an early
stage, since the defective region is a weaker one (x ,<i ), Y , and
then T, increase more rapidly than Y and T , respectively. But, Y ,
decreases, although it is still higher th'an Y . This implies that the
strain-hardening plays a leading role in this first stage, and then it,
in fact, is showing a tendency of strain-uniformization. (Notic that a
slope of 1 in the plot of Y , or Y versus Y just corresponds to a
uniform strain state). However, with increasing Y , the thermal
softening induced by temperature rise (Eq.(3)) enhences gradually. At
i i i
\
-J
)

?1- \

/f H
/

V
m\ \
/

O 10 20 0 10 20 0 10 tO
£a(H) ^H> U(%)
Fig. 1. Evolution of strain, strain-rate and temperature
in both regions.
484

Yft=s 5H in the present example, then, v d begins to increase with y ,

as well as both v d and T d increase accelerately. This implies that tfte
thermal softening plays a leading role in the secend stage. Obviously,
the minimum point of v d corresponds to a transition from a strain-
uniformization process to a strain-localization process. Of course,
whether the transition happens or not, in general, depends on the
material properties and the external loading conditions. At last, the
accelerated strain-localization process, as can be expected, leads to a
dramatically increase of all v y and T. at v «16X, while v
decreases abruptly. Thus, the third stage corresponds to the so-called"
thermo-viscoplastic instability or adiabatic shearing. It should be
noticed that the strain-rate plays different role in the whole process,
i.e., at the first stage, it plays, in substance, a -softening ■ role
due to d v d / d v a <0, while at the second and third stage it plays a
•hardening- role due to dv d /dv a >0, as pointed out by the author
(Wang, 1986).

For the different values of constant v by the same calculation

procedure, the effect of strain-rate upon strain-localization can be
studied. The results are shown in Fig.2. It can be seen that with
increasing v ft, the instability strain, i.e. the strain corresponding to
a dramatical increase of y &, decreases markedly. So the adiabatic
shearing is strain-rate dependent.

Similarly, varying the initial temperature T e from -200° to 50*C in step

of 50*C, the influence of environmental temperature on the adiabatic
shearing can be studied. The results are shown in Fig.3. It is obvious
that the lower the T e is, the smaller the instability strain is. So,
the adiabatic shearing is temperature dependent, too.

8 "£ o
o
o
o
o
o J
o
6 H
Vft)
4
2
t—_ 1 1 1 1
10 15

ig. 2. Strain-localization for the different val

of apparently constant strain-rate.
 485

Fig. 3. Strain-localization at different initial

Temperature.

Furthermore, to obtain a quantitative description of the critical

condition for strain-localization instability, the apparent strain
corresponding to Y J'Y =10 is tentatively defined as the instability
strain Y ., which is supposed to correspond to the occurence of
adiabatic shear band. Then the critical curve of Y . versus Y can be
„ „ - _ - . . . arly, for different f i a

Te ,a set of critical curves, Y ai. - Ya . can be plotted, as shown in Fig.5.

1 ' 1

4 J
s 9

L^
% 1
1
1 -J
X 1

HJ
1 |

> ^■■LBMMBJ
• 10 to oo 40

Fig. 4. Critical Y . - Y curve for the occurence of

adiabatic shear band at a given T .

58 -ttt -M *
*X \1 11 I1
w 2
\ I \
«l
1
\ V
1 . 1 ^
10 25
U i %>
Fig. 5. Critical Y . - Y curves at different
environmental temperature.
486

A conclusion can be drawn from Fig.4 and Pig.5 that not only the strain
(as in a critical strain criterion) but also the strain-rate and
environmental temperature are all the important factors which control
the dramatical development of strain localization or the occurence of
adiabatic shear band. Thus a reasonable criterion for adiabatic shearing
should be a thermo-viscoplastic instability criterion with three control
-variables, i.e. strain, strain-rate and environmental temperature. It
is interested to emphasis that such a criterion is not only consistent
with the authors' another model based on the maximum stress concept for
an apparent adiabatic stress-strain curve, but also in agreement with
the experimental results given by the authors.

ACKNOWLEDGEMENT

The research is supported by the China Natural Science Foundation.

REFERENCES

Bao, H.-S.,L. -L.Wang and W.-X.Lu (1989). Explosion & Shock Waves, _9, 109-119.
Bao, H.-S.and L.-L.Wang (1990). J. China Univ.Sci.fc Tech., 20, 18-24.
Batra,R.C.and Y.W.Kwon (1989).Acta Mechanica, 77, 281-297.
Curver,R.S.(1973).IntMetal.Effect at High Strain-rates (R.W.Rhode,
B.M.Butcher, J.R.Holland and C. H. Karnes. ed. ), p. 519. Plenum Press, New York.
Recht,R.F.(1964).J.Appi.Mech., 31, 189.
Lu,W.-X.,L.-L.Wang and Z.-Q. Lu (1986).Acta Metall.Sinica, 22, A317-320.
Semiatin,S.L.,G.D.Lahoti and S.I.Oh (1983). In:Mater ial Behavior under
High Stress and Ultra High Loading Rates (J.Mescall and V.Weiss, eds)
p. 119,Plenum Press, New York.
Semiatin,S.L.,M.R.Staker and J.J.Jonas (1984).Acta Net a 11., 32, 1347.
Wang, L.-L.,W.-X.Lu, S.-S. Hu and Z.-P.Tang (1987). In : Macro- and Micro-
Mechanics of High-Velocity Deformation and Fracture, pp.395-406,
Springer-Verlag, Berlin.
Wang, L.-L (1986). Proc.Int.Symp.Intense Dynamic Loading and Its Effects
(Z.-M.Zheng and J.Ding, eds).pp.787-790, Science Press, Beijing.
Wang, L.-L.,H.-S. Bao and W.-X.Lu (1988). Jour.de Phys., 49, C3/207-214.
Zener,C.and J.H.Hollomon (1944). J. Appl. Phys., 15, 22.
WS2h2

AN EVIDENCE OF MELTING ALONG ADIABATIC SHEAR BAND IN

A HIGH-SPEED SHEARING PROCESS

M. GOTOH and M. DHNO

Department of Mechanical Engineering, Gifu University,
1 - 1 Yanagido, Gifu 501-11, JAPAN

ABSTRACT

A commercially pure aluminum (Al) is sheared by a circular punch at a high

rate (10 m/s) with the aid of the drop-hammer testing apparatus. Not only the
occurrence of the adiabatic shear band (A.S.B.) but also melting along it is
clearly demonstrated by measuring the micro-Vicker1s hardness distribution
over the sheared-off surface, by the optical microscopy of the sheared sect-
ion showing a thin layer with a different microstructuure from the adjacent
smooth shear flow region, by the mirror-like appearance of the sheared-off
surface, and above all by a theoretical analysis of the shearing process.

KEYWORDS

Plasticity; adiabatic shear band; high rate shearing; aluminum

TESTED MATERIAL

The material tested here is a commercially pure aluminum (Al) of (lA)-hard-

ness whose nominal thickness is 10 mm. Its chemical composition is given in
Table 1. The mechanical tensile properties are measured in which the strain-

Table 1. Chemical composition of aluminum tested.

Si Fe Cu Mn Mg Zn Ti other Al

0.06 0.32 0.02 0.00 0.00 0.01 0.02 0.01 99.56

hardening property is expressed by the n-th power law as a = Ke" .

The diameter of the circular blanks (specimens) ranges from kl mm to 90 mm,

while the diameter of the shearing punch is fixed kO mm. Therefore, the
breadth of the sheared-off rings ranges from 0.5 mm to 25 mm and the ratio of
it to the thickness does from 0.05 to 2.5.

TEST CONDITIONS
487
488
main body of machine
(6 m high)
operating
and
recording
pump panel

1.weight,2.hammer,3.displacement senser
i+.urethane rubber,5.clay,6.punch
7.ring piston,8.blank-holder,9.die
10.test piece,11.semi-conductor gauge

(General view of the impact (Schematic illustration of the

testing machine with drop hammer) setup for high-rate shearing)

Fig. 1 Testing Apparatus. Fig. 2 Main part of the apparatus.

The testing apparatus with a drop-hammer is shown in Fig.l whose capacity is

about U00 kgf-m. In the test, the hammer is lifted up to 5.^ m high and then
released to shear the blank (specimen) at about 10 m/s. In Fig.2, the main
part of the setup is illustrated. The punch is first set on the blank and
then the released hammer hits the punch dynamically. In the shearing operat-
ion, no lubrication is applied. The clearance between the punch and the die
is adjusted to be 0.1 or 0.05 mm by using the two dies of different bore dia-
meters. The edge radii of the punch and die are machined to be as sharp as
possible.

For comparison, a slow-speed shearing operation with the punch speed of 0.1
mm/s is also performed parallelly.

RESULTS AND DISCUSSIONS

Figure 3 shows a few examples of the lateral surface of the sheared-off blank
. It is observed from this figure that shearing at high-rate yields a bright
sheared surface over a wider area for a smaller clearance, whereas shearing
at low-speed yields a dull (rough) sheared surface with a narrower fractured-
area (= the zigzag white zone at the upper edge) for a smaller clearance.
This difference in the appearance of the sheared-off surface suggests that the
 489

I l

"H
c l e a r a n c e O HR |
O.linm 1
• LS
1 D HR
■ 0.05mm
■ ■ LS 1
6 0" ■
0.1 c = 0.05 O
(a) low-speed
• ■ 1
• 1
o | 1 " 1
•
O a O f t '
5 0"
o a ? 8 1
a D I
•
i —r— 1 1 1 '

c = 0.1 c 0.05 position from burr (mm)

(b) high-rate
[sheared-off disk]
c = clearance (HR: high-rate; LS: low-speed)
Fig. 3 Examples of sheared-off sur- Fig. k Micro-Vicker's hardness distri-
face of 80 mm diameter blank.(disk) bution over sheared-off surface.

shearing process at high-rate differs from that at low-speed.

Figure h illustrates the micro-Vicker's hardness distribution along the shear

-ed-off surfaces of the disks. This figure clearly shows that the hardness
increases from the shear-drop side to the burr side in the slowly sheared-off
blank corresponding to the process of shearing. Moreover, it demonstrates
that the hardness in a high-rate shearing is almost invariable along the sur-
face, which suggests that the whole shearing process is fulfilled in almost
the same condition.

If the circular rigid ring as well as the blank-holder is employed at the

periphery of the blank in order to constrain the radial extension of the
sheared-off ring, the deformation of this ring is almost completely prevented
, and the hydrostatic pressure in the shearing region will become very high,
which contributes to avoid fracturing of the material and thus to make a good
sheared-off surface. Figure 5 shows an example obtained under the complete
constraint condition for the blank of U3 mm dia. (= 1.5 mm in breadth of the
sheared-off ring). It is observed in this figure that the surface of the disk
sheared at a low speed looks still dull, while the surface at a high-rate is
very bright and even looks like a mirror.

Figure 6, (a) and (b) show the chemically etched cross-sections of the shear-
ed-off rings which correspond to Fig.5, (a) and (b), respectively. From these
pictures it is clearly found that the shear flow concentration along the
shearing face is far stronger in the high-rate shearing than in the slow
shearing. Furthermore, in Fig.6,(a) we clearly find that the thin layer (of
490

(a) high-rate (b) low-speed

Fig. 5 Surface view of the disk sheared-off under almost
complete constraint.

(a) high-rate (b) low-speed

Fig. 6 Sectional micrography of the sheared-off ring
corresponding to Fig.5.

about 0.05 mm thick) whose micro-structure looks different from that of the
main matrix and in which no flow lines can be seen. This evidence together
with Fig.3(b), Fig.i+ and Fig.5(a) surely implies that this thin layer may be
the so-called adiabatic shear band (A.S.B.) which is nowadays well-known to
appear in a high-rate shearing. However, Fig.5(a) and Fig.6(a) might account
for beyond A.S.B.. Namely, it suggests strongly that melting of the material
could have occurred in this A.S.B.. The following simple theoretical check
may ascertain this point.

In the past, the A.S.B. has been studied much experimentally even in Japan (
Yanaihara et al.,1982, Ito et al.,1987). Measurement of the temperature in
the A.S.B. has also been attempted (Hartley et al.,1987, Marchand et al.,1988
). The theoretical study on the A.S.B. has also been performed by several
investigators (Fressengeas et al.,1987, Molinari et al.,1987). Especially the
formula of the width of A.S.B. was proposed and a few experimental checks of
it were done (Bai,1982, Dodd and Bai,1985, Kobayashi and Dodd,1988). A few
numerical simulations of the formation of A.S.B. have also been reported (
Lush and Anand,1989, Tomita and Shindo,1989). However, the rigorous compari-
son of the theory with the experiment can only be done by the use of the
analytical formula. Therefore, here we employ the formula of A.S.B.'s width
by Dodd and Bai to understand the experimental result described above, though
it does not assume melting of the material in the A.S.B..
 491
The half width of the A.S.B. is given t>y the following equation:
X = (KT»/T» Y * ) 1 / 2 , (1)
where K = heat conduction coefficient, T* = temperature in A.S.B., T* =
shearing stress in A.S.B., and y* = shearing strain rate in A.S.B.. This equ-
ation was derived from the instability analysis in a simple shearing. Kobaya-
shi and Dodd (1988) re-wrote (l) into the following form:
-,1/2
X= MY y,)/PC f} (2)
where Y m a x = maximum shearing strain in A.S.B., Yi = instability strain, p -
material density, c v = specific heat, and y = mean shearing strain rate in A.
S.B.. Yi is given as
y± = - n s pc v /{$Ox/8T)}, (3)
where n s and 3 are found in the reference,

The material properties required for calculation are given from the handbooks
(1972, 19T8). They and the calculated value of X are listed in Table 2. This
shows an excellent agreement of the
Table 2. Physical properties of the theory (Aca]_) with the experiment.
material tested and the half width
of the adiabatic shear band by the Now let us examine the possibility of
calculation and the experiment. melting in the A.S.B.. In the above
calculation, we can deduce that the
material Al material temperature at the onset of
the A.S.B. is about 150°Cf considering
p [kg/m ] 2680 *exp 0.05mm, the equation (3) and
the dependency of T on T. On the other
cv [J/(kg.°K)] 860 hand, the temperature rise can be
K [W/(m.°K)] 239. ^ evaluated from the energy equation
8T/3T[MPa/°K] -0.039 pcy(3T/3t) = q.oy,

n 0.15 where t = time, q = plastic work-heat

transition ratio = 0.95, and a = equi-
Yi 9.886 valent stress, from which we get
Ymax 11.3k AT = 0.226x(^.Ay). (U)
1+
Y [/s] 5X10 And we know from the strain-hardening
property that
A ca i [mm] 0.057
^0 = ^3 T 0 = K.(Ay//3) n , (5)
A eX p [mm] 0.05
where n = 0.15, K = 129 (MPa), and o"0
= flow resistence at room temperature.
From the handbook we find O/OQ= O.85 at T = 150°C. Using these values in (k)
and (5), we obtain Ay = 5.0, Namely, ai the onset of the A.S.B., the local
shearing strain amounts to 5*0. In the||experiment, the clearance between the
punch and die is set 0.05 mm. Therefore, the punch stroke at the onset of the
A.S.B. is evaluated as about 0.25 mm (= 0.05x5.0 mm), though the deformed re-
gion won't be limited within the clearance area. Once the A.S.B. is formed,
the_ shearing stress T in it.will be kept constant thenceforth at the value T
= 0//3 and a = 129x(5.0//3)°*15*0.85 = 128 (MPa).

Since then the simple shearing continues within the A.S.B.. We know the melt-
ing point of the material (Al) to be 6U3°C. Therefore, the additional shear-
ing strain at the onset of possible melting is easily estimated as follows:
Ay = (6U3 - 150)/(0.226xF),
where a" = 128 (MPa). That is, Ay = 17. Therefore, the punch stroke at this
492
instant is s = (IT + 5)*0.05 = 1.1 (mm). Namely, if instantaneous melting is
assumed to occur, the material melts at the punch stroke of 1.1 mm. Thence-
forth the shearing process goes on in the melted state.

CONCLUSION

Though some idealization about the extent of the deformed region was made in
the above consideration, it can be deduced from the experiment and a theoret-
ical examination here that the A.S.B. of about 0.05 mm wide is formed at the
punch stroke of 0.25 mm and even melting of the material in A.S.B. takes
place very probably at the punch stroke of 1.1 mm and thus the material melts
during almost the whole process of the high-rate shearing of a commercially
pure aluminum with 10 mm thickness. Here the punch speed of 10 m/s and the
clearance between the punch and the die of 0.05 mm were used.

ACKNOWLEDGMENT
This work isr'supported by the grant from the Japanese Educational Department.

REFERENCES

American Society of Metals (ed.) (1978). Metals Handbook, Ninth Edition.

pp.65-67.
Bai,Y.L. (1982). Thermo-plastic instability in simple shear. J.Mech.Phys.
Solids. 32, 195-207.
Dodd,B. and Y.Bai (1985). Width of adiabatic shear bands. Materials Science
& Technology, 1_, 38-^0.
Fressengeas,C. and A.Molinari (1987). Instability and localization of
plastic flow in shear at high strain rates. J.Mech.Phys.Solids, 35.,l85-211.
Hartley,K.A., Duffy,J. and R.H.Hawley (1987). Measurement of the temperature
profile during shear band formation in steels deforming at high strain
rates. J.Mech.Phys.Solids, 35, 283-301.
Ito,M., Yoshida,F., Inoue,M. and M.Ohmori (1987). Combined effects of
hydrostatic pressure and punching speed on blanking behaviors of an
aluminium. J.Jpri.Soc.Tech.Plasticity, 28, 698-705. (in Japanese)
Japanese Soc. Light Metals (ed.) (1972). Aluminium Handbook, pp.227-2^7.
Asakura-Shoten, Tokyo, (in Japanese)
Kobayashi,H. and B.Dodd (1988). Formation of adiabatic shear bands in steel
and titanium twisted at dynamic rates. J.Jpri.Soc.Tech.Plasticity, 29»
1152-1158. (in Japanese)
Lush,A.M. and L.Anand (1989). Shear localization in viscoplastic solids —
Thermal aspects. In: Advances in Plasticity (Proc. Plasticity'89; A.S.
Khan and M.Tokuda, eds.), pp.U55-^58. Pergamon Press, Oxford.
Molinari,A. and R.J.Clifton (1987). Analytical characterization of shear
localization in thermoviscoplastic materials. Trans.ASME, J.Appl.Mech.,
5^., 806-812.
Marchand,A. and J.Duffy (1988). An experimental study of the formation
process of adiabatic shear bands in a structural steel. J.Mech.Phys.Solids.
36 , 251-283.
Tomita,Y. and A.Shindo (1989). Strain localization behavior of thermo
elasto-qriscoplastic blocks under plane strain tension. In:Advances in
Plasticity (Proc. Plasticity1,89; A.S.Khan and M.Tokuda, eds.), pp. 1*73-1*76.
Pergamon Pre s s, Oxford.
Yanagihara,N., Saito,H. and T.Nakagawa (1982). Measuring of temperature in
the shearing region at high speed shearing. J.Jpri.Soc.Te ch.Plasticity, 23,
71-78.
 WS2h3

DYNAMIC VOID GROWTH IN RATE SENSITIVE MATERIALS

H. KLOCKER and F. MONTHEILLET

D6partement MateYiaux, Ecole des Mines de Saint-Etienne,
158 cours Fauriel, 42023 Saint-Etienne Cedex 2, France.

ABSTRACT
The influence of inertia on void growth during high strain rate deformation of ductile materials
is theoretically investigated by a Galerkine weighted residuals method. It is shown that inertia
effects are noticeable for strain rates larger than 103s_1, high triaxiality ratios (£°° £ 1) and
increase with the void radius. They are expected to reduce both the growth rate and anisotropy
of damage. Therefore, they are likely to play an important role in the process of dynamic ductile
fracture.

KEYWORDS
Damage; ductility ; dynamic loading; inertia effects ; plasticity; void growth.

INTRODUCTION
Fracture in ductile metals is generally caused by the growth and coalescence of voids (Gurland
and Plateau, 1963). Tension tests under high speed loading have often revealed a linear
relationship between flow stress and strain rate a= a 0 + pe, as well as a significant increase in
ductility with strain rate (e.g. Regazzoni and Montheillet, 1985). The latter can be partly
attributed to the improved stability of the elongation : necking occurs later and develops more
slowly than in the low strain rate quasistatic range. It has been shown by a simple mechanical
analysis that this can be attributed to both the linear flow rule and the inertia effects (Doyon et
al.f 1989). However, an increase in strain rate has been observed to improve the 'intrinsic
ductility' of the material as well, i.e. to diminish the damage growth rate. The aim of this paper
is therefore to analyze theoretically the influence of inertia on the growth of a cavity during high
strain rate deformation of the material.

Very few models including inertia effects are available to date. The growth of a spherical void in
an infinite, perfectly plastic material submitted to remote dynamic axisymmetric loading has
been investigated by Glennie (1972), starting from the classical velocity field of Rice and
Tracey (1969). More recently, two simple cases, viz. a cylindrical cavity submitted to axial and
axisymmetric radial remote loads, and a spherical void submitted to uniform remote mean
stress, have been dealt with by Klocker and Montheillet (1990). These early works show that
inertia effects tend to decrease the cavity growth rate, provided the remote mean stress is large

493
494
enough. However, the dynamic growth of a spheroidal (elongated or flattened) cavity, as well
as the possible interaction between shape and volume changes, have not yet been addressed.

In the present work, a spheroidal cavity in an infinite von Mises rate sensitive matrix submitted
to remote axial tension strain rate e and uniform triaxiality C,°° is considered. These loading
conditions correspond to the tensile test of a round bar with an axisymmetric notch or crack, as
shown in Fig. 1.

Fig. 1. Geometry and loading conditions.

QUASISTATIC LOADING OF A LINEAR VISCOUS MATERIAL

The exact velocity field in the case of a linearly viscous (newtonian) matrix without inertia
effects has been recently determined (Klocker, 1991) by using the 'three potentials method' first
introduced in linear elasticity by Papcovitch (1932) and Neuber (1944). By using the condition
of volume conservation, it was shown that velocity is the sum of four terms :

u + a .I1*a 2 g + a3I3 2
(1)
where u is the homogeneous remote velocity ; g and g denote two velocity modes,
associated with homothetic void growth and void distortion without change of volume,
respectively ; the third mode g 3 contributes to both volume and shape changes. It should be
noted that the latter had never been taken into account in the previous models of cavity growth.
g 1 , g 2 and g3are functions of the mean radius R = (a+b) / 2 and excentricity e = (a-b) / (a+b) of
the void. For a spherical void (e = 0), the expressions in spherical coordinates of the three
velocity modes are particularly simple :
3 A. 2
1*1 - R 3 /r* f 8? = ( 3 s i n 2 9 - l ) R 5 / 3 r 4 \ g? = (sin 2 eJR 3 /r
(2)
ge = 0 si sin2 9 R 5 /3r 4 ge = 0

The scalar coefficients are then determined by the kinematical equations

a = C ( A ) + aig'(A)
(3)
b = ur(B) + aig}(B)

where the points A and B are defined in Fig. 1, and the additional condition that the shear stress
 495
Gre, hence the shear strain rate e^ should vanish on the surface of the cavity. For any given
geometry (R, e), the.above three equations allow ai, 0C2 and 0C3 to be expressed as functions of
pie time derivatives R and e. It should be noted that such a form of the velocity field leads to
6re = 0 on the void surface, whatever the flow rule of the surrounding matrix. Furthermore, it
was verified that the normal stress component on is also zero on that surface in the newtonian
case, which proves that the exact velocity field was found. For a spherical void, the expressions
of the scalar coefficients in spherical coordinates reduce to
a i = R/R-7e/5+e/2
cc2 = - 6e/5 (4)
cc3 = 16e/5 - 3e/2

THE GALERKINE WEIGHTED RESIDUALS METHOD

In the^case of dynamic loading, the inertia forces py = p du/dt depend on the unknown velocity
field u. Hence, no variational principle can be used to approximate the exact solution. Thus the
following method was adopted here : the equilibrium equation div a - py = 0 is equivalent to
the condition

I I div a - p y . w dv = 0 (5)

for any weighting function w, where the integral is extended over the volume of the matrix.
Hence, an approximate solution will be found by prescribing that eq. (5) should be fulfilled for
some finite set of weighting functions.
The exact solution eq. (1) was chosen as a general form, R and e being now considered as
optimization parameters. For a spherical cavity, the scalar coefficients of the three velocity
modes (2) were assumed to be given by the same expressions (4) as in the exact solution. The
acceleration Y was then derived in spherical coordinates. For a spheroidal cavity, the same
velocity modes were still employed, so that calculations could be simplified by the use of
spherical coordinates. The scalar coefficients were then determined by the kinematical equations
(3) and the additional condition thatEro should vanish on the surface of a spherical void of same
mean radius R as the actual cavity. Thus the excentricity of the spheroid is taken into account in
the expression of die velocity field.

Since two optimization parameters, R and e, have to be determined, only two weighting
functions are necessary. The velocity modes g 1 and g 2 were chosen for that purpose, which
provides a set of two coupled second order differential equations (pi (R, e, R, e, R, e) = 0
(i = 1,2), which were solved numerically. This Galerkine weighted residuals method gives the
exact solution in the two special cases of a spherical void in an infinite matrix submitted to
remote hydrostatic tension, and a spheroidal cavity in a linearly viscous matrix submitted to
quasistatic loading. It is therefore expected to provide a good approximation for the general case
of a non linear dynamically loaded matrix.

INFLUENCE OF INERTIA ON VOID GROWTH

Although calculations were carried out for a jnaterial exhibiting a linear relationship between
flow stress and strain rate, viz. a = G0 + Pe, the special case of a perfectly plastic matrix
(P = 0) will be considered here, in order to bring into evidence the influence of inertia without
any rheological strain rate effects.

Figures 2a and b show the strain rate dependences of the normalized growth rate R/eR and
distortion rate X/kX of a spherical cavity, where X = a/b denotes the aspect ratio of the spheroid
(here X = 1). Under quasistatic loading, these two quantities would not depend on e. At high
strain rates, however, inertia effects tend to lower the growth rate (Fig. 2a) and the absolute
496
value of the distortion rate, which is negative for the triaxiality ratios considered (i.e. the void
undergoes flattening) (Fig. 2b). Both effects are more pronounced at high triaxiality. Figs 3a
and b show that the effects of inertia significantly increase with the cavity radius R. These
conclusions are in agreement with the results of a simple dimensional analysis, which indicates
that inertia effects, should be proportional to the squares of the cavity radius R and the remote
tension strain ratee (Klocker, 1991).
The case of a spheroidal void is illustrated by Figs 4 and 5, corresponding to moderate (C°° = 1)
and high (£°° = 4) triaxiality ratios, respectively. In the first case, the volume growth is rather
low (for e = 1, R ~ 4 RQ, Fig. 4a) and is associated with an elongation of the cavity (for e = 1,
e ~ 0.5, i.e. X ~ 3, Fig. 4b). The increases of the mean radius and excentricity are both slightly
reduced by inertia, although the effect on theradiusbecomes significant only at strains larger
than 0.4. Inertia effects are much more pronounced in the case of high triaxiality. The volume
growth is very fast (for e = 0.03, R ~ 3 R0 if R0 = 20 urn, Fig. 5a) and is now associated with
a flattening of the cavity (for e = 0.03, p ~ - 0.1, i.e. X ~ 0.8 if RG = 20 ^im, Fig. 5b).
Furthermore, Figs 5a and b show that the effects of inertia strongly increase with the initial
radius of the void, which confirms the above conclusions.
These results show that, during high strain rate deformation of a ductile material, inertia is
expected to reduce both the growth rate and anisotropy of damage. The first effect is equivalent
to an apparent decrease of the remote triaxiality ratio, whereas the second one is equivalent to an
apparent increase of the latter. This is different from the rheological strainjate effects, which are
generally also present at high strain rates : for a linear flow rule b=c0+pe, a strain rate increase
reduces the growth rate, but tends to slightly increase the distortion rate of the cavity (Klocker,
1991).

CONCLUSIONS
(i) Inertia effects on void growth during high strain rate deformation of ductile materials were
brought into evidence by a theoretical analysis. They become noticeable fore > 103 S"1 and
remote triaxiality ratios £°° > 1.
(ii) Inertia effects tend to decrease both the volume growth rate and the elongation or flattening
rate of the cavities. Thus, they are expected to reduce the growth rate and anisotropy of damage.
(iii) They strongly increase with strain rate, triaxiality, and the initial radius of the cavity.
Therefore, they are likely to play an important role in the process of dynamic ductile fracture or
crack propagation by void coalescence.

REFERENCES
Doyon, J., H. Klocker and F. Montheillet (1989). A simple model for the interpretation of
high strain rate tension tests. In : Advances in Constitutive Laws for Engineering Materials
(FT Jinghong and S. Murakami, Eds), Bd I, pp. 359-364. International Academic
Publishers, Beijing.
Glennie, E.B.(1972). The dynamic growth of a void in a plastic material and an application to
fracture. J. Mech. Phys. Solids, 20, 415-429.
Gurland, J. and J. Plateau (1963). The mechanism of ductile rupture of metals containing
inclusions. Trans. Am. Soc. Metals, 56, 442-454.
Klocker, H. (1991). Analyse theorique de la croissance d'une cavite dans un materiau
viscoplastique. These, Ecole des Mines, Saint-Etienne, France.
Klocker, H. and F. Montheillet (1990). Influence of flow rule and inertia on the ductile growth
of voids. Nucl. Eng. Des., in press.
Neuber, H. (1944). Kerbspannungslehre. J.W. Edwards, Ann Arbor MI.
Papcovitch, P.F. (1932). Solution generate des equations differentielles fondamentales
d'elasticite, exprimee par trois fonctions harmoniques. C.R. Acad. Sci., 195, 513-515.
Regazzoni, G. and F. Montheillet (1985). High strain rate ductility in uniaxial tension : a
review. In : Int. Conf. on Mechanical and Physical Behaviour of Materials under Dynamic
Loading, pp. 435-444. Les Editions de Physique, Paris.
Rice, J.R. and D.M. Tracey (1969). On the ductile enlargement of voids in triaxial stress fields.
/ . Mech. Phys. Solids, V7, 201-217.
 497

-b-

Fig. 2. Strain rate dependence of the normalized growth rate (a) and distortion
rate (b) of a spherical cavity in a perfectly plastic matrix. The mass per
unit volume is p = 8,960 kg/m3 (copper).

-b-

5 10 15 20 5 10 15 20
R (/^m) R (/^m)

Fig. 3. Influence of the cavity radius on the normalized growth rate (a) and
distortion rate (b) of a spherical cavity in a dynamically loaded
perfectly plastic matrix (p = 8,960 kg/m3).
498

Fig. 4. Dependence on remote strain of the mean radius (a) and excentricity
(b) of an initially spherical cavity in a perfectly plastic matrix with
(p = Pcu) or whithout (p = 0) inertia effects, in a case of moderate
triaxiality.

Fig. 5. Dependence on remote strain of the mean radius (a) and excentricity
(b) of an initially spherical cavity in a perfectly plastic matrix with
(p = pcu) or whithout (p = 0) inertia effects, in a case of high
triaxiality. The influence of the initial radius of the void is also shown.
WS2h5

A CONTINUUM DAMAGE THEORY FOR HIGH STRAIN RATE

DEFORMATIONS OF METALS WITH APPLICATION TO
IMPACT PROBLEMS

O.T. BRUHNS

Institute of Mechanics I, Ruhr-University Bochum,

D-4630 Bochum, F.R. Germany

ABSTRACT

The behaviour of metals under dynamic loading is described by introducing a con-

tinuum damage theory, which is also valid for nonisothermal processes. Microstruc-
tural changes are modelled by internal variables, e.g. damage due to shear bands
is described with a second order tensor. Dislocation induced viscoplastic deforma-
tions are modelled using a flow rule of the overstress-type.

KEYWORDS

Viscoplasticity; damage; shear bands; dislocations; finite deformations; impact.

INTRODUCTION

In many methods for the analysis of impact loaded structures S, a near field S n
in the vicinity of the point of impact and a far field Sf are distinguished, which
are separated by the boundary dSnf. In general, S n is deformed inelastically, the
state of stress is three dimensional and propagation phenomena are of importance.
On the contrary, elastic behaviour prevails in Sf, concerning the state of stress
the approximations of beam, plate or shell theory are valid and the characteristic
times of the structural behaviour are large compared with L/c. Here L denotes a
typical length of the structure and c is the velocity of propagation of acceleration
waves. Hence the solution in Sf can be expanded in eigenfunctions corresponding
to the lower eigenfrequencies, provided plausible assumptions are made about the
stresses on dS n f .

Structural failure under dynamic loading, however, frequently depends on the be-
haviour in S n . There are exceptions of this observation, e.g. when a focussing of
waves leads to failure at points of Sf? , but nevertheless we are convinced that con-
stitutive modelling and numerical simulation of the behaviour of S n deserves more
attention if one aims to predict structural failure. According to what has been said

499
500
about the state of stress in S n , a complete continuum mechanics description is
required.

During a vertical impact of a blunt steel projectile against a steel target, the target
plate fails by "plugging" due to shear band formation and by "spalling" due to
cracks, which are nucleated by the tensile wave reflected on the rear side (Shockey
et al., 1979). Further investigations (Curran et al., 1981) have shown that two types
of mechanisms contribute to the inelastic behaviour of metals under dynamic load-
ing, i.e. dislocation processes and (with a larger characteristic length) damage proc-
esses. The latter comprise nucleation, growth and coalescence of defects like micro-
voids, microcracks or micro shear bands. In vertical impact problems, shear band
formation has been found the most important of these damage mechanisms.

A defect will be called a microdefect if its extension is small compared with the
linear dimension of a representative volume element AV; otherwise it will be named
macrodefect. During a typical loading process, nucleation and growth of these mi-
crodefects may finally result in the nucleation of a macrodefect at time t = t*. The
time interval CO, t*3 will be described within the frame of continuum mechanics.

For t > t*, we have to deal with the growth of macrodefects (either macrocracks
or macro shear bands) in a damaged solid and thus elements of fracture mechanics
have to be included to complete the constitutive relations. However, even for this
phase an accurate description of phase 1 is necessary since otherwise the failure
criteria could be based on physically unrealistic values of variables.

In this paper we will concentrate on the description of phase 1 processes. To this

end a continuum damage theory is developed, which takes into account damage due
to shear bands (Bruhns and Diehl, 1989; Diehl, 1989). This theory is valid for strain
rates from 10~4 sec" 1 to 10 s sec" 1 and for arbitrarily large deformations and rota-
tions. The model has been implemented into 1-D (Diehl, 1989) and 3-D axisymmetric
(Fornefeld, 1990) finite element codes. Some numerical results for vertical impact
problems have been reported by Fornefeld (1990) and Bruhns (1991).

A CONTINUUM DAMAGE THEORY

General considerations

Consider a representative volume element AV as a polycrystal containing a finite

number of defects like stress concentrators etc. The motion of this element may
be defined by averaging values over AV, e.g. D the rate of deformation tensor is
the average effect of the different mechanisms that contribute to the motion in
the disproportionately stressed grains of AV.

The continuum damage theory is characterized by the additive decomposition of this

rate of deformation tensor according to

D = Dr + Dj, Dj = D d a + D d t + D s = D d + D s (1)

where D r and Dj are reversible and irreversible (inelastic) parts, respectively. Dj

contains contributions D d a of athermal dislocation motion, D d t of thermally acti-
 501
vated dislocation motion and D s of micro shear band formation. Additional varia-
bles are introduced in order to describe microstructural changes and to formulate
necessary yield and loading conditions. The identification of these variables is based
on an approximate homogenization method which is explained in Bruhns and Diehl
(1989). We here simply refer to the results of this method. Let

0 = { X a , X t , x, x, ^ Z, a q } , 0 = {u, Adi} (2)

be the set of internal and process variables, where X a and Xt are different kine-
matic hardening tensors related to the athermal and thermally activated dislocation
motion, respectively, and x is an isotropic hardening parameter related to the total
dislocation density N. The microstress concentration tensor x represents an average
of local stress concentrations in the vicinity of microdefects. # is an average of
local temperature concentrations, Z is a symmetric positive definite damage tensor,
and u = N m O D / N is the quotient of mobile and total dislocation densities. Further-
more Adl is an average of local dislocation induced deformations in the vicinity of
microdefects and otq is a vector-valued thermal variable which is related to heat
flux vector q.

For the description of nonisothermal processes the specific free enthalpy g is in-
troduced as a function

g = g ( 0 , 6; Q) , (3)

while the process variables (j do not alter the energy of the solid.

The constitutive law

The constitutive law comprehends:

i) the state function for the specific free enthalpy, from which the reversible
strains and the specific entropy are deduced,
ii) evolution laws for the internal and the process variables Q and £f, and finally
iii) flow rules for Dd a , D^t, Ds anc * t n e inelastic spin Wj.

According to the nonlinearity of inelastic material behaviour some of the flow rules
and evolution laws are subjected to yield and/or loading conditions.

The decomposition (1) is motivated by introducing a so-called intermediate configu-

ration (Lehmann, 1984). The evolution laws and flow rules are first formulated for
variables with respect to this intermediate configuration and thereafter transformed
to the actual configuration. This conversion includes multiplications with the rever-
sible part F r of the deformation gradient and is simplified in the present case
since in metals only small reversible changes of the shape occur.

i) Reversible part of deformations

Contrary to what is usually adopted in the formulation of elastic-plastic constitu-
tive relations we no longer maintain the assumption that the inelastic deformations
will not influence the reversible behaviour. This is especially due to the fact that
damage will influence the material properties (stiffness) in the elastic domain.

The reversible part of the rate of deformation tensor thus becomes

502

, — t r ( 8 ) l )J + - 2k a t © l (4)
2tiA 3 1+ v A

for an instantaneously isotropic material. Herein ^t (shear m o d u l u s ) , v (Poisson's

ratio) and a^ (thermal expansion coefficient) are the material p a r a m e t e r s of the
undamaged elastic material. The influence of the damage t e n s o r Z on the elastic
r e s p o n s e is introduced by functions

A = d e t ( F r ) = A(d, 0, Z ) , f = f(0, C := IIZ I (5)

o
F u r t h e r m o r e the symbol (•), e.g.

d := d - ( W - W ; ) d + d ( W - W s ) (6)

e x p r e s s e s a special objective time derivative (Jaumann-type rate) introduced in the

intermediate configuration with Wj the inelastic spin (see e.g. Dafalias, 1984, 1985).

ii) Flow rules - part 1: Dislocation induced inelastic deformations

The c o n t r i b u t i o n s of the athermal as well as the thermally activated dislocation
motion to the dislocation induced inelastic deformations are introduced as associa-
ted flow rules (normality rules) related to different yield surfaces

Dda= [ Y a ( u , . . . ) ] a < I C a > N a if (7)

^ d ' - X a ' M d ' - X a 1 ) - g a ( x , G,u) * 0 and

(8)
ICa = 2;(d' 6 >0
A dQ

Ddt= Y t ^ - ^ t j t N t if
(9)
F^-Va'"^-^'"^^) *gt<*.©. "> * °
where

Na Nt «'-Xa (10)
lld'-XJ

are the normals to the surfaces F a = const, and F^ = const., the square b r a c k e t s
here and in the following mean

x if F y ^ 0,
[x]v = (11)
0 otherwise

and the symbol <•> denotes a Maccauly bracket with respect to t h e loading c o n -
dition LCy > 0. Fy ^ 0 is a yield condition for changes of a variable ^ e ( / J u 5 ) ,
and the prime ( )' as usual d e n o t e s the deviatoric part of a tensor. Here and in
what follows functions Yy, <Dy and gy have been introduced as in normal plasticity
sxcept an additional dependency of some of t h e s e functions on the p r o c e s s variable
A. Moreover different functions are used for the description of t h e different mecha-
nisms t h a t c o n t r i b u t e to the motion. As it is usually t h e case t h e contribution of
 503
the athermal motion Dd a is given with a rate independent relation whereas D^t is
introduced as rate dependent. Thus D^ is described by two parts of different mathe-
matical nature. The transition of this relation from rate independent for slow proc-
e s s e s to a rate dependent behaviour is accomplished with the variable u.

Neglecting here for moderate up to high strain rates the contribution of the ather-
mal dislocation motion we have D^ = D^t-

iii) Flow rules - part 2: Shear band induced processes

The second part that contributes to the inelastic deformations is given by

Ds= M s < * Q > i r flidn1 rII ^ «2>

-^x1 i1 - - ^ - t r x - g s ( O) ** 00 and
and I
(13)
£ C S = - j - ( - | " x ' - v s l ) • ( t + mx)> 0.

We note that herein the yield and loading conditions for the damage processes are
formulated in (x, &)-space rather than in (d, 6 ) - s p a c e as in the case of the dislo-
cation processes, since damage is connected with local stress and temperature con-
centrations within the material. Moreover, damage processes depend on the local
hydrostatic pressure through tr (x) . Furthermore

x := ? - x tr(D) (14)

is a second objective time derivative which has been introduced in connection with
the transformation to the actual configuration.

iv) Flow rules - part 3: Inelastic spin

Following some ideas of Mandel (1971), Dafalias (1984, 1985) has introduced the con-
cept of plastic spin where

W := O + Wj (15)

W is the total spin, Wj is the inelastic spin defined as antisymmetric part of the
inelastic velocity gradient and Q is explained as rigid body spin of the substructure,
which differs from the material spin W. We note that herein the reversible part
of the total spin has been neglected for the assumed small reversible distortions.
According to this concept the inelastic spin (or Q, respectively) is given by a pro-
per constitutive law. Therefore similar as in (1) Wj is decomposed into

W| = W d t ♦ W s (16)

the different parts that contribute to the motion, where here the above simplifica-
tion has already been taken into consideration. Since the contribution of the damage
to the motion can be assumed small compared with the thermally activated dislo-
cation motion W s will be neglected and thus

Wi = T ( u )
- t*^ i Sin^i ) i ifFt
*° (17)

Here Wj is introduced in a form of the same type as (9). We note that this form
504
differs somewhat from the relations of Paulun and Pecherski (1987), where with
the use of the representation theory different tensor functions are given. Further-
more similar as has been mentioned by Dafalias (1990) the overstress-function 0
of (17) will also be taken from (9), i.e. <DW = <Dt.

v) Evolution laws - part 1: Dislocation variables

The evolution of the hardening of the material is here described in an analogous
way as in usual viscoplasticity

Xt= Act(x)Dd -[rt]t||Xt||Nt

(18)
x = k(x)d-Dd - l(x)(e-60)[rx]tx

where ct(*), k(-) and l(-) are functions of the average dislocation density and the
second terms on the right side express possible recovery of the material.

vi) Evolution laws - part 2: Damage variables

It is known from the theory of composites that the local stress concentrations x
can be related to the overall stresses d e.g. by

x =I> d (19)

(Dvorak, 1982) where I > is a positive definite material tensor. This relation here
will be generalized in the form

x = r > d + d 4 x x - mt (20)

where m ( ) and d 4 ( ) are yet undetermined functions of ||t || and the process vari-
ables.

For the evolution of the local temperature concentrations we adopt

x
S = [®e]v ; ^ Fv = ~ z ' * x ' " 8v * 0 <21)

whereas the evolution of the damage tensor Z may follow

Z= [ 0 z ] z < I C z > ( N n + N g ) if (22)

F z = - ^ x1 • x1 - - j - trx - g z (&) * 0 and

LCZ= -A
H K^ A
- x ' - v z l ) • (x ♦ mx)> 0. (23)

Herein in a specific form N n and Ng describe changes of Z due to shear band nu-
cleation and shear band growth, respectively. Z itself contains informations about
average shear band size and average shear band orientation and can be used in for-
mulating failure criteria.

vii) Evolution laws - part 3: Thermal variables

We introduce

Sq = A grad 6 - - £ j Oq , (24)
 505

where the objective rate (•) is according to (6) defined as

Sq = a q - ( W - W ^ a q (25.)

for vector-valued variables. With an appropriate choice of the specific free e n -

thalpy function g, we can derive q = -(fcAq)Oq from the entropy inequality (see
e.g. Kosinski, 1975) and thus find

t q q + q = - A f c grad 9 , (26)

where k is the heat conductivity. (26) is known as the Maxwell-Cattaneo law of

heat conduction.

viii) Evolution laws - part 4: Process variables y

The evolution of the process variables u and A^l is finally described by
c2
u + c u + j " < u - u*eq'
eq) = 0 ; with c = c 0 ( a + v p ) (27)

where Vp := max{0, IID || + x©} is a sufficient measure to describe the process ve-
locity and u e q ( ) is the equilibrium value of u which for different values of v p can
be determined from experiments (e.g. Shioiri and Sakino, 1988).

Adl= A 2 Y d l [ > d l ] v ifjjj ♦ ( t r D ) A d i ; if F v * 0 (28)

Identification of material parameters

A strategy for the determination of the material parameters was presented by For-
nefeld (1990). Since experiments with high strain rate deformations are characterized
by non-homogeneous states of stress and strain, the interpretation of experiments
is difficult and fitting the parameters to experimental curves requires the numerical
solution of an initial boundary value problem. Therefore the identification process
represents an iterative procedure where an initial set C of parameters is chosen
such that the simulation of fictitious homogeneous deformations gives plausible
results. C is modified until the numerical simulation coincides with experimental
results.

A useful mathematical tool for this iteration is the evolutionary strategy. This is
a statistical optimization method for engineering systems, which imitates the prin-
ciples of biological evolution like mutation and selection and which was introduced
by Rechenberg (1973). The evolutionary strategy easily circumvents relative minima
of the cost function, where classical deterministic methods are "trapped".

Some results for homogeneous uniaxial states of stress

The main features of the constitutive model of equations (4) to (28) can be illustra-
ted in the case of uniaxial states of stress. From o-e-curves which differ in e and
the initial temperature (Diehl, 1989) we can observe:
- an increasing flow stress with increasing i,
506
- a decreasing flow s t r e s s with icreasing 0,
- damage induced softening at larger strains only for sufficiently large s.

These observations are in agreement with experimental r e s u l t s . Further predictions

of the model in the case of cyclic t e s t s , relaxation t e s t s , strain rate jump t e s t s
etc. can be found in Diehl (1989) t o g e t h e r with predictions for combined t e n s i o n -
torsion t e s t s . Several time integration m e t h o d s (explicit and implicit) were used
for t h e integration of the rather stiff system. The explicit Fehlberg algorithm was
found t o be t h e m o s t efficient one (Fornefeld, 1990).

REFERENCES

Bruhns, O.T. and Diehl, H. (1989). An Internal Variable Theory of Inelastic Behaviour
at High Rates of Strain. Arch. Mech., 41, 427-460
Bruhns, O.T. (1991). Shear Band Formation in Impact Problems. In: Nonlinear Com-
putational Mechanics - a State of the Art (P. Wriggers and W. Wagner eds.),
Springer-Verlag (to appear)
Curran, D.R., L. Seaman and D.A. Shockey (1981). Linking Dynamic Fracture t o Micro-
structural Processes. In: Shock Waves and High Strain Rate Phenomena in Metals
(M.A. Meyers and L.E. Murr, eds.), pp. 129-169, Plenum Press, New York,
Dafalias, Y.N. (1984). The Plastic Spin Concept and a Simple Illustration of its Role
in Finite Plastic Transformations. Mech. Materials, 3, 223-233
Dafalias, Y.N. (1985). The Plastic Spin. J. Appl. Mech., 52, 865-871
Dafalias, Y.F. (1990). The Plastic Spin in Viscoplasticity. Int. J. Solids Struct., 26,
149-163
Diehl, H. (1989). Ein Materialmodell zur Berechnung von Hochgeschwindigkeitsdefor-
mationen metallischer Werkstoffe unter besonderer Berlicksichtigung der Schadi-
gung durch Scherbander, Report No. 66, I n s t i t u t e of Mechanics, RU Bochum
Dvorak, G.J. (1982). Mechanical Properties of C o m p o s i t e s . In: Mechanical Behaviour
of Anisotropic Solids (J.P. Boehler, ed.) M. Nijhoff Publ.
Fornefeld, W. (1990). Zur Parameteridentifikation und Berechnung von Hochgeschwin-
digkeitsdeformationen metallischer Werkstoffe anhand eines K o n t i n u u m s - D a m a g e -
Modells, Report No. 73, I n s t i t u t e of Mechanics, RU Bochum
Kosinski, W. (1975). Thermal Waves in Inelastic Bodies, Arch. Mech., 27, 733
Lehmann, T. (1984). The Constitutive Law in Thermoplasticity, CISM C o u r s e s and
Lectures No. 281, Springer-Verlag
Mandel, J. (1971). Plasticite classique et viscoplasticite, CISM C o u r s e s and Lectures
No. 97, Springer-Verlag
Paulun, J.E. and Pecherski. R.B. (1987). On the Application of the Plastic Spin C o n -
cept for the Description of Anisotropic Hardening in Finite Deformation Plasticity.
J. Plasticity, 3, 303-314
Rechenberg, I. (1973). Evolutionsstrategie, F. Frommann Verlag, S t u t t g a r t
Shioiri, J. and K. Sakino (1988). Comparison of Flow S t r e s s of Aluminum at High
Rates of Strain Calculated on the Basis of Ultrasonic Study of Dislocation Beha-
vior with Directly Measured Ones. In: Impact Loading and Dynamic Behaviour of
Materials (C.Y. Chiem, H.-D. Kunze, and L.W. Meyer eds.), Vol. 2, pp. 793-800,
DGM, Oberursel
Shockey, D.A., L. Seaman and D.R. Curran (1979). Microfailure Models and Their
Application to Nonlinear Dynamic Fracture Problems. In: Nonlinear and Dynamic
Fracture Mechanics (N. Perrone and S.N. Atluri, eds.), AMD-Vol. 35, pp. 79-105,
ASME
WS2h6

ON THE RELATION BETWEEN THE PENETRATION RESISTANCE OF

CERAMIC TILES AND THEIR DYNAMIC PROPERTIES

Z. Rosenberg1, S.J. Bless2, Y. Yeshurun1,

and N.S. Brar2

1-RAFAEL, P.O. Box 2250, Haifa, Israel

2-University of Dayton Research Institute
Dayton, Ohio 45469 U.S.A.

ABSTRACT
The ballistic efficiency of ceramic tiles is best determined
by the thick backing technique in which the residual
penetration of the projectile is measured after it penetrates
the ceramic tile. Using long rod penetrators and steel
backing plates we have demonstrated that Tate's modified
Bernouli model can be applied to ceramic tiles. Thus, the
penetration resistance of ceramics can be described by a
single strength parameters, Rt. R t is closely related to the
HEL of ceramics.
KEYWORDS
ballistic efficiency, penetration resistance, ceramic tile,
compressive strength, shear strength, fracture toughness, tile
confinement.
INTRODUCTION
Research on ceramic materials for armor applications has been
performed for over 30 years. The extensive work of M. Wilkins
and his colleaguest1/2! is by far the most comprehensive study
in this field. Their experimental configuration consisted of
bonding a thin ceramic tile (6 to 10 mm) to a ductile back
plate of comparable thickness, and determining the ballistic
limit velocity for this sandwich against 7.62 mm armor
piercing (AP) projectiles. It turns out that results are
relatively insensitive to ceramic strength. Therefore, we
have suggested t3'4J a different configuration, the thick-
backing technique, in order to better determine the ballistic
potential of ceramic tiles. The ballistic efficiency of the
tile is determined by measuring the residual penetration of
the projectile into the thick metallic backing which supports
the tile. We have shown that the efficiency is a linear
function of a specific strength parameter y/p where y is an
effective strength of the ceramic and its density (p).
507
508
Int6l we have used the thick backing technique is order to
evaluate the ballistic performance of ceramic tiles against
long-rod penetrators. We have shown that Tate's theory for
metallic targets^7! can be applied to the ceramic long-rod
interaction and that in particular, a penetration resistance
parameter R t can be assigned to the ceramic, as for metals.
In this theory, penetration is quasi-steady and according to a
modified Bernoulli equation[7]

VipptV-U) 2 + Yp = Vipt\J2 + R t
where V and U are impact and penetration velocity,
respectively, p p and p t are projectile and target
density,respectively. Y p and R t are the "effective strength
of the projectile and the target, respectively.
EXPERIMENTAL TECHNIQUES
Long rod projectiles made of a tungsten alloy (with 7% iron
and nickel) 80 mm long and 8 mm in diameter were launched with
a 20 mm smooth bore gun at RAFAEL Ballistic Center. Impact
velocity and yaw were determined prior to impact with a set of
flash x-rays. The ceramic tiles were glued with epoxy to
thick steel plates of rolled homogeneous armor (RHA). The
tiles were either glued on the face of the steel plate or were
embedded in it with a steel cover plate 10 to 12 mm thick.
The purpose of these configurations was to check whether one
obtains a different R t value for the confined ceramic. R t
values were determined with the aid of the residual
penetration in the steel backing and a computer code based on
Tate's equations for the steady-state penetration processt7!.
Changing R t as a parameter until the code reproduces the
residual penetration depths resulted in R t values for the
tiles we have tested.
RESULTS AND DISCUSSION
Table 1 lists all the relevant data for the ceramics we tested
in this study and the R t values obtained from Tate f s model.
Rt values are compared with the Hugoniot elastic limits of the
different materials. Tate found that R t for metallic targets
are in the range of 3 to 4 times their Hugoniot elastic limit
(HEL) while Y p is roughly equal to the HEL of the projectile
material. Tatet8! explained the high values of R t by
considering the spherical cavity expansion oft 9 ].

The most striking fact about the ceramics which we tested is

that unlike metals their R t values are roughly equal to their
HEL values. Thus, their resistance to penetration is lower
than what would be expected when considering the simple Tate
analysis.
 509

Table l. Summary of Results for Different Ceramics.

Density HEL (kb) Rt (kb) R t (kb)
Material (g/cc) [Ref] t h i s work from [10]
AD-85 3.42 60 [15] 58 —
B4C 2.50 160 [18] 63 52
SiC 3.17 150 [18] 75 63
TiB2 4.48 50 [18], 77
75[20],
110[18]
Soda Lime G l a s s 2.50 64 25 —
Fused S i l i c a 2.20 80 — 36
A£N 3.25 92 66 —
AfN Confined 3.25 92 94 —

Sternberg!10] lists R t values for several ceramics which were

obtained by sphere impact experiments. His values are also
near the respective HEL values of the ceramics. He correlates
the ratio Rt/H (H = indentation hardness) with the fracture
surface energy (7) through Grady's analysis for the fragment
size in a fractured brittle solid! 11 ]. This analysis results
in a linear relation between Rt/H and y1/3 which is followed
quite closely by the ceramics studied by Sternberg.Forrestal
and Longcope!12] developed a dynamic cavity expansion analysis
in brittle materials to account for the R t values. Their
analysis shows that the physical parameters which govern the
R t values are the compressive strength of the ceramic and the
pressure dependence of the shear strength. The compressive
strength can be taken as its static value or from the HEL.
The shear strength of ceramic materials at high pressures can
follow one out of three modes: (1) it can remain nearly
constant at its value at the HEL-elasto perfectly plastic
behavior, (2) it can decrease towards zero as pressure is
increased elasto-hydrodynamic behavior, or (3) it can increase
with pressure-pressure hardening. These three behaviors are
shown schematically in Fig. 1 for uniaxial strain loading in
which the Hugoniot curves of the ceramics are shown along with
their hydrostatic curves.

The shear strength is related to the offset of the Hugoniot

from the hydrostatic compression curve.
The only direct method to measure shear strength at high
pressures is by embedding thin piezoresistive gauges in plate
impact experiments. We developed techniques to embed
commercial manganin gauges to measure principal stress!13] and
lateral or transverse!14] stress. The shear stress is half the
difference between the two principles stresses. We have
obtained results for AD-85 alumina! 15 ], soda-lime glass! 16 ],
aluminum nitride! 17 ], and TiB 2 .
510

Volumetric Strain

Fig. 1. The three possible behaviors of ceramic materials

at high pressures.

Of the materials tested, AD-85 alumina and AfN show an elasto-

perfectly plastic behavior in the sense that the shear
stresses remain constant above the HEL up to stresses 2 to
3 times the HEL value. Glass loses its shear strength at
about 100 kb (HEL « 65 kb) while TiB 2 has a strong pressure
hardening effect. Kipp and Gradyt18! measured Hugoniot points
and release curves for several ceramics and found SiC behaves
elasto-plastically while B4C loses shear strength at high
shock pressures.
We may now examine the relation between Rt/HEL ratios to the
shear strength above the HEL. Rt/HEL « 1 for both AD-85 and
A£N, and these two materials show elasto-plastic behavior.
However, SiC is also elasto-plastic while Rt/HEL « 0.40. This
low value is similar to B4C and the two glasses, for which
shear strength decreases above the HEL. Thus, the correlation
between Rt/HEL and the shear strength behavior at high
pressures is not very clear. The situation for TiB 2 is
clouded by the uncertainty in the HEL value. Measured wave
forms indicate the dominate HEL-like behavior is at 110 kbt18!
or 75 kbt2°], giving Rt/HEL = 0.7 to 1. Some
yielding may occur at 50 kb t18! giving Rt/HEL = « 1.5,
suggesting that perhaps Rt/HEL > 1 is possible for ceramics,
as with metal.
We have also found that R t values may increase when a cover
plate is used. R t increased from 66 to 92 kb for A£N, when a
 511
cover plate was used while it did not change for AD-85. This
indicates that the role of the fragmented material is
different in these two materials. While for A£N it is
important to keep the comminuted material in the projectile's
path, it is not so with alumina. We also noticed that AfN
fragmented to many very small particles, and we speculate that
these have a major role in the long rod erosion process, as
discussed by Sternbergt 1 0 1.
CONCLUSIONS
The interaction of long rods with ceramic tiles is a very
complex process. Even so, it was shown that one can apply
Tate's steady state analysis and assign a strength parameter
(Rt) to the ceramic in order to describe its resistance to
penetration. The magnitude of R t falls between 50 to 100 kb
for the ceramics which we examined. R t apparently depends on
the compressive strength and on fracture toughness.
ACKNOWLEDGEMENTS
This work was supported in part by the U.S. Army Research
Office under Contract No. DAAL03-88-K-0203.
REFERENCES
1. Wilkins, M.L., C.F. Cline and C.A. Honodel, Light Armor
UCRL-71817 (1969).
2. Wilkins, M.L., C.F. Cline and C.A. Honodel, 4th Progress
Report of Light Armor Program UCRL 50694.
3. Rosenberg, Z., S.J. Bless, Y. Yeshurun and K. Okajima "A
New Definition of Ballistic Efficiency Based on the Use of
Thick Backing Plates," Presented at the Impact 87
Conference in Bremen F.R.G. (1987)
4. Rosenberg, Z., Y. Yeshurun, Int. J. Impact Enq. 2:3 57
(1988) .
5. Rosenberg, Z., Y. Yeshurun and Y. Tsaliah "More on the
Thick Backing Technique for Screening Ceramics Against
Armor Piercing Projectiles," Presented at the 12th Int.
Symp. on Ballistics, San Antonio, Texas, (Oct. 1990).
6. Rosenberg, Z. and Y. Tsaliah Int. J. Impact Eng. 9.: 247
(1990) .
7. Tate, A., J. Mech. Phvs. Solids 15;387 (1967).
8. Tate, A., Int. J. Mech. Sci. 2£:9 (1986).
9. Bishop, R., R. Hill and N.F. Mott, Proc. Phys. Soc..
London 57:3 147 (1945).
10. J. Sternberg, J. App. Phys. .65:3417 (1989).
11. D.E. Grady, J. App. Phys. 5J3:322 (1982).
12. Forrestal, M.J. and D.B. Longcope, J. App. Phys. 67:3669
(1990).
13. Rosenberg, Z., D. Yaziv and Y. Partom, J. App. Phys.
11:3702 (1980).
14. Rosenberg, Z. and Y. Partom, J. App. Phys. 58..-3072 (1985).
15. Rosenberg, Z., D. Yaziv, Y. Yeshurun and S.J. Bless, J.
A P P . Phvs. 62..-1120 (1987).
16. Bless, S.J., N.S. Brar and Z. Rosenberg, 309-312, Shock
Waves in Condensed Matter (1987) North Holland (1988).
512
17. Brar, N.S., S.J. Bless and Z. Rosenberg, "Response of
Shock-Loaded A1N Ceramics Determined with in-Material
Gauges," Int'l. Conf. on Shock Wave and High Strain Rate
Phenomena in Materials (Explomet 90), San Diego, CA,
(August 1990).
18. Kipp, M.E. and D.E. Grady, "Shock Compression and Release
in High-Strength Ceramics," Sandia Report No. SAND89-1461
(1989).
19. Shockey, D.A. et al., Int. J. Impact Ena. .9:263 (1990).
20. Yaziv, D. and N.S. Brar, J. de Physique, £9:C3-683 (1988).
WS2h7

The Penetration of Circular Thin Metal Sheet

by Conical Projectile

K.Raminishi, N.Taneda, S.Kawano and S.Tanaka

Department of Mechanical Engineering,

Faculty of Engineering, Yamaguchi University,
2557 Tokiwadai, Ube, Yamaguchi, 755, Japan

ABSTRACT

Penetration tests on thin circular sheets using conical projectiles were

carried out in order to clarify the dependence of the energy-absorbing
capacity on mechanical properties involving fracture toughness. In
addition, the authors presented formulae for estimation of the energy-
absorbing capacity of thin metal sheets under penetration. By comparing the
estimated values with the experimental ones, it was clear that the proposed
formulae were valid for assessment of the energy-absorbing capacity of thin
sheet.

KEYWORDS

Penetration; Fracture; Energy-absorbing Capacity; Thin Metal Sheet

INTRODUCTION

The study of projectile impact against thin metal targets has long been of
interest to designers of shields for the containment of missiles such as
turbine blades in aero-engines and fragment resulting from an explosion in
process or power plants etc. However, penetration phenomena is not yet
explained generally, because the physical processes involved in the
penetration of targets by projectiles are extremely complex.

We have conducted quasi-static penetration tests (punch speed 0.04mm/s and

1.8mm/s) and dynamic penetration tests (drop type: impact velocity from 1 to
5 m/s, and missile type: from 20 to 80 m/s) using thin metal sheets in order
to clarify the effect of mechanical properties involving fracture toughness,
plate thickness and projectile velocity on the energy-absorbing capacity.
On the basis of the above experimental results, the authors proposed
formulae to estimate the energy-absorbing capacity of a thin metal sheet.
The calculated values from the proposed formulae were compared with the
experimental results.

513
514
EXPERIMENTAL PROCEDURE

Materials

The sheet materials used in this study were cold-rolled carbon steel, SPCC,
(plate thickness h=1.0mm) for motorcars, corrosion-resisting aluminum alloy,
5083, (h=1.0, 1.5, 2.0 and 2.5 mm) for super express trains and extra super
duralumin, 7075,(h=l.0mm) for airplanes. The mechanical properties and
fracture toughness are given in Table 1, where J;n i8 the J-integral value
of the initiation of stable crack growth. On the tensile strength, 7075 is
two times as high as SPCC. On the J;n value, however, 7075 is smaller than
SPCC by one order and about three orders, respectively.

Penetration Test

We carried out quasi-static penetration tests in which a punch, which was

the same shape as the projectile, was pushed into the centre of the specimen
which was installed on the support stand with a fixed board and placed on
the bed of a universal testing machine as already reported (Kawano et al.,
1988). The punch load and travel were detected by a load cell and
strokesensor. In addition, the crack length following penetration of the
punch was measured from photographs taken from beneath the specimen. The
same methods were carried out for drop type penetration tests. Missile type
penetration tests were carried out with a projectile, whose mass was 80.7g,

Table 1 Mechanical properties and fracture toughness

Material Thick- Young's Yield Tensile Elon- Jin

ness nodulus Point Strength gation
h,mm E,GPa a y ,MPa au,MPa s,% kN/m
SPCC 1.0 207 254 353 40 310
5083-H32 1.0 70 260- 369 15 70
1.5 75 150 308 24 120
5083-0 2.0 74 145 304 23 100
2.5 76 147 319 23 100
7075-T6 1.0 67 487* 551 14 28
* 0.2* Proof Stress

/ \'
i i

1 &^
300 »< " '" »»
H
" ; L »2o.s J
Fig.l Specimen and projectile configuration
 515
accelerated by compressed air with the experimental equipment as already
reported (Kaminishi et al.» 1990). The shape and the dimensions of the
specimen and projectile are shown in Fig.l. The impact velocity was
measured by means of two parallel light sources focused on photodiodes being
broken in series by the passage of the projectile.

EXPERIMENTAL RESULTS

We carried out quasi-static penetration tests using two different punch

velocities (Vis=0.04mm/s and 1.8mm/s) to examine the effect of the punch
velocity. Figure 2 shows the relationship between the punch load, P, and
punch travel, X, for SPCC. The following three regions could characterize
the deformation behavior of a thin plate under penetration, as shown in
Fig.2, within the punch velocity of the present experiment.

First, the specimen deforms largely until the initial circumference crack is
generated (region I). Secondly, some cracks then progress radially from the
circumference crack, and crack extension and petal bending proceed
simultaneously according to the punch travel (region II). Finally, crack
progress stops and the punch load becomes constant when the contact part of
the punch and the plate enters the parallel section of the punch (region
III). Moreover, results for SPCC were similar to those for 5083 and 7075.

The effect of the impact velocity on the punch load was seen in region II
and at the boundary with region I, and the load increased by approximately
20 percent over a 45-fold increase of impact velocity. Under these
conditions, dynamic flow stresses do not change with velocity differences.
Therefore, fracture toughness of SPCC is thought to depend largely on the
strain rate. On the other hand, the effect of the impact velocity was not
seen as for the V-X curve of 7075. It is thought that this was because 7075
is not easily affected by the strain rate.
5
Punch Velocity
J O.OAmm/s:
z 4 /I 1.8 mm/s:

3
S

0 20 40 60 80
Punch Travel A , mm

F i g . 2 P-X curves

ESTIMATION OF ENERGY-ABSORBING CAPACITY

Formulation

The energy-absorbing mechanism of a thin metal sheet under a conical

projectile until b a l l i s t i c limit i s classified into two types as shown in
516
rc
©BJ P
\ \^
/
' 1\ uz \
5*
\ r ,''^ \
\ /
A \/
/ z NAeA^ .<CT.) A
R/ r<j
'I /
/[c

Fig.3 Deformation of a sheet before crack initiation

Fig.2. In region I, the deformation of a thin sheet may be approximated as

that of a membrane with a fixed end, as shown in Fig.3. The formulae for P
and X in n-power hardening plasticity are given as follows.

P = 2*hftrdcos20« C ( In ~r~ ) (1)

ho
©A
tan ( - ;
X = rd ( 1 - sin0p ) + rdCos2©«ln ( (2)
tan ( - j j - )
ToCOS2 ©ft
COS©B = (3)
rc
In [h C (In -—- ) "] - I n [hcC (In -^- ) "] - 2 j i (l ) = 0 (4)
n he
where ro is the projectile nose radius, rc is the blank radius, he is the
sheet thickness at the bottom of the punch, fi is the coefficient of
friction, c is plastic coefficient, n is strain-hardening exponent, 0 A is
the angle between the horizontal line and the end of "the contact zone" and
0 e is the complemental angle of the slope of the specimen at the fixed end.

Crack initiates when 0 A reaches a certain specific v a l u e , 0or w h i c h is

determined following equation using Hill's localized necking condition.

In ( (5)
sin0o

E n e r g y - a b s o r b i n g c a p a c i t y b e f o r e c r a c k i n i t i a t i o n , Ue, i s n u m e r i c a l l y
obtained by s u b s t i t u t i n g E q s . ( l ) and (2) i n t o the f o l l o w i n g e q u a t i o n .

Ue=J PdX (6)

0
where Xi is found by replacing 0 A in Eq.(2) with 0Af

In region II shown in Fig.2, the failure mechanism of a thin sheet under

penetration can be explained by the following models. Taking the case of
the number of cracks, N=4 for example, the petals are turned over along the
straight lines connecting the crack tips and the curvature radius of the
petals vary in proportion to the crack length as shown in Fig.4. It is
considered that the energy-absorbing capacity of a thin sheet under
penetration after crack initiation, UT - lie , is evaluated by the sum of
 517

Fig.4 Deformation of a sheet after crack initiation

propagation energy of the crack, the strain energy associated with bending
of the petal and the strain energy associated with bending of the fixed end,
Hence, dlh/daT can be expressed in the following equation.

£T " u'h + Ic - sin( IT > + ZH eos(

T" > (7)

Where dai is total crack length, Ec« is the energy of crack extension per
unit area under penetration, obtained from the method explained previous
paper (Kaminishi et al.. 1990). Then, it is thought to be able to express
dynamic dlh/daT by using oi and Ec# under consideration of the effect of the
strain rate. The following equation is obtained if there is a straight line
relationship between Ece and log e approximating the a r for convenience.

at = U r ) s ( i + ^'io* TYiTT"} ' Ee#

" (Ee#)s ( l +
^ alot Tvlfr } (8)

Comparison between Theoretical Results and Experimental Ones

The UT - ai diagrams from calculating by proposed formulae Eqs.(6) and (7)

are given in Fig.5, together with the experimental results plotted by
symbols. Table 2 shows the material constants used in this calculation. The
calculated values and the experimental values agree fairly well for all
sheets and impact velocities. From these comparison, it is clear that the
proposed formulae are valid for the assessment of the energy-absorbing
capacity of thin metal sheet under penetration.

Table 2 Material constants

Material Thick- (ath (Ec.)s D fix 0*

ness
h,M NPa kN/i
SPCC 1.0 350 700 0.22 0.05 0.28
5063-H32 1.0 342 170 0.16
1.5 258 280 0.32
0.02 0.25
5083-0 2.0 258 230 0.30
2.5 258 240 0.28
7075-T8 1.0 552 26 0.12 0.0 0.0
518
Quaii-Statie Dynaa e(Drop Type)
h-l.Oua b-1 . O n
150 Experiment
[ Experiaent
SPCC : • SPCC
7075 :A
5083 : ■ !
7075 : A
5083 :■
:•
Calculation W Calculation
=> 100

vt
E x p . ( a T) u .

en Cal.(a T) LI
C
50 \
LU I/9
[• .
-^r^ n
40 BO 120 0 40 80 120 0 120
Quasi-Static Dynamic(Drop Type) [Dynaaie(Miaaile Type) |
250 5083
Expriaent
L 5083
Experiaent \\ \ 5083 1
Experiaent
b-l.Oma : f)
b-1.5™ :A
h-1.Omm
:•
h-1.5ma : A
1
.,♦
h-l.Omn : •
1 h-1.5ma :
t
1 I
200 b-2.0mn :■ f b-2.0mm
:■ 11 f h-2.thnm :± J
h-2.3nas
Calculation
:♦
H b-2.5ma
Calculation:♦ y
h-2.5ma
Calculation
"^ //
'*
1bU
♦ ! Ol
/^
CD
C
100 ♦
■J y i
+yS>A
^^*
1 ♦yT
XA
LU
50
n
^ ^
0 20 40 60 80 0 20 40 60 80 0 20 40 60 80
Crack Length aT , m m
Fig.5 Comparison of energy-absorbing capacity between
calculated results and experimental ones

CONCLUSION

The penetration of circular thin m e t a l sheet by conical projectile was

studied and the following results were obtained.
1. Fracture toughness is as predominant as the yield point (proof stress)
and ultimate strength for energy of the energy-absorbing capacity.
2. The total work done during penetration varies in proportion to total
crack length.
3. On the basis of the experimental results, the authors proposed formulae
to estimate the energy-absorbing capacity of sheet.
4. By comparing the estimated values with the experimental ones, it was
clear that the proposed formulae were valid for assessment of the
energy-absorbing capacity of thin metal sheet.

REFERENCES

. Rawano, R. Raminishi, M. Yamashita and S.Shimizu (1988). Energy-Absorbing

Capacity of Ductile Thin Metal Sheet Under Quasi-Statical Penetration by
Conical Punch. JSME Int. J.. Vol.31. No.l. 108-115.
• R a m i n i s h i , S. Rawano, T. Nanba and M. Taneda ( 1 9 9 0 ) . Dependence of
Energy-Absorbing Capacity on Mechanical Properties Under Penetration. JSME
Int. J. Vol.33. No.3. 297-302.
. Raminishi, S. Rawano and M. Taneda (1990). The Effect of Target Thickness
under Penetration of Aluminum Alloy Plate. Proc. RSME/JSME Joint Conf.
Fracture and Strength 1 90. 442-447.
WS2i2

CHARACTERIZATION OF DELAMINATION AND FIBER

FRACTURES IN CARBON FIBER REINFORCED PLASTICS
INDUCED FROM IMPACT

Klas LEVIN
The Aeronautical Research Institute of Sweden(FFA)
P.O. Box 11021, S-161 11 Bromma, Sweden.

ABSTRACT

This investigation addressed the damage shape and size distribution in laminated carbon fibre
reinforced plastics subjected to impact. Unique shapes of delamination at each interface and fibre
fracture in each ply occurred for such factors as material toughness and impactor tip diameter
for a range of impact energies. However both toughness and impactor tip diameter had an effect
on the size distribution especially at lower impact energies where the damages were preferably
located in the lower part of the laminate. However the effect decreased at higher energies where
a more symmetrical size distribution occurred. Moreover a rotation of a stacking sequence did
not alter the delamination shapes and sizes.

KEYWORDS

Carbon fibre reinforced plastics, impact damage, deply technique, delamination, fibre fracture,
damage distribution

INTRODUCTION

Composite materials are used in a variety of aircraft structural applications. In particular

laminated carbon fibre reinforced epoxies have appeared as outer skins; as such they are
exposed to impacts in manufacturing and service. Of largest concern are the impacts which are
hardly visible for the naked eye. These are of hazardous nature since they are liable to escape
detection with regular inspection methods yet still render the structure susceptible to an overall
failure. Even though much attention has been devoted to study the effect of impact damage on
residual compression strength, e.g. Guynn et al. (1985) and Levin (1986) these studies are not
sufficient to fully understand the controlling processes of structural degradation by impact-
induced damage. A general lack of systematic studies concerning the damage mechanisms
involved is evident. Although the distribution of the delaminations has been shown to play a
major role in the post impact compression strength (Byers (1980) and Guynn et al. (1985),
however, fibre fractures and transverse matrix cracking can also strongly affect the compression
strength.

In previous quantitative studies of damage distribution in laminates have been mainly concerned
with delamination distribution; determined using the deply technique (Guynn etal.(\9S5)) and
519
520

sectioning (e.g. Joshi et a/.(1987) and Gosse et A/.(1988)). The fibre fracture distribution has
only recently been investigated by Poe (1988) but his work dealt with impact damage in
extremely thick rocket cases.
This research is directed to establish the damage distribution in a number of low-velocity impact
damages. The object was to determine the damage shape and size distribution through the
thickness of laminates for a range of impact energies from low energy up to energies causing
barely visible impact damages. Another object was to evaluate how the damage shape and size
distribution was influenced by factors such as matrix toughness and impactor tip diameter. A
deply technique was applied to obtain quantative characterization of the delaminations and fibre
fractures.

EXPERIMENTS

Specimen Configurations and Impact Conditions

The panels were fabricated with commercially available carbon fibre reinforced epoxy materials:
HTA7/6376 and T300/914C, in the form of unidirectional prepreg tape. HTA7/6376 has an
improved toughness in comparison to T300/914C. The materials were cured in an autoclave
held at 180°C for one hour. After curing the qualitity was examined using ultrasonic C-
scanning. Three different stacking sequences with 24-plies were included: (90/0/90/0/-
452/+452/90/0/-45/+45)s, (902/0/902/+45/902/-45/902/0)s and (02/90/02/-45/02/+45/02 /90) s .
The first stacking sequence was tested for both material systems, whereas the two other stacking
sequences were only made of HTA7/6376 composite materials.

The low velocity impact testing was conducted on panels clamped in a rigid steel rig with a
800mm long and 200 wide cutout. Two impact damages were imparted to each panel along the
longitudinal centre line and spaced 280mm apart, symmetrical with the respect to the lateral
centre line. In this program all the impact events were subjected due to low velocity and large
mass falling weight with 015 and 30 mm hemispherical tip guided in a tube. Three testing
energies were evaluated up to the limit to obtain barely visible impact damage (BVID). Barely
visible impact damage was defined as an impact with a 2 mm deep dent in the front surface.
De-ply technique

The first step in utilizing this technique is to infiltrate the damaged area with a penetrant solution
which serves as a carrier for a metal salt intended to precipitate on the fracture surfaces. The
solution was similar to that in the works of Freeman (1982) and Guynn et al. (1985): 10% by
weight of gold chloride, 1/3 by volume of distilled water, 1/3 by volume of isopropyl alcohol
and 1/3 by volume of KODAK Fotoflo 600.

It is important that the damaged area be fully infiltrated with the penetrant. To accomplish this
the panel was loaded in three point bending in order to reopen the matrix cracking and
delaminations. An abundance of solution was applied and the panel was allowed to soak for
about 10 minutes. In some cases it was possible to apply the solution directly into the rear
surface damage by injection. The panel was then dried for a few days at 70°C to remove the
solvent which can result in unwanted by-products from pyrolysis. The matrix is partially
pyrolized in an oven at 400°-450°C with an inert gas environment. This allowed the separating
of each laminate into individual plies. The plies were examined and damage pattern were drawn
on transparent plastic films while all details were collected under the microscope during the first
unstacking operation. Since matrix cracks are parallel to the fibre direction they were reproduced
on the films of the ply opposite to that in which the crack actually existed. With these transparent
films it was possible to obtain a good three-dimensional view of the damage. The results on
each impact condtion was based on two deplied impact damages.
 521
RESULTS AND DISCUSSIONS

The greatest problem with the deply technique is to know whether the penetrant has infiltrated
the damage sufficiently. To evaluate the extent of infiltration non-destructive methods are
available; X-rayradiographyunfourtunately has the same problem and furthermore, only gives a
two-dimensional image; pulse-echo ultrasonic C-scanning provides only a quasi three-
dimensional image of the damage, and reveals no matrix andfibrefractures, only the extension
of the largest delaminations where each successive delamination is hidden by any previous
delamination. However the delamination patterns from the deplied specimens were found in
good agreement with ultrasonic C-scanning and the X-ray radiography images. The method
gave also possibility to reconstruct the distribution of fibre fractures through the thickness.
However, matrix cracks are generally obscured by the delamination markings so that the method
can only be used to determine matrix cracking outside the delamination region. Small
delaminations in the near-surface region can also be a problem to detect. A typical example of
markings from a deplied impact damage is given in Fig. 1.

For a quantative representation of the damage through the thickness, the delaminations at each
interface were characterized by their area. Since interfaces between two adjoining plies with the
samefibredirection can not be deplied and do not contain any delaminations they were excluded
from examination. Extended lines or steps of thefibrefracture generally occur in the plane of a
ply at some oblique angle to the fibre direction. These have been quantified by measuring their
projected length perpendicular to thefibredirection.

The shape of the delamination can be described as a more or less distorted peanut shape
extending predominantly in the direction given by the fibre directions of the ply below the
delamination as shown in Fig. 1. In most cases and especially where the difference in fibre
angles between adjacent plies is 45° the shape is distorted. From markings it can be observed
that the delaminations are often bounded by matrix cracks. The markings indicate also that
matrix cracking occurring, at an early stage, forces the propagating delamination to jump to the
next interface below. This delamination continues to propagate but in alternate direction from
previous interface. In cases where the mismatch angle is 45° in the new interface the
delamination propagates in a continuous manner. Otherwise it is likely to be terminated.
However, at high impact energy such smooth extension of delaminations are less prone to be
found as enough energy for fibre fracture becomes available thus distorting the delamination
shape. Only in the interfaces where the difference in ply orientation is 90° are more fully peanut
shaped delamination observed. These delaminations are less sensitive to distortions by large
fibre fractures.

For all cases, an increase in impact energy results in a greater delamination area as shown in
Fig. 2 for the quasi-isotropic T300/914C-laminate. Ignoring the large rear face delamination,the
histogram in Fig. 2 indicates that delamination sizes at greater impact energies follow a binormal
distribution symmetrical in respect to the midplane of the stacking sequence. The rear face
delamination is induced from a bending crack in the last ply (Rechak et al. (1987)).
In Fig. 3 the effect of composite material toughness and impactor tip diameter on the
delamination area, for a low energy impact of 20J, is given for each ply interface. The figure
indicates that delaminations are firstly initiated at critical interfaces preferably at locations in
lower part of the laminate. At higher impact energies near-impact surface delaminations are
prone to be created. The influence of material toughness can be readily observed. In almost all
interfaces the delamination area is substantially greater in the more britde composite T300/914C.
In case of impacts using a smaller impactor a more fully developed delamination state has been
reached at 20J. Moreover, larger impactor tip diameter can cause greater delaminations through
the whole thickness without creating a BVID. These differences are diminished at higher impact
energies.

In the two non quasi-isotropic stacking sequences, for which stacking sequences were rotated
90 degrees to each other, the shape of delamination was the same. Also the delamination area
concided for the two stacking sequences. This indicates that the local geometry i.e. relative ply
522
orientation is the determining factor for delamination shape and size. This is in accordance with
Liu's(1988) model where the size and shape of delaminations are determined by the ratio of
bending stiffness between two adjacent plies.
Fibre fractures occur at 20J particularly at the lower part in the impact damage as shown in Fig.
4 with the smaller impactor causing extensive fibre fractures already at this energy. The fibre
fracture length does not differ significant between the two materials. When the impact energy is
increased a more uniform and symmetrical fibre distribution occurs with slightly larger fibre
fractures in lower half of the laminate. Also a slight effect of the impactor tip diameter on the
fracture size was indicated. Impacts with larger impactor result in larger fracture sizes.
However, the fibre fracture sizes were more dependent on the dent depth actually occurred for
the individual impact damages.

The extension of the fibre fractures in a ply coincides mainly to the fibre direction of the ply
above. Also the fibre direction of the ply below has some effect at high impact energies. Two
types of fibre fractures, which both seems to be initiated from matrix cracks, are noticable. One
where the fibre fractures pass directly below the impact site predominantly occurring in the
lower part of the laminate and these which pass a distance from the centre with preferable
location closer to the impacted surface. However, at higher energy these fracture modes tend to
occur parallel in the same ply.

CONCLUSIONS
A deply technique was used to characterize the damage state in laminates subjected to impact.
The method gave quantitative data of the delaminations and fibre fractures in impact damages
through the thickness. The results from the deplied samples showed that an unique shapes of
the delamination in each interface and fibre fractures in each ply occurred. For the thin laminates
tested in this program at low impact energy the delaminations and fibre fractures predominandy
were appeared at lower part of the damage. Impacts with a small impactor results in larger
delaminations and fibre fractures than for impacts with a large impactor. Improved material
tuoghness resulted in better resistance to delamination but the effect diminished at larger impact
energies. Also at large energies a more symmetrical distribution was found. Finally a rotation of
a stacking sequence did not alter the shape and size distribution.

ACKOWLEDGMENT

The author is grateful to B. Tornquist, B. Pierrau, L. Delhage and A. Linder for their patient
and devoted experimental assistance. J. Theskan, P. Sindelar and R. Olsson are also kindly
acknowledged for their support and valuable discussions. This work was supported by the
Swedish Defence Material Administration.

REFERENCES
Byers, B.A. (1980). Behavior of Damaged Graphite/Epoxy Laminates under Compression
Loading. NASA-CR-159293
Freeman, S.M. (1987). Characterization of Laminar and Interlaminar Damage in
Graphite/Epoxy Composites by the De-ply Technique. Composite Materials: Testing and
Design (Sixth Conf.), ASTM STP 787, pp. 50-62.
Gosse, J.H. and P.B.Y. Mori (1988). Impact Damage Characterization of Graphite/Epoxy
Laminates. Proc. ASC Third Techn. Conf., pp. 344-353.
Guynn, E.G., and T.K. O'Brien (1985). The Influence of Lay-up and Thickness on Composite
Impact Damage and Compression Strength. 26th Struct., Struct. Dyn.and Mat. Conf., AIAA,
pp. 187-195.
Joshi, A.P. and C.T. Sun (1987). Impact Induced Fracture in a Quasi-Isotropic Laminate. / .
Comp. Techn. Res., Vol. 9, pp. 40-46.
 523
Levin, K. (1986). Effect of Low-Velocity Impact on Compression Strength of Quasi-Isotropic
Laminate. Proc. ASC First Techn. Conf., pp. 313-325.
Liu, D. (1988). Impact-Induced Delamination - A View of Bending Stiffness Mismatching. / .
Comp. Mat., Vol. 22, pp. 674-692.
Poe, Jr. C.C. (1988). Simulated Impact Damage in a Thick Graphite/Epoxy Laminate Using
Sphereical Indenters. Proc. ASC Third Techn. Conf., pp. 334-343.
Rechak, S. and C.T. Sun (1987). Optimal Use of Adhesive Layers in Reducing Damage in
Composite Laminates. Proc. 4th Int. Conf. Comp. Struct., pp. 2.18-31.
Sendeckeyj. G.P.(1983). NDE Techniques for Composite Laminates. AGARD Specialist's
Meeting on Characterization, Analysis and Significance of Defects in Composite Materials,
London, U.K.

<* 9
<t>
1 % !
AB-B 1 - 2 AS-B 2 - 1
■«•
AS 3 - 4

6>
%
4p ■a* 1
6> |90°
AB-B 1-9
AB-B 6*7

a*
AS-B 10 - It AS-B 9-10

A8-B 11-14

AB-B 13 - 14

A8-B 14 - IS

AB-B IS - 16 AB-B 16 - 17

AB-B IS - 19

AS-B 20 - 21
■ of
1°:
AS-B 22 - 23 AB-B 21 * ::
j|-J0°

Fig.l Markings of a typical damage pattern in the HTA7/6376

quasi-isotropic laminate impacted with 25J and a 015mm
impactor. (Fibre direction in the ply below the interface is
given)
524

INTERFACE PLY ANGLES

Fig. 2 Examination area in each interface of the T300/914C quasi-
isotropic laminate. Impactor tip diameter is 030mm

INTERFACE PLY ANGLES

Fig. 3 Delamination area in each interface of the quasi-isotropic
laminates. Impact energy is 20J.

PLY FIBRE ORIENTATION

Fig. 4 Fibrefracturelength in each ply of the quasi-isotropic

laminates Impactor tip diameter is 030mm
WS2i3

FRACTURE BEHAVIORS OF HIGH STRENGTH BEARING STEEL

IN IMPACT TORSIONAL FATIGUE AND ITS DEFECT SENSITIVITY

M. SHffiATA*, M. YAMASHTTA*, H-W. GAO*,

H. NAKAYAMA**, H. NOSE*** and I. SAKAMOTO***

* R&D Center, Koyo Seiko Co., Ltd., Kokubu Higanjyo-cho,

Kashihara-shi, Osaka, 582, JAPAN
** Faculty of Junior College of Automobile Industry, Osaka
Sangyo University, Daito-shi, Osaka 574, JAPAN
*** Faculty ofEngng., Osaka Sangyo University, Daito-shi
Osaka, 574, JAPAN

ABSTRACT
In order to systematize the impact fatigue behavior of metallic materials, impact
torsional fatigue tests were conducted on a high carbon chromium bearing steel;
JIS. SUJ2 with ultimate tensile strength of 2000~2500MPa. The results indicate that
the strength in impact torsional is almost the same as that in non-impact torsional
fatigue in contrast to the results of mild carbon steels. And furthermore, it is revealed
that fatigue fracture nuclei in torsional fatigue are not the preexisting defects such
as inclusions but small shear mode surface cracks despite that fracture nuclei in
rotating bending fatigue are restricted to the inclusions in most cases.

KEYWORDS
Impact fatigue; torsional fatigue; bearing steel; fractography; defect sensitivity.

INTRODUCTION
Investigations on impact fatigue of metallic materials conducted hitherto indicate, as
a general trend, that the strengths in impact fatigue are lower than those in non-
impact fatigue under push-pull and bending load conditions (Nakayama et al.,
1985), while strengths under repeated torsional impact load are higher than those in
non-impact torsional fatigue (Gao et al., 1990). But it must be noticed that these
experimental facts are restricted to relatively low strength steels and/or alloys, and
recently Tanaka, et al. indicated that the crack growth rate in impact push-pull
fatigue was the same as those in non-impact fatigue (Tanaka et al., 1990). Such a
trend in impact fatigue investigations suggests that impact fatigue data for high
strength alloy steels are needed to systematize the impact fatigue properties of
metallic materials. From this point of view, a series of torsional fatigue tests was
carried out on a high strength bearing steel with high cleanliness, JIS.SUJ2, under
non-impact and impact load conditions. And furthermore, on the basis of
fractographic observations, difference in defect sensitivity depending on repeated
load patterns is also discussed.
525
526

Table 1. Chemical composition (wt%).

~C SI Mn P S Cr Mo O
1.01 0.31 0.31 0.012 0.006 1.54 0.02 0.0008

Table 2. Condition of heat-treatment and monotonic tensile properties.

Ultimate tensile Proof Elongation Reduction Hardness

strength stress of area
Quenching Tempering
°B
(MPa)
<%.2
(MPa)
8
(%)
4>
(%)
H
RC

1008K, 40min 453K, 2hr., A.C. 2461 1667 1.0 2.3 61.8
O.Q. (343K) 523K, 2hr., A.C. 2275 2167 1.0 2.0 58.3
573K, 2hr.f A.C. 2265 1981 4.0 9.0 56.3

Fig. 1. Shape and sizes of specimen; (a) for rotating bending fatigue,
(b) for torsional fatigue, and (c) shape of hole notch.

MATERIAL, SPECIMEN, TESTING MACHINES

AND EXPERIMENTAL PROCEDURE

High carbon chromium bearing steel, JIS.SUJ2, supplied as spherodized bars of

23mm in diameter was used as experimental material, whose chemical
composition, and heat-treatment conditions and their monotonic tensile properties
are listed in Tables 1 and 2. They were tempered with different temperature after
machining to the specimen shapes indicated in Fig. 1, and then grind-finished. Two
types of specimens were used in this study; one was hour-glass type specimen and
another was hole-notched specimen with two holes drilled axisymmetrically of a
diameter of 70,100 or 200 [im.

Two types of impact torsional fatigue testing machines were used in this study; one
was a vibro-motor type torsional impact fatigue testing machine with a loading
frequency of about 30Hz, and another was a weight drop type one with a loading
rate of about 2.5Hz. Figures 2 and 3 show examples of impact torsional stress
patterns obtained by these machines. The torsional stress amplitude T a was defined
as a half of the peak to peak value of the stress patterns and an application of a fully
reversed torsional stress was counted as one stress cycle. Stress rise time of the
impact stress generated by the vibro-motor type testing machine is longer than that
by the weight drop type one by about twice. Therefore, the former impact stress is
called weak impact and the latter one strong impact hereafter. Additionally, 4-point
uniform rotating bending fatigue testing machine with a rotating rate of about 3420
rpm' was also used to obtain reference data.
 527

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Fig. 2. Impact torsional stress Fig. 3. Impact torsional stress
obtained by vibro-motor obtained by weight-drop
type testing machine. type testing machine.

EXPERIMENTAL RESULTS AND DISCUSSION

Impact Torsional Fatiaue Strength

In Fig. 4 are shown the results of fatigue tests for JIS.SUJ2 specimens tempered
with different temperature in non-impact torsional, strong and weak impact torsional.
fatigue. This figure indicates that difference in fatigue strength due to the difference
in the stress patterns can not be observed in any tempering condition. Previous
studies by the authors revealed that the strength in impact torsional fatigue is higher
than that in non-impact torsional fatigue through the experiments done on relatively
low strength carbon steels and an alloy; JIS.S10C (ultimate tensile strength; OB
=358 MPa), JIS.S45C (GB =555 MPa) and JIS.SCM435(o B =1081 MPa). But, the
results of this study do not coincide with those results.

Recent study on impact push-pull fatigue of a high strength alloy steel ( O B « 1 800
MPa) indicates that the fatigue crack growth rates in impact fatigue are almost the
same as those in non-impact (Tanaka et al., 1990). And, such a crack growth
behavior in impact fatigue is discussed reasonably from their dynamic stress-strain
responce; the metallic material with high sensitivity to strain rate in its monotonic
stress-strain behavior shows a trend to take higher crack growth rate in impact
fatigue than in non-impact fatigue. The results of the present study seem to be
explained from the same view point suggested by Tanaka, et al.

The results of reference fatigue tests obtained under rotating bending conditions are
shown in Fig.5. When compared with Fig.4, it is clear that the scatter of fatigue life is
smaller in torsional fatigue than in rotating bending fatigue.

Fractoaraphic Observations

In Figs. 6 and 7 are shown microfractographs of fractured surfaces under rotating

bending and torsional fatigue load conditions. Microfractograph in rotating bending
fatigue shows clear fish-eye pattern at the fracture originating site. Area analysis by
electron probe micro-analyzer revealed that the core of the fish-eye is AI2O3 of
about 20|im in diameter. On the other hand, in the cases of fracture surfaces in
torsional fatigue, shear mode small surface cracks play a role of fracture origin, and
528
1200
Tempering Non Weak Strong
temp. (K) impact impact impact
©
453 O © •

°
1000
523 A A A
0)
573 □ m ■
•a
3 800

E ► < ■

600
. A
^ 1 ^
' D 4
400 -

200
10 10 10 10
Number of stress cycles to failure N
Fig. 4. Torsional fatigue strength of smooth specimen.
^ 1400

10 10" 10' 10"

Number of stress cycles to failure N
Fig. 5. S-N curves of smooth specimen in rotating bending fatigue.

they grow to Mode I large cracks after reaching the total length of about 100^im.
These observations indicate that non-metallic inclusions such as AI2O3 are not a
predominant factor for fatigue failure in the case of torsional fatigue. Such a
difference in fracture mode mainly depends on the difference in the magnitude of
shear stress component at specimen surface between rotating bending and
torsional load conditions. And additionally, it is assumed that the defect sensitivity is
lower in torsion than in bending. In order to confirm this point, a series of non-
impact fatigue tests was conducted by using hole-notched specimens.

Fatigue Strength of Hole-notched Specimen

S-N data of hole-notched specimen in rotating bending and torsional fatigue are
shown in Figs. 8 and 9, respectively. Analytically, difference in elastic stress
concentration factor by these three hole-notches is negligible because their
diameters are small in comparison with that of specimen. So, S-N curves in both
 529

Fig.6. Fracture originating site in Fig.7. Fracture originating site in

rotating bending fatigue. weak impact torsional fatigue.
(aa=1222MPa,N=6.40xl05, (Xa=589MPa, N=4.38xl()6
Tempering temp.=453K.) Tempering temp.=453K.)

^ 1400 Key Diameter of hole d(mm)

10 O Smooth
Q. D 70
s« 1200
o ^^ V Q O I]
■
100
200
D
T>^0
0)
■o
3 1000
Q.
o->
E
CO
D
~ 800
CO ■ — ^ _ 1_
_ _^_ _ _

^n7Ta&
CO

fc;
- "" -—
£
*« ■Cr^cJ
.>,^ —^-^
600 ■■fr*^

400 ____^^_J____ , ,
10 10 10 10 10
Number of stress cycles to failure N
Fig. 8. S-N curves of hole-notched specimen
in rotating bending fatigue.
CO
Q. Key Diameter of hole d(^im)
1000
° Smooth
D 70
C 100
0) ■ 200
•o
~ 800 " \ ^ \ 0
Q.
E
CO
CO
CO
2
CO
600
^^^^fe-^

400
10* 10s 10° 10' 10°
Number of stress cycles to failure N
Fig. 9. T-N curves of hole-notched specimen
in non-impact torsional fatigue.
530

O Rotating bending fatigue

• Torsional fatigue

800 L

o> 6004

400
0 100 200 300
Hole diameter d ( urn)
Fig. 10. Relationship of fatigue limit and hole notch diameter.

figures indicate the defect sensitivity of the material. Fatigue strength in rotating
bending fatigue shows abrupt decrease with the increase in diameter of the hole.
On the other hand, in the case of torsional fatigue, fatigue limits are almost the same
regardless of the difference in the hole diameter, and furthermore four specimens
broke at the site apart from the hole notch (data points with cross, x, in Fig. 9.).
These facts indicate clearly that torsional fatigue strength is insensitive to material
defects, which agrees with the fracture mode of smooth specimens mentioned in
preceding chapter. Dependence of fatigue limit on the hole diameter is represented
in Fig. 10 for respective load conditions. This figure indicates that the torsional
fatigue strength of SUJ2 alloy steel is not so affected by the defect in spite of the
high sensitivity to defects under rotating bending load condition.

CONCLUSIONS

Major conclusions obtained in this study are summarized as follows:

(1) High carbon chromium bearing steel, JIS.SUJ2, takes almost the same fatigue
strength in non-impact and in impact torsional fatigue. And fatigue fracture mode in
torsional fatigue quite different from that in rotating bending fatigue; fracture origin in
torsional fatigue is not inclusions but shear mode small surface cracks.
(2) JIS.SUJ2 shows high sensitivity to defect in rotating bending fatigue, but
torsional fatigue strength is scarcely affected by defect.

REFERENCES
Nakayama, H. and T. Tanaka (1985). Lecture on fundamentals and applications of
impact problems of materials (5. Impact fatigue). Jour.Soc. Mat. ScL, Japan. 34.
1483-1489. (in Japanese).
Gao, H-W., M. Shibata, M. Yamashita, H. Nakayama, H.Nose. and I. Sakamoto
(1990). Impact torsional fatigue fracture of steels. Koyo Engng. Journ., No.138.
32-39. (in Japanese).
Tanaka, T., K. Kinoshita and H.Nakayama (1990). Impact fatigue characteristic of
martensitic stainless steel and the relationship between the impact fatigue crack
growth behavior and the dynamic stress strain response of material. Proc.
Dynamic & Design Conf., JSME., No.900-44(B). 163-166. (in Japanese).
WS2J1

DYNAMIC CRACK PROPAGATION IN BRITTLE POLYMERS

T. SHIOYA and R. ISHIDA

Department of Aeronautics, University of Tokyo

7-3-1 Hongo, Bunkyo-ku, Tokyo, Japan

ABSTRACT

Dynamic crack propagation in brittle polymers is studied in the combination of continuum

mechanics analysis and microscopic consideration. The crack path is predicted by the use of
energy balance method. Analytical interpretation is given for the path direction change at
high propagation velocity. Related running experiments crack is executed in brittle PMMA
plate in fixed sided condition. Microscopic feature of the fracture surface is examined. The
mode change of the surface with the crack propagation velocity is shown from parabolic pat-
tern region to crazing and micro-branching region. The transition from micro-branching to to
macro-branching of the crack path is discussed in terms of applied loading energy.

KEYWORDS

Dynamic crack propagation; crack path; polymer; brittle fracture; micro-mechanism; Lagrangian.

INTRODUCTION

Fracture of brittle polymers is characterized by crack propagation with high velocity. Crack
propagation path has been investigated in dynamic continuum mechanics (Shioya et al., 1983,
Fujimoto et al., 1985). According to the analyses, in a fixed sided plate, the crack tends to
run towards the center line when the crack propagation velocity is small, however it turns to
deviate from the center and goes toward the fixed side in case of high propagation velocity.
These analyses are within continuum mechanics and postulate no branching of the path. In ac-
tual crack propagation branching is often observed at high velocity of propagation. There
have been several theories of branching, mainly postulating a criterion based on the stress
condition in continuum mechanics. However, such phenomena depend much on material natures as
well as loading conditions, and therefore should be examined by microscopic point of view
together with macroscopic analysis.

In the present study, the crack path is analyzed and interpreted in terms of energy relations.
Related experiments of crack propagation are conducted in brittle non-crystalline PMMA plate.
The fracture surfaces are observed in detail by a scanning electron microscope. The surface
formation energy is evaluated. Through the experiments and analyses, fracture mode transi-
tions are discussed in the aspects of microscopic mode transition of fracture surface together
with macroscopic branching conditions.

CRACK PATH ANALYSIS

The authors formally analyzed the running crack path problem by g e n e r a l i z i n g the
Griffith(1921) energy balance concept. (Shioya et a l . , 1983, Fujimoto et a l . , 1985) The
analysis is reviewed here briefly with some additional interpretations. The Lagrange • s equa-
tion of motion is described as,

531
532

0.5 V/////////////////////^^^^^^
V/Vs low high

-0.5

Fig. 1. Schematic Explanation of Running Crack Path in Fixed Sided Plate.

_d,_9L_x _9L_
(D-

where L = T - U is the Lagrangian, T is the kinetic energy, U is the potential energy, q and q
are the generalized coordinate and generalized velocity, and N.is the non-conservative force.
Taking the crack tip position as the generalized coordinate, tne differential equation (1) can
be integrated to obtain the whole crack path. In case of fixed sided plate, the crack tends
to take a path towards the center line of the plate in case of low propagation velocity,
however, it turns to go away from center line (to the fixed side) in case of high velocity un-
der the assumption of no branching (Fig. 1 ) . The change of path direction can be interpreted
by examining the sign of energy change as follows. The potential energy U and the kinetic
energy T are the functions of the crack tip position (X, Y) and its propagation velocity V,
and in case of Mode III, they are expressed in form of,

U(X,Y,V) E (Yjxf^V) - AX + B
(2)
T(Y,V) T (Y)xf 2(V),

where, X is the position of the tip in the propagating direction, Y is taken in the width
direction, A and B are the constants. The f 1 (V) and f«(V) are given analytically. The func-
* #
tions E (Y) and T (Y) are obtained numerically, however, they are similarly shaped as shown
in Fig. 2. Thus, the Lagrangian L can be expressed as,

L(X,Y,V) = L (Y)xf (V) + AX - B

(3)
f 3(V) = 0.5(V/V s) 2/(1-(V/V 8) 2} 1 / 2- { 1 - ( V / V B ) 2 } 1 / 2,

where V is the shear wave velocity of the material. The derivative of L with respect to Y
changes its sign with f g (V) so that the change of sign f 3 (V) which is at V = (2/3) 1 /^ 2 V =
0.82V corresponds to the transition velocity of the crack path direction (Fig. 3 ) . Basically
same concept may be applied to the case of Mode I, however, the analysis and the interpreta-
tion become more complicated. Numerical simulation of crack path for Mode III and I has been
shown (Shioya et al., 1983, Fujimoto et al., 1985). It may be worthwhile to emphasize that
the above analysis is based on the total energies of the system and does not Include the
analysis of near crack tip condition. Therefore it should be realized that the theory does
not give a local path bending condition but it gives a general tendency of the crack path.
 533

*_J
*"
* "
LU

- 0.5 0 0.5
Y/h

Fig. 2. Energies of System in Width Direction. E :Potential, T :Kinetic, L :Lagrangian.

Fig. 3« Lagrangian vs. Propagation Velocity.

534

PROPAGATING DIRECTION
a

Fig. 4. Fracture Surface of PMMA at Various Propagation Velocity

 535

EXPERIMENT

Experimental Procedure

The fracture experiment was conducted in a brittle PMMA plate. The elastic wave velocities
were measured by an ultrasonic transmission method as V = 1945m/s and V =1205m/s, where v. and
v are dilatational and distortional elastic wave velocities, respectively. Slender rectan-
gular shaped specimens were used with the longer sides rigidly fixed after tensile loading.
The crack was triggered at the shorter' side of the specimen plate after fixing the longer
sides to specified tensile displacement. The crack propagation was along the longer sides
direction (Mode I ) . The propagation velocities were measured by the use of electrically con-
ductive paint.

Crack Path

The crack path tends towards to the center line in low propagation velocity range as expected
by the analysis. However, the path transition velocity 0.82V has not been attained due to a
rapid increase of the dissipation energy (fracture surface forming energy) with the propaga-
tion velocity V, and due to occurrence of bifurcations in some cases. This suggests that on
s t u d y i n g the crack path, it is not sufficient to analyze only by continuum mechanics
(macroscopic analysis) but, it requires at the same time to examine the mechanism of fracture
surface formation and branching at microscopic level.

Fracture Surface Analysis

The crack surface has different patterns depending on the crack propagation velocity V. The
parabolic line patterns appear at relatively low velocity. These parabolic lines are the in-
tersection lines of the crack fronts of the main crack and the microcracks which nucleate,
grow and coalesce into the main crack. The pattern changes in shape and density with the
crack velocity V. Typical fracture surfaces in the parabolic region observed by SEM are shown
for different crack velocities in Fig. 4 (a) and (b). From the SEM photos, it becomes clear
that the nuclei sites are always indented so that the material is elongated to some amount to
form voids before joining to the main crack. The depth of the nuclei which form the parabolic
pattern increases with the crack velocity, however, it remains in the order of several micron
meter. From the configuration of the parabolic pattern, the stress at the starting point of
micro-crack propagation can be calculated by the dynamic stress intensity factor (Shioya, et
al, 1988). This gives the criterion of. micro-fracture initiation and the critical stress in
case of the present material is H O MPa.

In case of intermediate loading energy, as the crack velocity is accelerated to a high

velocity range, the smooth parabolic fracture surfaces turn to rough crazing surfaces. Often
these crazing regions and the parabolic regions appear alternatively along the propagation
direction (Fig. 4- ( c ) ) . The depth or thickness of the crazing is the order of several 10s
micron meter, which is much larger than that of parabolic patterns. Corresponding opposite
fracture surfaces do not form cavity shape. These facts imply that the mechanism of craze
formation is different from that of the parabolic pattern.

As the applied loading energy becomes further higher, the craze size or thickness becomes
deeper so that the mode can be regarded as microscopic branching. These microscopic branches
can sometimes develop to macroscopic branches or the macroscopic bifurcation of the crack path
at high applied loading level (Fig. 4 (d)).

Fracture Surface Formation Energy

In the terminal velocity, the applied strain energy per unit length in the X direction is in
equilibrium with the crack surface formation energy per unit length (energy release rate).
The surface formation energy is calculated from this relation. Figure 5 shows the relation
between the surface formation energy and the crack propagation velocity. The energy increases
with the velocity gradually in the low velocity region, however, the increase rate rises
abruptly at about 4.50 m/s, which corresponds to the transition velocity from the parabolic
region to crazing region. At about V = 6$0 m/s, the energy increases without increasing the
propagation velocity. This corresponds to the macroscopic branching of the crack path, sug-
gesting that the applied energy plays an important role for the macroscopic branching
condition.
536

-« *-*[

200 400 600 800

CRACK PROPAGATION VELOCITY Y ( m / s )
Fig. 5. Surface Formation Energy vs. Crack Propagation Velocity.

CRACK PATH AND BRANCHING

As to the macroscopic branching condition, the measured branching velocity of about 60 X of

the shear wave velocity might be explained by the circumferential maximum stress in the sin-
gularity at the crack tip (Toffe, 1951). However, the experiment also claims that the actual
branching is the joining of microcracks to the main crack so that the singularity in the con-
tinuum mechanics theory does not have definite meaning as the criterion of branching. Since
the transition from crazing, micro-branching to macro-branching seems to be continuous, the
mechanism of branching is closely related with the craze and micro-branch formation. However,
there are many cases in the experiment that at almost same velocity range, some develop to
macro-branching, while, others remain micro-branching. It may be natural to consider that
craze and micro-branching is a necessary condition and that some additional condition exists
for macro-branching. Since the applied energy seems more important for macro-branching than
the propagation velocity, the concept of total energy described in the path analysis may give
the additional condition for macroscopic branching. In order to make this argument clear,
dynamic elasticity analysis of bifurcating crack becomes necessary to specify the Lagrangian
energy of the system.

CONCLUSIONS

Pynamic crack propagation in brittle polymers is studied macroscopically and microscopically.

The general tendency of crack path direction can be estimated by analytical energy method.
Microscopic fracture surface mode depends on the crack propagation velocity. The macroscopic
branching requires microscopic surface mode condition and macroscopic energy condition.

REFERENCES

Fujimoto,K.and T.Shioya(1985).A study on path of dynamic crack propagation.Journal de

Physique,£6-C5,233-238.
Griffith,A.A. (1921).The phenomena of rupture and flow in solids. Phil. Trans. Roy. Soc. London.
A221,163-198.
Shioya,T. and K.Fujimoto(1983).A theoretical study on the running crack path by energy balance
method.Trans.Japan.Aeronau.Space Sci.2£,2^6-257.
Shioya,T.,I,Koga,K.Fujimoto and R.Ishida(1988).Micro-mechanism of dynamic crack propagation in
brittle materials.Journal de Physique,£2-03,253-260.
Ioffe,E.H.(1951).The moving Griffith crack.Phil.Mag.42,739-750.
WS2J2

CXEAVAGB PRACEURE UtVER SHORT PULSE LOADING AT LOW TEMPERATURE

H. HOMMA, Y. KANTO and K. TANAKA

Department of Energy Engineering

Toyohashi University of Technology
Tempaku-cho Toyohashi 441 Japan

ABSTRACT

Cracks in SM50A, steel for welding structure chilled at -40 to -160 C were
loaded by various stress intensity pulses with durations of 20, 40, and 80
us to generate experimental data of critical stress intensity levels for
crack instability. Fracture surfaces were observed by a scanning electron
microscope to examine cleavage nucleation origins ahead of the crack tips.
The obtained experimental results were discussed from the minimum time
criterion and the crack tip plasticity.
The critical stress intensity obtained by the minimum time criterion
was decreased as the temperature was lowered. The cleavage nucleation
origin approached the crack tip as the temperature decreased.

KEYWORDS

cleavage; short pulse? minimum time; stretched zone; low temperature.

INTRODUCTION

Crack instability is strongly affected by loading rate and test temperature

especially in body-centered cubic metallic materials as low carbon steel.
ASTM standard E399 provides a test method for fracture toughness
measurement under rapid loading. However, there is a restriction of
loading rate so that stress field in a specimen could remain to be quasi-
static.

For the very rapid loading under which the stress field near a crack tip is
significantly affected by inertia, we lack reliable crack instability
criteria and experimental data. The crack instability criteria proposed
heretofore are classified to two types. One of them is based on the
quasi-static concept that a crack becomes unstable immediately when a
fracture parameter evaluated by fully dynamic analysis equals or exceeds
the critical value(Achenbach and Brock, 1973, Lehnigk,1 973). The other
takes into account of time effect that the crack instability is brought

537
538

about when t h e f r a c t u r e parameter equals or exceeds t h e c r i t i c a l v a l u e f o r

a certain period(Ka11hoff a n d S h o c k e y , 1 9 7 7 , Homma e t
al^, 1983,Kalthoff,1986) . The p e r i o d i s c a l l e d "minimum t i m e " o r
"incubation time". In t h e previous work, values of t h e minimum time for
t h e s t e e l for welding s t r u c t u r e , SM50A(Japanese I n d u s t r i a l Standards) a t -
40 C and -80 C were o b t a i n e d (Homma e t a l . , 1 9 9 0 ) . The aims of t h i s work
a r e t o generate experimental data of crack i n s t a b i l i t y a t lower temperature
t h a n -80C and t o examine the minimum time c r i t e r i o n for cleavage f r a c t u r e
in s t e e l a t t h e low temperature with crack t i p p l a s t i c i t y .

EXPERIMENTAL PROCEDURES

Material and Specimens

Material used in the experiment was the steel for welding structure SM50A
and its chemical composition and mechanical properties are indicated in
Table 1. Three kinds of specimen configurations shown in Fig.1 were
prepared to generate 80 y s , 40 y s and 20 s duration stress intensity
histories when the specimen was loaded by one point bending(Bohme and
Kalthoff,1982).

Test temperatures were -120 C and -160 C which are much lower than the
transition temperature of the steel so that the whole fracture surface
would be covered by cleavage.

Loading Device and Measurement of Dynamic Stress Intensity Histories

The loading device is shown in Fig.2. The projectile was launched by

opening the solenoid valve. The pressurized gas flew into the barrel at a
high speed and pushed the projectile to accelerate it against the load
transfer rod contacting with the mid-point of a specimen. The specimen
was loaded by one point bending due to the transmitted stress wave from the
rod since the specimen had no supports. Impact velocity was controlled by
the gas pressure.

Dynamic stress intensity history experienced by a crack was measured by a

strain gage mounted 7 mm far from the crack tip according to the method
developed by Dally and Sanford(1987).

RESULTS

Critical Stress Intensity for Crack Growth

The maximum value of dynamic stress intensity pulse measured by the strain
gage method is plotted against the pulse duration as a parameter of crack
growth event in Fig.3 for the test temperature of -120 C. The open circle
means that the crack did not grow under the stress intensity pulse and the
solid circle means that the crack grew under the pulse. A critical value
of dynamic stress intensity for the crack initiation was defined as the
middle of the adjacent solid and open circles. The critical value is
shown as a function of the stress intensity pulse duration in Fig.4
including the previous results at -40 C and -80 C(Homma et al,1 990). It
is indicated that the critical values for 40 and 80 s durations are almost
same and those are much smaller than the value for 20 s duration. It is
also seen that there is temperature dependence of the critical value.
 539
Observation of Cleavage Fracture

Fracture surface near the initial crack tip was observed by a scanning
electron microscope. For all the experimental conditions, the whole of
fracture surface was covered by the cleavage. The cleavage was always
nucleated ahead of the initial crack tip. The nucleation origin can be
detected by tracing back flow direction of river patterns to the flow
origin. The origin was a flat and smooth facet, and its direction almost
equaled the macro-scopic fracture surface direction. The distance
between the initial crack tip and the nucleation origin was measured and is
shown as a function of the temperature in Fig.5. It was noticed that the
nucleation origin was almost independent of the pulse duration while it is
significantly dependent on the test temperature higher than -120 C as shown
in the figure.

DISCUSSION

The critical maximum value of dynamic stress intensity pulse significantly

increased at the duration of 20 us as shown in Fig.4. The steep increase
is well explained from the minimum time criterion(Kalthoff and
Shockey, 1 977). The critical stress intensity determined by the minimum
time criterion is shown as a function of the test temperature in Fig.6.
It is seen that the temperature effect is significant in the range of
higher than -120 C.

The nucleation origin of the cleavage will be considered in association

with the plastic zone. Dynamic yield strength of the material was
estimated by the equation given in ASTM standard E399 Annex 7. The
dynamic yield strength was indicated in Table 2 for 80 us duration pulse.
The calculated plastic zone size is listed in Table 2. Comparing these
results with the nucleation origin of cleavage fracture, it is seen that
the cleavage fracture was initiated 1 to 2 times of the plastic zone size
far from the initial crack tip. Since average grain diameter of the used
steel is around 50 urn, only one or three grains will exist in the plastic
zone. The cleavage was nucleated at one to three grains ahead of the
crack tip. Especially, the cleavage fracture at the temperature of lower
than -120 C was nucleated in the grain adjacent to the crack tip of which
the cleavage plane was approximately parallel to the macro-scopic fracture
surface. When the crack was loaded by the critical stress intensity, the
elastic stress at the nucleation origin can be calculated by

a = K//27rr (1)

The calculated stress is also indicated in Table 2. It is seen that the

elastic stresses for -120 C and -160 C are equal to each other and are
around twice as large as those for -40 C and -80C.

Hahn et al(1959) reviewed the proposed several dislocation models for the
cleavage fracture and explained their experimental data using a dislocation
model. In all the dislocation models, the cleavage fracture is initiated
by the pile-up of dislocations against an obstacle such as the grain
boundary and inclusions. In this experiment, dislocations were emanated
from the crack tip and piled up at the nucleation origin. Stress
concentration ahead of the pile up of the dislocations is approximately
proportional to the number of the piled dislocations if the static
equilibrium is kept. The calculated elastic stress at the nucleation
origin may be enhanced to the cleavage stress by the stress concentration
540
due to the piled dislocations. Namely, the number of piled dislocations
at the temperature of -40 and -80 C will be around twice as large as that
at -120 and -160 C. Emanation of the dislocation from the crack tip
blunts the tip in proportion to the number of emanated dislocations.
Measurement of stretched zone width (szw) at the crack tip was made for the
fractured specimens and the results are shown in Fig.7. Although the szw
at -40 C is too large in comparison with the other results, this result is
compatible with the result of the elastic stress in facts that the values
of szw at -120 and -160 C are almost equal and that the value of szw at -80
C is around twice as large as those at -120 and -160 C. The szw for 20 ys
duration at -40 C and -80 C was relatively larger than those for 40 ys and
80 ys durations. This can be understood if it is considered that movement
of dislocations emanated near the instance of the crack initiation is not
ceased, so that the static equilibrium is not kept and that the static non-
equilibrium state is more enhanced under higher loading rate to emanate the
dislocations more and to blunt the crack tip more.

CONCLUSIONS

Experiments on crack instability under short pulse loading were made at low
temperatures of -120 and -160 C using steel for welding structure SM50A so
that cleavage fracture would predominantly take place at the crack
initiation. The following conclusions were obtained:

1 . The maximum stress intensity experienced by a crack at the crack

instability was much larger for 20 ys-duration stress intensity pulse than
for 40 and 80 ys-duration stress intensity pulses. This was well
explained by the minimum time criterion.

2. The cleavage fracture nucleation origins were around 20 urn far from the
initial crack tip for the both temperatures while those were around 170 and
100 urn for -40 and -80 C respectively.

3. The stretched zone size at the initial crack tip could be well explained
qualitatively from the calculated elastic stress at the cleavage nucleation
origin and the dislocation dynamics.

REFERENCES

Achenbach,J.D. and Brock,L.M. (1973).in Dynamic Crack Propagation,

G.C.Sih,Ed., Noordhoff, The Netherlands, p.529
Bohme,W. and Kalthoff,J.F.( 1982). International Journal of Fracture,
20-1,p.139
Dally,J.W. and Sanford,R.J.(1987). Experimental Mechanics, 27-4 p.381
Hahn,G.T., Averbach,B.L., Owen,W.S., and Cohen.M.( 1959). in Fracture,
Averbach et al Ed., The M.I.T. Press, USA, p.91
Homma,H., Shockey,D.A., and Murayama,Y.(1983). Journal of the Mechanics and
Physics of Solids, 31-3, p.261
Homma,H., Kanto,Y and Tanaka,K.(1990). To appear on ASTM STP for the
proceedings of symposium on "Rapid Load Fracture Testing" April 22-27
1990, San Francisco USA
Kalthoff,J.F. and Shockey,D.A.(1977). Journal of Applied Physics, 43-3,
p. 986
Kalthoff,J.F.(1986). Engineering Fracture Mechanics, 23-1, p.289
Lehnigk,S.H.(1973). in Dynamic Crack Propagation, G.C. Sin, Ed., Noordhoff,
•Hie Netherlands, p.333
 541

Table 1. Chemical compositiDn and Table 2. Dynamic yield strength, and

mechanical properties plastic zone size, nucleation
origin add elastic stress
(a) chemical com position
Teap 1 Dynamic yUkTlnaatk: acne Ommmtjn BafltfeatxMB
(C) atrangth(MPa) a t o e t i a ) odglnAiB) a t the obgWGPa)
Material C Si Mn P S Fe
-40 695 124 165 1.06
-80 790 56 106 1.10
SM50A <0.2 <0J5 <1.5 <0.04 <0.04 Re. -120 936 33 22 2.00
-180 1184 19 20 2.01

(b) mechanical properties

Yield Tensile Strain Young's
Material Elongation
Point Strength n.e Modulus

Unit (MPa) (MPa) (%) 00 (MPa)

SM50A 422 588 31 0.25 206000

50
Pre-crack Temp=-120*C
• Crock grew

I 40 e Crock did not grow.

■IV, » 30
'N^-
E^
o
c w
Q Q) 20
r
t-
\ ^ — I
73 0)
o| E <D
b 10
X -*-"

, 50
i
l \ 50 1
•Li 2
oco

. UKX) X£B 1

0 20 40 60 80 100
pre-crack
Stress Intensity
Pulse Duration To (//sec)

\i ol

i
* |%,
8 n
Fig»3. Maximum stress intensity for
crack initiation as a function of
pulse duration
L I'M Ts &

Pig.1. Specimen configuration

IOJECTILE
BARRL

/ LOAD TRANSFER ROD SPECIMEN

MgH b=B=t4
SOLENOID STRAIN GAUGED
REDUCTION VALVE

DIGITAL
MEMORY
[—rrrF
I L- = — ;
Th-m}—rcfRCUIT

MICRO X-Y PLOTTER

COMPUTER

n g . 2 . Loading device
542

250

200 h

iZ.2

o
o

-200 -160 -120 -80 -40

0 20 40 60 80 100
Stress Intensity Temperature (°C)
Pulse Duration To (//sec)
Fig.4. Critical stress intensity for Fig. 5. Cleavage fracture nudeation
crack initiation as a function of origin as a function of temperature
pulse duration

60 — i — i 1 1 |

D
50 -
Q_
v-—s
20 1 1 i 1
O

■o
a
40 r
AT= I6}isec
J • To=20jisec
■ To=40jisec
:*: | o To=80/isec •
CD • —
30 AT= Ifyisec
m
-j E o
10 L
AT= 15 fisec
i_ in
•+- 1
CO CDc 0 n
n
h • ■ -\
o 8
£Z 20 AT= 11/isc-c
- Temp= -40*C 1 M
■
O
(J • Temp= -80*C o
10 L Temp=-120*C J
a
u_
O ° Temp=-160'C

0 i . _l i i
. . . . i i 1 1
0 20 40 60 80 100 -200 -160 -120 - 8 0 -40
Stress Intensity
Temperature (°C)
Pulse Duration To (/isec)
Flg.6. Critical stress intensity for crack Flg.7. Stretched zone width as a
initiation as a function of function of temperature
temperature
WS2J3

T H E ELASTIC-PLASTIC A N A L Y S I S OF A CRACK

ON BIMATERIAL INTERFACE U N D E R D Y N A M I C LOAD

X. D. WANG

Department of Mechanics, Peking University,Beijing 100871,

P. R. China

ABSTRACT

The elastoplastic behavior of an interface crack under transient load is investigated. The materials are assumed
to be elastic—perfectly plastic and Dugdale's model is used to describe the plastic deformation near the inter-
face crack tips. Then the governing equations in the form of integral equation, which can describe the moving
boundary between elastic and plastic regions are formulated. Numerical results for crack tip opening and slip-
ping displacements and the length of the plastic region are obtained by solving the above equations. The results
obtained indicate that, for an interface crack, the slipping displacement at the crack tip has significant effect
on the failure of the crack.

KEYWORDS

Interface; Crack; Elastoplastic; Dynamic; Fracture.

INTRODUCTION

In studing the fracture initiation in a nonhomogeneous structural material, considerable attention has been di-
rected to the interface crack, both for static and dynamic loads (for examples, Williams, 1959; Comninou,
1977; Srivastava et al. , 1978). While, these solutions are mostly for linear elastic medium. In recent
works, the elastoplastic stress field near the interface crack tip was analyzed under static loading condition for
some special cases (Shin et al. , 1988,1989; Zywics et al. , 1989,1990). So far as the corresponding dy-
namic problem, little attempt has be made.

In this paper, the elastoplastic behavior of an interface crack under transient load is investigated. The materi-
als between which the crack hes are assumed to be elastic—perfectly plastic, furthermore, Dugdale's model is
adopted, that is, the plastic deformation region near the crack tip is assumed to be in the shape of a line, and
the stresses in it are assumed to satisfy Mises' yield condition. For elastic—perfectly plastic materials, there is
no singularity near the interface crack tip,so the physically unreasonable features caused by the oscillatory sin-
gularities given by the elastic solution (Williams, 1959) disappear. For this problem, since the length of the

543
544

plastic region varies with time, a moving boundary which represents the boundary of the elastic and plastic re-
gions should appear. Governing equations in the form of integral equation are formulated by the method of
Fourier and Laplace transforms coupled with the technique of inverting the transforms. The boundary of the
plastic region is not prescribed in the formulation of the problem, therefore, the equations mentioned above
can be used to investigate the elastoplastic behavior of an interface crack under transient load. From these e-
quations, numerical results for crack tip opening displacement and slipping displacement are obtained for typi-
cal examples. The results obtained indicate that, for an interface crack, the slipping displacement at the crack
tip has significant effect on the dynamic failure of the crack.

FORMULATION OF THE PROBLEM

Consider a crack which lies on the interface of two dissimilar infinite elastic—perfectly plastic media, as
shown in Fig. 1. The problem is assumed to be symmetric to y—axis. According to the assumptions given
above, the plastic deformation region near the crack tip can be described as a line—shape region (see Fig. 1 ) ,
here x=a(0 represents the tip of the plastic region.

i
.y

X
\ W\^^rr7\p- ' / / ■
/ / /
t c ^ c
a (t) a(t)
»

Fig. 1 Dugdale's model for an interface crack

Without any loss in generality, the half length of the crack is assumed to be c= 1, and the external load can
be assumed to act on the crack surface and the line—shape region of the plastic deformation. Therefore, the
stress on the crack surface can be expressed as
<rjt(x,o,0 = Pi(z,t),j = 1,2 |*| < 1 (1)
while in the plastic region
<ri2(x,o,0 = p>(*,0 + ( 7 ( j ( 0 , i = l » 2 , 1 < \x\ < a ( 0 , (2)
where p, are the known stresses acting on the crack surface, and ati are the stresses in the plastic region caused
by the plastic deformation,j=l,2 correspond to x and y axes respectively. Furthermore, Mises* yield condi-
tion must be satisfied in the plastic region, that is,
< + 3a?2 = a\ (3)
where aY is the minimum of the yield stresses of the two materials,
orr = min {arri,ar2} (4)
The stresses should be non-singular at the tip of the plastic region, that is, the stress intensity factors there e-
qual to zero,
# , ( 0 = 0, KiiO = 0 (5)
which are the auxiliary conditions used to determine a(t) and a* (or <r,2).

Let U j ( x , y , 0 be the components of the displacement vector. Making use of Fourier and Laplace transforms
given by

the problem can be formulated in terms of two unknown dislocation density functions defined by

Then making use of the continuty conditions of the stresses and displacements on the interface, and the bound-
ary conditions (1) and (2), the problem is reduced to the solution of the following integral equations;

where a=a(0 ,a=a(r) and P*>(fc,j=l,2) and the kernals of the integral equations given by

where a,/?,mtj(s,p) are given in the Appendix, and

In the expression (12), it remains to invert the Laplace and Fourier transforms. It fact, mkj(s,p) are homo-
geneous for s and p, that is, for any real constant / > 0 , the following relation exists

For such kind of functions, the inversion of Laplace and Fourier transforms can be obtained in closed form
(Wang, 1988), the result is

where ^*>(»/) = m» i (jy,l),^»,(i,j=l,2) are material constants given in the Appendix, and the superscripts
' + ' and '—' refer to the branches for /« (01,02,^,^2)^0 and /.(ai,a 2 ,/ffi,#)^0, respectively, in the
complex T? plane (r)=s/plal ,a2,filyfi2 are given in the Appendix), and R°k, correspond to the effect of Stone-
ley wave.

From above results, equations (9) and (10) become

 + —f1 ? i ( £ , 0 / ( x - oOadt - a^Cx/ayt)
it J - i
(21)
l i ( z _
+ JX/ " * ' ' " " T)[a^(£,T) - a ^ > ( $ , r ) ] ^ T = pi, |x| < a (O

- T r ^ [ sign(x/a - S)[aJ 2 ($,0 - a ^ 2 ( ^ , 0 ] ^

+ — P ^ ( ^ , 0 / ( x - a ^ ) a ^ + a^(x/a,0
7T J - l

+ ^^_FZi(x--a$,t- r ) [ a ^ ( ^ , T ) - a ^ ( 4 , T ) ] r f # T = p2, |x| < a ( 0 (22)

where ^ ( £ , 0 = ? » ( a ( 0 £ , 0 , j = l , 2 .

NUMERICAL SOLUTION OF THE PROBLEM

Since the stresses are non-singular at the tip of the plastic region, \x | = a ( 0 , it can be concluded that ^ , and
9>2 are non-singular at |<*| = 1. Therefore, $>i and $>2 can be expressed as

^ ( £ , 0 = ( 1 - <*2)*f>2.(0tf2.(O (23)

^ ( $ , 0 = ( 1 - $2)*1>2.-1 ( W 2
- 1 (
^ (24)
•-1

where A2.,B2,-i are unknown functions of time, U2m,U2.-l are second kind of Chebyshev Polynomials. Substi-
tute above expressions to ( 2 1 ) , ( 2 2 ) , a system of non-singular derivative-integral equations can be obtained:

2 ^ + 1 . 2 . ( 0 ^ 2 . ( 0 + a(0e2*+i(0 = J W i - ?2*+i (25)

.-i

J ^ . b - i C O ^ - ^ O + a(Oe 2 *(0 = P2k - ?2* (26)

where fc=0,'**,oo; djtl and e ; ( j , J = l , o o ) are the corresponding coefficient matrixes, and
2
Pu+l ~ j_Pl ( 1 _ £ 2 ) ^ » * ~ J - l ? 2 (1 - 4 2 ) ^ (2?)

while ? , - ( j = l ,••• , o o ) correspond to the integral terms, with respect to T, in (21) and ( 2 2 ) . Truncating the
Chebyshev Polynomials at n = iV, equations ( 2 5 ) , ( 2 6 ) provide 2 N + 2 equations for /l2.»#2.-i> and <7,i(or
a,2). The problem can be solved by integration step by step; while, in each step, iteration must be made for
0.1 (Or (7,2 ) .

If the solution of the above equations has been obtained, the crack tip slipping displacement (<50 and opening
displacement (<52) can be obtained,

<>i(0 = J V ( x , 0 < * x , (J 2 (0 = \'<p2(x,»dx (28)

RESULTS AND DISCUSSIONS

Numerical calculations have been made for special examples to illustrate the dynamic elastoplastic behavior of
an interface crack. The material constants are taken to be :
a. Ei = 2. 13 X 10l2dyn/cm2, yx = 0. 2 0 , pi = 5. 6?/cm 3 ;
b. E2 = 1. 05 X 1012<fyn/cm2, y2 = 0. 20, fh = 5. Sg/cm't
c. E2 = 3. 50 X 10ndyn/cm2, y2 = 0. 20, p2 = 5. $g/cm3;
 547
1
ar - 3. 50 X lOM^/cm .
while the load functions pi(*,0 and ft(x,0 are taken to be,
f i ( s , 0 - 0, ft(x,0 = - 7. 00 X WH(t)ii%/cml
The numerical results of the length of the plastic region (e=a—c) and <$i ,<5j for material combination a—6 are
plotted in Pig. 2 and Pig. 3, respectively i and the corresponding results for material combination a—c are plot-
ted in Fig. 4 and Fig. 5, where CmtM=min{CLl>CTltCLltCn} and CL1,CTi>CLt,Cn are the velocities of P and
SV waves for the upper and the lower half spaces, respectively. It can be seen that both 6X and 6\ reach maxi-
ma after the initiation, men approach the corresponding static results. Similar is the length of the plastic re-
gion (e=a—c). The above results are similar, on the whole, to the results for the stress intensity factors in
the corresponding elastic problem (Sin etal. , 1972). The present results show that the crack tip slipping dis-
placement (<$i) is of the same order of the crack tip openning displacement (<5j). It can be concluded directly
that the shear deformation near the crack tip on the interface has significant effect on the dynamic failure of
the interface crack. This paper is a preliminary analysis to the effect of plastic deformation on the dynamic
failure of an interface crack. Although only two special examples are given, the results do confirm the signifi-
cant effect of the slipping displacement at the crack tip. It should be noticed that the possible unloading of the
plastic deformation near the crack tip is not considered here, and this will be discussed in our forthcoming pa-
per.

REFERENCES

Comninou, M. (1977). J. A&. Meek. ,44^, 631-636.

Shih,C. F. e£al. (1988). J. Appl. Meek. ,55,299-316.
Shih,C.F.etal. (1989). J. Appl. Meek. ,56,763-779.
Sih, G. C. etal. (1972). Int. J. Sotiis Struc. ,7,977-993.
Srivastava,K. N. e£al. (1978). Int. J. of ^Vocftire,_14,i45-154.
Williams,M. L. (1959). Bulletin of the Seismoboical Society of Awerico,49,199-204.
Wang,X. D. (1988). Doctoral Dissertation, Harbin Institute of Technology, China.
Zywicz, E.etjd. (1989). J. Appl. Meek. ,56,577-584.
Zywicz, E. et al. (1990). Int. J. of Fracture,42,129-143.

APPENDIX

In equations (13),(14),m 4> (s,p) are given by,

m n (*,p) - A ^ D W K o i - H - ifrs*) + *i(arM - AfiS^/F
m„(*,j) -A«- 1 [fli- 1 A«(«r 1 r| ~ 4A*1) + *TlfiM(<Xlri - 4^««)]F
m12(a,r) =m 21 (*, ? ) - tufar1^ - 2A)G(aflrI - 4#**) - (oT»rf - 4ft« , )(«f I ri - 2^,)]/F
where F = sipxs~x - aTls)Q(<nlrl - 4fits*) 4- mCfiiaT1 4- At«fO
-h 2* , (af 1 r, - 2fil)(aTlrt - 2&) + s(fits~l - a*ls)(arlr\ - ift^Q-1
and Q=tH/fti, *$=?*/(%}* K}=ri/Cliia1=si+Kl,fl=z8l+tf9rl=8t+fl, where >=-4 and >=*2 refer to
the upper and the lower half spaces, respectively, while, a and fi are give by
o — 2/4[>i + * - < * • + /*i)]/Co
fi = - 2/n[(At + * ) ( * • -f 2 A ) 4- Ot + A ) U I + 2A«i)(?]Ct
where C,=[(l-hO)(A,-h/«,)-h2/i,)][(H-<0(A 1 -h/i 1 )-f2/i,]. In (19), tf,are given by,
tf, **MtQKM + Ktti)/(kiKx -f MTt). <At = A ( * I 4- G*I)*I*I/(*I*I 4- fcfi).
548

0.0
0 2 4 6cm 0 2 4 6cm

Fig. 2 Length of the plastic region (a—b) Fig. 3 Crack tip slipping and opening
displacements (a—b)

e (10" 1 cm)
1.0 2.Oh

0.5

tc m . n
I 1
0.0
0 2 4 6cm 0 2 4 6cm

Fig. 4 Length of the plastic region (a—c) Fig. 5 Crack tip slipping and opening
displacements (a—c)
WS2J4

DYNAMIC FAILURE OF BRITTLE MATERIALS:

MICROMECHANICS AND EXPERIMENTS

G. Ravichandran

Graduate Aeronautical Laboratories

California Institute of Technology
Pasadena, California 91125, U.S.A.

ABSTRACT

A micromechanical theory for damage evolution in brittle materials under high strain rate
loading is developed which includes the critical conditions for growth of microcracks. The
damage evolution is related to the number (Weibull distribution) and the average size of
microcracks. The theory provides a relation between the impact strength and the imposed
strain rate for brittle microcracking solids. An experimental technique for obtaining reliable
high strain rate deformation and failure properties of brittle materials using the split Hopkinson
pressure bar is presented.

KEYWORDS

Ceramics; damage; dynamic; impact; micromechanics.

INTRODUCTION

Brittle materials such as monolithic ceramics and ceramic composites are finding increasing
applications and there is a need to design them for resistance against impact loading. Ceramics
and ceramic composites are in general very hard and brittle and hence their failure occur at
strains of less than 1%. An understanding of damage evolution under dynamic loading
conditions is important in the analysis of structures made of such brittle materials. Past
investigations have shown that damage in the form of microcracking and/or microplasticity
plays an important role in deformation and failure of monolithic ceramics at stresses even
below the Hugoniot elastic limit (HEL) under dynamic loading conditions; see Grady (1977),
Lankford (1981), Longy and Cagnoux (1989), and Raiser ex al. (1990).

In the present study, a micromechanical theory for failure of brittle materials under high strain
rate loading is developed, including the critical conditions for growth of microcracks. Results
from mechanics of dynamic fracture (Freund (1990)) are used to develop a quantitative
understanding of damage evolution in brittle materials. The damage evolution and
accumulation is related to the degradation of the elastic moduli of the material. The
micromechanical theory is applicable for both tensile and compressive damage and is illustrated
using a one dimensional problem. The impact strength of the material is correlated with the

549
550
imposed strain rate. A recently developed experimental technique based on the split Hopkinson
bar that can be used to study the high strain rate behavior of brittle materials is briefly
described.

MICROMECHANICS OF DAMAGE EVOLUTION

In monolithic ceramics and ceramic composites, the damage evolution is intimately related to
microcracking at defects such as pores, inclusions, second phase particles and grain boundary
junctions; see Evans (1990). In the present study, the kinetics of microcracking and its
evolution under stress wave loading is modeled using concepts from dynamic fracture
mechanics (Freund (1990)) and the associated degradation of elastic moduli (Budiansky and
O'Connell (1976)).

Assume that there are N nucleation sites per unit volume and the nucleating microcracks are
assumed to be randomly oriented penny shaped cracks of average radius <a>. For randomly
oriented and dilute distribution of penny shaped microcracks, the elastic modulus of the
microcracked solid is related to the average density of microcracks through the following
relation (Budiansky and O'Connell (1976))

».l-»(l-vW>
where E and v are the Young's modulus and Poisson's ratio of the uncracked solid and the
barred (-) quantities correspond to that of the microcracked material. The cracks are assumed
to grow at a constant velocity v and the instantaneous average crack size <a(t)> is given by,

<a(t)> = vt (2)

The crack density N is assumed to have a Weibull distribution in relation to stress a and can be
written as:

I
— -
G I
0
'
, am

(3)
where a is the dimensionality of the cracks, a 0 is a threshold stress for microcracking, and m
is a Weibull constant; see Freund (1990).

A possible mechanism for microcracking under applied compressive and tensile loading in
polycrystalline materials is shown in Fig. 1 (a) and (b). The microcracking is shown to be
occuring at grain boundary junctions which act as stress concentrations or precipitors of flaws.
The same mechanism could hold for inclusions and voids where microcracking can occur due
to local tension, even under applied compressive loading. From dimensional analysis and
modeling considerations, the local tensile stress a/ in the vicinity of the crack can be related to
the prevailing stress a in the material,

a / = |a|g(E,v,fl)
(4)

where g(E,v,d) is a dimensionless factor that depends on the material properties such as E and
v, and #, which is to indicate the dependence on the size and the orientation of the crack, and
 551

also factors such as the frictional characteristics of the crack. This dimensionless factor g(...)
can be evaluated only through a detailed modeling of the micromechanism for damage; for
example see Horii and Nemat-Nasser (1984) and Ashby and Hallam (1988). For the present
study it suffices to know that Igkl. In the present analysis the stress o is replaced by o/ in
Eqn. (3) enabling one to study damage due to either tensile or compressive loading.

(a) (b)

Fig. 1. Mechanism for microcracking due to local tensile stresses

at grain boundaries in polycrystalline materials:
(a) under compression, (b) under tension.

Freund (1990) has presented an elegant analysis for microcracking of solids under constant
strain rate and uses an effective modulus for a microcrack distribution with a high degree of
geometric regularity. In the present analysis, the effective modulus result for randomly
oriented microcracks of Budiansky and O'Connell (1976) is used and follows the methodology
presented by Freund (1990).

By making use of the equations (2) and (4) in (1), and taking a = 3 (dimensionality of the
penny shaped crack) in Eqn. (3), a relation for the instantaneous modulus of the microcracking
solid at a given location can be written as:

(5)

where P is a constant given by

16
P= 1-v
(6)

When a material element is subjected to a constant strain rate e o, the stress o in the specimen
can be expressed as a function of the reduced modulus,

c(t) = E e 0 t (7)

Introducing £ = a(t)/a 0 and making use of equations (4), (5) and (7), the stress in the material
element can be written as,
552

3m
$ = - -e 0 tU P ^|-l) (?) H^|-l)
(8)

Parameters such as a 0 , b, and m have to be determined experimentally. The parameter g in

Eqn. (4) is assumed to be unity for illustrative purposes. H(.) is the Heaviside unit step
function. Using Eqn (8) one can study the effect of strain rate on the deformation response of
the material. The parameters used in this study correspond to a Weibull constant m = 1,
Poisson's ratio v = 0.25, and for the threshold stress (E/a0)= 1000. The characteristic length
scale b is taken to be 1 mm and an average crack velocity v =1000 m/s is assumed. A non
dimensionalized strain rate r is used in the calculations (see Freund (1990)) and is defined as,

E b'
r = —
v~e°
(9)
Equation (8) is used to obtain the stress-strain curves and are shown in Fig. 2 for normalized
strain rates r = 1,5,10, 50, and 100. r = 1 corresponds to an actual strain rate of 100 s'1.

vt/b

Fig. 2. Stress-strain curves for a microcracking solid for different

strain rates, r = 1, 2, 5, 10, 50, and 100.

Each of the stress-strain curves in Fig. 2 exhibit a maximum and this is termed as the impact
strength, a s , for the strain rate, r, and can be obtained from the relation,

§w-» (10)
 553

where ts is the time corresponding to the maximum in the stress-strain curve shown in Fig. 1.
Equation (10) can be explicitly written using Eqn. (8)

3m /.*\ 3
.-4»fc..r(s).. (ii)

By using (11) in (8), the impact strength o s at constant strain rate can be related to the time ts,

* - ( • • #
(12)
where q 0 is a constant given by

q0=
64(l-v) (13)

q 0 = 0.368 for v=0.25; Eqn. (13) has the same form as the result found in Freund (1990).

0 100 200

Fig. 3. Impact strength a s and time t$ as functions of strain rate r.

The impact strength as at constant strain rate can be obtained using (8) and (11), for m = 1,

,1/3
^=0.5 1+
AH£ (14)
554

Equation (14) is an important result in rate dependent behavior of brittle materials, providing an
explicit relation between the impact strength and the imposed strain rate. The impact strength
increases with increasing strain rate. The impact strength a s and the time ts are plotted as
functions of the strain rate r in Fig. 3.

EXPERIMENTS

Recently, the conventional split Hopkinson pressure bar has been modified for application to
testing very hard and brittle materials. This new technique involves two modifications to the
conventional Hopkinson pressure bar: (a) a thin copper plate is glued to the impact end of the
incident bar and (b) the strain is measured directly by attaching strain gauges to the sample.
The presence of the copper plate introduces a ramp-like stress pulse in the incident bar. While
this limits the strain rates at which the test can be performed, it does preclude the sudden
straining of the sample, as in the conventional split Hopkinson bar. The stress in the sample is
measured from the transmitted pulse. Thus, reliable stress-strain curves and failure strength
for hard ceramic based materials can be obtained at moderately high strain rates of about 50-
500 s"1. The experimental technique has been described and analyzed in detail by
Ravichandran and Isaacs (1990). This technique has been used successfully in studying the
dynamic behavior of boron-carbide/aluminum cermets; see Ramesh and Ravichandran (1990).
It is also currently being used at the California Institute of Technology to investigate the effect
of strain rate on impact strength of materials in microcracking solids. The results from these
experiments will be correlated with the analysis presented in the previous section.

ACKNOWLEDGEMENT
The support provided by the California Institute of Technology is gratefully acknowledged.

REFERENCES

Ashby, M. F. and Hallam, S. D. (1986). The Failure of Brittle Solids Containing Small
Cracks Under Compressive Stress States. Acta Met., 34, 497-510.
Budiansky, B. and O'Connell R. J. (1976). Elastic Moduli of Cracked Solids. Int. J. Solids
Structures, 12, 81-97.
Evans, A. G. (1990). Perspective on the development of high toughness ceramics. J. Am.
Ceram. Soc, Tl, 187-206.
Freund, L. B. (1990). Dynamic Fracture Mechanics. Cambridge University Press, Cambridge.
Grady, D. E. (1977). Processes occuring in shock wave compression of rocks and minerals.
In: High Pressure Research-Geophysical Applications ( M. H. Manghnani and S.-I.
Akimoto, eds) Academic Press, 389-438.
Horii, H. and Nemat-Nasser, S. (1983). Brittle failure in compression: splitting, faulting and
ductile-brittle transition. Phil. Trans. Roy. Soc, London, A319. 337-374.
Lankford, J. (1981). Mechanisms responsible for strain-rate dependent compressive strength
in ceramic materials. / . Am. Ceram. Soc, £4, C-33-C34.
Longy, F. and Cagnoux, J. (1989). Plasticity and microcracking in shock loaded alumina. / .
Am. Ceram. Soc, 21, 971-979.
Raiser, G. F., Clifton, R. J. and Ortiz, M. (1990). A new plate impact experiment for studying
microcracking in ceramics. Mech. Materials, in press.
Ramesh, K. T. and Ravichandran, G. (1990). Dynamic behavior of a boron carbide-aluminum
cermet: experiments and observations. Mech. Materials, in press.
Ravichandran, G. and Isaacs, J. B. (1990). A high strain rate testing technique for testing
brittle materials. Exp. Mech., under review.
WS3a1

Simulation of Probabilistic Fatigue Crack Growth

Hiroshi Itagaki

Department of Mechanical Engineering and Material Scince, Faculty of

Engineering, Yokohama National University, Yokohama, Japan

ABSTRACT
A method is presented for estimation of the probability distribution of fatigue crack growth
life and reliability assessment of structures by simulating material resistance to fatigue crack
growth along a crack path. The data for the simulation can be obtained from a few fatigue tests.
The material resistance is treated as a spatial non-Gaussian (eventually Weibull, in this report)
random process. The non-Gaussian random fields simulation method proposed by
Shinozuka.et al. is applied with statistical data obtained experimentally.

KEYWORDS

Fatigue Crack Growth, Material Resistance, Probability Distribution

INTRODUCTION

Experimental studies on the randomness of fatigue crack growth have been performed( for
examples Itagaki et al. 1972 ;Kitagawa et al.. 1986; Tanaka et al.. 1979 ; Tanaka et al.,
1981; Ortiz etal.. 1986). Some deal with the means and variance of material properties and
some focus on the characteristics of materials as spatial random processes. There have also
been several attempts to construct theoretically a fatigue crack growth model for the safety
evaluation of fatigue sensitive structures ( Ishikawa etal. t 1984; Kozin etal.. 1981; Lin etal..
1985; Okamura etaL> 1975; Wu etal.-1986). Such a model assumes fatigue crack growth as
a random process and,therefore, needs to know the stochastic nature of material parameters
before any its practical application. For this purpose not only mean and variance of growth rate
but also the spatial distribution of resistance are necessary. The authors studied the spatial
correlation of fatigue crack growth rate of a steel using fractographic data some yeas ago (
Itagaki et_aL,1972). The method may be said appropriate to get data for the analysis of very
short crack growth such as order of millimeter or fractions of millimeter but not good for the
analysis of longer propagation of fatigue cracks. It is, therefore, necessary to find an
appropriate experimental method of data acquisition for such a purpose.
In the previous study (Itagaki et al.. 1989), the crack growth rate was assumed to be
given by
da/dN = C (AK) m (1)
where, m and C are material constants, called hereinafter as growth rate exponent and
557
558
coefficient, respectively, and as a one-dimensional Weibull distribution
99.9
random process model of fatigue crack growth,
only the growth rate coefficient, C, was treated as a
99.0 f SJ
random variable along the crack path while the 90.0 L AK= 15.4 MPatfn jf f
80.0
exponent, m, was assumed as constant at any point. 70.0
The obtained probability distribution function of 50.0 LAK=25.3MPaVm ff
material resistance to fatigue crack growth seems [• _. \
30.0
dependent of the stress intensity factor range
1 7# :
AK.(Fig.l) It implies the assumption of a constant 10.0
m is not adequate. Therefore, the variation of the 3 *
exponent, m, should be taken into account and a 1 r i
parameter Ko should be introduced in the growth
law to make the dimension of C fixed while the
:I
exponent, m, changes. Namely, 1.0
•AK=20.2MP«fin
\
1 ' :*
m
da/dN = C (AK/KQ) (2) •
where, the dimension of the parameter Ko is same 0.1 C 1 —i 1 — i — i — I _ JI_

as that of the stress intensity factor range AK. 2 5

Then, the statistical analysis of the material l/c(x),xl0 1 0
parameters becomes possible even the exponent, m, Fig.l. PDF of resistance l/c(x)
fluctuates.
(ItagakietaL 1988 ).

VARIATIONS OF THE PARAMETERS IN THE CRACK

GROWTH LAW

Using eq.(2), the variations of the parameters, m and C, can be examined as follows.
The logarithm of the growth rate is given by

log(da/dN)=logC+m(logAK-logK0) (3)
The expected value of log(da/dN) is

E[log(da/dN)]=E[logC+m(logAK-logK0)]
=E[logC]+E[m](logAK-logK0) (4)

The variance
oflog(da/dN),^, is
<% =E[{log(da/dN)-E[log(da/dN)])2]
=<£+<£ (logAK-logKo)2+2 alcm(iogAK-logKo) (5)

where <*\c is the variance of logC, o^ is the variance of m, crlcm is the covariance between logC
and m.
The possible assumptions on m and C are,
1) m and C are constant (Paris et al., 1963),
2) m is constant and C is random ( Kanazawa et al. ^ 1979; Kimuraetal., 1983: Lin ,
1983; Ichikawa eiaL,1984 ; Sakai et al., 1979 ),
3) m is random and C is constant,
4) m and C are random variables (Fujii et al.. 1979; Ichikawa et al., 1985; Tanaka etal.
1981; Kitagawa et_aLil986; Okamura et al., 1975 ).
These can be checked easily by observing the variance of logarithm of the crack growth
rate,°v, with AK controlled tests. Namely, if ^ is non-zero, the assumption 1) is not
 559

appropriate. If <\ depends on AK, then the assumption 2) may not be true. If Aa^ is always
positive, the assumption 3) may be also rejected. If 1), 2) and 3) are negated, the fourth
assumption can be regarded as a reasonable one.
Let mi be the value of m of the i-th specimen, AKj be the stress intensity factor range
applied to this specimen, and C(x) be the value of C at point x along the crack path, then the
eq.(2) is rewritten as
da/dN=C(x)(AKi/Ko)mi (6)
Let Ci be the mean value of C(x) and (da/dN)j be the mean value of crack growth rate of a
specimen, then
- (da/dN)i=Ci(AKi/Ko)mi (7)
If the mean value of C(x) of all specimens are approximately same, the logarithm of
(da/dN)i is given by
log[(da/dN)i]=logCi+mi{logAKi-logK0)
-logCo+mi{logAKi-logKo} (8)

where, Co is the mean value of C(x) for all specimens, logCo ~ logQ. The expected value of
log(da/dN)i is expressed as

log[(^)i]=log Co+m{logAKi - logKo}

(9)

The standard deviation of log[(da/dN)i], o \ i , is given by

a
vi = a m l k r k o l (10)

where, ki=logAKj, ko=logKo-

As shown in eq.(10), if there is no variation due to m, then, there is no variation in the

mean value of crack growth rate.
On the other hand, if the mean value of C(x) in a specimen is not constant and m is

constant, the standard deviation of log(da/dN)i is independent of AK and given by

a = a
vi Ci (11)

where, °~ci is the standard deviation of logCj.

EXPERIMENTAL RESULTS

In the following the experimental results with a high tensile strength steel, 18mm thick
BS4360(GR50D), for marine structures are cited from referce[ Itagaki et al.T 1990 ] as an
example. The results are listed in Table 1. The test conditions are also given in the table.
Discussion of the Assumptions
The variance of log(da/dN), <\, for each AK value is computed by equation (5), and is
plotted against logAK in Fig.2. <\ is not always zero, thus the assumption 1) is not
reasonable. The assumption 2) can be negated for it depends on AK value. It seems always
positive, then the assumption 3) is also rejected. Therefore, the assumption 4) may be
reasonable.
560

Probability Distribution of the

Parameters Table 1. Test condition and results.
specimen AK mean of -*«*- co.vof^*- c.o.vofZ(x)
m
Estimation of Kn and Cn_ Using no.
(MPiffi) dN
(m/cycle) (%)
dN
(%)*
the assumption 4), the standard 1BS08 21.8 6.26 xlO"' 13.7 3.60 13.9 1
deviation of the logarithm of the 1BS09
1BS10
21.8
21.8
5.61
5.52
15.2
14.6
3.88
3.92
14.2
14.0
mean growth rate, <*vi is computed, IBS 11
4BS01
21.8
21.8
6.58
7.65
14.0
15.7
3.48
3.10
14.7
15.4
and is plotted against logAK as 4BS02 21.8 7.98 2.78 199 15.5

shown in Fig.3. As is seen, the 2BS01

2BS02
28.0
28.0
1.75 xlO"7
1.83
11.6
11.4
179
149
11.4
11.8
relation between o\i and logAK can 2BS03
2BS04
28.0
28.0
1.80
1.85
10.1
9.5
160
142
10.9
9.4
be described by equation (10). In 2BS0S
2BS06
28.0
28.0
1.90
1.85
8.9
10.4
124
142
9.1
11.1
this figure, the standard deviations 2BS07
2BS09
28.0
28.0
1.84 10.0
12.7
145
124
10.3
116
1.90
for the AK values which are smaller 2BS10
| 2BS11
28.0
28.0
1.78
1.76
115
14.5
168
175
13.2
14.4
than the parameter Ko are made 1 3BS02 34.2 3.06 x l O 7 8.5 175 8.4
negative to plot. The least square 3BS04 34.2 3.00 10.9 141 10.5
3BS0S 34.2 3.17 9.5 3.49 8.8
error method is applied to estimate 3BS06 34.2 3.10 7.9 3.05 6.9
the parameter Ko of 32.6MPa m 1 / 2 3BS07
3BS08
34.2
34.2
3.08
196
10.9
7.1
2.93
115
10.6
6.9
and the standard deviation of 3BS10 34.2 2.99 6.6 135 6.2

exponent m as 0.34. 5R01

SR02
43.5
43.5
5.76 xlO' 7
5.12
9.5
9.1
165
125
9.4
8.4
If m is assumed as a Gaussian 5R03 43.5
43.5
5.74 9.5 164 9.1
1DS02 6.42 7.5 3.03 7.3
random variable with the mean m 1BS04 43.5 6.36 9.2 199 8.6
1BS0S 43.5 6.02 15.1 181 11.1
and the variance G^ to estimate the * mean ofZ(x) = 3.81 xlO6
value of Co as follows.

0.03

0.02

0.01

o.oa 100
log AK (MPaVm)
log AK (MPaVm )
Fi
Fig.2. Relation between the variance of g- 3 - Relation between the standard deviation of
log (da/dN). the logarithm of mean growth rate log AK.

The logarithm of the mean growth rate for specimen i, log(da/dN)i =V[t follows Gaussian
distribution with the mean value,
logCo+(lq-ko), and variance, Gm(ki-ko)2.
Let the data obtained by fatigue tests be VI, V2,..., Vi,..., Vn. The likelihood is

1 " { n ^ l e x p j - i ^ l o g C ^ C V ^ j
L= (12)
Tf2Jto„ l-iVM \ i=i 2(ki-k0)2<£ |
The maximum likelihood of logQ) and m arc
 561

M ,
M Si
1*1 (kj-kp)2 ^i-^oj
logCo= i = l I (13)
MS2- S\
M

i=l ^i-^o (ki-ko)2J

nT= (14)
MS2- S?
where
M M
X
si=y-L- s2=I
M (ki- ko)
2
(15)

The variance of the exponent m, Oft, is

« ivtvi-logCo-mtki-ko)] 2
(16)
^ " M^i=i (ki-ko)2

where, the value of G§i must be the same with that estimated by eq. (10).
Using eqs. (14),(16) and (13), the mean value, the standard deviation of the exponent m
and logQ) are estimated. Obtained values are Ifi =3.2,am=0.34,logCo= 2.01x 10 -7 .

Probability Distribution of the Resistance Coefficient Determining the parameter Ko and the
value of m for each specimen, the parameter C(x) can be obtained by eq.(6) with the computed
growth rate at point x. Since the inverse of C(x) seems better for describing the material
property (Ortiz et al.. 1986: Itagaki et al.. 1989: Itagaki et al.. 1990), z(x)=l/C(x) is used
in the following, and called as growth resistance coefficient.

z(x)=l/C(x)= (AK/Ko)m dN/da (17)

As is seen, the growth resistance coefficient z(x) fluctuates very frequently within the
specimen. The results are summarized in Table 2 (for AK=21.8 and 43.5MPaml/2).

Table 2. Test results (AK= 21.8 and 43.5 MPaml/ 2 ).

specimen AK mean of ^N co.v of JN co.v of z(x)

no. (MPtvra) (m/cyde) (%) (%) •
1BS08 21.8 6.26 xlO* 13.7 3.28 13.8
1BS09 21.8 5.61 15.2 3.55 14.1
1BS10 21.8 5.52 14.6 3.59 14.0
1BS11 21.8 6.58 14.0 3.15 14.6
4BS01 21.8 7.65 15.7 2.78 15.4
4BS02 21.8 7.98 15.1 2.67 15.5
5R01 43.5 5.76 xlO*7 9.5 3.10 9.4
5R02 43.5 5.12 9.1 2.69 83
5R03 43.5 5.74 9.5 3.08 9.0
1BS02 43.5 6.42 7.5 3.47 7.3
IBS 04 43.5 6.36 9.2 3.44 8.5
1BS05 43.5 6.02 15.1 3.25 11.1

a ofz(x) = 4.30x10°
562
All data of z(x) are plotted on the Weibull probability paper, Fig.4. A 3-parameter Weibull
distribution function, Fz( z |a,p,7 ) is used to fit the data. The parameters a ' P and 7 are
estimated by the direct search optimization method (these values are a=3.67,P= 4.47x106, ? =
2.65x106 ). From all data of z(x), the auto-correlation function is determined as shown in
Fig.5. The function, CXP(_ bol x l ) c o s ( 2rcfox )t j s a i s o shown in this figure with the arbitrarily
chosen coefficients.

Weibull distribution
99.9 r "
90.0 h e- b 0l x lcos(27cfox)
bo=0.1,fo=-L
^"[■Kn bo=0.2,fy=-L
ss io.o a=3.66
■a P=4-47xl066
1.0 L 7=2.65xl0 1536 samples

1 2 3 4 5 6 7 8 9 10

Resistance z , 106 Distance x , (xl0_3m)

Fig.4. Probability distribution of z(x) for all data. Fig.5. Auto-correlation function of z(x).

APPLICATION TO RELIABILITY ASSESSMENT

The so determined auto-correlation function, and the probability distribution are used for
reliability assessment withrespectto fatigue crack growth by numerical simulations.
potability distribution determine target power
Simulation of the Crack Qrpwft function of Weibull
random process Z(x)
spectral density function
SK0
To simulate the fatigue crack Fz(*x.P.TD
growth in a specimen, it is necessary zr
to generate a random m and a seriese give initial power
of z(x) along the crack path. For the spectrum, S&(f)

simulation of m, a truncated
Gaussian distribution function (m modification

=3.2,am=0.32) is used (2.0 £ m

^ 4.0 ). A non-Gaussian random simulate Gaussian random spectral
process simulation method proposed process, u(x) Z(x). S«f)
by Shinozuka, et aL is applied for
random process z(x) with the calculate corresponding convert Gaussian random
obtained auto-correlation function, probabilities, FJ(<H)
process u(x) into Weibull
#0
R(x)=exp(- 0.1 |X|)COS(2TIX/64), and
probability distribution function
Pz( z |a,p,7 ) (a=3.66,P=4.47x ; estimate probability distribution of
; growth life and reliability t
6 6
1 0 , 7 = 2 . 6 5 * 1 0 ) . The flowchart of Fig.6. Flowchart of the simulation of random
the simulation of random process process z(x).
z(x) is shown in Fig.6.
 563
Given a initial crack length ao, the relation between the crack length, a, and the number of
cycles, N, can be determined by the simulated data of m and z(x).
In Fig.7, 100 simulated growth curves under constant load amplituds are plotted (ao=30mm,
AP =17.7kN and AP =16.0kN). The experimental data ( Itagaki et al.. 1990 ) are plotted
together in the same figures. The simulated a-N curves are reasonable in comparing with the
experimental data. From these curves the probability distribution of fatigue life can be
estimated.

N (xlO5, cycles ) N (xlO5, cycles )

(a) (b)

Fig.7. a-N curves (AP constant).

CONCLUSION
For the safety evaluation and the reliability assessment of fatigue sensitive structures, not
only mean and variance of fatigue life but also the probability distribution is necessary. In this
study, a method is proposed to determine the distribution function of the fatigue crack growth
life from a small number of tests and numerical simulations. The Paris law,da/dN=C(AK/Kq)m,
is used, where the parameters C and m are treated as random variables. Several possible
assumptions with the parameters C and m are made and checked by observing the variance of
the crack growth rate. It is assumed that the variation of the crack growth rate consists of a
very small interval fluctuation due to C and a gradual and long range variation due to m,
which leads to the postulation that the mean of logC over a specimen is approximately same
for all tests and the value of m is almost constant within a specimen, but differs from specimen
to specimen.
Using the proposed model, the data obtained by stress-intensity-factor-controlled fatigue
crack growth tests are analyzed. The results of the statistical analysis show that the parameter
Ko can be easily determined experimentally, and the parameters C and m can be analyzed
separately with the above assumption.
The probability distribution functions of material parameters, z=l/C and m, and the auto-
correlation function of z are estimated from the experimental data of a high tensile strength
steel. It is shown that the distribution of the parameter, m, is approximately normal and
that of z is a 3-parameter Weibull.
For the simulation of the fatigue crack growth, the non-Gaussian random process
simulation method proposed by Shinozuka, et al. is applied for random process z(x)
with the obtained auto - correlation function and probability distribution function, and a
truncated Gaussian distribution function is used for m. The probability distribution of the
564

fatigue crack length after a given number of load cycles or that of the number of load cycles
for a crack to reach a given length can be estimated by repeating such simulations.
The merit of the proposed method is that only a small number of tests are required to
estimate the probability distribution function of fatigue crack growth life.
Since the interval of the data acquisition along the crack path is determined by the accuracy
of the experimental technique,the size of the crack to which this method is applicable is limited.
In this research, a large crack growth of the order of millimeter or centimeter is considered.

ACKNOWLEDGMENT

The authors acknowledge the discussion given by the members of the reliability
committee of the Society of Materials Science of Japan and also of the material research
committee of the Society of Naval Architects of Japan.

REFERENCES

Fujii, S., Nakagawa,T. and Hasimoto, K. (1979). Journal of JSME (A), 45-393,, 516. (in
Japanese).
Ichikawa, M. and Nakamura, T. (1985). Materials ,Vol.34, No.378, 321. (in Japanese)
Ichikawa, M.,Hamaguchi, M. and Nakamura T. (1984). Materials, Vol.33, No.364, 8. (in
Japanese).
Ishikawa,H. and Tsurui, A. (1984). Journal of JSME, 50-454, 1309. (in Japanese).
Itagaki, H., Ishizuka, T., Huang P. and Ueki, S. (1988). INALCO'88 Organizing
Committee, Tokyo, 3-38.
Itagaki, H., Ishizuka, T. and Huang P. (1988). ICAEM, Tianjin, China, F24.
Itagaki,H. and Shinozuka,M. (1972). Special Technical Publication 511 ASTM, 168.
Itagaki, H., Ishizuka, T. and Huang Peiyan (1989). Journal of the Society of Naval Architects
of Japan, Vol.165 , 253. (in Japanese).
Itagaki, H., Ishizuka, T., Huang P. (1990). Journal of JSME (A),Vol.56,No.252, (in
Japanese).
Kanazawa, T., Itagaki, H., Machida S. and Kawamoto, Y. (1979). Journal of the Society of
Naval Architects of Japan, Vol.146, 444. (in Japanese).
Keith Ortiz, Chieh Julius Kung and Horng-linn Perng (1988). Probabilistic Methods, ASCE,
21.
Kimura, Y. and Kunio, T. (1983). Materials, Vol.32, No.361,, 1144. (in Japanese).
Kitagawa,H., KwonJD., Nakasone,Y. and Shimazaki,T. (1986). Journal of JSME(A),
52- 480„1749. (in Japanese).
Kozin,F. and BogdanoffJ.L. (1981). Eng. Fract. Mech.,14, ,59.
Lin, Y. K., and Yang, J. N. (1983). Eng. Fract. Mechs., 18-2, 243.
Lin,Y.K. and YangJ.N. (1985). AIAA Journal, 23-1, ,117.
Ortiz,K. and Kiremidjian,A.S., Eng. Fract. Mech., 24-5,(1986),657.
Okamura,H., Watanabe,K. and Naito,Y. (1975). Reliability Approach in structural
Engineering (A. M. Freudenthal et al.), 243,Maruzen.
Paris, P. C. and Erdogan, F. (1963), Trans. ASME J. Basic Eng. 85, , 528.Sakai, T. and
Tanaka, T. (1979). Materials, Vol.28, No.312, 880. (in Japanese).
Tanaka,S., Ichikawa,M. and Akita,S. (1981). Int. J. Fracture, 17,R121.
Tanaka,T. and Sakai,T. (1979). Materials, Vol.28, 92. (in Japanese).
Wu,W.F. (1986). Prob. Eng. Mech. 1(4), 224.
Yamazaki, F. and Shinozuka, M., Stochastic Mechanics, 1, (1986), 211.
WS3a2

Estimating the Statistical Properties of

Fatigue Crack Growth
Using Spectral Analysis Technique

Tetsuya SASAKI
Graduate School, Department of Mechanical Engineering, University of Tokyo
7-3-1, Hongo, Bunkyo-ku, Tokyo 113 JAPAN

Shinsuke SAKAI and Hiroyuki OKAMURA

Department of Mechanical Engineering, University of Tokyo
7-3-1, Hongo, Bunkyo-ku, Tokyo 113 JAPAN

ABSTRACT
This paper presents a new stochastic model which treats the material's resistance against fatigue
crack growth as a spatial stochastic process evolving along the path of the crack. To obtain the
stochastic properties of the fatigue crack propagation process, constant AK tests were conducted
on several AK levels, and the parameters of the model were calculated by a spectral analysis
using the maximum entropy method (MEM), which accounts for the statistical correlation that
has been observed between adjacent fatigue crack growth rates. Using a proposed random crack
propagation model, Monte-Carlo simulations were also performed and satisfactory agreement
with the results of experiments were obtained.

KEYWORDS
Fatigue, Crack Propagation, Structural Reliability, Statistical Treatment, Spectral Analysis,
Distribution of Crack Propagation Fatigue Life, Random Crack Propagation Resistance

INTRODUCTION
The statistical properties of the distribution of crack propagation fatigue life are often needed for
structural reliability analysis based on fracture mechanics. Generally, many crack propagation
tests are required to obtain its statistical properties. However, the statistical characteristics can
be obtained with far fewer crack propagation tests, if the variability of the crack propagation
fatigue life is mainly due to the random nature of the crack propagation process. But we have
only limited information about the actual stochastic properties of fatigue crack propagation
process.

In this paper, the crack propagation resistance is treated as the randomly varying material

565
566
property. To obtain the stochastic properties of random crack propagation resistance, constant
AK fatigue crack growth tests were conducted on several AK levels. The stochastic properties
of crack propagation resistance were estimated using spectral analysis technique. To verify
the estimation, Monte-Carlo simulations were also performed and satisfactory agreements were
obtained.

FORMULATION OF THE STOCHASTIC MODEL

Deterministic models for fatigue crack propagation based upon the principles of fracture me-
chanics are generally of the form

± = Q(AK,R), (1)

where a = deterministic crack size, N = number of cycles, Q = non-negative function, AK =

the stress intensity factor range, R = the stress ratio.

In order to account for the random nature of crack growth, we suggest the following model for
deterministic loadings

± = ±Q(*K,R), (2)
where Z is random crack propagation resistance and a non-negative spatial stochastic process.
In this manner, the reciprocal of the growth rate, dN/da, is treated as the randomly varying
material property, rather than da/dN (Ortiz and Kiremidjian, 1986).

Because the stochastic properties of Z depends on the plastic zone size in front of the crack tip,
it can be evaluated not by AK increasing tests but by constant AK tests. In this way, Z will
be a stationary process, and the stochastic properties of dN/da are equivalent to that of Z. A
stationary process can be supposed to be ergodic, thus the ensemble mean E(Z) and the spatial
mean ~Z are standardized by definition as

E{Z) = Z = 1. (3)

ANALYTICAL PROCEDURE
In order to perform a spectral analysis, Z should be recorded at n points, spaced at equal
increments, Aa. Z&a>i is average crack growth resistance over the ith increment. The subscript,
Aa indicates the length over which the process is averaged. Consider the residuals of Z^a>i from

CAa.i = ZAa>i - 1. (4)

The discrete power spectral density function (P.S.D.) P<A#it and the discrete auto-correlation
function (A.C.F.) R^AmtL can be evaluated using the formula

(5)
Ma=)-v|S<~«>(-^)f
1 n~*
^a..L (* A a ) = ■—£ ^2 CAa,.CAo,i+*, (6)
 567
where ; = imaginary number, ib = lag number, L = nAo (total sampling length). To compute
eqn (5) effectively, the fast Fourier transform (FFT) is often used.

The discrete P.S.D. evaluated from eqn (5) includes the sampling effect which is written as

PU., = GU;Aa,L)P( =1-JSF [l - 1 - ^ r ] P(, (7)

where G - sampling effect filter (see Fig. 1), P c = true P.S.D., / = spatial frequency (Smith,
1962).

Though the F F T method evaluates the P.S.D. effectively, the maximum entropy method (MEM)
is better for the evaluation of the low frequency component of the spectral (Rodoski et a/., 1975)
which plays an important role for the stochastic analysis later.

EXPERIMENTAL PROCEDURE
Materials used in this study are SUS304 and Cr-Mo-V casting steel. Chemical composition and
mechanical properties are summarized in Tables 1 and 2. Specimen geometry is ASTM standard
compact tension type, with a width W = 50 mm and a thickness B = 12 mm. Specimens were
side grooved with an included angle of 60 deg. Side grooves which resulted in 25 % reduction
in thickness were used.

Constant AK tests were done using a personal computer-based testing system designed to be
used with a standard servo-hydraulic test frame. Fig. 2 shows the schematic diagram of testing
system.

Tests were run at stress intensity ranges of 12, 15, 18, 21 MPav/m. They are within the region
of stage 2 fatigue crack growth. 12 specimens were used for each material at AK = 15 MPaVm
and 1 specimen at other AK levels. All the tests were carried out at R = 0.1 in air at 15 Hz.
The accumulated number of cycles were recorded for each 0.20 mm of crack growth (Aa = 0.20
mm).

RESULTS AND DISCUSSIONS

Results

Effective R a n g e of D a t a The following analyses are performed using the data where Z is
considered to be stationary: 0.36 < a/W < 0.56 for Cr-Mo-V, 0.44 < a/W < 0.56 for SUS304.

Crack Growth Curves Fig. 3 shows the crack growth curves for 12 replicate tests at AK
= 15 MPax/m. It is apparent that the variability of crack growth depends on materials even
under the same condition.

Distribution of Z Sample data of Z at AK = 15 MPay'm was plotted on the log-normal

probability paper as shown in Fig. 4. It is quite apparent that log-normal distribution provides
a good fit. The same distribution also provides a good fit for Z at other AK levels.

Spectral Analysis of Z First, the P.S.D. of the residuals of Z is computed by taking the
Fourier transform of each test records, eqn (5). Next, the individual spectra are combined to find
the ensemble average spectrum, as shown in Fig. 5. It is apparent that the low frequency region
568
of the P.S.D. cannot be evaluated because of the sampling effect. Thus, the MEM is also used
for the evaluation of that region. The ensemble A.C.F. of the residuals of Z can be evaluated
by eqn (6) and is shown in Fig. 6. According to Figs 5 and 6, Z will be approximated by the
mixture of a first-order Markov process and a white noise process. The P.S.D. of a first-order
Markov process, PM, and the A.C.F., RM are given by
(8)
*w-=£?£*
RM(a) = fa exp(-c*Af a), (9)
and the P.S.D. of a white noise process, JV, and the A.C.F., Rw are given by

Pw(f)=fa (10)
Rw(a) = fa6(a), (11)

where 6 = Dirac's delta function.

The parameters of eqns (8) ~ (11) can be evaluated from the experimental data for 12 specimens
at AK - 15 MPaVm:

aM = 5 x 10m"1 fa = 4x 10"3 fa = bx 1(T7 for SUS304;

1 2
aM = 3 x 10m" fa = 2 x 10~ fa = 1 x 10"6 for Cr-Mo-V.

These parameters also provides a good fit for other AK levels (12, 18, 21 MPaVm).

Numerical Simulations of Z

To confirm the adequacy of the approximation of stochastic properties of Z, a Monte-Carlo

prediction scheme was used. The digital generation of sample functions of log-normal stochastic
process, eqns (8) and (10) are readily computed with the aid of the FFT algorithm (Yamazaki and
Shinozuka, 1988). Using the parameters evaluated from the experiment, numerical simulations
were conducted under the same conditions with the experiments at AK = 15 MPa^/m. The
ensemble P.S.D. computed with the results of simulations are also shown in Fig. 5. It is
apparent that the mixture of a first-order Markov process and a white noise process provides
a good fit. The simulated crack growth curves are shown in Fig. 7. They are very similar to
the experimental ones shown in Fig. 3. The coefficient of variation of simulated fatigue crack
propagation life also provides a good agreement with the experimental one.

CONCLUSIONS
The conclusions developed from this study can be summarized as follows:
(l)Fatigue crack growth resistance, Z is approximated by the mixture of a first-order Markov
process and a white noise process;
(2)The log-normal distribution provides a good fit for Z;
(3)The statistical properties of Z is independent of AK within the region of stage 2 fatigue crack
growth.

REFERENCES
Ortiz, K. and A. S. Kiremidjian (1986). Time series analysis of fatigue crack growth rate data,
Eng. Fract. Mech., 24, 657-375.
 569
Rodoski, H. R., P. F. Fourgere and E. J. Zawalick (1975). A comparison of power spectral
estimates and applications of the maximum entropy method, J. Geophy. Res., 80, 619-
625.
Smith, F. B. (1962). The effect of sampling and averaging on the spectrum of turbulence, Quart.
J. Roy. Meteorological Soc, 88-376.
Yamazaki, F. and M. Shinozuka (1988). Digital generations of non-Gaussian stochastic fields,
J. Eng. Mech., ASCE, 114, 1183-1197.

1.0 " T O ^ e J ^ I 1 1 1 1 1 1
S t r ani A a.p
1 2 Btl AD /
C o n v e rrt e c=> 1 6 Btl
0.8 T P e r s o nl a
C o m p urt e
Load C el l
Paralle
<0=s> w i th FP
U
\ . -
Iprogramnc b k_
l
0.6
j f O ^ For Cr-Mo-V
t I C oni Amp
. ~ I /O

o 1
, T .
> | s t rr aAl » P|
0.4 I For SUS304
- o S t r ani
1 2 0 t1 D/
A
C o n v e rrt e <=>
C \^.
Spe
0.2 Applicatio
n
A c t u n tr o . k- n e nl Tim e
0.0 f i . . _J 1
t M o n i tro
0 500 1000 1500 2000 Serv
o V o l v c HH
—Sj e rov U nti 1 MS-DO
S

Spatial frequency, m -1 ? A m p l i t ue d
1 S e rov Amp
. 1 ( Z)
F u n c t ino
- J __ + XY/10.Z
«-iii-
Fig.l S a m p l i n g effect filter.

Fig.2 Schematic diagram of test system.

Table 1 Chemical composition of the

material used (wt. % ) .

M a t e r i al C Si Mo P S Hi Cr Mo

SUS304 0.05 0.50 1.21 0.030 0.003 8.26 18.10

/
Cr-Mo-V 0.17 0.38 0.67 0 . 0 12 0.007 0.15 1 . 28 1.02

As V Sn Sb

0.010 0. 19 0.026 0.004

Table 2 Mechanical properties of the

material used.

M a t e r i al Y i e l d p o i nt T e n s i le strength E l o n g a t i on
(MPa) (MPa) (X) Fig.3 Crack growth for 12 replicate tests.
SUS304 266 679 56
Cr-Mo-V 466 637 19
570

X10"
~l i i i i i i i r~
Cr-Mo-V
AK=l5MP<iJfii

0.00 1.00 2.00 3.00 4.00 5.00

Spatial lag, m XI 0 " 3
Fig.4 Distribution of Z (log-normal
probability paper). xi o-
4.00
SUS304
AAr=15MPav/m

X I 0"
1.00 — 1 1 1 1 1— i—i—r - i
1
\ 4
1
Cr-Mo-V
0.80 AA,=15MPa>/m

0.60
"XFFT
[11\ Experiment 1 0.00 1.00 2.00
-I
3.00
I I
4.00
L_
5.00
UU Simulation - Spatial lag, m XI 0 " 3
0.40 T l \ \ -
1 1 \V MEM
/ - Fig.6 Auto-correlation function of Z
0.20
yr for ensemble(AA'=15MPa v /m).
0.00 l i i r "i . J1 1 1 1 L.

500 1000 1500 2000 2500

Spatial frequency, m _ 1

X I 0"8
1 1 — 1 I 1 1 1 1 1
2.00
N ^ ^ - v MEM SUS304 A
- ^ \ , A/C=15MPay5i
1.60

1.20 p/j \
\ll \
KV Experiment
.• Simulation U
f v
\ s
-
-
0.80

0.40 -
f i f*V I 1 1 __J 1 L_
0.00 500 1000 1500 2000 2500 15MPav/I5 "J
0.00
Spatial frequency, m-1 0.00 0.20 0.40 0.60 0.60 1.00
Load cycle XI 0 8
Fig.5 Power spectrum density of Z
for ensemble(A/C=15MPa>/m).
Fig.7 Crack growth for 12 replicate
simulation.
WS3a3

C O M P A R I S O N OF SOME PROBABILISTIC MODELS I N T H E

D U R A B I L I T Y ANALYSIS OF FATIGUE CRACK G R O W T H

Wen-Fang Wu
Department of Mechanical Engineering, National Taiwan University,
Sec. 4, Roosevelt Road, Taipei 10764, TAIWAN

ABSTRACT

Three probabilistic models describing the random fatigue crack growth and predicting its
corresponding durability are discussed in this paper. The first is a simple randomization
of Paris-Erdogan equation, the second a discrete Markov chain model and the third is
a Poisson process model. To examine the applicability and superiority of these models,
numerical examples are performed over experimentally obtained fatigue crack growth
data of twenty center cracked APFH 60 high tensile steel specimens. It is concluded
that all three models give us satisfactory results in the present study.

KEYWORDS

Probabilistic model; fatigue crack growth; durability; Markov chain; Poisson process.

INTRODUCTION

In the earlier stage of applying probabilistic method in the fatigue analyses, the atten-
tion was focused on the statistical treatment of fatigue data alone. Recently, in order to
gather more information than the usual statistical treatment, additional physical argu-
ments are incorporated into the probabilistic analyses of observed fatigue data. These
analyses may be classified into two groups, the first of them uses a model based on
the randomization of Paris-Erdogan's crack growth law and the second group utilizes a
model considering the continuous damage accumulation during the fatigue crack growth
instead of using Paris-Erdogan's law. Among many recent publications related to the
probabilistic or stochastic analysis of fatigue crack growth, Lin and Yang's (1983, 1985),
Tsurui and Ishikawa's (1984, 1985), Sobczyk's (1986), and Ihara and Misawa's (1988)
works all belong to the first group, while Bogdanoff and Kozin's works (1978, 1983) fall
into the second group. Since both Lin/Yang's and Bogdanoff/Kozin's models are based

571
572
on Markov theory, they should share some common advantages as well as shortcomings.
While in comparing several Markov approximations for the fatigue crack growth prob-
lems, Wu (1986) concluded that a transformed Poisson process model is in fact parallel
to both Lin/Yang's continuous Markov process model and Bogdanoff/Kozin's discrete
Markov chain model.

Many articles and examples have been published based on Lin/Yang's stochastic fatigue
crack growth model or other similar approaches. Likewise, Bogdanoff and Kozin have
also written many articles concerning the use of their Markov chain model. However,
to the best of the writer's knowledge, there are no article comparing the result from
applying both models separately to the same set of data. It is therefore the intent of
this article to apply different probabilistic fatigue crack growth models to the same data
set and make comparisons on the results.

PROBABILISTIC CRACK G R O W T H E Q U A T I O N

Using a linear elastic fracture mechanics approach, the fatigue crack growth rate can
frequently be described by the following Paris-Erdogan equation,

£ = C(AKr (1)

in which a is the crack size or half crack size, n is the stress cycle, C and m are material
constants, and AK is the stress intensity factor range defined as AK = Y(a)Acry/na
where ACT is the stress range and Y(a) is a geometric factor which will be assumed to
be one in the present analysis. From Eq. (1), the crack size after n stress cycles can be
obtained. Numerous experimental results show that even in well-controlled laboratory
conditions, the fatigue crack growth will produce considerable statistical dispersion.
In these experiments, according to Eq. (1), the only non-deterministic factor seems to
be C. Many attempts are therefore made to randomize C to produce sample fatigue
growth curves similar to those experimentally obtained. In this respect, C has been
considered as a random variable (Yang et a/., 1983), a random process (Lin and Yang,
1985), a stochastic field (Ishikawa and Tsurui, 1984; Tsurui and Ishikawa, 1985), or a
combination of those mentioned above.

For the simplest case, if C is considered a random variable, then the probability distribu-
tion of crack size at a given cycle n can easily be obtained once we know the probability
density of C. In the reliability analysis of fatigue crack growth, we may prescribe a
given critical crack size and find the reliability as the probability of the crack size not
exceeding the prescribed critical crack size. Accordingly, the knowledge of probability
density function of random cycles n to reach a given crack size may be important to a
designer. If we assume that C can be fitted from experimental data to be a log-normal
distribution, the probability density function of n to reach a can then be found as

fI l 1 / Hn-(logA-C')Y\
f {n) = p (2)
" v^°* \ s? 1
in which C* and a* are mean and standard deviation of C* = logC, and A is defined
as A = 2 (a1-™I2 - a j " m / 2 ) / (2 - m) (Aa)m %m'2 with OQ the initial crack size.
 573

The above discussion describes a very simple way to randomize Paris-Erdogan equation
in order to take into consideration the scattering behavior of the fatigue crack growth.
In some cases, the simple model is good enough to represent the experimental result.
In other cases, it may not be accurate enough for the representation of the real fatigue
crack growth. We will have to use a more complicated probabilistic model and the
analysis becomes much more involved although the basic idea is in fact the same.

B-MODEL

In a series of papers by Bogdanoff and Kozin, the Markov chain model is used extensively
to described the probabilistic behavior of the cumulative damage of fatigue failure,
fatigue crack growth and wear. Since the model was first proposed by Bogdanoff, it is
also recognized as B-model. In the B-model, a duty cycle (DC) is a repetitive period
of operation in the life of a component during which damage accumulates following the
Markov chain theory. Let the finite (discrete) damage states be denoted by { 1 , 2 , . . . , 6}
where 6 denotes failure, and let the discrete time be nd = 0 , 1 , 2 , . . . which are measured
in numbers of D C s and are irrespective of their durations. For a damage index D, the
random variable Dni denotes the damage state occupied at time nd with Prob[Dnd =
il = P»«0')- T h e (! x b) r o w v e c t o r Pnd = {p n <(l),p n<[ (2),...,p n<( (&)} denotes the
probability distribution of Dnd. An initial probability distribution of damage at the
beginning of the observation should be given and denoted by p 0 = {ni ,7r 2 ,..., 7rb_ x , irb}
and J^ x 7Ty = 1 where nb = 0 if no failed item is assumed to be put into service at
the beginning. For the fatigue crack growth problem, if the initial crack size is given
deterministically, consequently 7Ty = 0 for all j except that ^ = 1. For each constant
severity DC, the evolution of damage is characterized by a probability transition matrix
P with probability p3 of staying in the current state and probability q3 = 1 — p y of
going to the neighboring right state. This transition matrix has 6 — 1 state dependent
transition states, one absorbing state, and only unit-jumps in damage are permitted.
The unit-jump restriction can be lifted to make the transition matrix more complicated.
Moreover, if P is set to be time dependent, the damage model becomes a nonstationary
one.

It follows from Markov chain theory that p n d = p 0 P n * = p n<i _ X P. From this equation,
the distribution function of time to failure, the reliability and the hazard rate can all
be calculated accordingly. Of special interest is the cumulative distribution function of
DC nd to reach a given state j , which is derived analytically as

*.,„„-{a,-.<.-y*v-. «#;•_, (3)

In applying the above equation, the number of total states 6 and values of p and q are
determined from experimental data according to
6 = 1 + 1
^ % - ' r-*--**- ) (4)

where py is assumed to be constant and r = p / ( l — p). The mean failure time m and
its standard deviation b are obtained experimentally. It is noted that Eqs. (3) and (4)
can be replaced by their continuous equivalents for simplicity.
574

P O I S S O N MODEL

It is well-known that the mean of a Poisson process is equal to its variance at any time
of consideration. Statistical results from the fatigue crack experimental data indicate
that the growth behavior may be far from being able to be approximated by a Pois-
son process. Nevertheless, we can try applying a linear transformation to a certain
measurable quantity and it may result in a Poisson process. Before pursuing this any
further, the crack size a will be considered as the independent variable hereafter, while
the number of duty cycle n will be the dependent variable during the fatigue crack
growth. The rationale behind these assumptions are that a) the crack size a in reality
grows continuously while the duty cycle n is counted discretely; b) the divergence of
the Markov process can be avoided; and c) treating a as independent variable and n as
dependent variable is more consistent with many real fatigue crack growths according
to Kozin and Bogdanoff (1983).

From statistical analysis of experimental data, although n(a) cannot be approximated

by a Poisson process, there may be a linear transformation nt = ^n which makes nt(a)
closer to a Poisson process. Using the least squared-error technique, the optimal value
of 7 for the best approximation of nt (a) by a Poisson process can easily be found as

3E:J x As.-m.-a? ± y/(3z:°fc»M?)a- s (E:° M?) (E:° KM*)

1 = (5)
4£. n o *.-*?

where rajs and d[s are estimated means and standard deviations obtained from exper-
imental data, k[s are weights and n0 is the number of observed data points. If the
approximation of nt (a) by a Poisson process is considered acceptable, many probabilis-
tic descriptions related to the Poisson process can then be easily determined which can
be further transformed to represent the original fatigue crack growth. For example, the
probability distribution function of random number of cycle to reach a specified crack

Hin)
m a
Fnt[nt;mnt(a)}= £ «—.<«> 'nti ) (6)

where mnt (a) is the transformed mean curve and I (in) denotes the nearest integer of
in. The probability distribution function of the crack size a at cycle number nt, hence
n, can be calculated from the waiting time distribution of the Poisson process nt (a) as

,-mnt(a) I nn»]/(7n)-1 dmnt(a)

da
Fn« (7)
J a0 Mm) -1]! da

The crack exceedance curve, i.e. the probability of crack size to exceed a at a prescribed
time, F* (a), is then calculated as F* (a) = 1 — Fn (a). We can also use the present Poisson
process model to generate sample crack growth curves which are statistically consistent
with the experimentally obtained data.
 575

A P P L I C A T I O N A N D COMPARISON

To apply the three models discussed, experimental data for the fatigue crack growth
of a high tensile strength steel APFH 60 are studied in the present section. The data
set was obtained by Shimada, Nakagawa and Tokuno (1984). From the experimen-
tal result, the mean values and standard deviations of the number of cycles to reach
crack length 4.0, 4.5, 5.0, 6.0, 7.0, 8.0, 9.0 and 10.0 mm were calculated. As it has
been discussed in Shimada, Nakagawa and Tokuno (1984) that a simple randomization
of Paris-Erdogan equation resulted in moderately good approximation for the fatigue
growth data. However, the intermingling behavior of real fatigue crack growth curves
cannot be reproduced by just treating constant C in Eq. (1) as a random variable. A
more adequate approximation is therefore needed. In the present study, the B-model is
applied to the present data set. Each duty cycle is selected to be nd = 4000n where n is
the real number of stress cycles. If the critical failure crack size is selected to be 10 mm,
according to Eq. (4), the number of states to failure is found to be 26, and p and q are
found to be 0.444 and 0.556, respectively. After the needed parametric values are eval-
uated, the stationary Markov chain B-model is completely established. Using Eq. (3),
the cumulative distribution function of random time to failure or to reach a given crack
size can be evaluated easily. The crack exceedance curve can also be calculated from
Eq. (3).

The Poisson crack growth model is also applied to the present data set. From exper-
imental result and Eq. (5), it is found that 7 = 0.304. The probability distribution
function of random cycles to failure and to reach a given crack size can be calculated
from Eq. (7). The result for the distribution function of cycles to reach a = 7 mm is
shown in Fig. 1 in solid curve, the result from B-model is also plotted and denoted by
circles which is similar to the formal. Crack exceedance curves at n = 120,000 cycles
are also plotted in Fig. 1 in dashed curve and triangles representing Poisson process
result and B-model result respectively. The agreement, however, is not as good as those
probability distribution functions of random cycles to reach prescribed crack sizes.

Finally, simulation results for twenty crack growth sample functions are shown in Fig. 2
which are generated using Poisson process model. They have similar shapes as those
of experimental results. The intermingling behavior in many real fatigue crack growth
curves is also found in this figure. However, the simulation result does have some
deviation from the experimental crack growth curves due to the fact that the optimal
transformed factor 7 is not small enough. Although the model can preserve the entire
real crack growth tendency as well as the real crack growth behavior at those fitted
observation points, it may not be able to reproduce the crack behavior in the entire
cyclic range. This shortcoming may be overcome by either using a more complicated
nonhomogeneous birth process model or applying a nonstationary B-model.

CONCLUSION

Through the numerical study it is concluded that the simple probabilistic fatigue crack
growth model usually leads to moderately satisfactory result while the B-model and
Poisson model have better outcomes. Further comparison between the latter two models
576
shows that they both lead to almost the same degree of satisfaction. Since each of
these two models has its own advantages and shortcomings, a solid conclusion on the
superiority between them is still open for further research. The decision of which method
to use therefore depends on real life environments and the user's preference.

Crock S i z e , mm
6 7

100 125 150 175 200 225 50 100 150 200 250 300
T h o u s a n d Cycles T h o u s a n d Cycles

Fig. 1. Distribution function of cycles Fig. 2. Simulated crack growth curves.

and crack exceedance curve

REFERENCES
Bogdanoff, J. L. (1978). A new cumulative damage model, part 1. J. Appl. Mech.,
ASME, 45, 246-250.
Ihara, C. and T. Misawa (1988). A stochastic model for fatigue crack propagation with
random propagation resistance. Eng. Fract. Mech., 31, 95-104.
Ishikawa, H. and A. Tsurui (1984). A stochastic model of fatigue crack growth in
consideration of random propagation resistance. JSME Trans., 50, 1309-1315. (in
Japanese).
Kozin, F. and J. L. Bogdanoff (1983). On the probabilistic modeling of fatigue crack
growth. Eng. Fract. Mech., 18, 271-293.
Lin, Y. K. and J. N. Yang (1985). A stochastic theory of fatigue crack propagation.
AIAA J., 23, 117-124.
Shimada, Y., T. Nakagawa and H. Tokuno (1984). Reliability analysis of fatigue
crack propagation life by Markov chain. J. Soc. Mat. Set., Japan, 33, 105-111. (in
Japanese).
Sobczyk, K. (1986). Modelling of random fatigue crack growth. Eng. Fract. Mech., 24,
609-623.
Tsurui, A. and H. Ishikawa (1985). On the reliability degradation of fatigue crack prop-
agation. JSME Trans., 51, 17-22. (in Japanese).
Wu, W. F. (1986). On the Markov approximation of fatigue crack growth. Prob. Eng.
Mech., 1, 224-233.
Yang, J. N., G. C. Saliver and C. G. Annis, Jr. (1983). Statistical modeling of fatigue
crack growth in a nikel-based superalloy. Eng. Fract. Mech., 18, 257-270.
WS3a4
FATIGUE LIFE DISTRIBUTION ANALYSIS OF GFRP IN CONSIDERATION OF
SPATIALLY DISTRIBUTED RANDOM CRACK PROPAGATION RESISTANCE

Hiroshi Ishikawa*, Toshio Tanimoto**, Hidetoshi Ishikawa*** and Hitoshi Inomo***

* Department of Information Science, Kagawa University

2-1 Saiwai-cho, Takamatsu-shi, Kagawa 760 JAPAN
** Department of Materials Science and Ceramic Technology
Shounan Institute of Technology,
1-1-25 Tujido-Nishikaigan, Fujisawa-shi, Kanagawa 251 JAPAN
*** Department of Information Systems, Kagawa College of Technology
3202 Gunge-cho, Marugame-shi, Kagawa 763 JAPAN

ABSTRACT

The present paper deals with fatigue life distribution analysis of GFRP in considera-
tion of spatially distributed random propagation resistance utilizing the Tsurui-Ishikawa's
stochastic crack growth model. At least 20 replication tests under constant stress ampli-
tude are first performed at each stress level of four different levels to empirically char-
acterize the scatter in the number of cycles to failure. Then, the effect of random crack
propagation resistance in GFRP on the crack propagation life distribution is clarified,
and the statistical properties of the fatigue crack process for GFRP material is also in-
vestigated. Finally, discussions are made on the pertinent method for the quantitative
prediction of fatigue life of GFRP, which becomes undoubtedly of vital importance in the
reliability-based design and the reliable utilization of this material.

KEYWORDS

Probabilistic Fracture Mechanics, Tsurui-Ishikawa's Model, Random Crack Propagation

Resistance, Crack Length Distribution, Fatigue Life Distribution, GFRP.

INTRODUCTION

It is well known that the fatigue crack growth process is associated with various uncertain-
ties (Ishikawa et a/., 1984, 1989; Tsurui et a/., 1985, 1986). Among these uncertainties, in
particular, it becomes of vital importance to clarify the effect of random crack propaga-
tion resistance in the material on the temporal variation of the crack length distribution
and consequently, on the crack propagation life distribution, since actual materials used
in structural components will inevitably involve, to a degree, non-homogeneous micro-
structures which will tend to cause spatial randomness of the propagation resistance. In
this connection, Tsurui and Ishikawa have derived a generalized Fokker-Planck equation
to describe the temporal variation of the crack length distribution for locally stationary
random load and locally stationary random propagation rresistance, and then solved the
equation in a closed form to obtain a useful residual life distribution, which is termed as
the Tsurui-Ishikawa's model (Ishikawa et a/., 1984; Tsurui et a/., 1985).

577
578
On the other hand, composite materials have been extensively used as one of the main
structural components and, hence, the distribution analysis of their fatigue strength or
fatigue life becomes of crucial significance. Unfortunately, however, there are quite few
papers to date which deals directly with this theme on F R P in comparison to metals. In
this respect, the present paper proposes a useful method to perform fatigue life distribution
analysis of G F R P in consideration of spatially distributed r a n d o m crack propagation
resistance with the aid of the aforementioned Tsurui-Ishikawa's model.

S P E C I M E N P R E P A R A T I O N AND T E S T I N G P R O C E D U R E S

The material used consists of polyester resin as matrix and satin woven glass cloth as
reinforcement. T h e composition of the material is shown in Table 1. In Table 2, the
glass fiber content of the specimen and its mechanical properties are shown. T h e shape
and dimension of the specimen is shown in Fig.l. T h e material was fabricated by means
of a hand-lay-up method and was cut and machined into the specimen, in the direction
pararell to the warp of glass fabric.

Table 1. Material of the specimen. Table 2. Glass fiber content of the specimen
and its static properties

Matrix Polyester resin Weight content Wg 54.47 %

(polylite FG - 284)
Reinforcement Satin woven glass cloth Volume content Vg 35.78 %
(SLS-212)
Catalizer Methyl ethyl keton per oxid Tensile strength at 294.2 MPa
Hardener Cobalt naphthenate Bending strength ab 394.2 MPa
0.6%solution

_*e_
3U3
£ *=W
JQ3_
Unit : mm
Fig. 1. Fatigue test specimen.

Specimens were then kept for more than 48 hours under constant conditions of 23 ± 1°C
and 65 ± 5 % humidity. T h e fatigue test was conducted under the constant condition of
20°C all day long in the testing room at a speed of 3600 r.p.m. by using the rotating
bending fatigue testing machine, paying a particular attention both to the vibration of
the specimen and to the moment arm. At least 20 replication tests for each stress level
were performed in order both t o evaluate the scatter in the fatigue life on an empirical
basis and to compare with theoretical distribution.

S T O C H A S T I C FATIGUE CRACK G R O W T H MODEL IN

CONSIDERATION O F RANDOM PROPAGATION RESISTANCE

T h e Tsurui-Ishikawa's model utilized in the present study assumes the following stochastic
differential equation (1), as a natural extension of the Paris-Erdogan's crack growth law
(Eq.(2)), in the case of random propagation resistance a n d / o r random applied load:

dX/dn = eCnZ*x+VXx+1 (1) da/dn = C {AK)m (2)

 579
where a represents the crack length after n cycles of loading, X = a/ao the non-dimensional
crack length, C, m and € material constants, AK the stress intensity factor range, and
Cn and Zn are both the non-dimensional locally stationary random crack propagation
resistance and the stress amplitude. Based upon the comparison between Eqs.(l) and
(2), the following relationship is provided:

e = (C/oo)(5 0 v^^) m (3) A = m/2-l (4)

where a0 and s 0 are both normalization constants for crack length and stress amplitude,
respectively. The non-negative constant A in Eq.(4) is introduced in place of m.

As described in detail in the references (Ishikawa et a/., 1984; Tsurui et a/., 1985), the
residual life distribution H(n\x0i xc) of the number of cycles for a crack to propagate from
its initial length x0 to the length xc for the first time is given analytically with the aid of
Markov approximation method. When the applied load is deterministic with a constant
amplitude of ZQ = SQ/S0, the residual life distribution can be given as

r*-*-*-AeZ; 3&
2A+1
X^a {*o< > - (*0-* - XeZ^^E[Cn)nf^1)/X] /(2A + 1) j

H(n\x0, xc) = I ( in case of x^x > AcZj(A+1)E[Cm]n) (5)

f |x^^-AgZn^>E[C7.]n
A ^ o ( 2 A + 1 ) / ( 2 A + l)

(otherwise)

in which $ is the complementary function of the standardized normal distribution func-

tion and a is a parameter left unknown.

Although Eq.(5) contains E[Cn] and a as unknown parameters, E[Cn] is the quantity of
order one, independent of the number of cycles n. Hence, the constant e can be determined
so that E[Cn] = 1 holds. Consequently, a is essentially the only parameter left unknown.
At this point, the following quantity a is introduced as a measure of scatter with n being
the median of the life distribution:

J
a={V2^dH^> J| y (6) Xn — X-
(7)

It is reasonable that the quantity a can be used as a measure for the standard deviation of
the life distribution since c in Eq.(6) coincides exactly with the standard deviation when
H(n\x0i xc) follows a normal distribution. Prom Eq.(5), this quantity a is given as

c = ,ja {x0-(2A+1) - *:<"-»>} /(2A + l)/(eZ^) (8)

580
Assumed that h is used as a measure for the expected value, a measure for the coefficient
of variation of the distribution may be given as

<7 _ yJ(xc/x0)2X - (xjxp)-1 X2a

(9)
n (XC/XQ)X
- 1 ~^(2A + l)z0

This model has a great superiority over any other model (Ishikawa et ai, 1990).

FATIGUE T E S T RESULTS AND FATIGUE CRACK P R O P A G A T I O N

P R O P E R T I E S U N D E R C O N S T A N T STRESS A M P L I T U D E

Figure 2 represents the empirical S-N diagram based upon the experimental results under
constant stress amplitude. Figure 3 represents the empirical relationship between da/dn
and .AK (Amijima et a/, 1985). From this figure, the material constants, C and m, for
the sarin woven G F R P are obtained as 1.302 x 10" 3 1 and 21.09, respectively.

1 •/
140
130 /' ''''
I "l
4' j
<* 120 0
,fa,
f'.'
?/•*
/u
%h
V°
I 100 h ?' $'
$
1
1
1
I 90 I"
t
t
80
—o— m„n

7 8
io io
3 5 6
10 10" 10 10
Number of cycles to failure N

Fig. 2. Empirical S-N diagram. Fig. 3. Relationship between da/an and

AK for three kinds of G F R P .

FATIGUE LIFE DISTRIBUTION ANALYSIS BASED UPON

PROBABILISTIC F R A C T U R E MECHANICS

Determination of Parameters in Fatigue Life Distribution Model

The fatigue life distribution model under constant stress amplitude Z0 = SQ/s0 given
by Eq.(5) contains many parameters to be determined. First, values of A and e are
obtained with the aid of Eqs.(3) and (4) through values of m and C in Eq.(2). As for the
determination of x 0 , xc and a, though the maximum likelihood estimation method may be
applicable, the least square error method is adopted here on a practical basis. T h e value
of parameter a is to be determined such t h a t the variance a2 (a) around the regression
line becomes the minimum, by plotting the obtained fatigue lives (the number of cycles)
on a normal probability paper. In this case, the axis of abscissa represents u in $[u] in
Eq.(5) and the axis of ordinate the cumulative probability, which is estimated by use of
the mean rank method defined by H(n\x0, xc) = i/(n + 1). First, the median h and the
standard deviation a are obtained through fatigue life d a t a of a certain constant stress
amplitude S0 (in this case, 5 0 = 9 0 MPa). Next, with the aid of Eqs.(7)~(9), the critical
 581
value xc and the parameter value a are determined for the prescribed initial crack length
x0. Then, the ordered fatigue life data n; ( i = l , 2, 3, •••, n) are plotted on the normal
probability paper by use of the mean rank method and the variance <r2(a) is calculated
around the regression line. Finally, values of x0i xc and a are determined as a solution in
such a case where the variance a2 (a) becomes the minimum.

As a result of computation with the aid of the abovementioned procedure in case of S0 = 90

MPa, the value of the parameter a proves to take on 7.2713 x 10" 2 with x0 = 0.55 and
xc = 1.30. Figure 4 represents the fatigue crack propagation life distribution obtained by
use of those values in case of 5 0 = 90 MPa. In the figure, solid line is drawn by applying
the least square error method to the experimental data. The slope of this line is, needless
to say, concerned with the variance as a measure of the scatter in fatigue life and the
variance becomes smaller as the slope becomes steeper. As can be clearly seen in the
figure, the fatigue life data under constant stress amplitude of the satin woven GFRP
show a good agreement with the Tsurui-Ishikawa's model in consideration of the spatial
variation of the crack propagation resistance.

/
/ A ■ i
„*/ -/ /
'
/ '
% i/
/ J
A jy
/o° S*
/ /
/ /•
•
i i 1 1 1 in L_U.ll,IU l 1 nil • ... i.... i 1
1 0» 10° 10T 3 x 10T 5 x 10 4 10 8 10° 5 x 10(

Number of cycles lo failure N Number of cycles to failure N

Fig. 4. Fatigue crack growth life distri- Fig. 5. Fatigue crack growth life distri-
bution in case of 5 0 =90MPa. bution in case of S 0 =100MPa.

Propriety of Tsurui-Ishikawa's Model for Fatigue Life Distribution Analysis.

Comparisons are made between the theoretical distribution and the emperical ones of
fatigue life distribution under S0 being 100, 110 and 120 MPa, respectively, with the
aid of the parameter values obtained by use of fatigue life data under S0 = 90 MPa.
Figures 5~7 represent fatigue life distributions in case of 5 0 = 100, 110 and 120 MPa,
respectively. Every figure shows a good agreement with the Tsurui-Ishikawa's model.
This fact is considered to reveal the usefulness of the model in the fatigue life distribution
analysis of the satin woven GFRP.

By expanding this analytical procedure to the general case, the value of the parameter a
can be determined, which characterizes the scatter of life for the various types of GFRP
material. In other words, the procedure to determine distribution parameters can be
established with the aid of empirical data obtained comparatively easily, through the
application of the Tsurui-Ishikawa's model. Further, P-S-N curves can be also obtained
582
from the fatigue life distribution thus established and come to put into practical use in
the various field of reliability analysis.

I m / I
j ■ / I
I ■/ __J
1 ■/ I
I ■ / I
I ■/ I
I /m —— 1
If ■ j

!•• !•»
Number of cycles to failure
Number of cycle* to failure

Fig. 6. Fatigue crack growth life distri- Fig. 7. Fatigue crack growth life distri-
bution in case of 5o=110MPa. bution in case of 5o=120MPa.

CONCLUDING REMARKS

The present study is concerned with the clarification of the fatigue life distribution of
GFRP based upon the probabilistic fracture mechanics, by applying the Tsurui-Ishikawa's
stochastic crack growth model with a special emphasis on the randomness of the crack
propagation resistance involved in the material. As a result of this research, the model
proves to clarify the scatter in the fatigue life of GFRP under constant stress amplitude
loading.

By applying the present analytical procedure to various types of FRP materials, the values
of the parameter a can be accumulated, which characterizes the scatter in fatigue life for
FRP. This database will contribute to the clarification of the fatigue life distribution
and also enables to establish the procedure to determine distribution parameters in the
residual life distribution by use of empirical data obtained comparatively easily.

REFERENCES

Amijima, S., T. Tanimoto, T. Matsuoka and H. Ishikawa (1985). J. Soc. Mater. Set.,
Japan, 31, 286-292.
Ishikawa, H. and A. Tsurui (1984). A Stochastic fatigue crack growth model in
consideration of random propagation resistance. Trans. Japan Soc. Mech. Engrs.,
5fi, 1309-1315.
Ishikawa, H., A. Tsurui and H. Ishikawa (1989). Some aspects of structural reliability
assurance for random excitation processes. JSME International Journal, 32, 463-471.
Ishikawa, H. and A. Tsurui (1990). Reliability assessment of machines and structures
based upon stochastic fracture mechanics. KAGAWA-TECHNO, 2Q, 2-33.
Tsurui, A. and H. Ishikawa (1985). Theoretical study on the distribution of fatigue crack
propagation life under stationary random loading. Trans. Japan Soc. Mech. Engrs.,
5h 31-37.
Tsurui, A. and H. Ishikawa (1986). Application of the Fokker-Planck equation to a
stochastic fatigue crack growth model. Structural Safety, 4, 15.
 WS3b1

J O I N T 3 : A n Efficient Optimization Algorithm for

Calculation of the Joint Beta-Point in Parallel Systems
lb Enevoldsen & J.D. S0rensen, Department of Building Technology and Structural Engineering.
University of Aalborg, Sohngaardsholmsvej 57, DK-9000 Aalborg, Denmark

Abstract

In order to estimate the systems reliability of large structural systems it is often necessary to
estimate the systems reliability by use of parallel systems. An optimality criteria-based algorithm
for calculation of the joint /?-point in a parallel system is described and an efficient active set
strategy is developed and tested.

1. Introduction
Recently the calculation of the reliability of single failure elements (modelling potential failure
modes in e.g. structural elements) by first order reliability methods (FORM) has become a
well-established and acknowledged technique in practical reliability-based design, see e.g. Ho-
henbichler et al. (1987) and Madsen et al. (1986).
The next natural step is to establish efficient methods for estimation of the systems reliability.
So far, in reliability-based design mainly such models have been used where the potential failure
modes (failure elements) are modelled as elements in a series system (Level 1 systems analysis).
In large and complicated systems (e.g. structural systems with a high degree of statical indeter-
minateness) a better estimate of the systems reliability is determined by modelling the system
in a series system of parallel systems (levels > 1), i.e. failure of the system is defined as failure
of a parallel system, where more than one failure element have to fail simultaneously.
The problem of calculating the probability of failure of a parallel system in a FORM-analysis is
divided into two parts, namely 1) calculation of the probability of intersections and 2) determi-
nation of the joint /?-point where the limit state functions are linearized so that the intersections
can be determined, see section 2.
This paper concerns the calculation of the joint /?-point. In S0rensen h Thoft-Christensen (1989)
an optimality criteria (OTC) based algorithm is suggested for calculation of the joint /?-point.
A similar solution technique is suggested in Abdo & Rackwitz (1990) by use of a sequential
quadratic programming (SQP) formulation and introduction of a line search technique. None of
the papers exemplifies the techniques for calculations in a parallel system.
The main aim of this paper is to refine and implement the OTC-algorithm and in particular to

583
584
develop and examine an active set strategy which is very important for stability, cost and use of
the algorithm.

2. Reliability of a Parallel System

In FORM-analysis some of the quantities connected with uncertainty are modelled as stochastic
variables X = (X\, X2 ,'•'■, Xn) . m failure elements are assigned to the system each modelling
a specific potential failure mode at a specific point in the structure. The failure elements are
described by failure functions: g%i^x) = 0, i = 1,2, • • • , m. The failure function divides the
space for realizations ~x of X so that g%{x) < 0 corresponds to failure states and gi(x) > 0 to
safe states.

In FORM a £/-space of standardized and normally distributed variables is introduced by the

transformation X = T(U), and the failure functions are written gi(T(u)) = 0, i = 1,2, • • •, m.
If a system failure is defined by the event that N failure elements have to fail, each of the possible
failure paths of N failed elements can be modelled as a parallel system. The probability of failure
of a parallel system Pf is written as a probability of intersections: Pf = P(C\i=i{9i(^) < 0})

An approximation of the failure region is obtained by linearization of the safety margins M, =

gi(T(U)) in the so-called joint /9-point tl*, defined and determined from the following optimiza-
tion problem

min
u 1 = 5« T « (i)

s.t. </<(«)<0, t = l,2,---,iV

When the joint /9-point u* is determined the safety margins of the NA active constraints/failure
elements (i.e. <7i(«) = 0, i = 1,2, • • •, NA) are linearized

Mi~-aTU + 0i ,with a, = ^ ^ , and ft = aju\ t = 1,2,-• •, tfA (2)

The FORM approximation of the failure probability is written Pf = $i(—f3p) = $N A (~/?»?)

where 0P is the generalised reliability index of the parallel system, $NA ls
* n e -^A-dimensional
an( tne
normal distribution function /3 — (/?i,/?2r * * IPNA) ^ correlation coefficient matrix ~p is

determined by p = A A, with A = [ a i , a 2 , • • • , 5 ^ ] .
The above formulation will be used in this paper. For completeness the following is mentioned.
A better approximation of the probability of failure using intersections can be obtained by
including the inactive constraints, see Hochenbichler et al. (1987). A new linearization point
is calculated for each inactive constraint by modification of the optimization problem (1) so
the specific inactive constraint is forced to be active (i.e. an equality constraint). This is very
computer time consuming and will not be discussed further but the same solution techniques as
described in this paper can be used.
 585
In the formulation of (1) it was implied that at least one of the (i = 1,2, • • • ,N) constraints
was active in origo (<7t(0) > 0). If g%(0) < 0 for all i = 1,2, • • •, N constraints the safe domain
can be written as a union, see e.g. Hochenbichler et al. (1987). Hereby the calculation of /3P can
be performed by using the standard techniques for calculating the reliability of series systems,
see e.g. Madsen et al. (1986).

3. OTC-Algorithm for Joint /?-Point Calculation

In the following an OTC-based recursive algorithm is presented, see also S0rensen & Thoft-
Christensen (1989).
The OTC-algorithm is developed based on the Lagrange function and the Kuhn-Tucker (KT)
optimaiiity conditions of the optimization problem in (1) with A as the vector of Lagrange
multipliers. For a given iteration k and the corresponding values of the optimization variables
uk is the step length p to the next estimate u + 1 of the optimal point given by p = uk*1 — uk.
p is obtained by linearizing the KT-conditions (for an assumed correct active set) and neglecting
the second derivatives of the constraints with respect to the optimization variables u and keeping
the Lagrange multipliers constant. The KT-condition for the NA active constraints can then be
written

U A = 0
*+Pi + E * ^ ^ • «" = l,2,---,» (3)
>=i *

gi(uk) + Vgi(ukfp = 0 , i = l,2,---,NA (4)

If V 5 = [Vgi(uk),Vg2(uk),---,VgNA(uk)] and G = [gi(uk),g2(uk),-• ■ ,<7jvA(tr*)]T are

introduced the following matrix formulation is obtained

/ VG" p
—T - A = -G \
LVG 0 .
with the solution

A= - ( v E f v ^ r ^ V S uk - G) and p = - V ^ A - uk (6)

It is seen that the equations (5) are similar to the equations used in sequential quadratic pro-
gramming, see Gill et al. (1981) or Luenberger (1984). So the above approximation of the
Hessian matrix of the Lagrange function by the identity matrix gives a recursive formula:

u*+1 = -V<5A = v5(v^ T vS)- 1 (v5 T u A : - G) (7)

For NA = 1 (7) is the well-known Rackwitz-Fiessler algorithm for calculation of element reli-
ability indices. For iteration k the correlation matrix between the constraints is calculated by

p = A A. Hereby the gradients of the constraints can be written V G = — AN, where N is

586
a diagonal matrix of the Euclidian norms of Vgi(uk). Hereby (7) can be written, (see Abdo &
Rackwitz (1990))

u*+1 = -VSA = Tp~l(Xuk^ WlG) with \ = WlTlC&ruk +WlG) (8)

The correlation matrix of the constraints is always positive definite so the Cholesky decomposition
method can be used to solve the equations.

4. JOINT3, Stability and Active Set Strategy

The stability requirements for an algorithm for joint /?-point calculation depend very much on
the actual problem. Stability should most often be viewed in relation to solution accuracy and
calculation time and cost. The described formula (8) is easy to use. The difficult task and
the point where a major difference between algorithms can arise is in selection of the active set
strategy. How courageous an allowable active set strategy can be is problem dependent and fatal
for the convergence rate and stability of the algorithm.
After several considerations, see Enevoldsen (1991) the following algorithm JOINT3, see the next
page, is suggested.

It is seen that the algorithm requires that at least one of the constraints <7i(0), i = 1, 2, • • • , N
is greater than 0, i.e. only so-called "small intersections" are considered and it is only necessary
to calculate the gradients of the active constraints. The convergence checks are selected as
requirements for the objective function, the constraints and for the Kuhn-Tucker condition parts
(not for the sum but for the parts). Cj, €2 a n d €3 are selected from the author's experience
so the requirements become of equal importance. Furthermore, it is seen that the number of
equations is only NA which, compared toother techniques (e.g. sequential programming schemes
with NA + n equations), is a large reduction. The reduction is possible because of the simple
structure of the equations from the approximation of the Hessian matrix of the Lagrange function
by the identity matrix.

In algorithm JOINT3 techniques from sequential quadratic programming are used in step 3.
Functional values and gradients of all the constraints are necessary. A sub-iteration level is
introduced so that a new point is always calculated with an active set with positive Lagrange
multipliers and so that the linearized inactive constraints are not violated. The sub-iterations
do not require additional calculations of failure functions but additional solutions of (8).
The stability of JOINT3 is obtained because maximum one constraint can be deleted (smallest
negative multiplier) or added (most violated linearized constraint) in each sub-iteration in step
3 of JOINT3. In JOINT3 it can be more efficient to initialize the active set as only the most
violated constraints, i.e. NA = 1. Whether or not it is more efficient depends on the final number
of active constraints compared to the number in the initial set.
The decision in JOINT3 step 3 on whether a new constraint shall be added to the active set
based on the linearized constraint can be unprecise if the constraint is very non-linear. Thus it
can be a good idea to include a test-type line search technique (e.g. Goldstein-Armijo's principle,
see Luenberger (1984)) or the watchdog principle, see Chamberlain et al. (1982). However a line
search is expensive and the mistakes made in the active set will often be corrected during the
slow changes of the active set in the JOINT3-iterations.
 587
ALGORITHM JOINT3
Step 0 Initialize: k = 0, uk = 0, 7* = 0, A" = 6
Set 3 small positive convergence parameters €i, €2 and €3 (can be t\ = 1 • 1 0 - 3 ,
e2 = 1 - 1 0 " 4 a n d e 3 = 1 • 1 0 " 6 )
Calculate # ( 0 ) , i = 1,2, • • •, N. IF all # ( 0 ) < 0 STOP.

Step 1 For k = 0 Initialize the active set as the constraints with gi(uk) > 0, i = 1,2, • • • , N
For k > 0 calculate 0*(ufc) and V0;(U*), i = 1,2, • • •, N

Step 2 Convergence check (IF k > 0)

IF b ^ - T * - 1 ! < c i

andm^{k + E j G / A i ^ 1 l } < e 2
and gi(uk) < €3, z = 1,2, • • •, N
THEN STOP
ELSE k = fc -}-1

Step 3 Form V G and G and calculate A and u from (8)

IF Af > 0 for all i = l , 2 , - . - , A T A
and ^ ( u * " 1 ) + V f l f ^ u * - 1 ) ^ * - u ^ " 1 ) < 0 for all s £ I
GOTO Step 1
ELSE
Find the multiplier with the lowest value A m j n and the corresponding constraint Imin
G / and the constraint
Imax £ / w i t h $ r m a i a s m a x ^ ^ ^ - ^ + V ^ ^ - 1 ) ^ - ^ - 1 ) }
IF Xmin < 0 THEN
Delete Imin from the active set and form a new active set / ' with N'A = iV^ — 1
ELSE IF gmax > e4 » ( e 4 a small positive parameter, e.g. 1 • 1 0 - 2 )
Add Imax to the active set and form a new active set I' with N'A = NA + 1
Set 1=1' and NA = N'A
REPEAT step 3

5. Tests
Extensive tests of JOINT3 have been performed, see Enevoldsen (1991). JOINT3 was tested
against the two extended sequential quadratic programming based algorithms for non-linear
optimization, namely NLPQL by Schittkowski (1986) and VMCWD by Powell (1982). The tests
were performed with parallel systems of 20 elements in cases with few and many variables and
cases with low as well as high degrees of non-linearities in the problems. The tests resulted
in several conclusions, see Enevoldsen (1991), but in brief the tests showed that JOINT3 in
general is at least as stable and fast as NLPQL and VMCWD. In several cases JOINT3 is more
stable than NLPQL and faster than VMCWD. Further, JOINT3 becomes superior when the
tests examples become more non-linear and more complex.
588
6. Conclusions
An optimality criteria based algorithm (JOINT3) for calculation of the joint /?-point in a parallel
system is outlined, and it is explained how the systems reliability index in first order reliability
methods can be calculated.
It is shown that the number of equations to be solved during the iterations compared to usual
sequential programming based algorithms is much smaller due to the special structure of the
problem.
The presented J0INT3 algorithm seems to be fast and stable with a strong active set strat-
egy compared to standard non-linear optimization algorithms. Further, J0INT3 is small and
relatively simple and easy to programme.

7. References
Abdo, T. & R. Rackwitz (1990). /?-Point Algorithms for Large Variable Problems in Time-
Invariant and Time-Variant Reliability. In Proceedings. Presented at the 3rd IFIP WG7.5
Working Conference on Reliability and Optimization of Structural Systems. University of Cali-
fornia, Berkeley, USA.
Chamberlain, R. M., M. J. D. Powell, C. Lemarechal, H. C. Pedersen (1982). The Watchdog
Technique for Forcing Convergence in Algorithms for Constrained Optimization. Mathematical
Programming Study 16. North-Holland Publishing Company, pp. 1-17.
Enevoldsen, lb (1991). Reliability-Based Structural Optimization. Ph.D.-Thesis, Department of
Building Technology and Structural Engineering, The University of Aalborg, Denmark.
Gill, P. E., W. Murray & M. H. Wright (1981). Practical Optimization. Academic Press, Inc.
1981.
Hohenbichler, M. (1984). An Asymptotic Formula for the Probability of Intersections. Berichte
zur Zuverlassigkeitstheorie der Bauwerke, Heft 69, LKI, Technische Universitat Miinchen, pp.
21-48.
Hohenbichler, M., S. Gollwitzer, W. Kruse & R. Rackwitz (1987) New Light on First- and Second
Order Reliability Methods. Structural Safety, Vol. 4, No. 4, pp. 267-284.
Luenberger, D. G. (1984). Linear and Nonlinear Programming. Addison-Wesley, 2nd ed.
Madsen, H. 0 . , S. Krenk & N. C. Lind (1986). Methods of Structural Safety. Prentice Hall.
Powell, M. J. D. (1982). VMCWPj A FORTRAN Subroutine for Constrained Optimization.
Report DAMTP 1982/NA4, Cam&Tdge University, United Kingdom.
Schittkowski, K. (1986). NLPQL: A FORTRAN Subroutine Solving Constrained Non-Linear
Programming Problems. Annals of Operations Research.
S0rensen, J. D. & P. Thoft-Christensen (1989). Reliability-Based Optimization of Parallel Sys-
tems. In Procedings. Presented at the 14th IFIP TC-7 Conference on System Modelling and
Optimization, Leipzig, German Democratic Republic, July 3-7.
WS3b2

STOCHASTIC FIELD SIMULATION AND STRESS

FOR ORTHOTROPIC MEDIA

A. NISHITANI and S. SUGANUMA

Department of Architecture, Waseda University,

Okubo, Shinjuku-ku, Tokyo, Japan.

ABSTRACT

Random spacial variability of an orthotropic material property is discussed. The

simulation technique for generating the sample spacial irregularities is presented by
taking the orthotropic characteristics into account. Through the Monte Carlo cal-
culations by utilizing the simulation technique to represent the variabilities of the
elastic coefficients and applying the results to the finite element analyses, the ortho-
tropic stress variations are demonstrated.

KEYWORDS

Orthotropic material; spacial variability; stochastic field; material property; sample

function.

INTRODUCTION

The stress distributions for orthotropic media are fully dependent of elastic coeffi-
cients. Therefore the orthotropic stresses are seriously affected by uncertainty or
irregularity of the elastic coefficients. Considering the fact that wood is a typical
orthotropic and also a natural material, stochasticity of the material properties of
wood should be taken into account. For an orthotropic wood plate, Nishitani and
Matsui (1989) demonstrated the stochastic stress variability evaluation, which,
however, did not involve the spacial variability. This paper discusses the spatial
irregularity of the material property of an orthotropic wood plate, and presents the
simulation technique for generating the stochastic sample fields. The stress varia-
tions due to the elastic property fluctuating in space are also demonstrated.

SPACIAL IRREGULARITY OF ORTHOTROPIC PROPERTY

In dealing with an orthotropic wood, the y-axis is taken to be parallel to the wood
fibers, while the x-axis is to be perpendicular to them. The spacial fluctuation in an
589
590

orthotropic material property is supposed to be random. The random spacial varia-

biHty is assumed to be decomposed into two components: one is for the x-direction
and the other for the y-direction. From this assumption the following function
representing the orthotropic spacial irregularity is introduced:
or(*,y)-aJL*)+a 9 (y\*) with E[or(*,y)]«0, (1)
in which
as(x) : fluctuating component respect to the x-direction,
ay(y\x) : fluctuating component respect to the y-direction with x held fixed,
E[*] : the spacial average.

For a two-dimensional orthotropic wood plate the stress vector a is related to the
strain vector e by the relationship
<r«De, (2)
T CaB f ff T
in which * " [ * r , * f , f J , [ r j r 7 j and D is the elasticity matrix with the fol-
lowing five elastic coefficients:
Ex : Young's modulus with respect to the x-direction,
Ey : Young's modulus with respect to the y-direction,
G^ : shear modulus,
v^ : Poisson's ratio with respect to the x-direction due to the normal
stress in the y-direction,
i/^ : Poisson's ratio with respect to the y-direction due to the normal
stress in the x-direction.

In this study, only Ex1 Ey and G^ are regarded as random fluctuating in space
since they are of great significance among all the elastic coefficients necessary for
the two-dimensional problems (Nishitani, 1987). These three random fluctuating
coefficients are assumed to be identically represented by a(x,y) in the following
fashions:

l/Efayl-l/E^l+afry)}, (3)
l/^(xfy)-l/^{l+a(*,y)}, (4)

V^(*,yHl/G^l+a(*,y)}. (5)

SIMULATION TECHNIQUE FOR SAMPLE FIELDS

This section will be devoted to presenting how to generate the sample fields. Sam-
ple field with random spacial variability is generated by combining the simple tri-
gonometric simulation techniques generating the one-dimentional sample functions.
First of all, the field, in which sample irregularity will be simulated, is discretized
into Nx in the x-direction and into N$ in the y-direction. Then, the following pro-
cedures (a), (b), (c) are performed:
(a) a sample function ax(i) is generated by
*.-i .
* , ( 0 - 2 }J ^x(mAKt)AKxcos(imAKt+<l>t(m))y 1 = 1,2, • • • ,Nt, (10)
m-0
in which
 591

Sx : power spectral density function of ax,

AKX : wave number increment in the x-direction,
<)>x : random phase angle uniformly distributed between 0 and 2TT,

(b) for every s each Nx sample functions of 6cy(j\ i) are generated by

N
'~l I
a
» O I 0 - 2 E yS,(mAKv)AK9cos(vmAKy+<l>y(m)), i - 1 , 2 , • • • ,Nr (11)
m-0
in which
5 : power spectral density function of a ,
AK : wave number increment in the y-direction,
<f> : random phase angle uniformly distributed between 0 and 2TT,

(c) one complete sample field is generated by a(ij)=6cx(i)+a (j\i).

NUMERICAL EXAMPLES

Figure 1 shows an example for the spacial variability of a(x,y) obtained by a simple
experiment. In order to simulate the random fluctuating samples, the spectral den-
sities Sx and S must be estimated. From the variability a(t,i), given by Fig.l, the
spacial average with respect to the y-direction, ot r (t), is evaluated by

«*(«')=— E «(»".». (12)

^y m-0
which provides the power spectral density Sx without difficulty. In consequence,
the irregularity with x held fixed, a (j\i), is calculated by
«0'i «)=«(«.;) -*,(«•)• (13)

Fig.l Example of a(x,y) Providing VariabiUty of Material Property

592

Now that there are sample functions, or (jli), available for i = 0 to iV^—1, the Nx
kinds of spectral densities, Sj°J,Sjj * ' > £ « * > a r e obtained. In this paper, how-
ever, the average of these densities are employed along every Une parallel to the
fibers.

(14)

The spectral densities, Sx and S , thus evaluated are depicted in Fig.2.

With the spectral densities Sx and Sy substituted into Eqs.(lO) and (11), ax and cL
can be generated, respectively. Incorporating them into Eq.(13) leads to the result-
ing sample field a as shown in Fig.3. Comparing Fig.3 with the original variability

-154* 154*.

-154* 154*v

Fig.2 Spectral Density Functions for Random Orthotropic Fields

Fig.3 Generated Sample Field

 593
in F i g l indicates that the orthotropic characteristics of the irregularity fluctuating
in space are well simulated. Through the Monte Carlo calculations utilizing 1000
simulated sample functions of orthotropic random fields and applying the finite ele-
ment analyses, the stress variations of two dimensional wood plate subject to a con-
centrated tensile force F are presented. The finite element models are shown in
Fig.4, in which the smaller figure illustrates the liber direction, and the several
dimensions of the plate are provided in Table 1 as well as the elastic coefficients.
Figure 5 shows the standard diviations of <ry.

Table 1 Elastic Coefficients and Dimensions of Plate

Symbol Value Used for Analysis
E
*. 162,000 kgf/cm2
E 21,700 kgf/cm2
»
G
*v. 9,540 kgf/cm2
"xy 0.061
V 0.427
Ax 0.8 cm
Ay 0.8 cm
t (plate thickness) 1.4 cm

^y

I0i
iAx

H>
16 ><8- 12*tek ane AtS T
P
i\
IP

10

-*-y

Fig.4 Finite Element Model for Elastic Analysis

594

Fig.5 Standard Diviations of a

CONCLUDING REMARKS

In the sense of material property variations wood is one of the most significant
materials and also it is a typical orthotropic medium. The orthotropic stresses are
fully dependent of the elastic coefficients. Spacial variability of the elastic property
is hence necessary to be considered in performing an elastic analysis.

In this paper, simulation technique generating the stochastic sample fields is

presented. Sample field simulation is performed by taking the orthotropic charac-
teristics into account. Utilizing the generating technique and applying the finite
element method, the Monte Carlo calculations are conducted to provide the stress
variations for an wood plate subject to a concentrated load.

REFERENCES

Nishitani, A. (1989). Orthotropic Anarysts of Bolt-Jointed Woods , Waseda Univer-

sity doctoral dissertation, Waseda University
Nishitani, A. and Matsui, G. (1989). "Probabilistic Approach to Stress Distributions
for Orthotropic Wood Plates," Proceedings of the 5th International Conference
on Structural Safety and Reliability , ASCE, pp. 1847-1854
WS3b3

RESPONSE VARIABILITY AND RELIABILITY OF SIMPLE STOCHASTIC SYSTEMS

T. Takada
Ohsaki Research Institute, Shimizu Corp. 2-2-2 Uchisaiwai-cho
Chiyoda-ku, Tokyo, 100 Japan

ABSTRACT

Stochastic systems whose mechanical properties vary spatially are investigated in the present
paper. The stochastic response variability is analytically evaluated and the reliability issue is also
discussed.

KEYWORDS

Stochastic field theory; stochastic mechanical property; static indeterminacy; first excursion
probability; reliability problem.

INTRODUCTION

The spatial variability of the mechanical properties of systems can conveniently be represented by
means of the concept of the stochastic fields. To estimate the response of such systems, there are
some methods: stochastic finite element methods (Hisada and Nakagiri, 1981) and analytical
methods without using the discretization of stochastic fields (Shinozuka, 1987a; Bucher and
Shinozuka, 1988). This paper, using these analytical methods, emphasizes that the stochastic
response also constitutes a stochastic field particularly when the mechanical property is assumed
to be idealized as a continuous stochastic field, and therefore, this characteristics should be taken
into consideration even in the reliability problem.

STATICALLY DETERMINATE STOCHASTIC SYSTEMS

When systems are stochastic but statically determinate, the static equilibrium condition to the
static, deterministic external loads can fully determine the stress distribution of the systems. This
advantage of the systems is made use of to evaluate the stochastic response. To make the problem
simpler, a beam system is considered to consist of a single straight flexural beam. A stochastic
bending flexibility is assumed now to be expressed as in the following form:

(1)
m*) = ik{l+fix)}
595
596
where 1 /El (x) is a bending flexibility varying spatially and 1 jEJo is a mean value and / (x)
implies the zero-mean and one-dimensional homogeneous Gaussian stochastic field.

The deflection and deflection angle responses of the stochastic beam subjected to deterministically
distributed loads denoted by p (x) are now evaluated. The principle of complementary virtual
work can yield the following solution (Bucher and Shinozuka, 1988).

U {X) =
{ J(x) } = I £7o"h (t'x) M(t) ^ + fW*dt (2)

where u (x) is a response vector consisting of the deflection w (x) and the deflection angle 6 (x).
h (t, x) is a Green function vector associated with these two responses. M (x) is the bending
moment distribution. It can be observed in the above equation that u (a;) can be separated into two
parts: the deterministic and thefluctuatingparts. This characteristics cannot usually be seen in
statically indeterminate systems, as will be shown later. It is interesting to note that the fluctuating
part of the response can be expressed in terms of the convolution integration which is familiar in
the linear random vibration analysis.

Now focusing on the response statistics, the mean value can easily be evaluated by letting
/ (x) = 0 and the covariance function matrix associated with u (x) can directly be derived
from Eq. (2) as follows:

h
Cu„Ui,S2) = f f (jfir) (tuxi)ht(t2,X2)M(ti)M(t2)Rff(t2-h)dUdt2
(3)
where Rf/ (t) is an auto-correlation function of /(a;).

As seen in the above, the responses exhibit statistical non-homogeneity since the statistics are
dependent on the locations of interest. Of great interest to note is that this non-homogeneity results
from the boundary and loading conditions, as is quite similar to the initial and input conditions
in the random vibration analysis.

From the Fourier analysis, there exists the following transformation of Rff(t) into the
corresponding power spectrum density function S/f ( K) , which is known as a Wiener-Khintchine
transform (e.g. see Shinozuka, 1987b). Applying this transform to Eq. (3) and taking into
consideration that h (t, x) = 0 in the range t < 0 and t > U the covariance function matrix
can be rewritten:
+oo
Sff(n) V (K,X\) VU(K,X2) dn (4)
/ ■oo

where V (K,X) is called "a variability response function (Deodatis and Shinozuka, 1989)"
defined by:
V (*,*) = f °° Jjj-h (t,x)M(t) eiKtdt (5)
and V * ( K , x) is a complex conjugate of V ( K , x).

Now let us demonstrate a simple example, a canti-lever beam subjected to the concentrated force
P at the free end. We now take the following auto-correlation function of / (x):

Rff(0 = o? { l - 3 ( $ / 6 ) 2 } / { l + ( £ / 6 ) 2 } 3 (6)
 597
where oy is a standard deviation of / (x) and 6 is a correlation distance.

Figures 1 and 2 are the comparison between the standard deviation of the response from the Monte
Carlo simulation method (Shinozuka, 1987b) with 4000 sample size and those from Eq. (3). The
double integration appearing in Eq. (3) was done numerically. These comparisons show fairly
good agreements between the two evaluation methods.

Figures 3 and 4 show the variability response functions at a few locations. From these figures, the
higher fluctuating component of / (x) does not much influence on the variation of the response
since the variability response functions decay very quickly as n becomes large. The variability
response functions for other types of loading can be obtained in a same way. Importantly, these
variability response functions are dependent not only upon the boundary conditions but also upon
the loading conditions imposed.

Simulation (sample size=4000) Simulation (sample size=4000)

K| Eq. (3) eq Eq (3)
— - ^---ITTTT^

6/1=0.1

0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Non-dimensional Coordinate x/l Non-dimensional Coordinate x/l
Fig. 1. Standard deviation of deflection Fig. 2. Standard deviation of deflection angle

\ .6/1 = 0.1

\ 7^Sff(n)/(ojb/4)\

Fig. 3. Variability response function Fig. 4. Variability response function

of deflection of deflection angle

STATICALLY INDETERMINATE STOCHASTIC SYSTEMS

Since the stress response depends on the deformation in statically indeterminate stochastic
systems, the stress response also shows variability resulting from the mechanical property
variation. To analyze them, static indeterminate forces are introduced in order to satisfy the
boundary conditions which cannot be satisfied from equilibrium only.

The deflection and deflection angle responses at the location x of the single beam with raj-th
598
order of static indeterminacy can be written in the following:
mi
u ( x ) =uo(x) + ^2Bkuk(x) (7)
*=1

where uo (x) is a deflection response vector of the associated statically determinate system
subjected to the prescribed external loads, and u* (x) is a deflection response vector of the system
subjected to the A;-th static indeterminate force Bk. Since / ( x ) is assumed Gaussian stochastic
field, Ujt(s) can become Gaussian stochastic field. However, the resulting deflection and
deflection angle responses cannot constitute Gaussian stochastic field due to the non-Gaussianity
of Bk- Therefore, the statistics of the response u (x) cannot easily be obtained by simply taking
an expectation as seen in Eq. (3).

Thefirst-orderapproximation can conveniently be utilized to evaluate the response statistics.

Applying the Taylor expansion to Eq. (7), and taking up to thefirstorder, then we have

du (x) |
u (x) * u (x) | X H *,, + £ — L l \ ( X i (x) - (X< (x)» (8)
dXi '*>=<*>>V
1=1

where X,- (x) are the the stochastic fields and random variables involved in Eq. (7).

Once the responses are approximated as seen in the above, the covariance function matrix can
immediately be evaluated as follows:

^(x^^^^^^^l^^KAX^xOAX.C^)} (9)
•-1 ;=1
axi ' dXj

where (AX,- (xi) AX;- (X2)) are cross-covariance functions between the two stochastic fields.

To demonstrate the procedure mentioned above, a both-end fixed beam subjected to a

deterministically uniform loadpo is analyzed below. Using the auto-correlation function defined
by Eq. (6), the variances and cross-covariance of the deflection and deflection angle response can
be obtained from Eq. (9), as shown in Figs. 5 and 6. 4000 sample fields were used to evaluate
the response statistics in the simulation method. From these figures, the results based on Eq. (9)
agree well with those from the simulation although thefirst-orderapproximation was employed.

CT/=0.2 Simulation a/=0.2 - - - Simulation

" (sample size=4000) ■Eq.(9)
■Eq.(9)

Non-dimensional Coordinate x/l Non-dimensional Coordinate x/l

Fig. 5. Standard deviation of deflection Fig. 6. Standard deviation of deflection angle
 599

RELIABILITY ANALYSIS

In classical reliability analyses, the stochastic responses at the certain locations of systems
are selected as random variables not as stochastic fields, and the associated threshold is
probabilistically compared with them to evaluate the reliability. However, if one wants to
evaluate the reliability of stochastic systems, stochastic responses at a few selected locations
may not be enough to estimate "reliability as a structural member" since the stochastic responses
continuously and spatially fluctuate. This indicates the need of evaluating the probability that
the stochastic field stays in a safe region within an individual structural member. This is, indeed,
well known as thefirstexcursion problem. In the following, the probability that the deflection of
a single beam member exceeds a specified threshold level within the beam length is evaluated.

Let A w (x) be afluctuatingpart w (x)—(w (x)). The following probability that A w (x) exceeds
a certain threshold a is considered hereafter.

Pf(l,a) =Prob[Aw(aO > a : 0 < x < I] (10)

As mentioned before, Aw(x) becomes, in general, non-homogeneous and non-Gaussian

stochastic field. So, the first excursion theory must handle this non-homogeneity as well as
non-Gaussianity of the involved stochastic field. Many approximations have been proposed
for this end. Among them, Shinozuka et al. (1968) proposed the upper and lower bounds of
the probability for non-stationary Gaussian, zero-mean, stochastic processes. This bounding
technique is not allowed to be used due to the non-Gaussianity of the process of the response
of statically indeterminate beams. However, from Figs. 6 to 8, thefirst-orderapproximation of
Eq. (8) is reasonably good for evaluating up to the second-order statistics of the response. It
then follows that the approximate new Gaussian process given by Eq. (8) is used in statically
indeterminate beams.

From a reliability point of view, the above two bounds of the probability can be interpreted in
such a way that the lower bound is the probability of the excursion event at only one selected
location of the beam, while the upper bound takes into accounts of the excursions occurred at
every location of the beam.

Let us show some numerical examples. A canti-lever beam subjected to the concentrated force
at the free end is analyzed first. Figure 7 is a plot of the excursion probability versus a non-
dimensional threshold level, by applying the above bounds. From this figure, it can be said
that the two bounds of the excursion probability coincide with those from the simulation, and
therefore, use of one location (the free end of the canti-lever in this case) allows us to evaluate
a reliability as a member. Of course, this conclusion is only valid under the specified loading
condition.

On the other hand, Fig. 8 is a same plot when taking a both-end fixed stochastic beam subjected
to the deterministic and uniform load p. The resultsfromthe Monte Carlo simulation method fall
between the two bounds in most of the threshold range. The careful examination of the figure
points out that the simulation results get close to the lower bound in the large threshold level, and
furthermore they become below the lower bound in the larger threshold level. This may result
from thefirst-orderapproximation employed in Eq. (8). In the case of the both-end fixed beam,
an evaluation of "reliability as a member" is needed since there are some difference between the
two bounds of the excursion probability.
600

a/(PP/EI0) a/(pl*/EI0)
Fig. 7. First excursion probability of deflection Fig. 8. First excursion probability of deflection
(a canti-lever beam) (a both-end fixed beam)

CONCLUSIONS

This paper described a procedure to evaluate the response of simple stochastic structural systems
with mechanical property variation. The fundamental but essential mechanism and behavior of
the resulting stochastic response was made clear. Furthermore, a concept of "reliability as a
member" was combined with the classicalfirstexcursion problem.

REFERENCES

Bucher, C.G. and Shinozuka, M. (1988), "Structural Response Variability II," J. of EM, ASCE,
Vol. 114, No. 12, pp.2035-2054
Hisada, T. and Nakagiri, S. (1981), "Stochastic Finite Element Methods Developed for Structural
Safety and Reliability," Proc. of the 3rd ICOSSAR, pp.395-408
Shinozuka, M., Itagaki, H. and Hakuno, M. (1968), "Dynamic Safety Analysis of Multistory
Buildings," J. of ST, ASCE, Vol. 94, No. 1, pp.309-330
Shinozuka, M. (1987a), "Structural Response Variability," J. of EM, ASCE, Vol. 113, No. 6,
pp.825-842
Shinozuka, M. (1987b), "Stochastic Fields and Their Digital Simulation," Stochastic Methods in
Structural Dynamics, edited by Schueller, G.I. et al., Martinus Nijhoff Publishers, Netherland
Deodatis, G. and Shinozuka, M. (1989), "Bounds on Response Variability of Stochastic Systems,"
J. of EM, ASCE, Vol. 115, No. 11, pp.2543-2563
WS3c1

TWO-DIMENSIONAL STRESS-STRENGTH
INTERFERENCE MODEL FOR
RELIABILITY-BASED DESIGN*

Z.T.Gao, B.J.Fei, H.M.Fu, J.Ling

Beijing University of Aeronautics and Astronautics, China

ABSTRACT

The amplitude value and mean value for fatigue stress and fatigue strength are con-
sidered as two random variables in this paper. The two-dimensional probability distri-
butions of fatigue stress and fatigue strength are established, then a two-dimensional
stress-strength interference model is presented. This model will be better used for fa-
tigue reliability—based design.

INTRODUCTION

A great deal of work has been done in the reliability-based design by

M.Shinozuka[l],H.Ishikawa[2], J.N.Yang[3], E.B.Haugen[4] and the others, since
A.M.Freudenthal first presented this new concept. Research interest in the fatigue relia-
bility has grown rapidly in recent years, becouse of the inherent variability in fatigue
strength of materials as well as the statistical nature of random fatigue load.
Generally speaking, both the fatigue stress and the fatigue strength must be des-
cribed by two parameters: amplitude and mean, herein they are treated as two random
variables. On the basis of this principle, the two-dimensional probability distribution of
the fatigue stress and the fatigue strength are discussed along with the practical exam-
ples. Then a two-dimensional stress-strength interference model is presented.

OThe project of financial support by National Natural Science Foundation

601
602

TWO-DIMENSIONAL PROBABILITY DENSITY

FUNCTION OF FATIGUE STRESS

Statistical analyses show that the stress amplitude sa has a Weibull distribution or
a Normal distribution, and the mean stress sm has a Normal distribution. The
two-dimensional probability density function of fatigue stress may be illustrated by the
curved surface as shown in Fig.l.

Figure 1 probability density surface of fatigue stress

As an example, we acquired the data of 2178 peak values and vally values of fatigue
stresses measured from a machine part. By using the Rain-Flow Counting Method, we
can obtain the frequencies (number of occurrences) of stress amplitudes and mean
stresses as shown in Table 1.
Suppose the fatigue stress follows the two-dimensional Normal distribution, the
probability density function can be expressed as
 603
Table 1 . Fatigue stress frequencies

Smi l 2 3 4 5 6
s
Sai 50 100 150 200 250 300

1 40 9 0 75 0 21 0

2 80 0 48 0 120 0 42

3 120 45 0 162 0 57 0

4 160 0 61 0 129 0 38

5 200 27 0 69 0 33 0

6 240 0 36 0 63 0 24

7 280 0 0 16 0 10 0

Fatigue stresses sai, smj in MPa

h
(sa>sJ =
2na a >/l-i
cpj
2(1-p)
1
e-vs'
2p(sa-iix) (sm-ny) (sm-n
(1)
x y
'«
where n ,n ,a ,a and p are the parameters, their estimates are

1 v
(2)
" /-I

(3)

n-\
S^(^ f l / -? x ) 2 (4)

*,=J^hi*j<*.i-fi,)2 (5)

p=- S Z %(*.,-£,)(*«,-£,) (6)

From the data in Tablel, total cycle frequency n=1085, number of groups for
amplitude mx = 7, number of groups for mean my = 6. Vj is the frequency of ith group
for sai , Vj is the frequency of ith group for smj and Vy is the frequency corresponding to
sai smj. These estimates can be calculated as follows:
604

/2 = 139.87AfPa £ =\75.76MPa
^x ^y

a = 62.29 AfPa a =66A2MPa p = 0.02642

x y

Substituting the above values into Eq.(l), we obtain the probability density function of
fatigue stress.

T W O - D I M E N S I O N A L PROBABILITY DISTRIBUTION
FUNCTION OF FATIGUE STRENGTH

According to the identity of the probability of failure for fatigue strength

P(S min < S < S *) at a prescribed life N * and that for fatigue life P(N min < N < N *) at a
prescribed stress level S * (Fig.2), suggested by Weibull[5] and Tanaka[6], that is

P(Sm <S<S ) = P(Nmin <N<N ) (7)

s ,1
PDC OF FATIGUE STRENGTH

s*
h>/\. PDC OF FATIGUE LIFE

1 P - S - N CURVE
1 1 ^
N*

Figure 2 Probability density curves

Where Smin and N min are the minimum values of fatigue strength and fatigue life
respectively, and let f(N| S *) be the probability density function of fatigue life N at a
prescribed stress level S *:

P(Nmin <N<N*) = \N f(N\S * )dN (8)

We have the probability distribution function P(S) of fatigue strength:

P(S) = P(Smin <S<S*) = S" f(N\S * )dN (9)

N min

It is proved that Eq.(9) may be generalized to the two-dimensional probability dis-

tribution function of fatigue strength P(Sa,Sm) at any prescribed life N:
p S
( a>SJ = C. f(»\Sa,Sm)dN (10)
 605

When the fatigue life follows log Normal distribution, the probability density function
oflogNis
! f [logN-n(Sa,Sm)]2]
f(logN\S ,S ) = , expi 5 — > (11)

where /x(Sa,Sm) and c(Sa,Sm) are the mean of logN and the standard deviation of logN
at the stress level (Sa,Sm) respectively. Substituting Eq.(l 1) into Eq.(10), taking logN in-
stead of N, logNmin = - o o , and making the transformation of variable, let
lQKN-y(Sa,Sm) d(l0frN)
y
*(Smfm) *(Sa9Sm)
thus the probability distribution function (probability of failure) can be written as
loKN-rtSm,Sm)
P(S ,S ) = J *(5--5».) 1 -Y- (12)
2
v
a7 m ' J
-oo yf2^ e dY

Table 2 Results of statistical treatments

sm= 0 sm== 98
s
* ? a '****. s. ? d /0
^84.1

396.0 4.6174 0.0630 4.5544 372.4 4.6874 0.0270 4.6604

372.4 4.7065 0.0930 4.6135 333.2 5.0004 0.1770 4.8234

352.8 4.8690 0.1760 4.6930 313.6 5.1419 0.0780 5.0639

333.2 5.1395 0.1160 5.0235 294.0 5.3333 0.1030 5.2303

sm= 196 sm= 294

sa ft a l°*Ki s. ? CT to
***.
333.2 4.8034 0.0250 4.7784 313.6 4.7517 0.0463 4.7054

313.6 4.9479 0.0450 4.9029 294.0 4.9872 0.0720 4.9152

294.0 5.2147 0.1010 5.1137 274.4 5.2238 0.0936 5.1302

274.4 5.4254 0.0390 5.3864 254.8 5.5693 0.1169 5.4524

Now we find the mean /i(Sa,Sm) and the standard deviation (r(Sa,Sm) of logN.
Based on the fatigue testing of the notched specimens (stress concentration factor
Kt = 2) made of No.45 carbon steel[7], the results of statistical treatments are shown in
Table2. From the data, the expressions of the estimates Jx (Sa,Sm) and logNMl(Sa,S )
corresponding to 84.1% probability of survival are given by the two—dimensional
606
linear regression:

In the light of the statistical theory,

Substituting the estimates Eqs.(13) and (15) of /*(Sa,SJ and cr(Sa,SJ into Eq.(12),
P(Sa,Sm) is known for any prescribed life N.

TWO-DIMENSIONAL STRESS-STRENGTH
INTERFERENCE MODEL

The two-dimensional stress-strength interference model may be established when

the two-dimensional probability density function h(sa,sm) of stress and the
two-dimensional probability distribution function P(Sa,Sm) of strength are given.
It is well known that for the one-dimensional stress-strength interference model, the re-
liability level R can be defined as

Where h(s) and g(S) are the probability density functions of stress and strength
respectively . The probability distribution function P(s), ie, the probability of failure is

Hence Eq.(16) becomes

We extend it to the two-dimensional case, thus

Substituting Eq.(12) into Eq.(19),

The above expression (20) can be calculated by numerical method with the aid of com-
puter.
 607

REFERENCES

[1] Shinozuka, M., "Structural Reliability under Condition of Fatigue and Ultimate Load Failure",
Air Force Materials Lab., AFML-TR-68-234,1968.
[2] Ishikawa, H.,"A State-of-the-Art Survey of Reliability-Based Design of Structures", Journal
oftheJSSC, Vol.18,1982.
[3] Yang, J.N. and Trapp, W.J., "Reliability Analysis of Aircraft Structures under Random
Loading and Periodic Inspection",AIAA J., 12(12): 1623-1630,1979.
[4] Haugen, E.B., Probabilistic Mechanical Design, John Wiley & Sons, New York, 1980.
[5] Weibull, W., Fatigue Testing and Analysis of Results, Macmillan Company, New York, 1961,
pp.226-227.
[6] Tanaka,T., "Data-Base on Fatigue strength and Statistical Distribution Characteristics of
Fatigue Life and Fatigue strength", Proceedings of FATIGUE 84, Vol. II ,1984,
pp.1139-1149.
[7] Gao, Z.T. et al., Handbook of Fatigue Behavior of Aeronautical Metal Materials, Beijing
Institute of Aeronautical Materials, China, 1981.
WS3C2

JAPANESE ROUNDROBIN ANALYSES OF STABLE CRACK

GROWTH IN INHOMOGENEOUS CT SPECIMEN

G. YAGAWA 1}, S. YOSfflMURA l\ M. KIKUCHI2), S. AOKI3),

N.MIYAZAKI4), M. NAKAGAKI 5), T. NISHIOKA 6), N. MUKAIMACHI7),
S. SASAKI8), T. SHIMAKAWA 9), T. WATANABE 10)

1) Department of Nuclear Engineering, University of Tokyo,

7-3-1 Hongo, Bunkyo, Tokyo 113, Japan
2) Science University of Tokyo, Noda, Chiba
3) Tokyo Institute of Technology, Ookayama, Tokyo
4) Kusyu University, Higashi, Fukuoka
5) Kusyu Institute of Technology, Iizuka, Fukuoka
6) Kobe University of Marcantile Marline, Higashinada, Kobe
7) JGC Corporation, Minami, Yokohama
8) Nippon MARC, Shinjuku, Tokyo
9) Kawasaki Heavy Industries, Koto, Tokyo
10)Century Research Center, Nakase, Chiba

ABSTRACT

Elastic-plastic finite element analyses were performed on stationary as well as growing cracks in
welded CT specimens made of the nuclear pressure vessel A533B class 1 steel. Cracks were set
to be normal to the phase boundary of base metal and weld metal. Residual stress effects were
ignored. In a stationary crack regime, parametric analyses were performed by changing material
properties, i.e. Young's moduli and yield stresses, and the distance between the crack-tip and the
phase boundary. In a growing crack regime, generation phase crack growth analyses were
performed on four kinds of welded CT specimens with different crack-tip locations. The effects
of inhomogeneity on fracture parameters such as the J-integral were discussed in detail.

KEYWORDS

J-integral; crack growth ; generation phase analysis ; inhomogeneity ; roundrobin analysis

INTRODUCTION

Nonlinear fracture mechanics (NLFM) based on the J-integral (Rice, 1968) has been widely
utilized in the assessment of structural integrity of ductile materials (Yagawa, et ai, 1985,1989).
The NLFM was originally developed on the assumption that materials and structures are
homogeneous. Recently, various EPI (Elastic-Plastic fracture phenomena of Inhomogeneous
materials and structures ) problems have been increasingly important, related to the structural
integrity assessment of aged structures with weldment.

Aming at the development of some simple estimation schemes for crack growth resistance in
inhomogeneous materials and structures, we performed the roundrobin finite element analyses of
stationary cracks as well as stable crack growth in welded CT specimens, in which initial cracks
were set to be normal to the phase boundary between base metal (BM) and weld metal (WM).
Material properties used were obtained from uniaxial tensile tests of welded plate made of the
nuclear pressure vessel A533B class 1 steel. During crack growth experiments, histories of crack
growth were obtained as the relationships among a crack extension amount (Aa), an applied load
per unit thickness (P) and a load-line displacement (8). Generation phase simulations were
carried out by nine finite element codes.

The J-integral and other integral parameters (Aoki, et ai, 1981, Atluri et ai, 1984) were
evaluated with line integration techniques. As reference, the J-integral was also evaluated with
609
610

conventional empirical formulae such as the Merkle-Corten's formula and so on (Merkle and
Corten, 1974, Ernst et al.y 1981, Ernst, 1983). Through the comparison of those results, we
discussed the effects of material inhomogeneity on the fracture mechanics parameters.

ROUNDROBIN PROBLEMS

Materials and Specimens

Welded CT specimens were simply modeled as bimaterial CT specimens as shown in Fig. 1. The
materials #1 and #2 in the figure correspond to base metal (BM) and weld metal (WM),
respectively. Initial crack-tips were placed around the phase boundary. The material properties
of both metals were determined from uniaxial tensile tests on welded plate made of A533 class 1
steel. A uniaxial stress-strain relation of the material #1 is formulated as follows:
IF o<a Y S e=| (1)

IFa,aYS e - | + ( ( ^ - ( ^ f ) (2)
where Ej = 206 GPa, v = 0.3, o 1 = 550 MPa, n = 2.0 and E' = 500 MPa. For the material #2, a
similar relation was used, i.e. v = 0.3, n = 8.0, E' = 950 MPa. Young's modulus and yield stress of
the material #2 were parametrically changed to examine inhomogeneity effects. Residual stress
effects were ignored.

Stationary Crack Problems

In the analyses of stationary cracks, initial crack-tips were set to be in front of the phase
boundary, and the following three parameters were varied :

(1) The distance between the crack-tip and the phase boundary, i.e. 0.025 < c/b < 0.15,
(2) The ratio of Young's moduli of two materials, i.e. 0.70 < EyEj < 1.0,
(3) The ratio of yield stresses of two materials, i.e. 1.0 < G2Y!/olYS < 80/55.

The analyses were performed considering the following issues :

(a) Each participant chooses an appropriate mesh by himself.

(b) J A is calculated along various integration paths including a path set in material #1.
(c) J ^ is calculated by the Merkle-Corten's formula (Merkle, et ai, 1974).

Four participants performed those analyses. All the participants used eight-noded isoparametric
elements. The finest mesh consists of more than 2000 nodes, while the coarsest mesh does about
300 nodes. Three participants used the line integration technique for the J-integral calculation,
while the rest one used the virtual crack extension technique.

Growing Crack Problems

Analyzed here were one homogeneous and three welded CT specimens with different crack-tip
locations as shown in Fig. 1. 20 % side groove was machined in all the specimens.
(1) M5G specimen, which is a homogeneous CT specimen made of the BM.
(2) H5G specimen, in which a crack-tip is located in front of the phase boundary,
i.e. in HAZ part.
(3) F5G specimen, in which a crack-tip is located on the phase boundary.
(4) D5G specimen, in which a crack is located across the phase boundary.
The stress-strain relations used in the present analyses are basically the same as those of Eqs. (1)
and (2). Young's moduli of the materials #1 and #2 are taken to be 206 GPa and 175 GPa,
respectively, while their yield stresses are 550 MPa and 630 MPa, respectively. Generation
phase crack growth analyses were performed following the measured relationships among a load
per unit thickness (P), a load-line displacement (8) and a crack extension amount (Aa).
 611

Nine participants performed the present analyses. All the participants used eight-noded
isoparametric elements. The finest mesh consists of about 1300 nodes, while the coasest mesh
does about 500 nodes. Eight participants used the line integration technique for the J-integral
calculation, while the rest one used the virtual crack extension technique. All the participants
used a nodal release technique to simulate stable crack growth. The following fracture
mechanics parameters were plotted against Aa : the J-integral calculated along integration paths,
J ath, the J-integral evaluated by the Merkle-Cortens formula, JM<:(Merkle and Corten, 1974), the
modified J-integral by Ernst, J (Ernst, 1983), the deformed J-mtegral by Ernst et al.,J^ (Ernst et
ai, 1981), the T*-integral (Auuri et ai, 1984), the f-integral (Aoki et al.y 1981) and CTOA. It is
well known that the conventional J-integral calculated along integration paths loses any physical
meaning and a path independent feature when large-scale crack growth occurs. Nevertheless, we
calculated J A values along various integration paths because one of purposes of the present
analyses wfs to study the correlation of J alh with JM c , JM and JD during crack growth in
inhomogeneous materials.

RESULTS AND DISCUSSIONS

Stationary Cracks

As one of analysis results, Fig. 2 shows the J vs. 8 curve in the case of E ^ = 0.85, G2YS/olY$ = 80/
55, c/b = 0.025. All the results of the present analyses on stationary cracks in bimatenal CT
specimens can be summarized as follows :

(1) In a homogeneous case, J A and JM<: coincides with each other very well.
(2) J shows a good path independence feature even in bimaterial CT specimens.
(3) When o\J&YS is greater than unity, JH<: becomes larger than J tf|. In other words,
increase or the yield stress of the material #2 promotes overestimation of JM^,.
(4) When Ej/E, is smaller than unity, J,^ becomes smaller than J^.
(5) The above effects of (3) and (4) are more significant when a crack-tip approaches the
phase boundary.

In practical welded specimens, increase of the yield stress of weld metal and decrease of its
Young's modulus influence the JM^, evaluation competetively. However, it is anticipated that the
effects of increase of yield stress finally dominate the JM c behavior after a sufficiently large
yielding zone is developed around a crack-tip. It is also found that the difference of the JM _ and
J .values is only 10 to 20% at most in practical welded specimens. It can be concluded that
difference of material properties assumed in this study does not cause any difficulty in
experimentally evaluating the J values.

Growing Cracks

Figure 3 shows the calculated and measured crack growth resistance curves of M5G specimen,
where solid circles indicates the measured JD and others are calculated values, i.e. Jp (open
circles), J (open squares), J (open triangles), J ± calculated along the farthest path (dashed
line), and T* (solid line). The following observations can be derived from the figure.

(1) Calculated and measured JD values agree well with each other within 10 % difference.
(2) All the J values increase continuously in accordance with cragk growth, while the T*
value levels off after a certain amount of crack growth. The J-integral showed the
similar trend to the T*-integral although it is not shown in this particular case.
(3) The order of magnitudes of the J values is as follows : JM > JM^ > JD. It should be noted
that J A values have shown strong path dependence.

Figure 4 shows the crack growth resistance curves of H5G specimen. The following
observations can be obtained from the comparison of both figures.
612

(4) Crack growth resistance of M5G is greater than that of H5G, even if evaluating by any
J-integrals.
(5) The slopes of J-R curves of H5G are steaper than those of M5G.
(6) The T*-integral always levels off after a certain amount of crack growth, and the
magnitude of the T* of M5G is greater than that of H5G. In H5G specimen, the T*
increases gradually after crossing the phase boundary.

Those results may be attributed due to the fact that the HAZ part has lower initiation toughness
than both weld and base metals.

Figures 5 and 6 show the crack-tip strain and stress distributions of M5G and H5G specimens
along uncracked ligament, i.e. 0 = 0° at crack initiation. The crack-tip strain field is continuous at
the phase boundary, while the stress field shows jump of about 15 % of yield stress, which almost
corresponds to the difference of yield stresses of both materials. For the purpose of comparison,
the theoretical HRR fields (Hutchinson, 1968, Rice et al., 1968) using yield stresses of both
materials are plotted here. It can be expected that the HRR fields in a homogeneous material
regime may be adjustable to a stationary crack in a bimaterial regime. However, the analyses on
crack-tip fields during crack growth in homogeneous and bimaterial specimens also show that
the HRR slope disappears after a certain amount of crack growth.

CONCLUDING REMARKS
Elastic-plastic finite element analyses were performed on stationary cracks and growing cracks
in bimaterial CT specimens, whose material properties and crack growth histories were obtained
from fracture experiments of welded CT specimens made of A533B class 1 steel. The analyses
results clearly showed the quantitative effects of material inhomogeneity on fracture mechanics
parameters.

ACKNOWLEDGMENTS

This study was performed under the EPI program, and financially supported by Japanese utilities
and fabricators, and USNRC and Martin Marietta Energy Sytems, Inc. under Subcontract No.
19X-SD561V.

REFERENCES

Aoki, S., K. Kishimoto and M. Sakata (1981). Energy-release rate in elastic-plastic fracture
problems. Trans. ASME, J. Appl. Mech., 48, 825-829.
Atluri, S.N., T. Nishioka and M. Nakagaki (1984), Incremental path-independent integrals in
inelastic and dynamic fracture mechanics. Engrg. Fract. Mech., 20, 209-244.
Ernst, H.A., P.C. Paris and J.D. Landes (1981). Estimations on J-integral and tearing modulus T
from a single specimen test record. ASTM STP 743,476-502.
Ernst. H.A. (1983). Material resistance and instability beyond J-controlled crack growth. ASTM
STP 803,1-191-213.
Hutchinson, J.W. (1968). Singular behavior at the end of a tensile crack in a hardening material.
J. Mech.Phvs. Solids, J6,13-31.
Merkle, J.G.and H.T. Corten (1974). A J-integral analysis for the compact specimen,
considering axial force as well as bending effects. Trans.ASME, J. Press.Vess.Tech., 96,
286-292.
Rice, J. R. (1968). A path-independent integral and the approximate analysis of strain
concentration by notches and cracks. Trans. ASME.J. Appl. Mech., 35, 376-386.
Rice, J.R. and G.F. Rosengren (1968). Plane strain deformation near a crack-tip in a power-law
hardening material. J. Mech. Phys. Solid, 16, 1-12.
Yagawa, G., Y. Takahashi and H. Ueda (1985). Three-dimensional fully plastic solutions for
plates and cylinders with through-wall cracks. Trans. ASMEJ.Appl. Mech., 52, 319-325.
Yagawa, G.and K. Ishihara (1989). Cleavage and ductile thermal shock fractures of corner-
cracked nozzles. Trans. ASME, J. Press. Vess. Tech., I l l , 241-246.
 613

11mm

J)=20mm
63mm 0.1.2.3.4.5.6.7.8.9 11.11.2
8 (mm)

Fig. 1. Configuration and dimensions of Fig. 2. Calculated JM^ and J A vs. 8 curves
bimaterial CT specimen. of stationary cracks in inhomogeneous
specimen.

2.0
L.\)-
• JD(exp.) M5G • JD(exp.) H5G
A A
JM-C (homogeneous) JM-C (inhomogeneous)
© JD ° JD
D
o JM +'* JM
1.5 1.5
- - Jpath (farthest path) S o - - Jpaih (farthest path) /'

/A - :
X* ,' DA — T* /nl

1.0- ' B Z ° • •
' D « ° •
/ o§ : . •
/«• mat#l
0.5
/B °•
z

0.0- ' 1 ' 1 ' 1 ■ 1 ■

2 3 1 2 3
A a (mm) A a (mm)

Fig. 3. Measured and calculated crack growth Fig. 4. Measured and calculated crack growth
resistance curves of M5G specimen. resistance curves of H5G specimen.
614

u.«t -

L/(J/Jys) = 63 9=0°

0.3-
HRR in material #1 (Plane stress)
I ° M5G (Aa = 0.22mm)
I • H5G (Aa = 0.22mm)
ex
CO 0.2-

\° . Phase boundary
V®
0.1 - \ •
Material #2
^ . ,
Material #1 ^ . ^ ^ ^
mCtP
^~9 • • « « #
0.0- 1 ' 1
10 20
R/(J/ays)

Fig. 5. Comparison of crack-tip strain fields of M5G and H5G specimens.

1200

1000

800

~ 600 Material #1 Material #2

400
HRR in material #1 (Plane stress)
HRR in material #2 (Plane stress)
200 H M5G (Aa = 0.22mm)
H5G (Aa = 0.22mm)
0
10 20

R/Q/Oys)

Fig. 6. Comparison of crack-tip stress fields of M5G and H5G specimens.

 WS3c3

FATIGUE RELIABILITY ANALYSIS OF STEEL HIGHWAY BRIDGES

USING AN EFFICIENT MONTE-CARLO PROCEDURE

Wataru SHIRAKI a n d S h i g e y u k i MATSUHO

D e p a r t m e n t of Civil E n g i n e e r i n g , T o t t o r i U n i v e r s i t y , 4 - 1 0 1 ,
Minami, K o y a m a - c h o , T o t t o r i - s h i , 680, J a p a n

ABSTRACT

Risk e v a l u a t i o n of f a t i g u e f a i l u r e is p e r f o r m e d of s t e e l s t r u c t u r a l e l e m e n t s of
h i g h w a y b r i d g e s u s i n g a n efficient M o n t e - C a r l o p r o c e d u r e . F o r a t y p i c a l t y p e of
s t e e l g i r d e r b r i d g e t h e s t o c h a s t i c modeling of f a t i g u e p h e n o m e n a a n d p a r a m e t e r s
a r e made. I n modeling t h e u n c e r t a i n t i e s in t h e load d a t a s u c h a s t r u c k axle a n d
g r o s s w e i g h t s , h e a d w a y s , impact, s t r e s s r a n g e , g i r d e r d i s t r i b u t i o n , a n d volume
a r e i n c o r p o r a t e d . T h e n u m e r i c a l c a l c u l a t i o n s of r i s k of f a t i g u e f a i l u r e c l a r i f y some
s h o r t c o m i n g s i n h e r e n t in t h e c u r r e n t J a p a n e s e s p e c i f i c a t i o n s for s t e e l h i g h w a y
bridges.

KEYWORDS

Fatigue failure; risk analysis; steel highway bridge; efficient Monte-Carlo

p r o c e d u r e ; full p r o b a b i l i s t i c a n a l y s i s

INTRODUCTION

T h e l o a d i n g c o n d i t i o n s of h i g h w a y b r i d g e s in J a p a n h a v e become more a n d more

s e v e r e from y e a r t o y e a r d u e t o t h e r a p i d i n c r e a s e in t h e n u m b e r a n d t o n n a g e of
motor v e h i c l e s c r o s s i n g t h e b r i d g e s . As a r e s u l t , c o n c r e t e s l a b r o a d w a y s , s t e e l
b r i d g e c o m p o n e n t s a n d a t t a c h m e n t s a r e s u f f e r i n g from s e v e r e d a m a g e s much
quicker than expected at the design stage.

In t h e c u r r e n t J a p a n e s e d e s i g n specification for steel highway b r i d g e s , t h e r e a r e

no f a t i g u e p r o v i s i o n s e x c e p t for s t e e l d e c k p l a t e s . I t h a s b e e n p o i n t e d o u t t h a t t h e
p r i m a r y c a u s e of t h e d a m a g e s m e n t i o n e d a b o v e lies in t h e d e f e c t s of f a t i g u e
p r o v i s i o n s . Many e x p e r i m e n t a l a s well a s t h e o r e t i c a l r e s e a r c h e s for f a t i g u e of
h i g h w a y b r i d g e s h a v e b e e n p e r f o r m e d d u r i n g t h e l a s t d e c a d e . I n 1989 t h e new
v e r s i o n of t h e g u i d e l i n e for f a t i g u e d e s i g n of s t e e l s t r u c t u r a l e l e m e n t s a n d
a t t a c h m e n t s w a s p r o p o s e d b y t h e J a p a n S o c i e t y for S t e e l C o n s t r u c t i o n (JSSC,
1989). T h i s v e r s i o n i n c o r p o r a t e s s t a t e - o f - t h e - a r t f a t i g u e a n a l y s i s models a n d
d a t a . However, t h i s g u i d e l i n e is i n t e n d e d t o a p p l y for v a r i o u s s t e e l s t r u c t u r e s
other than highway bridges.

615
616
In this study, risk analysis of fatigue failure is performed on steel structural
elements of highway bridge using the model proposed by Nyman and Moses (Nyman
et ai., 1985). In the analysis the uncertainties in the load data such as truck axle,
gross weights, headways, impact, s t r e s s range, girder distribution, and volume
are incorporated. The probabilistic modeling of these uncertainties are made by
utilizing field data and laboratory testing data. The present study uses a
reliability evaluation program which is developed by the first author using an
efficient sampling technique, the IFMPUC (Iterative Fast Monte-Carlo Procedure
Using Conditional Failure Probability) (Shiraki, 1990).

From the calculation results, some shortcomings inherent in the c u r r e n t Japanese

specifications for steel highway bridges are pointed out, and then the necessity of
developing fatigue provisions is emphasized.

EFFICIENT MONTE-CARLO PROCEDURE

USING CONDITIONAL FAILURE PROBABILITY

For actual limit state functions of s t r u c t u r e g(x) where X=(Xi ,X2,—,Xn) is the
random vector of so-called basic variables, any basic variable Xi may very often
be expressed in the form
X, = g- , (x') (1)
where g ^x') is the inverse function of g(x) for x5 and is any continuous and
monotonous function in each of the variables of the random vector X'=(X1,X2,
— ,Xi_i ,X i + i, ••• ,X n ). Using this expression, the conditional failure probability,
PT°(X/), with given values X'=xf of all other variable except X;, may be expressed as
PT°(X , ) = 1 - F X « . X - ( X , | X ' ) (2)
where F X nx(x; I x') is the conditional cumulative distribution function of Xs with
given value X'=x\ In Fig.l the relationship between the conditional cumulative
distribution function F X i i x (xi | x') and the conditional failure probability PT°(X')
for the two dimensional case is shown. Assuming the statistical independence
between Xi and X* and using the conditional failure probability P T ^ X ' ) , then the
failure probability of s t r u c t u r e is given by
Pr = / P ° GOf.-GOfc- (3)
an i-
If X, is not independent of X', the evaluation of F Xi ,x(Xi | x') in Eq.(2) must be
performed by using the Nataf Model (Liu et ai., 1986). Using the importance

fxiv(xiy) : Conditional probability

density function

Pxir(xly) : Conditional cumulative

distribution function

1-Fxiv(£aly=a)
g(x.y) : Li«it s t a t e function

P,c(y-a)- 1 [ F X I Y U al y»a)

"PX|Y(€ il y-a)]

Fig. 1 Relation between Conditional Probability Function FXiy(x|y)

and Conditional Failure Probability Pf°(y)
 617
sampling density function hY_(x'), Eq.(3) can be rewritten
r,-Jr'.V
The mean values of the importance sampling density function h x (x') are selected
to be a point as the center of domain which contributes most to the total failure
probability. In this procedure the domain is defined as the mass center of failure
density Prc(x,)f2<'(x,i). Then, Eq.(4) may be estimated numerically by
(5)
''■T&'^&n
where N is the number of simulations. The calculation procedure is the same as the
procedure presented in the IFM procedure (Bucher,1988)

RELIABILITY ANALYSIS OF FATIGUE OF

STEEL STRUCTURAL ELEMENTS OF HIGHWAY BRIDGES

Stochastic Modeling of Fatigue Phenomena

The failure function for fatigue used herein is given by (Nyman et ai., 1985)

where g = failure function such that g<0 implies failure; D f = damage to cause
failure ; V = volume of traffic in t r u c k s p e r day ;t = life in days; N D = design
number of cycles (= 2 x 106 cycles); M = m k / m D = moment ratio; m k = factor
incorporating t h e effects of span type, axle spacings and weight distribution
among the axles which influence the bending moment range at any specific site k;
m D = design value of m K; G = g k / g D = distribution factor ratio; g k : girder
distribution factor given as t h e percent of t h e maximum bending moment
transferred to a single girder at site k, i.e. a property of t h e bridge and the
lateral positioning of the vehicle on the b r i d g e ; g D = design value of g k ;H = h k / h D
= headway ratio; h K = headway factor accounting t h e increment of bending
moment range by multiple t r u c k s loading on t h e bridge at the same time at site k;
h D = design value of h k ; 1 = 1 k / I D = impact factor ratio; I k = impact factor
representing t h e dynamic amplification of the bridge at site k; I D = design value
of I k ; S = S r%/S D = s t r e s s range ratio; S r t = true s t r e s s range defined as to
the s t r e s s r a n g e amplitude at N D ; S D = design stress; Lo
loadometer value; w : = weight of t h e i th truck at site k; and w D = design truck
weight.

In formulation of Eq.(6), Miner s law is used and it is assumed that a truck

crossing causes a single s t r e s s cycle. The parameters DT» V,M,G, H, I , S and Lo
in Eq.(6) are assumed to be the random variables.

Stochastic Modeling of Parameters for Fatigue

Moment Ratio (M). The moment ratio M is rewritten as

where Mk = bending moment range at site k; and MD = design value of M*.

According to Eq.(7) t h e probabilistic characteristics of M a r e estimated. In
estimation t h e traffic load models investigated by t h e Committee on Design Load
Development for Hanshin Expressway (HDL Committee, 1986) a r e used, and the
design vehicles a r e t h e TT-43 model (see Fig.2) in the Japanese Specification for
Highway Bridges (Japan Association of Road Engineers, 1980).
618

TT-43 Table 1 Mean Values and Standard Deviations

13t 12t 12t of Moment Ratio M
6t
40m 60m 80m
u 0.11588E+01 0.10202E+01 0.10146E+01
325 780 155 (cm)
o 0.58727E-02 0.37614E-02 0.27068E-02
Fig.2 Design Vehicle
Loading Model

The estimation results are shown in Table 1. In this table (i and a are the mean
value and standard deviation of M, respectively, and L is the span length of
simple beam model.
Distribution Factor Ratio ( G ) . According to the result of Nyman et al. (1985), the
mean value JLL and the standard deviation a of G are determined as follows; JLL =
0.374 and a = 0.0486.
Impact Factor Ratio ( I ). The probabilistic characteristics of the impact factor I K
are evaluated by using the results in the HDL report (HDL Committee, 1986). The
design impact is taken as the value in the Japanese Specification for Highway
Bridges(1980). The mean value JLL and the standard deviation a of I are shown in
Table 2 for the simple beam with span length L=40, 60, 80 (m).
Headway Ratio (H). Based on the definition given by Nyman et al. (1985), the mean
value u and the standard deviation o of H are evaluated by using the simulation
technique. In simulation the traffic load models reported by the HDL Committee
(1986) are used. The simulation results are shown in Table 3.
Loadometer Value ( L a ) . Using the simulation technique the mean value JLL and the
standard deviation a of L □ are calculated for the design vehicle model TT-43.
These values are as follows; ju = 0.1955 and a =0.012153.
Truck Volume ( V ) . The mean value JLL of truck volume is expressed in Average
Daily Truck Traffic (ADTT). A typical ADTT for the Hanshin Expressway Network is
3700 and will be the mean value used here. The standard deviation a is assumed to
be 370.
Stress Range Ratio ( S ) . The s t r e s s range ratio S is simply the t r u e s t r e s s range
S r t divided by the design s t r e s s range S D at 2x 106 cycles. The mean value ji and
the standard deviation a of S are computed by using the s t r e s s ranges S r t and
S D given in the guideline of fatigue design (JSSC, 1989). Table 4 shows the
computation results for five attachment categories.
Damage to Cause Failure ( D f ) . Miner's law is chosen here because it generally
provides good results and is easy to use. The mean value JLL and the standard
deviation a of D f are assumed to be 1.0 and 0.1, respectively.

The random parameters described above are all assumed to be log-normally

distributed.
Table 2 Mean Values and Standard Deviations
of Impact Factor Ratio I
40m 60m 80m
u 0.877 0.866 0.877

o 0.033 0.011 0.0058

Table 3 Mean Values and Standard Deviations

of Headway Ratio H
40m 60m 80m
u 0.10580E+01 0.10880E+01 0.11253E+01

o 0.18300E+00 0.20740E+00 0.25700E+00

 619
Table 4 Mean Values and Standard Deviations of Stress Range Ratio S

Attachments Attachment2 Attachnent3 Attachment4 Attachment5

S rt: u 188 126 164 235 323

(MPa) o 15 22 28 36 50

So (MPa) 155 80 100 125 155

S : u 0.121E+01 0.158E+01 0.164E+01 0.188E+01 0.208E+01
o 0.968E-01 0.275E+00 0.280E+00 0.288E+00 0.323E+01

Risk Analysis of Fatigue Failure

The f a t i g u e failure function defined by Eq.(6) has a high nonlinearity. For s u c h a

h i g h l y nonlinear limit s t a t e function t h e u s e of t h e IFMPUC mentioned early i s
effective.

Eq.(6) is rewritten t h e same t y p e of E q . ( l ) a s

n _ Vt_ M 3 G 3 H 3 I 3 T
Dr- N D • g3 ' U (8)
Thus, t h e conditional failure probability P T °(x') is e x p r e s s e d a s
Pr°(x') = 1- FOT(DT) (9)

Several calculation r e s u l t s are shown in Tables 5 and 6. These t a b l e s show t h e

f a t i g u e failure probability P* and s a f e t y index J3 of s t e e l s t r u c t u r a l elements of
highway b r i d g e s for v a r i o u s s p a n l e n g t h and for v a r i o u s attachment c a t e g o r i e s ,
r e s p e c t i v e l y . In t h i s s t u d y (3 is calculated b y / ? = - ® _ 1 (P T ) in which 0 _ 1 ( • ) i s t h e
i n v e r s e function of s t a n d a r d normal distribution function 0 ( • ). The s a f e t y
i n d i c e s obtained h e r e are c o n s i d e r a b l y small compared with t h e calculation r e s u l t s
p r e s e n t e d by Nyman and Moses (1985) for t h e AASHTO code. A reason for t h i s
d i f f e r e n c e lies in t h e d e s i g n v e h i c l e models. The J a p a n e s e model ( s e e Fig.2) has
l a r g e axle s p a c i n g s .

A f a t i g u e failure probability or a s a f e t y index that d o e s not v a r y significantly

with s p a n l e n g t h and attachment c a t e g o r i e s i s t h e goal for a n y d e s i g n model. It
can be s e e n from Tables 5 and 6 that t h e amount of d i f f e r e n c e between t h e failure
probabilities for t h e s p a n l e n g t h L=40, 60 and 80 (m) is not significant, but t h e r e
is a significant difference between t h e failure probabilities for each attachment

Table 5 Fatigue Failure Probability P« and Safety Index 0

for Various Span Length

40m 60m 80m

Pf 0.262976E-02 0.967893E-03 0.267471E-02

0 2.79 3.10 2.79

Table 6 Fatigue Failure Probability Pf and Safety Index 0

for Various Attachment Categories

Attachnentl Attachment2 Attachment3 Attachment4 Attachments

Pf 0.355120E-01 0.459188E-02 0.262976E-02 0.327037E-03 0.921716E-04

0 1.82 2.60 2.79 3.41 3.74

620
c a t e g o r y . T h i s is a s h o r t c o m i n g s i n h e r e n t in t h e g u i d e l i n e s of f a t i g u e d e s i g n in
J a p a n (JSSC, 1989).

CONCLUSIONS
T h i s p a p e r p r e s e n t s a r i s k a n a l y s i s of f a t i g u e f a i l u r e of s t e e l s t r u c t u r a l e l e m e n t s
of h i g h w a y b r i d g e s u s i n g a n efficient M o n t e - C a r l o P r o c e d u r e . T h e main r e s u l t s
a r e a s follows:
(1) T h e f a t i g u e f a i l u r e p r o b a b i l i t i e s a n d s a f e t y i n d i c e s of s t e e l s t r u c t u r a l
e l e m e n t s a r e c a l c u l a t e d for v a r i o u s s p a n l e n g t h of simple g i r d e r models a n d for
v a r i o u s a t t a c h m e n t c a t e g o r i e s . I t is p o i n t e d o u t t h a t t h e r e is a s i g n i f i c a n t
d i f f e r e n c e in f a t i g u e f a i l u r e p r o b a b i l i t i e s for e a c h a t t a c h m e n t c a t e g o r y .
(2) T h e s a f e t y i n d i c e s o b t a i n e d for t h e JSSC g u i d e l i n e a r e too low c o m p a r e d w i t h
t h o s e for t h e AASHTO c o d e . A r e a s o n f o r t h i s d i f f e r e n c e lies in t h e d e s i g n v e h i c l e
models w h i c h h a v e l a r g e axle s p a c i n g s . Development of t h e f a t i g u e p r o v i s i o n s a n d
p r a c t i c a l r e l i a b i l i t y - b a s e d d e s i g n method for h i g h w a y b r i d g e s in J a p a n is d e s i r e d
a s soon a s p o s s i b l e .
(3) T h e full p r o b a b i l i s t i c f a t i g u e r i s k a n a l y s i s is e f f e c t i v e l y p e r f o r m e d b y t h e u s e
of t h e IFMPUC.

ACKNOWLEDGMENTS
T h e a u t h o r s would like t o a c k n o w l e d g e f i n a n c i a l s u p p o r t for t h e i r s t u d i e s on
d e v e l o p i n g p r a c t i c a l r e l i a b i l i t y - b a s e d f a t i g u e d e s i g n m e t h o d of b r i d g e s t r u c t u r e s
from t h e Society of Materials S c i e n c e , J a p a n a n d t h e H a n s h i n E x p r e s s w a y P u b l i c
Corporation.

REFERENCES
B u c h e r C.G. (1988). A d a p t i v e s a m p l i n g - a n i t e r a t i v e f a s t M o n t e - C a r l o p r o c e d u r e .
Structural Safety, 5, 119-126.
HDL Committee (1986). Report on investigation of Design Load Systems on
Hanshin Expressway Bridges. H a n s h i n E x p r e s s w a y P u b l i c C o r p o r a t i o n
(in J a p a n e s e ) .
J a p a n Association of Road E n g i n e e r s (1980). Specifications for Highway
Bridges, M a r u z e n Book Co., T o k y o (in J a p a n e s e ) .
J a p a n Society for Steel C o n s t r u c t i o n (1989). Guideline of F a t i g u e Design, (in
Japanese).
Liu P.-L. a n d K i u r e g h i a n (1986). M u l t i v a r i a t e d i s t r i b u t i o n models with p r e s c r i b e d
m a g i n a l s a n d c o v a r i a n c e s . P r o b a b i l i s t i c E n g i n e e r i n g M e c h a n i c s , Vol.1,
No.2, p p . 1 0 5 - 1 1 2 .
Nyman W a n d Moses F (1985). C a l i b r a t i o n of b r i d g e f a t i g u e d e s i g n model.
Jour, of Structural Engineering, ASCE, Vol.111, No.6, pp.1251-1266.
H a n s h i n E x p r e s s w a y P u b l i c C o r p o r a t i o n a n d Society of Materials S c i e n c e , J a p a n
(1989). Report on Investigation for Developing Practical Reliability -
Based Design Methods for Fatigue of Bridge Structures (in J a p a n e s e ) .
S h i r a k i W. (1990). An e x t e n s i o n of i t e r a t i v e f a s t M o n t e - C a r l o (IFM) p r o c e d u r e a n d
its applications to time-variant s t r u c t u r a l reliability analysis.
Proceeding of ICOSSAR'89, Vol. , pp.1015-1018.
WS3C4

PROBABILISTIC F A T I G U E D A M A G E PROPERTIES OF M A T E R R I A L S

Pan Z E N G
Institute of Applied Mechanics, Southwest Jiaotong University,
Chengdu 610031, Sichuan Provience, P.R.China

ABSTRACT

Variety of natural damage exists in materials due to the inherent inclusions, small holes, etc., which will grow to make
materials failure under loading. According to a lot of experimental phenomena and engineering investigations of fa-
tigue, the following basic characteristics could be found: 1) irreversible damage process, 2) stochastic and probabilistic
aspest, 3) field effect. In order to describe the mechanical properties of materials, viz.PFDP(probabilistic fatigue dam-
age properties), the present paper propoeses a theoretical model from macroscope aspect aiming at its applications of
practical structures considering these properties. Some test results are illustrated to prove the efficiency of proposed
model.

KEYWORDS

Fatigue; Damage; Probabilistic.

INTRODUCTION

Most defects detected in practical components are randomly oriented or distributed, which could be considered as
their natural damage before loading and may become the main causes to lead the life of comeponent large scatter af-
ter loading. Such a complex situation has been a major difficult in the assessment of structural reliability. So far there
have been some useful investigations and researchs on continuum damage mechanics (CDM) including the work done
by Kachanov, Rabotnov, Ashby and Dyson, on micromechanism of fatigue process (Field and Behnaz, 1982; Baxter,
1983), on stochastic and probabilistic aspests of fatigue (Provan, 1980; Kozin et al., 1981), But there still exists a lack
of everall understanding and description of fatigue including its damage, probability and localed field effect. There-
fore there is an urgent need for studies on this topic, aiming at estimation of probabilisic distribution of fatigue life
(N) for structural components.

621
622

DESCRIPTION OF PFDP

Based on many investigations of fatigue both in microscope and in macroscope, the present paper, first, proposes the
basic hypotheses of PFDP (Probabilistic Fatigue Damage Properties), secondly, establishs the expression of
probabilistic damage for basic element, then, that for field or structure.

Basic Hypotheses of PFDP

(1) Isotropy of material

(2) Homogeneous distribution of natural damage before loading
(3) Developing model of mechanical damage could be described as
d D / d t = 0D (1)
where D is damage variable, fi: damage constant.
(4) The probabilistic character of fatigue life could be described by the well-known Weibull distribution or
Log-normal one.

Probabilistic Damage of Basic Element

Based on the basic hypothese (3), The equation of damage failure state for a basic element A V with original damage
D0(x,y,z) could be solved as follows, the curve is shown in Fig. 1.
Doe* = CF (2)
where CF is the critical damage constant of material.

0 t(failure life)

Fig. 1. Curve of damage failure state of material

According to hypothese (4), the probabilistic expression of the basic element A V in damage failure state could be
written as:
Fc(t,x,y,z) = l-exp{^(D0(x,y,z),t) - AV} (3)
where Fc(t,x,y,z) is the life failure rate for the point (x,y,z), 0~is the function vector for Weibull or Log-normal distri-
bution, A V is the damage space.

Eg.(3) means that the probabilistic damage produced by original damage D0(x,y,z) could be expressed in the
probabilistic distribution of life failure rate under failure state Eq.(2).
 623

Probabilistic Damage of Field

Based on the studies of element, by Weakest Linkage Theory of unequal strength, the expression of fatigue
probabilistic damage of field could be infered as:
F(t)=l- fl [1-Fe(t,xify,,zi)]

= 1 - limn[exp(^CD a (x l ,y, I 2.),t)AV | ]

= l-exp[J v T(D 0 (x,y,z),t)dV] (4)

where the subscript i denotes every element.

MATERIAL PARAMETERS OF PFDP

The basic probabilistic model expressed in Eq.(4), after simplified and modified on an assigned probabilistic distribu-
tion, could be used to estimate or predict the probabilistic distribution of the life (N) or Log-life (t) for a component
with original damage D0(x.y,z) if the material constants of PFDP are obtained. Some contents are given below.

PFDP Model on Log-normal Distribution

After mathematically simplifying for Eq.(4) at the maximum damage point P0(xo,y0,Zo), t h e density of probabilistic
distribution of fatigue life for a component with original damage could be estimated by
i , (t-vs)2
pjt) = T ex
P(- -} (5)
^2iT<
Where the subscript s denotes structural component, the t means lg—life, y^ al are the mean value and variance
in Log-normal distribution, which could be calculated by following formulae:
ys= - i l U - R G / M g D ^ - U - R G / M g C , , ] (6)

'•Td;K1~RO«) ,b
.-c,-R°.)'b.|«DJ (7)
J v

in which
equivalent damage variable at point P0
RG( equivalent damage gradient at point P0
f factor for the mean stress caused by loading
damage space
0,lgCF,b„b2: material constants of fatigue damage failure state in PFDP
Ai,A2,B1,B2: coefficients of damage gradient

PFDP Model on Weibull Distribution

After similar treatment for Eq.(4) at point P0(x0, y0, z^, the Weibull distribution form of the density of probabilistic
624
distribution of fatigue life for a component could be estimated by
m N-0 m . N-0 m
Pw(N) = - ^ ( — ^ ) B ' - ' « P l - < — M - - 1 (8)

Where m„ a„ 0, could be calculated by yt and a\ of formulae (6) and (7) ( Zeng et al., 1988 ). Here N indicates
the fatigue life.

Implementation of Testing for Material Constants

It is important to obtain the material constants of the proposed model before its application. The p-s-n testing is
usually used to investigate probabilistic properties of fatigue, which actually is the probabilistic s-n testing. Here,
two schemes of fatigue p-s-n testing have been suggested to obtain the material constants of PFDP based on the
proposed model.
a) p—s-n testing scheme using the standard small smooth and notch specimens.
b) p-s-n testing scheme only using notch specimens.
After having the basic testing data, the regression method would be used to solve the PFDP material constants.

EXAMPLES AND VERIFICATIONS

Some examples and verifications are given for material 40Cr, on both Log-normal distribution and Wwibull one.
Using p-s-n testing scheme a), the PFDP material contants on Log-normal distrbution are obtained as follows:
0=0.07546, lgCF = 3.1254 (lgMPa)
b, = -2.0967tx 10"7(m3), b 2 =7.67l7ix 10-8 (m3 / lgMPa)
A, = -2.2942, A2 = -2.2917
B, = -0.1411, B2 = -0.1215
Then applying PFDP model on Log-normal distbution the paper estimates the probabilistic distribution of fatigue
life (N) of another five kinds of specimens under various loading, which are compared with the results of fatigue test-
ing shown in Tab. 1.

Table 1. The results of testing and estimation

on Log-normal distribution

Testing conditions
Specimen no. Testing results Estimated results

1
C y c l e

Pa(kN) Pm(kN) Mean(lgN) Variance Mean(lgN) Variance

ASP-21 22.6 0. 4.9652 0.1228 5.1162 0.1712

ASP-22 17.1 5.5 5.6036 0.2228 5.7150 0.1641
ASP-23 17.1 0. 6.0306 0.2034 5.7490 0.2273
ASP-31 12.6 0. 5.1388 0.1058 5.2497 0.1239
ASP-32 12.6 6.6 4.7764 0.0758 5.1972 0.0833
 625
The corresponding reliability curve of specimen No. ASP-31 is presented in Fig.2. Also, the PFDP model on
Weibull distribution is applied in the current examples and verifications, and the reliability curve of ASP-31 is illus-
trated in Fig.3.

Estimated curve
Testing curve

50 100 150 200 250

Number of cycles ( x 103)
Fig.2. Reliability curve of ASP-31 on Log-normal distribution

Estimated curve

Testing curve

50 100 150 200 250 300

3
Number of cycles ( x 10 )

Fig.3. Reliability curve of ASP-31 on Weibull distribution

As compared with the results of testing data, the results estimated by PFDP model have given the better prediction. A
relatively larger data scatter in fatigue data is observed as shown in Fig.2 ang Fig.3, which is obvious characteristic of
fatigue therefore needed the probabilistic methods to describe it, and the common methods in fatigue design are very
difficult to do it.

SUMMARIES

A major area of interest nowadays is the probabilistic problems of fatigue and its application, the present paper has
626
made an effort on probabilistic fatigue damage properties of materials, which indicates a way to deal with these of fa-
tigue. Some contents are summarized as follows:
(1) It is suggested that some basic hypotheses about isotropy, homogoneous, developing model and probabilistic dis-
tribution form of damage, which are considered as the foundation of PFDP model.
(2) It is studied that the equation of damage failure state, the expressions of probabilistic damage of basic element and
field.
(3) PFDP model on Log-normal distribution and Weibull one have been established to estimate the probabilistic dis-
tribution of fatigue life for a component under loading. And two testing schemes for obtaining the material
contants of PFDP model are suggested.
(4) Some examples and verifications have shown that the proposed PFDP model could give the better prediction of
probabilistic distribution of fatigue life.

ACKNOWLEDGEMENT

The author expresses his thanks to Prof. X.L.Yu, Prof. X.F.Sun for their help, Mrs. L.Y.Zhang for her help in writ-
ing of the Paper.

REFERENCES

Ashby, M.F. and B.F. Dyson (1984). Creep damage mechanics and micromechanism. In: Proc. 4th Int. Conf. on
Fract. Mech., Vol.1, pp. 3-30. New dehli.
Baxter, W.J. (1983). Oxide films: quantitative sensors of metal fatigue. ASTM STP 811.
Field, J.L., F.Behnaz and R.N.Pangborn (1982). Characterization of microplasticity developed during fatigue. In:
Proc. A Conf. on Fatigue Mechanisms Spor. by ASTM E-9, pp. 78-90. Dearborn.
Kachanov, L.M. (1958). The time to failure under creep condition. Izv. Akad. Nauk., SSSR. Tekh. 8,26-31.
Kozin, F. and J.L. Bogdanoff (1981). A critical analysis of some probabilistic models of fatigue crack growth. Engng.
Fract. Mech.,20, 597-603.
Provan, J.W. (1980). A fatigue reliablity distribution based on probabilistic micromechanics. In: Defects and
Fracture(G.C.Sih,ed.), pp. 105-130. McGraw-Hill, New York.
Rabotnov, Y.M. (1969). Creep problems in Structural Members. North-Holland, Amsterdam.
Zeng, P. (1988). Studies on Probabilistic Fatigue Damage Mechanics. Ph.D. Dissertation, Tsinghua University, Beij-
ing.
WS3d1
SCATTER AND TRANSFERABILITY OF FATIGUE DATA AT
SERVICE LOADING

K. Heckel and Ch. Kra

University of the Federal Armed Forces Munich,

Werner-Heisenberg-Weg 39, D-8014 Neubiberg, FRG

ABSTRACT

The two-parameter Weibull-distribution and the Basquin-law were used to

define a scatter band function. This function enables to predict the
fatigue behavior of other components as tested. To apply the model, the
following assumptions must be true for all components under considera-
tion: The fatigue crack must nucleate from the surface, the material,
the state of the surface and the stress history (stress-time dependence)
must be the same.

KEYWORDS

Scatter band function; transferability; prediction of fatigue; fatigue

strength; fatigue life.

INTRODUCTION

A machine part or a test specimen can only sustain a service or fatigue

loading if no fatigue crack is initiated. This means that in macroscopi-
cally homogeneous materials, each surface element has to sustain crack
initiation. Due to the fact that fatigue data show a natural scatter, it
is possible to determine only the reliability R. If reliability (R(i))

627
628
of the z surface elements is known, the reliability of the whole part
(R) is given by multiplying the R(i) of all the surface elements (theo-
rem of compound probability):

R = J^Rd) • <D
i=l

This fundamental equation is independent of the type of the distribu-

tion-function to describe R(i).

The sample size in fatigue results is not large enough to decide by

statistical methods for the benefit of one or another distribution
function. There are three main reasons which endorse to favour the two-
parameter Weibull distribution-function (Weibull, 1939). The Weibull
distribution-function:

is physically well-founded (weakest link concept),

has a good handling,
is conservative in the estimation of the reliability.

The distribution function describes the probability

F - 1 - R (2)

that a maximum stress o initiates a fatigue crack after a number of N

cycles. Assuming that a is constant on the whole surface S of an (un-
notched) specimen the reliability is given by:

R(a) = 1- F(a) = exp [- f- (^-)k] (3)

(N - const) o v
o

where o and k are the two Weibull parameters (of the reference speci-
men: S = S ) , which can be determined by fitting of eq.(3) to experimen-
tal results, for instance by maximum likelihood estimation (MLE). If the
specimen under consideration has the surface S, eq.(3) gives R.
 629
In the case of an inhomogeneous stress field at the surface

the surface is divided into such small elements dS that the stress can
be regarded to be constant at the element. According to eq.(l) and (3)
it finally follows:

The size faktor Z enables to calculate R for arbitrary shaped parts

provided that the stress distribution a (x,y,z) is known.

To describe the scatter of the number of cycles to initiate a crack at

constant a it is assumed that, in the range of consideration, k is
max °
constant and a — o (N) follows the Basquin-law:

If eq.(6) is put into eq.(5) one finally receives:

Eq.(7) is the common description of the scatter band of the normalized

o /a . and N/N . lifetime function (Heckel, 1987).
max7 0 ' 0

APPLICATION

The applicability of equ.(7) to transfer fatigue data of constant ampli-

tude tests between specimens of different shape was demonstrated in many
previous publications. To examine the applicability of eq.(7) at service
loading, a great number of fatigue tests with a standard random load se-
quence of Gaussian type and the standard load sequence MiniTWIST were
performed. Two different CT-type specimens and four notched flat bar
specimens of different shape, made from 7075 T 7351 alloy, were used
630

(Fig.l). The specimens were axially loaded in the tension range.

— 20 —

M s P
n

^
,

1* loo J

CT25 CT40
> - 2.5 p - 4.0
u- 22.5 a n- 25.0

Fig.l. Dimensions of test specimens in mm, thickness: 14 mm

To determine the size factor Z, the stress integral according to eq.(5) was
evaluated by FEM. The stress integral depends on k. The size factor Z,
which is the quotient of two stress integrals, is in the range of conside-
ration practically independent of k. The size factors of the specimens
(related to the reference specimen FLA1, Z = 1) which were used for predic-
tion, are listed in table 1. To fit the experimental results of a reference
specimen (Z = 1) to eq.(7), the three parameters o , n, and k must be de-
termined. There is a fundamental difficulty to determine n with sufficient
accuracy from a limited number of tests. According to a suggestion in
Haibach (1989) n was chosen to be 0,2. The parameters o and k were then
fitted to experimental results by MLE.

The test results which were determined with specimen FLA 1 were used to fit
2
eq.(7). The following expressions were received (a in N/mm ):

0,2 12,70
mX a
N
r> • n T r, r

9633 ] ]

M 0,2 7,29 (8)

Gaussian: R — exp [-Z [ N
8484 ] ]

MiniTWIST: R = exp [-Z [

 631
Table 1. Tests and size factor Z

specimen number a load size f a c t o r 1

max 2
(Fig.l) of tests N/mm sequence Z

FLA 1 22 624 Gaussian 1,00

FLA 1 16 558 Gaussian 1,00
FLA 2 17 554 Gaussian 6,29 1
FLA 2 18 498 Gaussian 6,29
FLA 3 19 551 Gaussian 2,54
FLA 4 18 530 Gaussian 10,00
CT 25 32 632 Gaussian 0,91
CT 40 26 653 Gaussian 1,57

FLA 1 13 652 MiniTWIST 1,00

FLA 1 20 555 MiniTWIST 1,00
FLA 1 13 478 MiniTWIST 1,00
FLA 4 20 556 MiniTWIST 10,00

Inserting Z from Table 1, the eqs.(8) can be used to predict the fatigue
behaviour of the other specimens. The test results which were experimen-
tally determined with the specimens FLA 2, FLA 3, FLA 4, CT 25 and CT 40
were used to control the prediction according to eq.(8). For this pur-
pose the test results of these specimens were also fitted to eq.(7).

1 - -?
/ //
/
/ /
FLA 2
/ FL.A 3 /l
1U / ,
9- / /
8 - / ■i CT25 Jv Gaussian
,- 6
c
7
° - / >TLA2 / 'FLA u
o / 1'
♦ CTA /
U 3
/ / /
•o
Q) / / / /
Q. /
O
ID
o / /
/
J
/
/ //
2 /
/
/
♦ FL/> U Nlini rwisT
/
m5
- 5 /
10
10 I 3 k (3 5 7 3 3106 1 \ I 5
N 50% experimental

Fig.2. Comparison of N50% prediction and N50% experimental

632
Fig.2 shows the comparison of the predicted and experimentally deter-
mined number of cycles to initiate a fatigue crack at a reliability of
R = 0,5 (= N50%).

CONCLUSION

The transferability requires:

same, macroscopically homogeneous material,

same surface conditions,

same load sequence,
same kind of crack initiation.

No less than 30 tests are desirable to determine the parameters of the

scatter band function (eq.(7)).

It was shown that the proposed model is very suitable to transfer

fatigue date at service loading from a reference specimen to specimens
of different shape. The predictions are predominantly conservative.

REFERENCES

Basquin, O.H. (1910). The Exponential Law of Fatigue Tests, Proc of the
ASTM. 10, 625 - 630
Haibach, E. (1989) Betriebsfestigkeit. VDI-Verlag GmbH, Dusseldorf
Heckel, K. (1987). Scatter and Size Effect at Fatigue Loading, Proc.ICM-5.
Beijing. China 3.-6.6.87, Vol.1 587 - 593
Kra, Ch. (1989). Fatigue Life Description of Randomly Loaded Notched Speci-
mens Based on the Statistical Size Effect, Diss. UniBw-Munich, FRG (in
German) (1989)
Weibull, W. (1939). A Statistical Theory of the Strength of Materials,
IV A, Stockholm, Sweden, Handlingar Nr. 151.
WS3d2

A PROBABILISTIC CRACK GROWTH MODEL

BASED ON NONLINEAR DAMAGE ACCUMULATION

F. Ellyin

Department of Mechanical Engineering

University of Alberta
Edmonton, Alberta, Canada T6G 2G8

ABSTRACT

A probabilistic crack growth model based on nonlinear damage accumulation criterion is

presented. The nonlinear damage function account for the effect of loading sequence. The
resulting simulation model is compared to the experimental data, and the results of an earlier
linear damage model. The nonlinear damage model indicates better correlation with the
experiments. It also has a better physical interpretation of the phenomenon.

KEY WORDS

Crack growth; cyclic loading; damage zone; fatigue failure; nonlinear damage; probabilistic
simulation.

INTRODUCTION

The strength of a structural member is reduced due to the presence of a crack (or deflect), and
the subsequence crack growth results in further weakening of the member. The damage
tolerant design methodology allows for the crack growth to a certain limit, as long as the
residual strength of the member is greater than the applied load effect. A strategy of periodic
inspection is then instituted to detect cracks (defects) of a predetermined size, e.g. see Ellyin
(1985). The damage tolerant design methodology therefore requires the ability to predict crack
growth in a probabilistic manner. Also, in making risk assessment studies of critical
components in a system, there is a need to incorporate statistical aspects of the crack growth
process.

A brief survey of investigations on the probabilistic crack growth modelling is given by Ellyin
& Fakinlede (1985). Two major inputs are required: (i) a suitable damage function, and (ii)
a failure criterion. The damage function quantifies the damage accumulation rate, and is
directly related to the applied load. The failure criterion specifies the critical value of the
damage function at which the material fails. In most investigations, a linear damage rule is
used which results in reduced computation effort. However, such a damage law has certain
633
634
disadvantages, e.g. it cannot predict the effect of loading sequence. Recently, Ellyin and
Fakinlede (1988) have presented a probabilistic crack growth model based on a nonlinear
damage accumulation criterion. The damage function takes cognizance of the effect of
loading sequence.

In this paper a probabilistic simulation by a nonlinear damage accumulation will be outlined.

FORMULATION

The probabilistic crack growth model is developed based on the following assumptions:

(i) There exists a damage zone (DZ) ahead of a crack tip, beyond which the accumulation
of damage is insignificant. The damage zone is taken to coincide with the reversed
plastic zone.

(ii) The damage zone is divided into finite material elements with fatigue damage
resistance (FDR) that are random observations from the same probability distribution,
see Fig. 1.

(iii) The material elements mentioned in (ii) are so dimensioned that macroscopic
(continuum) laws apply.

(iv) At each material element damage accumulates according to the following nonlinear
damage law.

Nonlinear Damage Law

A material element subjected to a given stress/strain or energy level, may accumulate damage
at each cycle. When the absorbed energy reaches a certain level, cracks may initiate. In an
energy versus life plot, the ensemble of these crack initiation points will form a curve, as
shown in Fig. 2, which is termed damage curve. The method of constructing the critical
damage curve is explained by Golos and Ellyin (1988). Cycling beyond the damage curve
would cause the initiated cracks to propagate. Fatigue failure of a small material element
would take place after a certain amount of crack growth. The fatigue failure curve shown in
Fig. 2 is mathematically expressed by

AW = K Nf + C (1)

where AW is the strain energy density per cycle, Nf the number of cycles to failure, K and a
are material constants. The constant C is the nondamaging energy associated with a material*s
fatigue (endurance) limit in a virgin one step loading state, i.e. fatigue limit associated with
the crack initiation stage. For all crack propagation stages, the material has an "apparent"
(reduced) fatigue limit defined by AW , see Fig. 2.

The strain energy density, AW, in (1) could either be the plastic energy, AWP (hysteresis
energy), or the total energy, AW1, which is the sum of the plastic energy and the elastic energy
associated with the positive stress.
 635
historical damage

• damage accumulated per cycle of loading

£ = fatigue damage resisance

crack >

i 4 3 2 1
Element No.
Fig. 1 Schematic illustration of material element in front of a crack and their fatigue
resistance and cumulative damage

log AW
Life Curve

-Damage Curve

n
1 N
f2 N
f1 N
end N
* log N f
Fig. 2 Variation of strain energy density versus number of cycles for both damage and life
curves and the definition of AW

A nonlinear damage accumulation law was proposed by Kujawski and Ellyin (1984) for two
step loading and later generalized by Golos and Ellyin (1987) for multiple loading steps. This
damage law for j levels of loading is given by:
) V Vi n.
/ ( A ^ i , AW2i...,AWp = (A)^«+(A) |n /n 3 2
*(/-!) + - ^ = 1.0 (2)
*Nt N72
4 J NTt/'-DJ
4

where m = log [(AW| - C)/AW*] i = l,2,...j (3)

and AWj = AW? + AWe+ (4)

636
AW? being the plastic strain energy density per cycle and AW^ is the elastic part of the strain
energy associated with the positive stress. In a uniaxial loading condition

A W = llSl (Ao-6o 0 )Ae* + 6o 0 Ae* (5)

l+n*

and

APP + = J - ( A £ + a )2 (6)
2£ 2

where n is the strain hardening exponent and 5a 0 is the increase in the elastic range for a
non-Masing material description, see Ellyin and Kujawski (1984). For an ideal Masing
material n = n' and Sa 0 = 0.

For each material element, the energy function f(AWj, AW2, ..., AW:) is evaluated at each
cycle. The failure criterion then becomes
f(AWv AWV ..., AWp = £ (7)

where % is a unit random variate. It is the random fatigue damage resistance (FDR) of each
material element location, Fig. 1.

Stress and Strain Field Ahead of a Crack

The elastic-plastic strain and stress distribution ahead of a crack commonly referred to as HRR
singularity fields, see Hutchinson (1983) when modified for the cyclic loading are:

Ac} = «'(-S£Q-)*'*» e„(n', 6)

(8)
A
°.y = a/-3£M-'-i o„(n', 6)

where a' = cyclic yield stress, E = Young's modulus, n' = cyclic strain hardening exponent,
r, and 0 are polar coordinates and e,y and o,y are dimension functions of n' and 0, and In,
is a function of n' only. Ae^, Aay and AJ are the range of cyclic strain, stress and J-integral,
respectively; and a' = (2E/a' )(a'/2K')^ n where K' is a coefficient with dimensions of stress
which appears in the cyclic stress/strain relationship, see Ellyin and Kujawski (1984).

The energy function, fCAW^ AW2, ...) is evaluated in front of the crack, using the HRR fields
(8). The number of cycles to failure at a loading step i, is obtained from an appropriate
fatigue failure criterion such as (1). When the damage resistance of an element i is exceeded
before all the other elements, then the random crack growth rate is given by:

(*°L) = Hi (9)
dN n
 637

where x* is the size of the material element in Fig. 1, and n is number of cycles spent at that
configuration.

RESULTS AND DISCUSSION

The predictions of the crack growth simulation model (9) will be compared with the
experimental results. It should be pointed out, however, that the experimental results are
deterministic while the proposed theory give a random growth rate output. The comparison
therefore has to be made with some measure of central tendency of the simulated probability
distribution. The median value is chosen for the comparison since it is least susceptible to the
input variance. Figures 3 and 4 show the comparison between the predicted median of the
probabilistic model and the experimental data for A516 Gr.70 steel, taken from Ellyin and Li
(1984) and an aluminum alloy 2219-T851 from Saxena and Hudak (1971). Included in the
figures are predicted median values of the linear probabilistic simulation of Ellyin and
Fakinlede (1985), using the statistical Miner's law.

- # ( H , o)
(10)
N.

where N indicates normal probability distribution, the mean value u : 1, and a is the variance
of the normal density function.

A516-Gr 70-Steel
X" = 7.432*10 s m
AK = 200.0MPaVm

£ b

p.
o _
*-« T
a, o

linear model
non-linear model
non-linear model
(Massing Behaviour)
I i|ini|iiii|mi|imi|Ui|n i i I i|iiii|ini|iiii|iiqi|i|UH ' l""l""WI'l'l1
ltf lrf lrf 103
Stress Intensity Factor, MPavm
Fig. 3 Comparison between predicted and experimental data for the crack growth rate vs.
stress intensity factor of A516 Gr. 70 steel
638

2219-T851-Aluminurri
X"= 5.140*10"'m
AK = 30.0MPaVm

linear model
non-linear model

10° 101 ltf

S t r e s s I n t e n s i t y Factor, M P a V m
Fig. 4 Comparison between predicted and experimental data for crack growth rate vs.
range of stress intensity factor of 2219T851 aluminum alloy

It is seen from both figures that the predictions of the nonlinear model are closer to the
experimental results than those of the linear model. In Fig. 3 also a comparison is made
between the predictions of evaluating the strain energy density function AW using either the
non-Masing material description or the ideal Masing one. The difference between the two
does not appear to be very significant in this case.

An interesting outcome of the simulated crack growth distribution is that it can be best
approximated by a log-normal density function. There is experimental results which support
this conclusion, e.g. see Bertrand, Lefebvre and Ellyin (1982).

REFERENCES

Bertrand, M., Lefebvre, D. and Ellyin, F. (1982). J. de Mecanique Theorique et Appliquee,

I, 1-18.
Ellyin, F. and Li, H.P. (1984), ASME J. Pressure Vessel Technol. 105, 255-260.
Ellyin, F. and Kujawski, D. (1984). ASME J. Pressure Vessel Technol. 106, 342-347.
Ellyin, F. (1985). Theo. Appl. Fract. Mech. 4, 83-96.
Ellyin, F. and Fakinlede, CO. (1985). Engng. Fract. Mech. 22, 697-712.
Ellyin, F. and Fakinlede, C O . (1988). Int. J. Fract. 36, 137-149.
Golos, K. and Ellyin, F. (1988). ASME J. Pressure Vessel Technol.
Golos, K. and Ellyin, F. (1987). Theo. & Appl. Fract. Mech. 7, 169-176.
Hutchinson, J.W. (1983). ASME J. Appl. Mech. 50, 1042-1051.
Kujawski, D. and Ellyin, F. (1984). Int. J. Fatigue 6, 83-88.
Saxena, A. and Hudak, S.J. (1971). Fracture Mechanics, ASTM STP 677, 215-232.
WS3d3

Hazard Rate of Structural Components under Fatigue Environment

Including Random Overloads

H. Tanaka*, T. Tanaka** and A. Tsurui**

* Dept. of Indus. &: Sys. Eng., Hiroshima Univ.

Higashi-Hiroshima, 724 Japan
** Dept. of Appl. Math. & Phys., Kyoto Univ.
Kyoto, 606 Japan

ABSTRACT

A method is proposed for estimating the hazard rate of structural components under fa-
tigue environment including random overloads. Fatigue crack growth processes are first
stochastically analyzed by the use of a Markov approximation method in consideration of
the retardation effect due to the overloads. Hazard rate of structural components which
allow the ductile failure as well as the fatigue one is then investigated with the aid of an
importance sampling simulation procedure. One of the interesting results shows that the
crack growth retardation due to overloads would rather much effect in the range of high
hazard rate.

KEYWORDS

Hazard rate; fatigue; random loads; retardation; stochastic crack growth; two-criteria ap-
proach; importance sampling.

1. I n t r o d u c t i o n

We often come across a situation in which the nonlinearity in fatigue crack propagation
processes cannot be disregarded. For instance, if the loading process is "strongly" random,
there will be a possibility of "overloads" that causes the retardation effect in the crack
propagation. In this case, we can not directly apply the Paris' law to describe the crack
propagation. On the other hand, if overload appears, we must take instantaneous ductile
failure into reliability analysis. Thus, the so-called two-criteria approach is required, which
allows fatigue and ductile failure modes.
In this paper, supposing a situation in which a structural component is operated under
random cyclic loads including overloads, we investigate the behaviour of its hazard rate.
A comcept of "delay time" is first introduced according to Arone's study (1986, 1987). By
utilizing a probability distribution function of the delay time resulted from the retardation
effect due to overloads, we then revise a probability distribution function we previously
639
640

obtained for components' residual life (Tsurui et ai, 1986; Tanaka et a/., 1987) so as to
reflect the retardation effect. Using this result, we approximately obtain a crack length
distribution function in view of the retardation effect.
In order to take the ductile failure mode into account, we have to construct a limit
state function reflecting the two failure modes simultaneously. Therefore, we use Burdekin-
Stone's failure criteria (Larsson et ai, 1978), which asserts that the component fails at least
one of the following two events takes place: (i) loading stress exceeds a critical value that
may depend on the current crack length, and (ii) fatigue crack length exceeds a critical
one.
Since the limit state function based upon the Burdekin-Stone's criteria is not simple
enough to calculate the hazard rate analytically, we lastly perform an importance sampling
simulation technique for the calculation (Tsurui et a/., 1989). This simulation method can
give an approximate value of the hazard rate with high accuracy in a very short CPU time.

2. Probability distribution of total delay time

In this section, we simply review the Arone's method (1987) to derive the probability
distribution of total delay time caused by random overloads.
We assume that the component is loaded with the over-stress superimposed on a con-
stant amplitude cyclic stress. Suppose that Xi(n) represents the crack length under the
retardation effect caused by the overload occurred at the n t -th cycle, and X(n) a virtual
crack length under the condition of no overloads. Let us define a delay time ndi(y) at a
crack length y as
ndi(y) = X-1(y)-r\y). (1)
Since the effect of the overload vanishes as time elapses, ndi(y) will converge to a constant
value as y —► oo. We call this limiting value ndi = l i m ^ ^ ndi(y) delay time due to the
overload occurred at the n t -th cycle.
If plural overloads occur, owing to the cross-effect, the total delay time will not become a
simple sum of each delay time. However, if the component is suitably designed, overloading
will take place as rare events. Therefore, we assume that the total delay time after n cycles
of loading is approximately given as Nd(n) = £ t n<j-, and that it has a stochastic nature
due to the randomness associated with the number and magnitude of overloads. Hence, we
treat the total delay time as a stochastic process. Let its probability distribution function
be
F(nd,n) = Pi[Nd(n)<nd]. (2)
To determine F(nd, n), we introduce the following transition probability distribution:

P(nd | n'd,n) = Pi[Nd(n^) < nd | Overload occurs at the ra-th cycle, Nd(n) = n'd\, (3)

where Nd(n^) represents the total delay time after n cycles of loading, including the delay
time due to the overload at the n-th cycle. Letting q(n) be a probability that an overload
takes place at the n-th cycle, we can derive the following equation:

F(ndi n + 1) = {1 - q{n)}F(nd, n) + q(n) £* P(nd \ rid, n)dn>dF{n'd) n), (4)

in which the integral in the second term is of Stieltjes type.

 641
If the transition probability P(nd \ n'd,n) is known, we can obtain the probability
distribution function of the total delay time F(nd)n) as the solution of Eq.(4) under the
adequate conditions. Arone (1987) has proposed a concrete expression for P(nd \ nd,n),
under the assumptions that (i) except for the overloads, the loading process is a constant
amplitude process, and (ii) a parameter associated with a magnitude of retardation effect
obeys an exponential distribution. In this paper, we revise it a little and use the following
transition probability distribution function:

[nd < n i ) ,
(nd > n'd and n^ + nd — n < 0),
P(nd | ridin) =
nd ~n'd V
exp (otherwize)
£(rioo + nd-n)j
(5)
in which p and f represent a shape and a scale parameters of the Wei bull distribution,
respectively. The quantity n ^ represents the number of cycles when the crack with initial
length x0 grows to infinity under the condition of no overloads.

3. R e v i s i o n of t h e Crack L e n g t h D i s t r i b u t i o n

Under the condition of no overloads, we assume that, according to Paris law, the fagitue
crack grows obeying the following stochastic differential equation:

^ = eCnZ*x+VXx+\ (6)
an

in which X ( n ) , Z n , C n , £, A represent crack length after n cycles of loading, amplitude of

loading at the n-th cycle, normalized propagation resistance at the crack tip after n cycles,
mean propagating resistance, material constant, respectively. We also assume that the
processes Zn, Cn are stationary, locally stationary, respectively.
If we can assume exponential decay of correlation for the coefficient processes Zn and
C n , the residual life distribution function H(n \ x0,xc) is given as follows (Tsurui et a/.,
1986; Tanaka et a/., 1987):

\sMcMzn
H(n\x0,xc) = $
X^G(n)
a0aj (2A + 1)

(2A + \)M?K
G(n) = - (x0 x
- \eMcM2Min[n, n^]) * } + e2M^a22nzn

. 2 2 2 /
Min[n,ncx
(*0 • \eMcMzn') A dn'
+e acaznz / eMcMznz
(7)
(XQX - \eMcMzn')

where M c , M 2 , o\, o\ represent the means and the variances of Cn, Z%>x+1\ respectively,
and XQ, XC the initial and critical crack sizes, and <£( •) represents a complementary function
of the standardized normal distribution. Let us denote a residual life distribution function
with retardation as Hn(n \ x0,xc) by taking the effect of random overloads into account.
Since the residual life distribution under the condition t h a t the delay time up to time n
equals to nd is given as H(n — nd \ XQ, XC), Hn(n \ x 0 , xc) is led to
rn
HR(n | x0, XC) = / H(n - nd \ x0, xc)dndF(nd, n), (8)
.'0
642

in which F(n<i, n) is the probability distribution function of the total delay time discussed
in the preceding section.
As we can neglect the probability t h a t the crack length decreases, paying attention to
the arbitraryness of x c , from Eq.(8) we can obtain a crack length distribution function with
retardation WR(X, n \ xQ) as

WR{x, n | x0) ~ 1 - HR(n \ x0i x). (9)

4. H a z a r d R a t e

In the preceding section, the crack length distribution function has been revised so as to
suit the fatigue environment including random overloads. Making use of the result, in this
section, we will give a method to calculate the hazard rate in consideration of two failure
modes, one is corresponding to a fatigue failure mode and the other an instantaneous
ductile one.
In order to take the two failure modes into account, we have to use the so-called two-
criteria approach. Moreover, in case of the calculation, as many uncertainty factors as
possible will be preferably taken into consideration. Random variables adopted in this
study are as follows :

(i) X\: Current crack size X(n) under the condition t h a t the initial size was x0,
(ii) X2: Initial crack size xQ,
(iii) X3: Loading stress at the n-th cycle cr(n),
(iv) X4: Yield strength ay,
(v) Xb\ Tensile strength <jti
(vi) X6'. Fracture toughness Kc.

For later convenience, we use a vector notation X = (A^, • • •, X6) as well.

Now, we will specify a limit state function g(X), the negative side of which corresponds
to the failure region. For this purpose, the Burdekin-Stone's criteria is often utilized to
lead

where Kj stands for the current stress intensity factor and KJC the critical stress intensity
factor. As is well known, K\ is usually the function of X\ and X j , and KJC has been
empirically expressed by Feddersen as a function of Xo, Xt, Xb and X6.
Under the circumstances stated in the previous section, it is obvious that the random
variable X$ takes an overload with probability q(n) and a normal-load (i.e. non-overload)
with probability 1 — q(n). As the result, it is convenient to consider two conditional hazard
rates h^N\n) and M°^(n), the former corresponds to the hazard rate under the condition
t h a t a normal-load takes place at the n-th cycle and the latter t h a t an overload takes place
at the n-th cycle. Each conditional hazard rate can be calculated with the conditional
probability density, that is

h^N\n) = / /A-(*,TC I X3 is a normal-load)d«, (11)

Jg(X)<0

h{°\n) = f fx(*,n\ X3 is an overload)d», (12)

 643
and the total hazard rate h(n) can be obtained through

h{n) = {1 - q(n)}h(N\n) + q{n)h(0)(n) (13)

By taking account of the correlations among the random variables, the probability density
will be expressed as

/ x ( * , n | •) = w*Xl^(xun\ x2)fx3(x2)fx3{x3 | -)/x 4 x 5 (x 4 ,a:5)/x 6 (^6), (14)

where with the aid of the result obtained in section 3,

W (15)
^{X^X>) =
WR{xc,n-l\x2y
because the hazard rate must be calculated under the condition that the component has
not failed yet up to the (n — l)-th cycle.

5. Numerical Studies

The integral in Eqs.(ll) or (12) is too complicated to be analytically carried out. So, we
will go through with the integrations with the aid of Monte-Carlo simulation technique, in
particular, the software package ISPUD (Bourgund et a/., 1986).
Type of distribution and its parameters of each random variable assumed are shown in
Table 1. Since the coefficients of variation of X± and X*> are both small, in this study, X 4
and X$ are, for simplicity, assumed to be independent of each other.

Random variable Type of distribution Mean value Coefficient of variation

Xi\X3 special type of Eq.(15) — —
x2 shifted exponential 2.5 [mm] 0.8
X3 (normal load) shifted Rayleigh 70 [N- mm" 2 ] 0.5
X3 (overload) Weibull 140 [N- mm" 2 ] 0.2
XA Weibull 515 [N-mm-2] 0.05
x, Weibull 587 [N-mm-2] 0.05
x6 Weibull 1641 [N-mm"1-5 ] 0.1

Table 1: Type of distribution and values of parameters

The parameters to specify the special distribution of X\ \ X2 are as follows :

Q 1.0 x 10~4 and 0.5 x 10"4 A 0.5 OiQ 1.0 [mm] £ 0.167
€ 1.0 x 10~ n [mm5-5N-3cycles_1] nz 1000 [cycles] P 1.7 °c 0.2

Table 2: Values of parameters of special distribution

Needless to say, Mz and az must be calculated from the distribution of ^(normal-load),

and Mc has been set to unity. xc is approximately set to the half width of the component
(500 [mm]).
Symbols tied by lines on Figs. 1(a) and (b) correspond to the log-scaled hazard rate
versus number of loading cycles for q = 1.0 x 10"4 and 0.5 x 10 - 4 , respectively. The triangle
644

q= 1.0 x 1 0 ' 4 q = 0.5 x 10" 4

X no overloads X no overloads

A failure by overloads x A failure by overloads

/" -
o failure by normal loads O failure by normal loads
/ ■

10"
5
/

r
\/r:
C
/ o- -°

^ ^ L ^ - L 1

10"-10
5 10
xlO4 cycles xlO 1 cycles
(a) (b)

Figure 1: Hazard rate

and circle symbols represent qhS°\n) and (1 - q)hSN\n), respectively. T h e former means
t h a t the failure is caused by the overload which occurs at the n-th cycle, and the latter by
the normal load. Then, the sum of both constitutes the hazard rate in case that overloads
are superimposed. For the comparison, the hazard rate in case of no overloads is also put
as the cross symbols on the figures.
These figures suggest that in the early stage of low hazard rate the failure caused by
overloads is rather important than the retardation effect of crack growth. Relating to the
assumption of the Poisson arrival of overloads, qh^°\n) changes slowly. On the other hand,
(l-q)h^N\n) changes rapidly, corresponding to the crack growth. T h e overload occurrance
rate q has a significant effect on the retardation, while, in this study, the effect of q on the
overload failure seems to be canceled out by the retardation.

References
Aron-e, R. (1986). Fatigue crack growth under random overloads superimposed on constant-
amplitude cyclic loacing. Engng Fracture Mech., 24, 223-232.
Arone, R. (1987). On retardation effects during fatigue crack growth under random over-
loads. Engng Fracture Mech., 27, 83-89.
Bourgund, U. and C. G. Bucher (1986). Importance sampling procedure using design
points, A User's Manual. Report No. 8-86, Institute of Engng Mech., Univ. Innsbruck.
Larsson, H. and J. Bernard (1978). Fracture of longitudinally cracked ductile tubes.
Int. J. Press. Vess. Piping, 6, 223-243.
Tanaka, H. and A. Tsurui (1987). Reliability degradation of structural components in the
process of fatigue crack propagation under stationary random loading. Engng Frac-
ture Mech., 27, 501-516.
Tsurui, A. and H. Ishikawa (1986). Application of the Fokker-Planck equation to a stochas-
tic fatigue crack growth model. Structural Safety., 4, 15-29.
Tsurui, A., J. Nienstedt, G. I. Schueller and H. Tanaka (1989). Time variant structural
reliability analysis using diffusive crack growth models. Engng Fracture Mech., 34,
153-167.
WS3d4

RELIABILITY ON FATIGUE UNDER STATIONARY GAUSSIAN NARROW BAND RANDOM LOADING

Yihui WU and Hingchu YAO

Graduate School. China Academy Of Railway Sciences

Beijing 100081. P. R. China

ABSTRACT

In this paper, a two block iterative Method on condensed matrix to calculate

the reliability on fatigue under stationary Gaussian narrow band random
loading is presented. Which was constructed on the assumption that the narrow
band random process is frequency determined but the amplitude is probabilistic.
And the cumulative function of the fatigue damage was taken as the limit state
function which is nonlinear, with correlative variables and non-Gaussian
distribution. The reliability index can be obtained given the S-N curve, the
loading time and the spectrum parameters.

KEYWARDS

Reliability, random, fatigue.

INTRODUCTION

Structures always failure due to fatigue under random loading. It is difficulty

to obtain a determined response history analytically for structure under random
excitation. The random vibration theory can give the power spectrum of the
response only. and if the excitation is Gaussian process, then the response is
Gaussian.

For the reliability on fatigue under random loading, two problems of the count
of fatigue damage cumulation and the calculation of the reliability need to be
sovlved. For the first aspect . there are the counting method on sampale process
based on S-N curve and miner's rule (ASCE 1982). which can carry out the
cummulative fatigue damage for every sample process, the method to calculate the
mean fatigue damage per cycle for stationary gaussian narrow band process ( Y. K.

645
646
Lin 1967. J. M. Tunna 1986) and for weakly non-Gaussian stationary narrow band
process (Juneber Jensen 1990). and the probabilistic model for cumulative
damage (Bogadanaof et al. 1985 ) . etc. And for the other we have the equivelent
damage random variable method (Yao 1984 ) . and the method of the assumed
probabilistic distribution of peak random variable (Yao 1984 ) . which transfer
the random process into an single variable based on the Miner's rule and S-N
curve. In this paper. the cumulative fatigue damage under narrow band random
loading is sumed linearity- for each cycle based the Miner's rule . The fatigue
damage for each cycle is the nonlinear function of the peak of the process. The
fatigue failure limit state function under the random loading is the summation
function, which is nonliner. with correlative and non-Gaussian distributive
design variables . For stionary Gaussian narrow band random loading, the peaks
have the Rayleigh distribution.

The reliability on the non-Gaussian distribution correlative variables nonlinear

limit state function can be solved using the advanced JC method (Li et al. 1987))
. But for the random loading process. the duration time to fatigue failure is
not small, which makes the numbers of the varibles of the limit state function
to be too large to calculate the reliability using the computer.

As the correlation parameter of peak is symmetrical and attenuative. a two block

iteration method was derived in this paper, which only includes calculating
condensed matrix. And this method can also consider the effect of mean stress
and the randomness of the creteria for fatigue failure. And for stationary non-
Gaussian narrow band load.thereliabi1ity can also be calculated with this method
if the peak distribution is able to be calculated.

LIMIT STATE FUNCTION

Peak Distribution. Correlation Function And The Correlation Matrix Of Peaks For
Stationary Gaussian Narrow Band Random Loading.

Given the response frequency(0 0 . bandwidth A w and the power spectrum Go . the
correlation function and the distribution density function are as follows :

R«* ( T ) « 2 G 0 / T C O S ( O ) 0 x ) s i n ( A w x/2) (1)

f R (r)« r / a „ * exp (-r2/ (2 a x 2 ) ) (2)

and
a*a - R*« (0)-G o A w
where
R x » ( ? ) : the correlation function for the process, x is the correlation
time. x - 2 n / u 0 for neighber peaks.
f R ( r ) t h e distribution density function for peak
r'the peak
a*2 : the variences of the process.
And the probability distribution function for peak F R (r) is

FR(r)~ l-exp(-rV(2G0Aco))

The Correlation Parameters And The Correlation Matrix For Peaks

To the ith and jth peaks, the correlative time x - \i- j| 2 n / w 0 . the correlation
parameter for the peaks p i} is
 P.j-Pji-«**in(|i-Jl«Au/u0)/(|i-j|*Au) (4)

If the loading time of the process is T. then the number of peaks L=Tco 0 /2n
which is always too large. From equation (4). p»j-**0 as i-j — ** . Set

w 0 /((l + l) n A u ) - e (e<<l).

Assuming

|i-j|>l. Pij-0 and 1 + 1 - ( o 0 / e n A o») (5)

then the correlation matrix is

l Pi P2 P 1 0
pi l P1 P 1-1 P i

P i-i P 1 1 P P i 0

p 1-1 p 1 1 p1 P i 0 0
Pi p 1-1 Pi 1 p1 P i - i P i0 0

p1 p 1 1 Pi

1 Pi

P J P I 1

in which

(6)

The Fatigue Damage and Limit State Function

The S-N curve is expressed as NS^-C. where S is the amplitude or range of the
stress. N is the number of eycles to fatigue failure under the stress level S.
m and C are constants of materials.

For zero mean narrow band process. S is represented by the peak or the difference
between the peak and trough. The S-N curve needs to be modified using the
Goodman rule if for non-zero mean narrow band process. The fatigue damage per
cycle from Miner*s rule is

The total damage under the random loading D is

648
from Miner's rule , the fatigue failure takes place when D > A ( A is 1. 0 or a
random variable ). Then the limit state function for fatigue failure is

From the equation (S). the limit state function is nonlinear. variables
correlative and non-Gaussain distribution. But the variables have the same
Rayleigh ditribution. And froa the correlation Matrix, the variables are paritial
correlative .

RELIABILITY ON FATIGUE UNDER STATIONARY GAUSSIAN NARROW BAND LOADING

Generally speaking. the reliability on fatigue under stationary Gaussian narrow

band loading can be calculated on the limit state function using the advanced JC
■ethod (as li 1987). in which. through the normalizing and independence .the
reliability index and failure probability can be carried out with the second
order moment aethod. But for the fatigue failure under random loading . the
number ofthe variables in the limit state function is too large to carry out the
calculation. A two block iteration aethod on condebsed Matrix to carry out the
reliability was constructed in the following.

The Two Block Iteration And Condensed Matrix

Using the first step iteration of the advanced JC aethod. setting the initial
parameters of design variables as the Bean. the new design point of the
variables is transfered as a condensed aatrix. In the second block iteration .
the design variables aatrix and correlation aatrix are condesned. the second
block iterationis the saae as the advanced JC aethod but on condensed aatrix.

The First Block Interation and the Condenced Matrix. Considering the amplitude
in the S-N curve, and the zero aean random process. then the stress level S is
peak r.

If the liait state function is G ( r i . r 2 r n ) . then the iteration equations

of the advanced JC aethod are as follows (Li 1987)

where.
r* : design point of the design variables.
R»: column aatrix of design variables at design point.
<X> : normal distribution function.
4> = normal distribution density function.
i|> : distribution function of design variables.
r : normalized design variable.
X r : diagonal aatrix of the variance of normalized design variables at
the design point.
 649
M? : column matrix of mean of normalized design variables at the design
point.
( V g ) r * : column matrix of the partial differentiation of the limit state
function with design variables at design point.
Pr the correlation matrix of design variables.
0: rel iabi 1 ity index.

Set the design point at the mean, the first block iteration and condensed matrix
are derived as follows

p - * - » [ F i i ( l O ] * l / [ 2 ( L - l + l) Z P.+ 2 , Z ( l - i ) p . ] 1 / * (13)

R*-Mr - 4 / a (14)
where.
R^ (1+1)#1 condensed column matrix of new design point for design
variables, in which
ri*- [ri*. r L « ] l and ri,-r L *.

ri*~ [ri». r < L - i > * ] T and ri«-r<L-i>x»

r(iti)x"[r<i*D*.r(i*j)t r<L-i-i>»] and
r<i*i>*T<i*a>*- r<L-i-i)» (15)
Mr .s (1 +1)*1 column matrix of mean for normalized design variables and

-F -n-{<i> [^- 1 (FR(n))]/f R (n)}o-MF R (n)J (16)

1 1
a - . n - * [*- (FR(n))J/{C*f„(n) [2 0.-1 + 1)2 Pl +2S(l-i) p ,]«'*}
• *i «-i )
(17

A : (1 + 1)*1 matrix of calculating coefficients and

i . - . n - H * [*-I(FR(n))]/fB(ii)»,[,z,pIj+ 2 P j ] / c (i<i) (18)

J =1 J *1
1
»c.»i>-2«n-M* [♦^(FHdiJJl/fBtn)} ! PJ/C (19)

To satisfy the limit state function, the variable vector needs to be modified as
follows :
Substitude eqation (14) into (8) (for A ~ l ) . then

r<i*i>*-{(C-2Zrls)/(L-2I)}1'-. (20)

Equations (13). (14) and (20) are the iteration equations for the first block
iteration .giving initial 0 and the condensed matrix of design variables R*.

The Second Block Iteration. The second block iteration is continued using
equations (9). (10). (11). (12) and (20) .with the condensed matrix .In which the
matrixies take the condensed form as R». The matrix of correlation becames (1+
1 ) * (1 + 1)

CALCULATION AND C0NCLUS1UNS

Calculation

The caculation of reliability index and failure probability with the two block
iteration method c*n be carried out through computer. given the design
parameters ( S-N curve. power spectrum of the loading, the main frequency, the
bandwidth, and theloading time). The flowchart of the iteration is as follows.
650
Imput caculating parameters
Go , A M . to o T and S-N curve

1
First block iteration with
equation (13). (14) and (20)

No Yes

Construct condensed matrix on

jU,£r and PT

No Second iteration with

equation (9). (10). (11). and (20)

Stop

For non-zero mean process. the effect of Mean stress can be taken into account
in S-N curve equation with Goodman rule. and the randon fatigue failure
threshold ( A ) can also considered. Which only change the limit syate function.
To non-Gaussian narrow loading. the peak distributioin is not Rayleigh (Y. K Lin
1967). but the reliabilty can be iterated with two block iteration method as the
peak distribution is able to be calculated.

Conclusions

With the two block iteration method presented in this this paper. the
reliability on fatigue under stationary Gaussian narrow band loading can
becarried out given the power spectrum, S-N curve and loading time. This method
can consider the effect of the mean stress. the random character of fatigue
failure threshold. And if the peak distribution of non-Gaussian narrow loading
is able to be calculated, the reliability index and failure probability can also
be calculated with the method.

REFERENCE

Y. K. Lin (1967). Erobabi1istic Theory Of Structural Dynamics. McGran-Hill. New

-
YoiT;. '
J. M. Tunna (1986). Fatigue Life Prediction For Gaussian Random Loads At The Design
State. ASCE. 1.16. No Em 116. 240-246
J. Juncher Jensen (1990). Fatigue Due To Non-Gaussian Response. Fatigue and
Fracture of En£ineerin£ Materials and Structure. 9. No. 3. 169-184.
M. C. Yao (1984). The Calculatio On Damage And Reliability Of Structure Materials
Under Variable Amplitude Loading (in Chinese). Research Report of
China academy of Rajlwav Science . Beijing.
ASCE Committee on Fatigue and Fracture Reliability (1982). Fatigue Reliability:
Variable Amplitude Loading. ASCE 108. No. ST1. 47-89.
J. L. Bogdanoff et al ( 1985 ) . Probabilistic Models Of Cumulative Damage . A
Wiley-Interscience Public ation. New York.
G.H.Li et al (1987). The Ccalculation Of Reliability On Correlative Variables
WS4a1

A DAMAGE STATISTICAL MICROMECHANICS

MODELIZATION TO A DISCONTINUOUS REINFORCEMENT
COMPOSITE ALUMINUM-CARBON.

P H . B R E B A N , D. B A P T I S T E , D. F R A N C O I S

Laboratoire MSS-MAT, CNRS - URA 850

Ecole Centrale Paris, Grande Voie des Vignes,
92295 Chatenay Malabry CEDEX, FRANCE

ABSTRACT
A new solid phase coextrusion process to manufacture metal matrix composites has been developed. As part of
this study, the influence of local concentration distribution on damage mechanisms of the composite was
investigated This has been achieved through an equivalent inclusion analytical approach based on a micro-macro
modelization. An analytical criterion for damage initiation has also been suggested. These results are compared
with in situ tensile tests performed inside a scanning electron microscope,where every stages of the failure
mechanism can be observed.
KEYWORDS

Micromechanics, statistics, damage, metal matrix composite.

INTRODUCTION

In order to better improve the mechanical properties by controlling the

manufacturing parameters, the influence of the microstructure has been evaluated through an
analytical modelization. A damage initiation criterion based on physical observations has been
suggested through the comparision of residual stresses and the local stress field around the
fiber when loading the composite.
The achieved results were compared with in situ tensile tests performed in the
SEM. A good agreement between calculations and experiments is noticed.
MICROSTRUCTURE OF THE COMPOSITE

The material selected for the experiments is a 1050A1 (A5) - 20vol.% T300 carbon
fibers reinforced metal-matrix composite. It was extruded at low speed and high temperature
according to the developed process. The final product is a plate of rectangular section (40 x
7mm 2 ) The material presents a good impregnation of fibers even in the middle of bundles
(figure 1). The aspect ratio of fibers (length divided by diameter) is relatively small, about 5 in
average. This parameter can be related to the geometry of the flow in the die, and it appears
here not to have been optimized. An important heterogeneity of local volume fraction can also
be noticed with some areas almost free of reinforcement and others with more than 50vol. %.
The last important point to be remarked is the large distribution of orientation of the fibers
compared with the extrusion axis (vertical on fig. 1). This disorientation occurred principally in
the plane of the plate. Thus tensile properties of the composite are not optimal in the extrusion
direction, but are improved perpendicularly.
653
654

ANALYTICAL MODELIZATION OF THE COMPOSITE BEHAVIOR

The important anisotropy of carbon fibers requires a three dimensional approach
taking into account all the coefficients of the stiffness matrix. An equivalent inclusion method
based on Eshelby's theory [2] has been chosen. Among different models, TANAKA and
MORI's model, presented by TAYA [3] in the case of metal matrix composites, appears to give
an explicit and relatively simple solution to the modelization of discontinuous metal matrix
composites. It had been tested previously on a 2124Al-25vol.% SiCw composite with a good
agreement with experiments. An attempt is made to clarify and generalize this approach in term
of a micro-macro relationship.

Fig. 1. Distribution offibersin the studied composite.

The macro scale corresponds to the elementary volume representative of the
structure. This volume includes all microstructural parameters such as distribution of fiber
length, disorientation of the reinforcement and local heterogeneity of volume fraction. The cell
is submitted to an uniform macro-stress E. The presence of numerous fibers locally disturbs
the uniform stress field. Thus the total stress field at any point of the space can be decomposed
into the uniform and disturbed stress fields (a). These two stresses can be associated to strain
fields through the stiffness tensor of the matrix (we assume that the properties of the aluminum
in the matrix are the same as the control metal):
£ = CmE0
<°>D-n=5iJj>dV = CmE
where < > D .Q denotes the average quantity over the matrix volume (D total
volume, Q fiber volume). The evaluation of a requires to write the behavior of a single fiber
surrounded with the others. Let us introduce at the micro scale a shortfibercharacterized by its
stiffness, aspect ratio and orientation in a small volume of matrix. The constitutive equation
completed with the equivalent inclusion theory provides a relation of localization where e*
represents the eigenstrain.
e* = Q(l/d,e,cp,C m ,C f )(E 0 +E)
Q is the localization tensor which only depends on the characteristic parameters of
thisfiberand of the matrix.
The homogeneization consists in writing that the disturbed stress field vanishes in
average over the entire volume of the composite.

I adV+ I adV = 0
Jt>a Ja
The problem can then be solved. The total strain field E associated to the uniform
stress field Z is determined
 655

E = Eo + j t l e*dV

The linear relation between Z and E gives the stiffness matrix of the composite.
*{'
Effect of the local volume fraction
One important microstructural parameter to be modelized is the effect of a local
volume fraction distribution. This has been achieved through the introduction at the micro-scale
of a term of short range interaction between the fibers (8*). 8* corresponds to the difference
between the eigenstrains calculated with the local volume fraction and the average one.

8*=e*(fi)-e*(f)

An extension of the modelization was carried out by TAYA and al. [4] to calculate
the coefficients of thermal expansion (CTE). The previous generalized formulation is also
extended to thermal loadings. The evolution of the CTE in the longitudinal and transverse
directions with the volume fraction of fibers for two different aspect ratios has been calculated.
In the particular case of carbon fibers, the increase of transverse thermal expansion for
composites with 25vol.% of fibers is noticeable. The value exceeds the CTE of the matrix and
can set a problem for an application requiring dimensional stability. The influence of the fiber
aspect ratio is negligible. Thermal residual stresses have also been calculated. This model gives
no influence of this stress field on the elastic constants but displays a translation of the
threshold surfaces.
The calculation of the criterion for plasticity has been done. The experiments on
DMMC have shown that strain localization involving local plasticity appears at very small
stresses nearfibertips without generating a macro plasticity. So a yield criterion has to take into
account the average stress over the matrix volume. An attempt was made by W. J. CLEGG [5]
to modelize the tensile behavior of particle reinforced MMC with a similar approach, using a
Tresca criterion for the matrix and involving elastic residual stresses. The aluminum is
supposed here to plastify according to a Mises criterion. When the stress £+<a>D-n reaches
the flow limit, the Hill criterion is assumed to be verified by the composite. Figure 2 presents
the influence of thermal residual stresses on the yield criterion. We can verify that the matrix is
initially in tension at least in the fiber axis. The important coupling between longitudinal and
transverse directions explains the behavior perpendicularly to the fibers.
600

400
• ' ■ »U* i*Bq

.♦* *++^
s Fig.2. Influence of the residual

■
■
■
,1ft*
•s M stresses on the yield surface of a
2024Al-20%vol. Gr composite.
£ 200 \\ (Aspect ratio of fibers 1/d = 10).
a » **
T ■
1 i
■♦
**
rfl
-3
is 1 ■ ■< \ * Q without residual stresses
-20 ■m
3 \* ♦ with residual
.s 4

M\
B
-40

-60
f***# *
9
i1

•»* *♦* f

-80
-400 -200 0 200 400
Stress perpendicular to the fibers (MPa)
656

APPROACH TO DAMAGE MODELIZATION

Experimental observations
In situ tensile tests on micro-samples have been performed in a SEM, in order to
identify the physical parameters of damage. The sample was chosen for its large distribution of
local volume fraction, at least at the surface. The different steps of damage can be listed :
+ strain localization in the bundles of fibers,
+ cavity nucleation at the fiber tips,
+ cavity growth and coalescence,
+ crack propagation with a plastic area in front of the crack tip.
We measured the load during the test which allows us to correlate the observations
to the macro-tensile behavior (figure 3). Cavity nucleation just begins when the stress reached
the macro-yield stress of the composite.

macro-yield stress
damage threshold . Fig. 3. The different steps ol
damage propagation correlated
to the macro behavior of the
studied composite.

0,2%

Damage initiation modelization

We are able to calculate the residual stresses at the fiber interface. Fracture surfaces
show that no reaction occured during the manufacturing process between carbon and matrix; so
only residual stresses assure the binding of fibers.
The physical damage phenomenon we modelize, is the failure of the interface between
the fiber and the matrix. The damage threshold is supposed to be reached when the normal
stress to the considerated point of the interface is equal to the residual stresses. Thus, a single
criterion allows the modelization of an anisotropic phenomenon. We can see a critical angle
corresponding to the transition between the interface at the fiber tip and the one along the fiber.
Figure 4 presents the evolution of the damage threshold surface with the fiber volume fraction
for a composite with a fiber aspect ratio of 10.
500-

400 v4n~1T~
j
fl — ♦ — f = 5%

1 300 H" — B— f = 10%

— ♦ — f=20%
- ■ — f=30%
■5 200 1 n _ □ — f=50%
■fir
100 11 Tin
11 ill)
j 1
f i it
0 i ■*■*

0 100 200 300 400 500

Stress perpendicular to thefibers(MPa)
Fig.4 : Evolution of the damage threshold surface with thefibervolume fraction with afiberaspect ratio of 10
 657

The decrease of the damage stress in both longitudinal and transverse directions
with the reinforcement rate is noticable. This tends to confirm the fact that damage first appears
in the areas with an important local volume fraction.
In order to clarify this point, we have introduced in the calculation of the damage
threshold surface the effect of a distribution of local volume fraction. The shape of the
concentration distribution has a negligible influence. Thus, the influence of rich in fibers areas
is clearly demonstrated.
Since we know the relation between the local volume fraction density and the
damage stress, we determine the proportion of damaged material as a function of the applied
stress. We presente, on figure 5, for different orientation of the tensile stress, the damage
probability, considering two different distributions of the locale volume fraction, but with die
same macroscopique volume fraction. We point out the importance of the shape of the
distribution on the mean value and the scatter of the damage initiation stress. The anisotropy in
the different directions is also well taken into account.
mm ° 1
j/w* T o°
J
0,8
f
£ 0,6
1
I 0,4
1 1 [■■■■■■■lll
0,2 10 20 30 40 50 60 70
local volume fraction
II
0,0 1 1 ■ ■ * ■

0 100 200 300 400 500

Tension stress (MPa)

1,0
f 90° ^ * - )° -p*-B
J1
1

[ 0°

L-
r
0,8

0,6

0,4
inn iii,—1
10 20 30 40 50 60 70
0,2 local volume fraction |

1 J*
0,0 ■ ■ 1 i
100 200 300 400 500
Tension stress (MPa)

Fig.5: Damage probability as a function of the applied stress for different directions of loading and two local
volume fraction distributions.
658

We point out the importance of the shape of the distribution on the mean value and
the scatter of the damage stress. For two similar materials, with the same mean value of the
reinforcement volume fraction, the most heterogeneous distribution will lead to a material twice
less resistant to the damage initiation than the one with an homogeneous distribution. The
anisotropy in the different directions is also well taken into account.

CONCLUSION

In this study, the influence of different microstructural parameters on the

mechanical properties of a Gr-Al composite has been investigated. A model has been presented,
based on a micro-macro relationship. This provides the influence of fiber length, distribution of
orientation and local volume fraction on the stiffness matrix, the coefficients of thermal
expansion, the Hill criterion for plasticity, and a criterion of damage initiation.
Taking into account the residual stresses generated by the cooling from the
manufacturing temperature, a configuration of bundled fibers with little matrix inbetween has
been shown to induce an earlier initiation of damage by cavity nucleation at the fiber tips.
Damage tends to propagate in the direction of the crack that is to say perpendicularly to the fiber
axis. The better configuration corresponds to homogeneously distributed fibers.
To go further in the modelization of the damage of DMMC, it appears indispensable
to take into account the void formation in the matrix through a local damage criterion that we
can build on the analytical modelization. This seems to be the best way to succeed in the good
prediction of a fracture criterion.
The developed models are included in a more general scheme to predict a damage
probability of a structure.

Acknowledgments - This work has been supported by the Ets R. CREUZET for the
manufacturing of the composites and the AEROSPATIALE, through a CIFRE contract.

REFERENCES

1 M. G. McKIMPSON and T. E. SCOTT (1989) Processing and properties of Metal Matrix Composites
Containing Discontinuous Reinforcement. Mat. Sci. Eng. A107. 93-106
2 ESHELBY J. D. (1957) The Determination of the Elastic Field of an Ellipsoidal Inclusion and Related
Problems. Proc. Rov. Soc. London Series A 241, 376-396
3 TAYA M. and MURA T. (1981) On Stiffness and Strength of an Aligned Short Fiber Containing
Fiber-End Cracks Under Uniaxial Applied Stress. J. Appl. Mech. 48,361
4 TAYA M. and TAKAO Y. (1985) Thermal ExpansionCoefficienis and Thermal Stresses in an Aligned
Short Fiber Composite With Application to a Short Carbon Fiber/Aluminium. J. Appl. Mech. 52.
806
5 CLEGG W. J. (1988) A Stress Analysis of the Tensile Deformation of Metal-Matrix Composites. Acta
Met 36 2141-2149
WS4a2
EVALUATION OF SCATTER IN STATIC STRENGTH OF CARBON/POLYIMIDE LAMINATES

T. SHIMOKAWA

Airframe Division, National Aerospace Laboratory

6-13-1 Ohsawa, Mitaka, Tokyo 181, Japan

and

H. MITSUMA

System Engineering Department, Tsukuba Space Center,

National Space Development Agency of Japan
2-1-1 Sengen, Tsukuba, Ibaragi 305, Japan

ABSTRACT

The objective of this study is to evaluate common scatter parameters from

many data sets of small sample sizes. Especially, the methods to average the
estimates of the coefficient of variation are proposed. Static tests for
smooth and circular hole notched specimens made of T-800H/PMR-15 carbon
polyimide laminates yielded various static strengths at four temperatures.
The mean and the averaged estimates of the standard deviation and coeffi-
cient of variation as functions of temperature are calculated from the ob-
tained data and evaluated. The distributional form of tensile strength in
the smooth specimens at room temperature is discussed.

KEYWORDS

Carbon/polyimide; static strength; temperature dependence; averaged standard

deviation; averaged coefficient of variation; distributional form.

INTRODUCTION

Scatter in mechanical properties of carbon fiber reinforced plastics is

generally much larger than that in metals. In designing composite struc-
tures, the design allowables must be determined on the basis of the scatter
parameters of mechanical properties. Therefore, the evaluation of scatter in
mechanical properties is very important.

With respect to mechanical properties, new advanced composite materials

generally have little accumulation of data. Most data published consist of
small sample sizes. Since the cost of specimens is very high, it is not easy
to obtain new data to evaluate the amount of scatter. However, if the esti-
mates of a scatter parameter are averaged, the averaged estimate ought to be
more reliable than individual estimate given separately.

The T-800H/PMR-15, carbon/polyimide, material is a high temperature polymer

composite and one of the promising candidates for the primary structures of
HOPE (H-II Orbiting PlanE), which is a small unmanned space shuttle techni-
659
660
cally studied at NASDA (NAtional Space Development Agency of Japan). Among
PMR-15 systems only a few data on the static strength of the Celion 3K and
6K/PMR-15 materials are published (McCleskey et al. 1982, Poveromo 1985).
The detailed evaluation of the T-800H/PMR-15 system has not been found so
far.

This study presents the methods to average the estimates of the mean and
scatter parameters derived from the data sets of small sample sizes, where
the normal distribution is assumed for the distributional form of mechanical
properties. Moreover, it is assumed that the difference among the means of
different samples is significant and each data set can not be mixed. Pre-
sented methods are applied for the static test results of the smooth and
notched specimens of T-800H/PMR-15 laminates at four temperatures. More-
over, the distributional form in the tensile strength data of the smooth
specimens obtained at room tempera-
ture is discussed using graphical —300-
plotting techniques and the statistic JLr
of the modified Kolmogorov-Smirnov Static
25.4- Tens.
goodness-of-fit test.

< 105 H
MATERIALS AND SPECIMENS -*|25.4f<- I
«3-
*
* 1 * 1 Static
The T-800H/PMR-15 laminates and i ! i
i i i i
Comp.
specimens were manufactured by two ♦
companies, A and B. The laminate ply -220-
lay-up is (45/0/-45/90)4s. Fig. 1 -110-
shows the specimen configurations. <J>6.35
Smooth and circular hole notched Tab
--&- Static
Tens.
specimens were used. The specimen
thickness is represented by the
nominal value calculated from the -105-
nominal prepreg tape thickness. Net <J>6.35 Static
area stress is used for stress in the HK- Comp.
notched specimens.

Fig. 1 Specimen configurations, unit=mm.

TEST CONDITIONS AND RESULTS

Tension and compression tests were conducted at NAL (National Aerospace

Laboratory), A, and B companies. Four data sets for each test case are
common, where each test case is defined by the combination of three items,
such as smooth or notched specimens, tension or compression tests, and a
test temperature. Four data sets come from the combination of the test
laboratory and laminate-manufacturing company, i.e., (NAL, A ) , (NAL, B ) , (A,
A), (B, B ) . However, there is one to three data sets in some test cases. The
number of observations in one data set is two to four, except for 30 in only
one data set. Test tern-
peratures were -100°C, Table 1 Number of specimens and number of
-50°C, room temperature, data sets within parenthesis.
and +300°C. At -100°C
and -50°C there is one Specimen & load -100°C -50°C RT +300°C
data set each and no
difference in the amount Smooth, tension 3(1) 3(1) 39(4) 10(4)
of scatter is assumed at Smooth, compression 3(1) 3(1) 14(4) 8(3)
these temperatures, and Notched, tension 3(1) 3(1) 13(4) 10(4)
the estimates of scatter Notched, compression 3(1) 3(1) 13(4) 10(4)
parameters at these low
 661
temperatures were averaged. In this case the temperature is represented by
-50°C in drawing graphs. Table 1 presents the numbers of specimens tested
and data sets.

Mean Strength

Strength considered is represented by x. Individual sample, i.e., data set,

is indicated by j, and the number of data sets by m. The sample size in the
sample j is denoted by n-:. An arbitrary strength observation is expressed by
x
Ji- The
"" mean in the sample j, fL,
" is given by
Oj = (Exj^/nj. (1)
When each sample is drawn from the populations with an equal variance, the
averaged mean is simply calculated by the arithmetic mean, jj,
y = (Enjty/Znj. (2)

Since in some test cases the

statistical test for the dif-
ference of the means was not 800
rejected, Fig. 2 indicates the
mean strength obtained from the 600
data sets separated by the
specimen manufacturer. This
figure reveals a rough estimate 400
of the mean strength. In case D Sm./Tens./A Sm./Tens./B
of the smooth specimens, the ■ Sm./Comp./A Sm./Comp./B
tensile strength drops slightly 200 o Nt./Tens./A Nt./Tens./B
following the rise of tempera- • Nt./Comp./A Nt./Comp./B
ture. The compressive strength _j i I L

decreases or does not change -100 0 100 200 300

with increasing temperature Temperature T °C
below room temperature, but
drops at 300°C. In case of the Fig. 2 Mean static strength.
notched specimens, as the
temperature rises, the tensile strength increases slightly or does not
change while the compressive strength decreases. The high strength of the
T-800H fiber contributes to the very high tensile strength in comparison
with the compressive strength in both smooth and notched specimens.

Evaluation of Scatter

The measure of scatter is represented by the standard deviation or coeffi-

cient of variation in the normal distribution. This study assumes that the
population standard deviation or coefficient of variation is equal or common
for all the data sets in each test case defined above. The estimates of the
scatter parameters obtained from each data set in one test case are averaged
and discussed.

Averaged Standard Deviation. The estimate of the standard deviation in each

data set, 6j, is given by

°j ■ [£(xji-Sj)2/(*j-l)]1/2- (3)
The averaged estimate of the standard deviation, i.e., the pooled estimate
of the standard deviation, with weights, a, can be calculated by the well
662
known formula,
8 = [KCnj-Daj2}/^-!)]1/2. (4)

Fig. 3 indicates the obtained results of the averaged standard deviation

calculated by Eq. (4). Besides a for the test case of the smooth specimens,
tensile tests, and at the low temperature, § of tensile strength in the
smooth specimens and a of compressive strength in the notched specimens are
not heavily influenced by temperature. As the temperature rises, a of ten-
sile strength in the notched specimens increases; however, the value of o at
300°C is considered too high. Meanwhile, 8 of compressive strength in the
smooth specimens decreases with an increase in the temperature. On compari-
son of § of tensile strength
and that of compressive gg
strength in the smooth speci- ^
mens, § of compressive strength 2:
is nearly equal to or lower
than that of tensile strength, 40
except for the test case at the
low temperature. On the other <o o
-p •«-
hand, in the notched specimens oo -P
§ of tensile strength is higher 20
than that of compressive
~* Notched/Comp.
strength. Hence, if the measure
of scatter is represented by
the standard deviation, the _i 1 i i i _j i »
-°100 0 100 200 300
amount of scatter in compres-
sive strength is not always Temperature T °C
higher than that in tensile
strength. Fig. 3 Averaged standard deviation estimates
with weights for static strength.

Averaged Coefficient of Variation The estimate of the coefficient of

variation, fj in one data set is calculated by

ni (5)
An appropriate method to average the estimates of the coefficient of varia-
tion has not been found in ordinary text books, the authors propose the use
of the following two formulas to get an averaged or pooled estimate, i.e.,
an unbiased estimate of the coefficient of variation with weights.

A simple approximated formula can be obtained by the use of the averaged

standard deviation of log-strength. The estimate of the coefficient of
variation, fL , is given by
n = [ex (inio-a )z-i]1/2
1 P L (6)
where 0"^ is the averaged standard deviation of log x. This formula is de-
rived from the fact that the normal distribution is well approximated by the
log-normal distribution when the coefficient of variation is not so large.

In order to average directly the estimates of the coefficient of variation,

the following formula, fu, is available. fi9 is an unbiased estimate of the
coefficient of variation with weights,
Z[c 2j n j /{i4-c 2j 2 (n 2 /n r i)}]
n2 = (7)
I[c 2j 2 /{l+c 2j 2 (r, 2 /n r l)}]
where l/c2-j is the constant to correct the bias of the sample standard
 663
deviation and a function of sample size n, H is the common population coef-
ficient of variation, r^ can be calculated by an iterative technique. Begin
with r|=ri0, where ri0 is the initial value of ri, such as fj-^. Then, calculate
f^, and let 11=^. Repeat this step and complete when ri and ri2 reach an equal
value. This formula is provided by one of the authors (Shimokawa, 1989).

Fig. 4 indicates fj-^ calculatedJ^y Eq. (6). Fig. 5 presents fL obtained by

Eq. (7). The estimates ru and f^ are very close to each other not only in
their tendencies but also^in
their values. Therefore, fj
represents either fj, or ru in
the following discussion. In
case of the smooth specimens,
besides fi of tensile strength
at the low temperature, fi's of
both tensile and compressive
strengths are approximately
constant regardless of tempera-
ture. Of course, their values
are apparently different. The
value obtained for compressive
strength is larger than that
for tensile strength. In case ~100 0 100 200 300
of the notched specimens, r)fs Temperature T °C
of both tensile and compressive
strengths are almost equal at Fig. 4 Averaged estimates of the coefficient
the low temperature and in- of variation with weights for static
creases as the temperature strength, calculated by Eq. (6).
rises. This value of tensile
strength becomes much higher fr* 10
than that of compressive <N
strength at +300°C. «cr
-p 8
c
0)
The averaged estimate of the
o cO 6
coefficient of variation of •r-
* ♦--r-
U- -P
compressive strength is higher <1)
10
O T-
than that of tensile strength O $- 4-
10
in the smooth specimens; howev- "O
<D
>

er, this relationship is re- D>4-

<0 O 2
versed in the notched specimens
except for the test case at the
low temperature. Since the -100 0 100 200 300
formula of the coefficient of Temperature T °C
variation is expressed by Eq.
(5), the tendencies shown in Fig. 5 Averaged estimates of the coefficient
Figs. 4 and 5 are roughly of variation with weights for static
explained by Figs. 2 and 3. strength, calculated by Eq. (7).

Distributional Form of Tensile Strength in Smooth Specimens

Thirty observations of tensile strength, S u , in the smooth specimens at room

temperature are plotted on normal and Weibull probability paper and illus-
trated in Fig. 6. Data fitness with a normal distribution is generally
better than with a Weibull distribution (with two parameters), though the
weakest value is exceptional. The statistic of the modified Kolmogorov-
Smirnov goodness-of-fit test (Mann et al., 1974) gives 0.077 for the normal
distribution and 0.126 for the Weibull distribution. This means that the
664
normal distribution fits quan- *s 99
titatively better with the
obtained data than does the
Weibull distribution.

CONCLUDING REMARKS

Static tests were carried out

for the smooth and circular
hole notched specimens of the
T-800H/PMR-15 laminates. The
mean and the averaged estimates
of scatter parameters of static 700 800 900 700 800 900
strength at various tempera- Tensile Strength S MPa
tures and the distributional Fig. 6 Distribution of tensile strength of
form of tensile strength in the smooth specimens at room temperature
smooth specimens at room tem- on normal and Weibull probability
perature were evaluated. Major paper.
results are as follows:

1. The tensile strength is much higher than the compressive strength in

both smooth and notched specimens.
2. The standard deviation of tensile strength is not always higher than
that of compressive strength.
3. The coefficient of variation of compressive strength is higher than that
of tensile strength in the smooth specimens. However, this relationship
is reversed in the notched specimens except for the test case at the low
temperature.
4. Distributional form of tensile strength in the smooth specimens at room
temperature fits better with a normal distribution than a Weibull dis-
tribution.

ACKNOWLEDGMENT

The authors wish to express their hearty gratitude to the collaborators in

obtaining the test results.

REFERENCES

Mann, N.R., Schafer, R.E., and Singpurwalla, N.D., Methods for Statistical
Analysis of Reliability and Life Data, John Wiley & Sons, 1974, p. 349.
McCleskey, S.F., Cushman, J.B., and Skoumal, D.E., "High Temperature Compos-
ites for Advanced Missile and Space Transportation Systems," Proc. AIAA/
ASME/ASCE/AHS 23rd Structures, Structural Dynamics, and Materials Conf.,
1982, pp. 212-222, AIAA Paper No. 82-0707.
Poveromo, L.M., "Polyimide Composites - Application Histories," High Temper-
ature Polymer Matrix Composites, NASA CP-2385, 1985, pp. 339-358.
Shimokawa, 1989, not published in English.
WS4a3

"Thermal Shock Tests of Epoxy Resin

with Disk Type Specimens"

Hidemitsu Hojo and Masatoshi Kubouchi

* Department of Industrial Engineering and Management,

Ninon University, College of Industrial Technology,
2-1,Izumi-cho 1-chome, Narashino-shi, Chiba-ken 275, Japan.
** Department of Chemical Engineering,
Tokyo Institute of Technology,
2-12-1, O-okayama, Meguro-ku, Tokyo 152, Japan.

ABSTRACT

The crack of LSI packages caused by thermal shock like the solder reflow-
ing, gives serious problem in electronic industry. Two types of specimen
were tested, and these thermal shock fracture behavior and cyclic life were
investigated from the point of reliability. As a result of the ring model
testing, cyclic life was found to obey the Weibull distribution. On the
other hand, thermal shock tests for LSI model indicated that there were two
patterns of cracking, circular type and diagonal type. LSI model was also
evaluated its life statistically considering failure mechanism, and data
agreed well with Weibull distribution. The life indicated maximum value
when solder bath temperature was 240 °C, because of the affair of thermal
stress and resin degradation.

KEYWORDS

Thermal shock; Thermal fatigue; Weibull distribution; Epoxy resin;

LSI package; Package crack; Moisture absorption.

INTRODUCTION

Epoxy Resin is now being used from large electrical products to miniature
electronic parts like IC packaging due to its good electrical properties.
With the request of high reliability for the resin products, the crack
resistance has become more and more important problem in this fields. In
this report, authors proposed the new test methods to evaluate the crack
resistance of epoxy resin by using cooling and heating thermal shock with
two types of metal inserted epoxy specimens.

665
666
EXPERIMENTAL METHOD

Three types of tests with ring model and LSI model specimens were made.

Ring Model

First of these tests was the heat cycle test using "ring model" specimen.
This test was used for the low cycle thermal fatigue of epoxy resin. As
shown in Fig.1(a), epoxy resin was casted into aluminum ring (60mm outside
diameter and 54mm inside diameter), and then machined to be 10mm thickness.

For this ring model, thermal cycle tests were conducted by putting the
specimens in a hot water bath and a cooling bath, using ice and water,
alternatively. Heating and cooling periods used were respectively 20
minutes , when the specimen was heated or cooled to be same temperature.
Then crack was inspected during the interval of changing the bath.

LSI Model

The second one was the thermal shock test using the disk type specimen
embedded aluminum chip as the model of the LSI resin package. It was desig-
nated as "LSI model". This type of specimen was made by epoxy casting, and
at the same time aluminum chip was embedded in the center of this disk with
60mm diameter. Figure 1(b) shows the shapes and three types of surface
treatment of aluminum chips.

For this model, thermal shock tests were conducted by cooling the preheated
specimen quickly. The specimen was fixed embedded chip side with heat
insulator, then it was put into the liquid nitrogen bath for 20 minutes.
After taking out of the bath the crack pattern was observed.

The third one was the cyclic thermal shock test with LSI model. Considering
the thermal shock in soldering process, this test was conducted by putting
the specimen into solder bath (200 to 280°C) and refrigerator (-40 to 40°C)
alternatively. Heating or cooling period was 30 minutes and this also
corresponded to the time when the specimen took flat temperature distribu-
tion.

R D
0 22(D)
2 22
5 22.5
8 23
12.5 25(Q)

(b)
Hea t i ns ula tor £:•:$:$:

Fig.l Shape and dimensions of two disk type specimens.

(a)Ring model, (b)LSI model.
 667
RESULTS AND DISCUSSION

Heat Cycle Test for Ring Model

For heat cycle tests of the ring model specimens, failure was initiated
from the interface of aluminum ring and epoxy resin by debonding, and then
crack was generated at the debonding edge and grown into epoxy resin.
This fracture process is shown in Fig.2. This resin crack step was defined
as the fracture of this heat cycle test.

Assuming Weibull distribution, test data were plotted as shown in Fig.3.

The test results for the specimen loaded temperature difference of 60, 64,
68, 72 and 76 K showed parallel straight lines, so that shape parameter "m"
was constant.

Figure 4 indicated Weibull plot of the test results for three epoxy resin
systems. The Weibull parameter M m" clearly shows the reliability of resin
systems.

(a) (b)

(c) (d)

Fig.2 Fracture process of ring model specimen;

(a)before testing,
(b),(c)debonded interface after few cycles,
(d)resin crack caused from the debonding interface.

VAT = 76K
D AT=72K
AAT = 68K
OAT=64K
OAT = 60K

10 20 30 50 100
n, cycle
Fig.3 Weibull distributions of heat cycle test results
with ring model specimens for five temperature
differences.
668

3 5 10 20 30 50 100
n, cycle
Fig.4 Weibull distributions for heat cycle test results
with ring model specimens for three resin systems.
resin A; DGEBA (epoxy equivalent; 450-500) + PA,
resin B; DGEBA (370-435) + PA + lOphr polyglycol,
resin C; DGEBA (370-435) + PA + 20phr polyglycol.

Thermal Shock Test for LSI Model

For LSI model specimens, two types of fracture pattern depended on test
conditions were observed. These fracture patterns are illustrated in
Fig.5. Figure 5(a) represents a conical crack along the edge of metal chip
(pattern A), and Fig.5(b) represents a crack along the diagonal of the chip
(pattern B).

Tests were made with five types of the embedded metal chips of which the
radius of curvature at the corner were changed. For circular chips, pat-
tern A was observed, and when square chip was used, the crack tended to be
pattern B. The specimen embedded square chip with rounded corner indicated
both pattern A and B, but changed the ratio of patterns A and B with the
radius of curvature. And the pattern B crack passed through the point where
the rounded corner join with the straight edge.

The surface treatment of the chip affected the fracture pattern, and
specimens with strong interface due to the sandblast treatment showed pat-
tern B, while the specimens with no treatment and also with weak interface
applied the silicon oil showed pattern A.

Fig.5 Fracture patterns observed in thermal shock tests

with LSI model specimens.
(a)circular type (pattern A ) ,
(b)diagonal type (pattern B ) .
 669

Cyclic Thermal Shock Test for LSI Model

Fracture appearance obtained in the cyclic thermal shock tests for LSI
model specimens was also divided two patterns, similar to the thermal
shock test result. When upper temperature of solder bath was higher than
200°C crack was tended to be pattern A (Fig.6(a)), and when lower than
200°C, then to be pattern B (Fig.6(b)) respectively independent of cooling
temperature.

In order to examine the effect of moisture absorption, the test was made
with the specimen which was immersed in 80 °C water 120 hours. Different
fracture pattern from A and B was observed. Figure 6(c) showed this frac-
ture pattern of cross-shaped crack above the chip region. Kitano et al.
(1988) evaluate the package cracking by means of moisture diffusion analy-
sis and stress analysis of packages. This fracture pattern in Fig.6 could
be explained by same method.

Similar to the ring model, life for cyclic thermal shock tests was studied
statistically. Weibull plot of the test results using 240°C (solder bath)
^ 0 °C (refrigerator) cycle for the specimen embedded square type metal
chip was shown in Fig.7. Test results does not show liner line on the Wei-
bull probability paper and this meant mixed Weibull distribution. Each
distribution will correspond to fracture pattern mentioned above.

The relation between MTTF (mean time to failure) and average temperature of
the cycle with constant temperature difference of 240 K is shown in Fig.8.
At average temperature of 120 C (upper temperature was 240 C) the life
became maximum. At higher than this temperature range the life decreased
and this means the degradation of resin from high temperature solder bath
(>240 C ) . And at lower temperature range data indicated less life, this
was due to thermal stress in the specimen becomes larger. Because elastic
modulus changes seriously above Tg, thermal stress becomes almost zero
(Shigeta et al.,1981). Therefore, when heat cycle using temperature range
higher than Tg, thermal stress will decrease and the life will increase.

(a) (b) (c)

Fig.6 Fracture surface of LSI model specimens for
cyclic thermal shock tests.
(a)200°C ^ 0°C, (b)240°C ^ 0°C,
(c)moisture absorbed before test.
670

T 1 1 1 1 1 1 1 1
99
90 -
^70 _
^ r
r*
^50
~30j ^
c C5 o o < ^
u-10
5r J
3
i 1 1 1 1 11II -l 1 1 1 1 1 III
1 2 3 5 10 20 30 50 100
n, cycle
Fig.7 Weibull distributions for cyclic thermal shock
test results for 240°C ==£= 0°C cycle.

10 [ 1 1 1 1- -—~ —1
AT = 240 K
i! 8|-
1 /\
° 6 \
^O- J
1 y°
1 -<r solder bath 1
1 ' ' i i i 1
60 80 100 120 140 160 180
Average temperature °C
Fig.8 Relation between MTTF and average temperature of
cycle with constant temperature difference, 240 K.

REFERENCES

Kitano, M. , A.Nishimura, S.Kawai and K.Nishi (1988). Analysis of package

cracking during reflow soldering process, IEEE Annu. Proc. Int. Reli-
ability Sympo., 90-95.
Kubouchi, M. and H. Hojo (1990). Evaluation method of thermal shock resist-
ance of epoxy resin based on fracture mechanics, J_;_ Soc. Mat. Sci. ,
Japan, 39, 202-207.
Kubouchi, M. , N. Haraki and H. Hojo (1990). Heat cycle test using epoxy
resin casted in cylindrical aluminum ring, J_^_ of Mat. Sci. Soc. , Japan,
27, 337-344.
Shigeta, Y., M. Ochi and M. Shimbo (1981). Shrinkage and internal stress
during curing of epoxide resins, J. Appl. Polym. Sci., 26, 2265-2277.
WS4a4

EVALUATION METHOD ON DISPERSION STATE

OF PARTICLES IN FINE PARTICLE DISPERSED
COMPOSITE MATERIALS BY X-RAY ANALYSIS

S. OKUDA and K. FUJISAWA

Department of Chemical Engineering, Doshisha University

Kamigyo-ku, Kyoto 602, Japan

ABSTRACT

In order to evaluate the dispersion state of filled fine particles in poly-

mer matrix, X-ray point analysis was carried out using EPMA, and micro-
scopical dispersion state of filler was evaluated from statistical treatment
of characteristic X-ray intensity.

KEYWORDS

dispersion; microdispersion, filler; particle filled composite materials;

EPMA; X-ray point analysis

INTRODUCTION

In fine particle dispersed composite materials, the dispersion state of

filled particles has strong influences on the mechanical properties of compo-
site materials. It is difficult to disperse submicron fine particles
uniformly in the polymer matrix. Additionally, the evaluation method of
micro-dispersion state is not established. Here, in order to evaluate the
dispersion state of filled fine particles, X-ray point analysis was carried
out by using Electro Probe X-ray Microanalyzer(EPMA), and microscopical
dispersion state of fillers was examined from the distribution of character-
istic X-ray intensities and their statistical treatment.

CHARACTERISTIC X-RAY AND PRINCIPLE OF ANALYSIS

Various signals which are generated by the irradiation of accelerated

electron on the specimen is shown in Fig.l. In this study, characteristic
X-rays were noticed. When an electron in ground state is collided with
accelerated electron or X-ray, atom is ionized and some electrons are eject-
ed and atom becomes excitation state, and characteristic X-ray is radiated
at same time. The wave length of characteristic X-ray is inherent to
element, and we can detect the kinds of element, and farther know concentra-

671
672

© Primary electron

©Back scattered
©Xray electron

© Photon ©Secondary
electron

Specimen [
©Absorbed
electron
© Secondary
electron

©Transmitted
electron

Fip,.l Behavior of accelerated electron in solid material

tion of element in the specimen.

The intensity of characteristic X-ray from the element A is defined as 1^,

and intensity of characteristic X-ray from standard sample where concentra-
tion of element A is known, is defined 1(A). And the ratio of these two
intensities denotes KA as relative intensity.
KA = - ^ (1)
When the concentrations in the specimen and standard specimen are defined
as C A and C ( A ) , next relation is approximately is established.

~ I 7 A ) = "C7A5= K A (2)

In this experiment, the intensity of X-ray analysis is converted directly

to concentration of fillers by calibration curve of intensity vs. volume
concentration of fillers.

STATISTICAL TREATMENT OF DATA THAT IS OBTAINED FROM POINT ANALYSIS

The relative comparison of statistical data from point analysis is useful

for the evaluation of dispersion. The standard deviation s is shown in
next equation.
s = [ z ( xi - x )2 / ( n - i )]1/2 (3)
Where, X is mean value, and ^ is sample size.
The standard deviation shows the scattering of data around mean value X,
and s/Vf shows the scattering per unit volume concentration of fliers.
s/vf and s may be used as measures of dispersion.

EXPERIMENTAL APPARATUS AND SPECIMEN

EPMA(Electron Probe X-ray Micro-Analyzer)

 673
X-ray analyzer which was used in this experiment is EPMA (Shimazu Mfg. Co.,
Ltd., EPM 810), and scanning type electron microscope (resolution is 150A)
is co-equiped. The maximum accelerating voltage is 30 KV.

Samples
The polymer matrix used is epoxy-acryl type vinylester(Showa Polymer Co.Ltd.
: Ripoxy®806),the fillers are almina(Sumitomo Chemicals, ALM®41 and AKP®30)
and calcium carbonate(Maruo Calcium Co., Ltd.; Kalfain®100, Kalfain®200 and
Super®SS). Table 1 shows the filler's geometry and characteristic X-Ray
wave length.

After vinylester resin was mixed with almina or calcium carbonate by mortar
for two hours, cobalt naphthenate 0.5 vol.% and metylethyl keton peroxide
1.0 vol.% were added. After mixing, samples were pressed to sheet by press
machine.and cured. Three directional samples were cut from the sheet, and
they were contained into phenol resin block.
Table 1 Filler geometry and characteristic X-ray wave
length
Filler Filler Material Mean Geoaetric Analytical Characteristic
oaae grade type diaaeter standard eleaent X-ray
deviation wave length
DPso.ua g.(-) (A)
Aluaina ALM-41 Raw 2.50 1.89 Al Kj 8.34

Grinded 0.19 2.32

Kalfain-100 Raw 0.23 1.49

Calcina Kalfain-200 Raw 0.12 1.74 Ca Ki 3.35

carbonate Super-SS Raw 2.25 2.04

Grinded 0.75 2.01

Table 2 X-ray point analysis conditions

Accelerating voltage E , kV 12 , 20

I n t e g r a l time I.T. , s 4

Beam diameter 4 , #m 1-150

Number of sampling point N , - 100

The contained sample was polished of its surface, and Au was coated in the
thickness of about 200A by vacuum evaporater.

X-ray point analysis by EPMA

For the purpose to know the dispersion of fillers, point analysis was
carried out by mechanical scanning on 1024 points in one direction of the
sample. The analytical condition used in this work is shown in Table 2.
The diameter of primary electron beam was changed from lym to lOOym, and
gained data were introduced to computer, and statistical treatments were
carried out.

EXPERIMENTAL RESULTS AND CONSIDERATIONS

674
Calibration curves
Fig.2 shows the calibration curves of almina and calcium carbonate. The
linear relationships are established between volume content Vf and X-ray
intensity. These inclinations are independant upon matrix polymer or
filler's particle sizes, but is dependent upon the kinds of filler.

Relation between beam diameter $ and standard deviation s

When the beam diameter is changed, the changes of standard deviation of
filler concentration are shown in Fig.3 and Fig.4 respectively. Except
ground sample of calcium carbonate Super-SS®, standard deviation is kept
constant until beam diameter reaches some critical values, and then has a
tendency to decrease straightly.
In the case of particle size of fillers is large, for example alumina or
calcium carbonate Super-SS®, the value of standard deviation becomes large,
and critical beam diameter $ c becomes several times of mean particle size.
On the contrary, in the case of small particle size fillers, the value of
standard deviation is relatively small and size of critical beam diameter
$ c becomes large. Especially, the ground material of calcium carbonate
Super-SS didn't show any decrease of standard deviation even more than lOOym
of $ c . This means that in spite of fine particles, the cohesion strength
of particles is not so strong, and it assumes some voidage between particles
is remained.
10*1 1
Beam diameter ft :100ym
Acceleratmq voltage, kV
Alumina
Calcium carbonate

10V

10 100
Volume content vf . vol°/o

Fig.2 Calibration curves

 675
Evaluation of dispersibility from filler's volume concentration
The relationship of filler's volume concentration Vf and value of standard
deviation devided by volume concentration is shown in Fig.5.
It can be seen from this figure that S/Vf is decreased as the increase of
filler's volume concentration, and accelerating voltage has an influence
on S/VF vs. Vf curves too. On the different size filler of same kinds,
S/Vf value is lower for almina ALM41®(mean diameter is l.lOym) than for
almina AKP30®(mean diameter is 0.39ym). This is due to the increase of
aggregation of finer fillers. On calcium carbonate, Kalfain200®(mean
diameter is 0.17ym)is treated on its surface by fatty acid and chemical
affinity with matrix resin is superior. Therefore, S/Vf values shows the
lowest value in whole volume^content.
Concerning about the histogram of filler content, the mode content of filler

100 I I ' l| I 1 1 | l i i i| —r

Filler : Alumina
50 Accelerating voltage : 20kV
Filler content : 20vol%

O Raw material*
A Grinded m a t e r i a l *

• 10
|

■o
&

0.5I -I l I I I I I I
5 10 50 100 500
Beam diameter 0 , um

Fig.3 Effect of beam diameter on standard deviation

100 . i i M | r i iT T T T
n— 1 1—i | i i i i | 1 r—-rq
Finer : C a C 0 3
Super-SS O Raw material*
50 - Accelerating voltage : 20kV
• Grinded materials
■1
' Filler content : 20vof%

- Kalfaln200 A Raw material* 1

£ . _o KalfalnlOO □ Raw m a t e r i a l *
J
O
o
• 10
: d
n
> 5 - —• 1_ H
e ■fl
V
■o A
m
•o
•e

s
1

0.5 11111 i_ 1 L_Lu 1 I I I 1 1 1 1 1 1 1 1 1 1 -uJ

Li
0.5 5 10
Beam diameter # , pm

Fig.4 Effect of beam diameter on standard deviation

676
2.0

Baam tflamatar : 6pm

12 20
Alumina A L M - 4 1 O

CaC03 Kalfaln200 A A

20 30 40 60 70
Voluma contant vF ,

Fig.5 Relation between s/Vf and Vf

corresponds well with the volume concentration of filler.
And the comparison with the shape variation of histogram gives also the
information of microscopical dispersion.

CONCLUSIONS

The dispersion of alumina and calcium carbonate fillers in vinylester resin

as matrix was examined by characteristic X-ray analysis.
By the analysis of changing beam diameter, it is possible to evaluate the
relative dispersion morphology of fillers.
And it can also gain useful knowledges about dispersion from the relation
between S/Vf value and Vf ( S is standard deviation, and Vf is volume
concentration of filler ).
From these experiments, it was confirmed that this X-ray point analysis
method is useful for the evaluation of microscopic dispersion state of fine
particles in the composite materials.
WS4a5

RELIABILITY EVALUATION ON MECHANICAL CHARACTERISTICS OF CFRP

Z.Maekawa*, H.Hamada*, A.Yokoyama*,

K.Lee**, S.Ishibashi***

* Faculty of textile science, Kyoto Institute of Technology

** Graduate Student, Kyoto Institute of Technology
Matsugasaki Sakyoku Kyoto 606 JAPAN
*** Toray Industries. Inc.

ABSTRACT

A study was conducted to evaluate the reliability of the longitudinal

tensile properties of unidirectional CFRP laminates. Four kinds of CFRP
were tested in order to examine the factors of variability of mechanical
properties and get the information concerning reliability improvement.
Statistical distributions of the mechanical properties were obtained from
the tensile tests with large sample size. As a result, toughened matrix
resin can yields a pronounced improvement of the reliability of CFRP and
shift of the strength to higher values, but the degree of improvement
depends on the combination of fiber and matrix.

KEYWORDS

Unidirectional CFRP laminate; reliability; toughness; tensile strength.

INTRODUCTION

In this paper, the tensile properties and those variabilities of

unidirectional CFRP were examined. Generally, the tendency is that the
coefficient of variation (CV) of unidirectional CFRP tensile strength is
large when compared to metal material,e.tc. but the scatter differs
remarkably depending on the material used^ '. A few reports have pointed
out that matrix resin effects the strength of composite but the effect on
the variability of the strength has not been reported^ *'. In this paper,
we will pay attention specifically to the effect on the variability of the
composite strength caused by the matrix resin to obtain the information
concerning the reliability improvement. Moreover, the variation of
mechanical properties caused by the composition method of fiber and matrix
will be examined. Finally, an examination was added about the effect on
the variability of strength by temperature caused by the large temperature
dependency of the matrix in a high molecule system composite.

EXPERIMENTAL PROCEDURE
677
678
s
I I a 4
06
1
L
Strain Gage
h—55—*
as id o*

es^i
I Qis20
175 mm
UJ — L » .1 W=25

_L
1 ' 1.25 W (mm)
1 "8
J | J=L

60 —
(C)
(B)
\
Fig. 1 Geometry of test specimens.
(A) Composite tensile specimen (C) Compact tensile specimen
(B) Resin fracture toughness test specimen
The CFRP used in this experiment is unidirectional carbon fiber/epoxy
laminate. Two types of PAN based carbon fibers, "Torayca" T300 and T800
(Toray Ind., Inc.), are used. Two tvpes of epoxy resin systems formulated
by Toray Ind. are also used; 177 C cure types of #3601 and #3631. A
schematic drawing and the dimensions of the test specimen are shown in
Fig.1(A). The tensile tests were conducted by an Instron universal testing
machine at three temperatures: -4.0°C, room temperature and 100°Cin
accordance- to standard ASTM D3039. Tensile tests were conducted in
accordance with the standard JIS K7113-1981 to obtain the mechanical
properties of two matrix resins, #3601 and #3631, used in this examination.
A schematic drawing and the dimensions of the test specimen are shown in
Fig.l(B). Moreover, a neat resin toughness test was done as the toughness
of the matrix resin is closely related to toughness of the composite. The
neat resin test was conducted on a compact tension specimen (CT). Resin
panels were cut into the test specimens by diamond tools and the pin was
made by the drill as shown in Fig.1(C). CT tests were conducted in
accordance with the standard ASTM E399-83 in three conditions of -40°C,
room temperature and 100°C atmosphere.

EXPERIMENTAL RESULTS

VARIATION OF MECHANICAL PROPERTIES

The results of the tensile tests on four types of unidirectional CFRP are
summarized in Table 1. The coefficients of the variation of the elastic
modulus are observed to be 2-3 percent as well as metal material. However,
the scatters of strengths are considerably higher than that of metal
material, especially, the coefficient of variation of strength in
T300/#3601 indicates very high value. These experimental results suggest
that matrix resin strongly Influences the scatter of strength with regard
to T300 specimens and weakly influences T800 specimens. The results of the
tensile tests of T300 specimens in three temperature condition are shown in
 679
Table 1 Mechanical properties of Odeg. composites.

Relnforclnc fibers Fiber Tonsil* strtnrth Ultlsate strain Dastle sodvlw Polsson's ratio
/Xatrix rains alicnient N seanOlPa) C.V.00 N seanOC) C.Y.00 II sean(GPa) C.V.00 11 fan(-) CV.CO

T300/33601 0# 278 1515.3 10.7 276 1.06 9.5 Z75 138.0 2.1 276 0.334 3.3
T300/S3631 0' 74 1740.5 6.3 74 1.22 5.2 74 135.5 1.3 74 0.339 2.8

T800/83601 0' 79 2S18.4 3.0 56 1.45 2.6 77 182.2 1.9 77 0.353 3.3
T 8 0 0 / * 3 831 0* 279 2572.7 4.8 244 1.45 3.9 276 165.7 2.8 278 0.349 5.7

Table 2 Mechanical properties of Odeg. composites

in three temperature conditions.

leinforeini fibers Tespsrators Tensile strencth Oltltatt strain Elastic sodulu Polsson's ratio
/Matrix rains (X) N sean(MPa) C.V.00 N aean(*) C.V.00 n Bean(GPa) C.Y.00 K aeu(-) CV.00

-40 40 1397.3 13.1 39 0.96 12.4 39 139.7 1.6 39 0.322 6.3

T300/33601 Root Tea?. 278 1515.3 10.7 276 1.06 9.5 275 138.0 2.1 276 0.334 3.3
100 37 1635.6 7.8 23 1.10 8.0 24 139.7 2.1 24 0415 6.9

-40 40 1514.2 11.6 40 1.06 10.2 40 136.0 1.1 39 0.336 6.6

T300/*3631 Roos Tesp. 74 1740.5 6.3 74 1.22 5.2 74 135.5 1.3 74 0.339 2.8
100 38 1602.9 6.2 32 1.10 7.4 37 135.6 1.9 36 0.329 6.0

Table 2. The strength of T300/#3631 at room temperature, however, is the

highest but the tendency of the scatter of the strength to decrease with
the temperature increase also eas seen.

FRACTURE MODE

The typical fracture modes obtained in this experiment are shown in Fig.7.
Two different fracture modes are displayed for the T300/#3601 specimens.
One is straight failure normal to fibrous axis, and the other is brushy
failure. Two kinds of T800 specimens show the brushy fracture mode
respectively. The T300/#3631 specimens show the mixed mode between straight
and brushy failures.

Failure of unidirectional CFRP is initiated by fracture of fibers because

the fracture strain of fibers is much lower than that of matrix material.
As is often mentioned, what happens after a fiber break depends on the
interfacial bonding strength^' ', fracture energy of the fiber and
toughness of the matrix resin. The straight fracture may be caused by the
growth of a transverse crack accompanied with fiber and matrix breakages,
while the brushy failure may be caused by the growth of a crack parallel to
the fiber. The difference in fracture modes between T300 and T800
specimens is considered to be caused by the magnitude of the fiber fracture
energy. Since using the toughed matrix in T300 specimens can suppress the
straight failure, T300/#3631 specimens may have only a failure mode and
slightly small scatter at the given strength. On the other hand, two types
of T800 specimens also can have one failure mode and considerably smaller
scatter at the given strength.

As shown in Fig.2(A)-(B), two kinds of fracture modes, similar at room

temperature, were observed at -4-0°C on the T300/#3601 specimen when the
influence of the temperature was examined. In the case of 100°C,
T300/#3601 specimen, the brushy fracture mode as shown in Fig.2(E) was
observed. It is thought that the toughness of the matrix resin improves
when the temperature rises thus the progress of the microscopic failure and
680

T300/#3601 T300/#3631

T800/#3601 T8Q0/#3631 I
|RoomTemp. P H — ' ■""■ mm
Fig. 2 Typical fracture modes of CFRP specimens.

the brittle fracture in the composite is suppressed.

CONSIDERATION OF STRENGTH VARIABILITY FACTOR

EFFECT OF MATRIX RESIN

Two kinds of fracture modes were shown and large scatter of strength was
observed in T300/#3601 specimen at room temperature. Frequency distribution
of the strength data of T300 and T800 specimens are shown in Fig.3. As for
otrorif/th distribution oT T300//B601 specimen, it io thought that two
different distributions as shown in the figure, are mixed and it appears
that a different process exists together in fracture. In the case of
T300/#3601, the fracture mode, as shown in Fig.2(c) was observed a lot, it
is thought that the cause of the low side of the strength of the mixing
distribution is formed by causing such a fracture. It is believed that
the cause of scatter was increased by causing such a fracture. As for the
T300/#3631 specimens at room temperature, only one kind of fracture mode
was shown and the strength distribution is composed by a single
distribution, and the scatter of the strength is comparatively small. This
difference of T300/#3601 and T300/#3631 specimen is thought to be cause by
the difference of the matrix resin used.

DEPENDATION OF TEMPERATURE

The tensile property of the T300 specimen in the three temperature

conditions is shown in Table 2. As for strength, strain and the scatter, it
was shown to change largely by the temperature. In the case of T300/#3601,
the tendency that the strength would increase and the scatter would
decrease with a temperature increase was observed. However, the strength of
T300/#3631 at room temperature was the highest, but the tendency of a small
scatter was also seen in the high temperature case of T300/#3631 specimen.
Frequency distribution of the strength data of T300 specimens are shown in
 681

T300/»3601 -M"t T300/»3631 -nn

j H H K I ,l—JflULI

1200 1600 2000 600 1200

TtnsH. Sttwjl* IHW

Fig. 3 Frequency histograms of Fig. K Frequency histograms of

tensile strength data in room tensile strength data in three
temperature condition. temperature conditions.

Fig. 4.- Two different strength distributions are mixed in the case of
T300/#3601 at room temperature. If the temperature lowers, the scatter of
strength of the composite increases because the distribution of low side
strength increases and the distribution of high side strength decreases.
When rising the temperature, it wa shown that scatter was small because
the distribution moves to the high strength side and the data whose
strength is extremely low decreases and becomes a single distribution. In
the case of T300/#3631, the distribution of strength at room temperature
was the highest and the strength distribution was composed by single
distribution, but if the temperature lowers, the scatter will increase
because the two different strength distributions are mixed. When
temperature is rising, there is a tendency for small scatter, but the
strength of the composite decreased because the strength of the matrix
resin decreased.

Next, the relation between energy release rate of cured neat resin and
tensile strength of T300 specimen is shown in Fig.5- Strength of average
value and standard deflection are shown in this figure. The side of the
axis in this figure is the energy release rate of the cured neat resin that
is required by crack though the unit area progresses. The tendency that the
strength of the composite would increase and the scatter of strength would
decrease with the increase of matrix toughness was confirmed. Moreover, the
relation between the energy release rate of cured neat resin and the
variation of composite strength is shown in Fig.6. It was clearly shown
that the scatter of strength decreases when toughness of matrix resin is
high. It is thought that the progress of the microscopic failure in
composite is obstructed and the brittle fracture is suppressed when high
toughness matrix is used so it clarified that toughness of matrix resin is
an important factor by which the strength and the variation were decided.
682

2000

40 60 80 100 120 140 160 40 60 80 100 120 140 160

Energy Release Rate Energy Release Rate
of Cured Neat Resin (N/m) of Cured Neat Resin (N/m)

Fig. 5 Relationship between energy Fig. 6 Relationship between energy

release rate of cured neat resin and release rate of cured neat resin and
tensile strength of composite. coefficient of variation of Odeg.
composite strength.

CONCLUSIONS

The principal results are summarized as follows;

(1) The variation of elastic properties is small, but the variation of
strength and strain is large as compared with metal material.
(2) That toughening the matrix resin generally yields a improvement of the
reliability of CFRP and shifts the strength to higher values, but the
degree of improvement depends on the combination of fiber and matrix.
(3) The scatter of strength decrease when the temperature rises.

REFERENCES

(1) Z.Meakawa, Reinforced Plastics Vol 34, No. 1_, pp,23-28(1988)

(2) P.E.McMahon and D.G.Taggart, "Effects of Carbon Fiber Strain and Resin
Characteristics on Optimum Composite Performance," Proceedings of the 4th
International Conference on Composite Materials, pp.529-536(1982)
(3) Ch.Baron, K.Schulte, and H.Harig, "Influence of fibre and Matrix
Failure Strain on Static and Fatigue Properties of Carbon Fibre reinforced
Plastics," Composite Science and Technology, 2£, pp257-272(1987)
(4) S.Yamane, T.Hiramatsu, and T.Higuchi, " 'TORAYCA' T1000 Ultra High
Strength Carbon Fiber and Its Composite Properties," Proceedings of the
32nd International SAMPE Symposium, pp.928-937(1987)
(5) T.Norita, J.Matsui and H.S.Matsuda, Proc. of the 1st Intern. Conf.
Composite Interfaces, pp.123-132(1986)
(6) T.Uematsu, A.Matsuki, T.Ikeda and H.Fukuda, Proc. of the 3rd Japan-U.S.
Conf. on Composite Materials, pp.719-726(1986)
WS4b1

INVESTIGATION OF CRUSHING STRENGTH OF SiaN* BALLS FOR

CERAMIC BEARINGS FROM A STATISTICAL POINT OF VIEW

M.ICHIKAWA , T.TAKAMATSU , N.OKABE and Y.ABE

* Dept. of Mechanical and Control Eng., Univ. of Electro-

Communications, Chofu-shi, Tokyo 182, Japan.
** Toshiba Corporation, Tsurumi-ku, Yokohama 230, Japan.

ABSTRACT

Crushing tests of S13N4 balls for rolling bearings were carried out for two purposes: to
investigate the statistical properties of the crushing load Pc, and to investigate the size
dependence of Pc. For the former perpose, SisN* balls with the diameter 3/8inch (9.525mm)
were tested. For the latter purpose, Si3N* balls with the diameter of l / 8 ~ 3/4inch (3.175
— 19.05mm) were tested. From the experiments, it was found that Pc followed a two
parameter Weibull distribution with the shape parameter m p c 2il3, and that Pc depended on
the ball radius R as Pcoc R* with A ^ 1 . 8 . Furthermore, a probabilistic theory of crushing
strength was proposed. The experimental results could successfully interpretted by the
proposed theory.

KEYWORDS

Ceramic bearing; silicon nitride; bearing ball; crushing test; crushing load;
statistical property; size effect; Weibull distribution.

INTRODUCTION

Ceramic bearings using silicon nitride were recently developed, and put into service under
various severe conditions. As in steel bearing balls, high static strength and high rolling
fatigue strength are required to ceramic bearing balls. With respect to static strength, the
ring crack (Hertz crack) initiation load was studied (Fujiwara et. al, 1988). In the present
paper, the crushing load Pc is studied as a measure of static strength. Pc is the compressive
load at which final fracture of a ball occurs. As tensile fracture strength of ceramic materials
is associated with large scatter, it is expected that there is also large scatter in the crushing
load Pc. Furthermore, it is expected that scatter of tensile fracture strength brings an
influence to the size dependence of Pc. A few data on the size dependence of Pc are found
in literature (Rokkaku et al., 1988), but it is difficult to derive a definite conclusion. Thus,
in the present paper, crushing tests were carried out on SisNi balls in order to study the
statistical distribution and the radius dependence of the crushing load .

683
684

Fft
Fig.l. Crushing test method.

Then, a probabilistic theory of the crushing strength was proposed. The theory is based on
the assumptions that tensile fracture strength of a volume element of a ball follows a two
parameter Weibull distribution and that a median crack which leads to final fracture is
initiated when the tensile stress beneath the contact zone exceeds tensile fracture strength of
the corresponding volume element. The predictions by the theory on the statistical
distribution and the radius dependence of the crushing load were shown in good agreement
with the experimental results.

EXPERIMENTAL PROCEDURE

Ceramic balls tested are SiaN* balls for rolling bearings. The fabrication process of the
balls is as follows: near-net-shaped pressureless sintering-* hot isostatic pressing (HIP)
^surface finish. Mechanical properties of SisN* tested are as follows: density 3.24 g/cm3,
Young's modulus 304 GPa, Poisson's ratio 0.28, Vickers hardness 1476, and fracture
toughness 7.6 MPa • m1/2. Employing JIS B 1501 method, crushing tests were carried out by
compressing two balls of the same size as shown in Fig.l. An Instron type testing machine
was used. Two kinds of crushing tests were carried out: tests for investigating statistical
properties of the crushing load Pc, and tests for investigating the radius dependence of Pc.
In the former, SisN* balls with the diameter 3/8inch (9.525mm) were tested, and in the
latter, the ball diameter was varied in the range of l/8~3/4inch (3.175~ 19.05mm).

EXPERIMENTAL RESULTS

Fracture Appearance

When two balls of the same size were compressed against each other as shown in Fig.l,
two cases were observed. In the first case, one ball exhibited final fracture whereas the
other kept the original spherical form. In the second case, both of the two balls exhibited
final fracture. Fig.2(a) shows an example of the ball which exhibited final fracture and was
restored to the original state of sphere. Fig.2(b) shows an example of the ball which did not
exhibit final fracture. It is seen from Fig.2(b) that ring cracks (Hertz cracks) and median
cracks (radial cracks) are formed. This implies that final fracture is preceded by formation
of ring cracks and median cracks. It is also seen from Fig.2(a) that final fracture occurs
along the vertical planes involving the loading axis. Comparing this macroscopic fracture
 685

(a) (b)
Fig.2. Fracture appearance, (a) a ball which exhibited final fracture,
(b) a ball which did not exhibit final fracture.

path with geometry of a ring crack and a median crack, it is reasonable to consider that
final fracture is caused by median cracks, not by ring cracks.

Statistical Distribution of Crushing Load

20 pairs of Si3N<* balls with the diameter 3/8inch (9.525mm) were tested at the crosshead
speed V=10mm/min. Furthermore, 5 pairs were tested at V=1.0mm/min, and another 5 pairs
were tested at V=0.1mm/min. Fig.3 shows the mean crushing load at each crosshead speed.
It is seen from Fig.3 that within the range of V in the present experiment, the crushing load
is not influenced by the crosshead speed. Thus, the data obtained at V=10, 1 and
O.lmm/min were pooled. Fig.4(a) shows the pooled data of the sample size 30 as plotted on
Weibull probability paper. It is seen that the crushing load follows approximately a two
parameter Weibull distribution whose distribution function is expressed as

F(Pc)=l-exp[-e-)mpc ] (1)
ro

The shape parameter m pc was estimated as mpc=12.8.

In addition to the above tests, tests aiming at a preliminary study of proof test effects were
carried out on 20 pairs of SiaN* balls with the diameter 3/8inch (9.525 mm). In these tests,
load was increased up to a prescribed proof load and then unloaded rapidly. The crosshead
speed on loading was taken as V=1.0mm/min. In testing of first 10 pairs, the proof load was
chosen as 24.5kN (2500kgf). In this case 7 pairs exhibited final fracture on loading. In
testing of another 10 pairs, the proof load was chosen as 22.54kN (2300kgf). In this case, 2
pairs exhibited final fracture on loading. Thus, the censored data of the sample size 20 was
obtained. Adding this data to the above crushing test data, the data of the sample size 50
was obtained. This data was plotted on Weibull probability as shown in Fig.4(b). It is again
seen that the crushing load follows a two parameter Weibull distribution. The shape
parameter m pc was estimated from Fig.4(b) as mpc=13.1, which is quite close to mpc=12.8
estimated from Fig.4(a). It should be noted that m pc is the shape parameter for the
686

1 10
Cross head speed V mm/min

Fig.3. Mean crushing load Pc as plotted against crosshead speed V.

1
2 o
o
a.

20 30 40 20 30 40

Crushing load Pc KN Crushing load Pc KN

(a) (b)
Fig.4. Weibull plot of the crushing load Pc. (a) complete data of sample size 30.
(b) censored data of sample size 50.

distribution of the crushing load, and is different from the usual Weibull modulus obtained
from bending or tension tests.

Radius Dependence of Crushing Load

SisN* balls with the diameter ranging 1/8—3/4inch (3.175—19.05mm) were tested in order
to investigate the radius dependence of the crushing load. Two series of tests (Series F-l
and Series F-2) were carried out. Figures 5(a) and 5(b) show the experimental results. Each
+ symbol in these figures corresponds to one pair of balls. It is seen that a power law holds
between the crushing load Pc and the ball radius R. Using the method of least squares,
Pc=1.563Rx-,f><> (Series F-l) and Pc=1.374R1 (Series F-2) were obtained (Pc:kN,
R:mm). Hence, Pc varies with R as

PccxR* (A -1.8) (2)

 687

(a) (b)
Fig.5. Dependence of the crushing load Pc on the ball radius R.
(a) Series F-l, (b) Series F-2.

3 A 5 10 20 30 3 A 5 10

Diameter D.mm Diameter D.mm

(a) (b)
Fig.6. Variation of Pc/D2 on the ball diameter D.
(a) Series F-l, (b) Series F-2.

It is noted that A is smaller than 2. Pc/D2 is sometimes used as an index of crushing

strength, where D is the ball diameter. Figures 6(a) and 6(b) show Pc/D2 as plotted against
D. It is clearly seen that Pc/D2 is not constant but decreases with increase of the ball size.
As the maximum contact pressure q m a x is proportional to (Pc/D 2 ) 1/3 , Figs.6(a) and 6(b)
imply that crushing strength cannot be completely specified in terms of the maximum
contact pressure.

For comparison, crushing tests were also carried out on SisN^ balls before surface finish.
Four series of tests were carried out, which were denoted as UF-1, UF-2, UF-3 and UF-4.
It was found that unfinished balls also followed eq.(2). Fig.7 shows comparison of Pc vs. R
relations for finished and unfinished balls. Only regression lines are shown. It is noted that
the crushing load of the unfinished balls is almost the same as that of the finished balls.
Hence, the crushing load can be evaluated before surface finish.
688

500,

200

Fig.7 Comparison of the crushing load Pc before and after suface finish.

~d>Oe

Fig.8 Tensile stress induced by contact of two balls.

THEORETICAL CONSIDERATION

Before constructing a probabilistic theory of crushing strength, we compare the ring crack
initiation load and the median crack initiation load. When two balls of the same size are
compressed against each other as shown in Fig.l, the radius of the contact circle, a, is given
by a=[(3(l-i> 2 )PR)/4E] 1/3 and the maximum contact pressure q m a x is given as follows
(Timoshenko et al., 1970).
3P 6E^P
(3)
'in a2 ;r(l-OR2

As shown in Fig.8, the radial tensile stress o r is induced in the thin skin layer outside the
contact circle, and the circumferential tensile stress o Q is induced around the loading axis
(z axis) beneath the contact circle. The former is responsible to ring crack formation and the
latter to median crack formation. The tensile stress o r at the surface (z=0 plane) varies with
 689

r asa z (z=0)=a max .i(a/r) for r^a, and a m a x , i is given by C7max,i=(l-2i> )q max /3
(Timoshenko et al., 1970). Hence, o max,i=0.147qmax for v =0.28. The tensile stress a Q
on z axis varies with z as (Hamilton et al., 1966)

o e(r=0) = q max [(l+ v)( - tan" 1 - -1) + — 1 - 5 : ] (4)

a a 2(a +z )

The maximum of a ^ (r=0) appears at z=2.1a, and this maximum o max.z is obtained as
o max,2=0.00702qmax for u =0.28. Comparison of o m«x,i and a m a x ,2 shows that the
former is much larger than the latter. Hence, it is reasonable to consider that ring cracks
first appear, and then median cracks appear. When a median crack extends to the ball
surface, it appears as a radial crack.

Noting that final fracture is caused by median cracks, we next derive the median crack
initiation load. The derivation is somewhat similar to one for Hertz crack formation in
indentation fracture of a glass plate by a steel ball (Oh et al., 1967). The distribution of the
tensile stress o Q around the z axis which is responsible to median crack initiation is
changed by appearance of ring cracks. Due to axial symmetry, however, it may still be
expressed after ring crack initiation by the following general equation.

a Q = O maxf(z,r)=kiqmaxf(z,r) (5)

where a max is the maximum of a Q . ki is the non-dimensional coefficient defined by

o max=kiqmax. Assume that tensile fracture strength a f of a volume element dV is
randomly distributed in space and follows a two parameter Weibull distribution with
Weibull modulus m. Then, its distribution function, G(cTf), is expressed as
Of m dV
G(af)=l^xp[-( )m — ] (6)
Oo Vo

where Vo is the reference volume for which the scale parameter a o is defined. Let o M be
the value of a m a x in eq.(5) at the instance when a median crack is initiated, and H(aM) be
the distribution function of a M. From eq.(6), H(<7M) can be derived as
1 o f) aM Vcff
H(aM)=l-exp[ ■ —( )mdV] = l-exp[-( )m—-] (7)
y Vo Oo Oo Vo

where Veff is the effective volume, and is proportional to R3 in this case. That is,

VCff=k2R3 (8)

where k2 is a non-dimensional constant. Let PM be the median crack initiation load, and
O (PM) be the distribution function of PM. From eqs.(3), (7) and (8), <D (PM) can be obtained
as
k2R3 ki 3 6E2 PM _
O(PM) = i^xP[ — - { — 3 - -sz—^-r -r-r" ] (9)
Vo oo n (1- v ) R
As the relation between PM and the crushing load Pc has not been known, we tentatively
assume the following relation based on a dimensional consideration
690

Pc PM „
k3( (10)
iP = iR^
where ks and a are non-dimensional coefficient. Let ¥(Pc) de the distribution function of
Pc. From eqs.(9) and (10), it follows
k2R3 ki3 6E 3 Pc Un mn
1/a m/3
¥(pc) = i-exp[ - — { — 5 - -r:—^r (-T—T) } 1 (ID
Vo oo n (l-v ) ksER
According to eq.(ll), the crushing load Pc follows a two parameter Weibull distribution.
This is in agreement with the present experiment. It also follows from eq.(ll) that the
curshing load depends on the ball radius R as Pcoc R* with A =2-9 a /m and that the sape
parameter of the distribution of the crushing load, m p c , is m/(3 a ). On the other hand, the
experimental value of m p c is about 13. From m/(3a )=13, A is predicted as A =2-9
a /m=2-3/13=1.77. This value of A is in good agreement with the experimental value A
2i 1.8. Thus, both of the statistical distribution and the radius dependence of the crushing
load found in the present experiments can be interpretted by the proposed theory.

CONCLUSIONS

(1) It was found experimentally that the crushing load Pc of SisN* balls for cermic bearings
followed a two parameter Weibull distribution with the shape parameter m p c ^ 1 3 .

(2) It was found experimentally that Pc varies with the ball radius R as Pcoc R A with A
21I.8. Thus, A is smaller than 2.

(3) A probabilistic theory of the crushing strength of ceramic balls was proposed, and both
the experimental results (1) and (2) mentioned above could be interpretted by the proposed
theory unifiedly.

The authors wish to thank Mr.K.Nishida of Toshiba Corporation for his help in this study.
Thanks are also due to Miss T.Hohjo, Mr. H.Yuhara, and Mr. N.Shindoh, graduate students
of University of Electro-Communications for their help in the experiment. A part of this
study was supported by Grant-in-Aid for Scientific Research, Ministry of Education,
Science and Culture, Japan.

REFERENCES

Fujiwara,T., T.Yoshioka, T.Kitahara, S.Koizumi, H.Takebayashi and T.Tada (1988). Study

on Load Rating Property of Silicon Nitride for Rolling Bearing Material. J.Japanese Soc.
Tribologists, 33, 301-308.
Hamilton, G.M. and L.E.Goodman (1966). The Stress Field Created by a Circular Sliding
Contact. Trans. ASME, J.Appl.Mech., 33, 371-376.
Oh.H.L and I.Finnie (1967).The Ring Cracking of Glass by Spherical Indenters.
J.Mech.Phys.Solids, 15, 401-411.
Rokkaku K, H.Takebayashi and K.Nishida (1988). Performance and Application of Ceramic
Bearings. Koyo Engineering Journal, No.133, 63-71.
Timoshenko, S.P. and J.N. Goodier (1951), Theory of Elasticity, McGraw Hill.
WS4b2

PROOF TESTING OF CERAMIC MATERIALS SUBJECTED

TO CYCLIC LOADING

T. HOSHIDE, N. SATO and T. INOUE

Department of Mechanical Engineering, Kyoto University

Sakyo-ku, Kyoto 606, Japan

ABSTRACT

A numerical simulation for two distinct materials and an experiment using

an alumina were conducted to investigate the effect of the stress rate in a
proof testing on the subsequent fatigue behavior. The simulated result
revealed that as increasing the unloading stress rate the minimum life be-
came longer and finally approached to the largest value, while the minimum
life was not affected by the loading stress rate. In the experiment, the
proof testing was found not to be efficient for the subsequent fatigue
properties unless the unloading stress rate was selected to be adequately
higher. The life distribution could be estimated by the band region be-
tween two extreme distributions associated with the crack geometry.

KEYWORDS

Proof testing, fatigue, stress rate, crack growth, statistics, ceramics

INTRODUCTION

The proof testing for ceramic materials has been proposed as an effective
procedure to exclude components with lower strength, which are not allow-
able in structural design. The investigations on proof testing applied to
fatigue strength have also been conducted experimentally or theoretically
(Ito et ai., 1983, Yamauchi et al,, 1984, Hoshide et al., 1990, Hamanaka et
al, , 1990). However, it has not been clarified how the stress rate during
proof testing and the crack growth characteristics affect the failure prob-
ability during proof testing and the subsequent fatigue behavior.

In the present paper, the effects of the loading and unloading stress rates
on the subsequent fatigue properties were investigated by a numerical
simulation based on the previous theoretical study (Hoshide et al., 1990)
for two materials with distinct crack growth characteristics. Experimental
study using an alumina was also conducted to investigate the effect of the
proof testing condition on fatigue strength.

691
692
THEORETICAL ANALYSIS

Formulation of Fatigue Life after Proof Testing

The loading pattern in proof testing to be analyzed is a triangular type,

which is characterized by the proof stress G p, and the constant loading
and unloading stress rates & L and & u. Some relevant equations derived
in the authors' work (Hoshide et al., 1990) are summarized below.

The crack growth laws used in the analysis are

for the crack growth under cyclic loading, and

for the crack growth due to the slow crack growth (SCG), so-called. In the
above equations, the equivalent crack length 1 - a Mo2 (Yamada et al.,
1984, Hoshide et al, , 1984) is introduced, where a is the crack length and
Mo is the magnification factor in the evaluation of stress intensity fac-
tor. If the cumulative distribution function Fi(l) of 1 is given, the
cumulative distribution function FN(NX) of fatigue life is presented as

The relation between fatigue life Nx and a specified equivalent crack

length lx is given by

The crack length lmax in the specimen before proof testing corresponding to
the maximum crack length in the surviving specimen is given by the follow-
ing equations, according to the unloading rate & u. For

and for 6 u ^ & uo ,

where o" *min is the minimum fracture stress in the unloading process; i.e.

The constants in the above equations are as follows; A=1/(TC n'2C q), q=(n-
2)/2, B=1/(7C s'2Cs'r)t and r=(s-2)/2. The crack-length parameter lo is the
factor to take account of the crack-size effect in the fracture mechanics
analysis (Kitazumi et al., 1989), and Kc is the fracture toughness.

The minimum life Nmin is evaluated as Nx calculated by substituting lmax

for lx in (4), and the failure probability PP in the proof testing is
presented as Pp = 1 - Fi(lmax).
 693
Testing Conditions and Parameters Used in Numerical Simulation

A sintered alumina with 96% purity (AI2O3) and a sintered silicon nitride
(Si3N4) are examined as model materials. Unless the stress rates are
specified, 6" i=100MPa/s and & t/=1000MPa/s are used. The proof stress o" P
is 1.5 times of the maximum stress o" a in the subsequent fatigue test,
which are conducted under the sinusoidal loading of 40Hz and the stress
ratio /^0.05. The value of o" a is 300MPa for AI2O3 and 600MPa for Si3N4.

The constants in the crack growth equations (1) and (2) are 05.68X 10" 14 ,
n=11.3, CS=1.38X 10-8 and s=5.5 for AI2O3, and O 2 . 6 3 X 1 0 " 2 4 , n=21.1,
Cs=4.50X 10 - 4 0 and s=40.7 for Si3N4, respectively, where da/dN is described
in m/cycle, da/dt in m/s and K in MPa/~ln. These parameters were obtained
by using the procedure proposed in the previous study (Hoshide et al.,
1988). The toughness Kc is 3.7MPaV~m in AI2O3 and 7.0MPaV"ln in Si3N4.

The magnification factor Mo is set the constant of 0.654 corresponding to

the case of semi-circular surface crack, although it may change depending
on the crack geometry. The cumulative probability function Fi(l), which
has been obtained in another three-point bending test, is adopted as the
initial crack distribution. The parameter lo is assumed to be 0M m.

Effect of Stress-Rate on Life Distribution

0.999i

'KT'

licr*

KT*
1 K)2 tf Kf 1C
Number of cycles . Nt
Fig.l Effect of loading rate on fatigue life
distribution in alumina.

1 5 10 50 100
<JL(MPQ/S)

Fig 2 Dependence of minimum life and failure

probability on loading rate.
694

0.9991
9 6 * AliOs

-crl

Siof

1 102 & K)6 K)8

Number of cycles , Ni

Fig.3 Effect of unloading rate on fatigue l i f e

distribution in alumina.
K)6

!S
.5? 104
B

! tf

XX) 500 1000

<X(MPa/5)

Fig.4 Dependence of minimum life and failure

probability on unloading rate.

Figure 1 presents the relation between the life distribution and the load-
ing stress rate o"i in AI2O3. As increasing & L , the cumulative probabil-
ity FN becomes higher compared at the same life. However, the minimum life
Nmin does not depend on 6"x. The similar tendency is also found in Si3N4.
The relations of Nmin and the failure probability Pp in proof testing
against & L for both materials are indicated in Fig.2. Higher &L
results in lower Pp. Compared at the same 6*1, Pp is higher in AI2O3 than
in Si3N4. The variation of Pp against 6" x is larger in AI2O3 than in Si3N4.

The effect of the unloading stress rate & u on the above strength
parameters after proof testing is shown in Figs.3 and 4. When increasing
& u, the minimum life shifts toward higher fatigue life region, and becomes
closer to the highest life that has been calculated for the case without
SCG (Hoshide et al., 1990). Pp is independent of & u in the region of more
rapid unloading. When & u becomes less than & uo given in (5), however, Pp
increases significantly. In this situation, too, higher Pp and larger
variation of Pp are observed in AI2O3 than in Si3N4.

As above mentioned, the effect of stress rate during proof testing on

fatigue strength is larger in AI2O3, which is more sensitive to SCG. It is
concluded that the fracture mechanics properties of the material under con-
sideration are so important in the selection of the stress-rates.
 695
EXPERIMENTS AND COMPARISON WITH ESTIMATION

Material Tested and Experimental Procedure

The material tested was an alumina with 96% purity. The Young's modulus
and the mean three-point bending strength are 349GPa and 414MPa, respec-
tively. Specimens with the dimensions of 4X 5X 25mm were as-fired. The
loading mode was three-point bending with the span length of 20mm, by con-
trolling the maximum stress. The proof testing was conducted using a tri-
angular loading with & L =100MPa/s. The proof stress and the unloading

1
"■" 1 1 1

i
1 ' ~r
961AUOJ
1 Ob-MOMPQ
OOOO 0 -
[ ft* MOM*
■?eooo|
*
40 h o o ooo o \

o o a>oo o \
1 i i i i iL 1 _

1 K>2 10* 10* 10

N u m b e r of cycles , Nf

Fig.5 Effect of unloading rate on fatigue life.

Q99h
if 0.90k " ^ A U Oj
p 0t=300MPa
*a50F CTp=380MPa
>> P 0u=8000MPa/s

I
|0.05|-

I
a
O2 10* tf
Number of cycles . Ni

Q99l c i — i — i
' / ) J ' 1

if 0.90l-
961 AlzOi
/ r / S _
E 01=300 MPa ^ / j y \ / -
F
"0.50F Op=380MPa j
0U = 40 MPa/s ^ ^ Itff
o 0.10
L
/ / M> —
_j

8 0.05 L
/ a*_
H
j 06~
V Q8

/1 i il 1. 1 1 1
K)2 Kf tf tf
Number of cycles , Ni

Fig.6 Estimated fatigue life distribution.

696

stress rate were changed to observe their effects on fatigue strength. Ten
specimens were employed in each testing condition. The fatigue tests of
specimens surviving in the proof testing was conducted under the sinusoidal
loading of 40Hz and R=0.05. All tests were done in an ambient atmosphere.

Experimental Results and Estimation of Life Distribution

The effect of o" p on the fatigue life Nf appeared in the truncation of

lower life. Larger proof stress was found to result in higher minimum
life. Figure 5 presents the effect of & v on Nf. As shown in the figure,
the proof testing with cr t/=40MPa/s is not effective on the minimum life,
contrary to the case of higher & u.

The subsequent fatigue life is estimated by using the formulation as al-

ready mentioned. Same parameters in the simulation were also used in the
estimation, except for 1O=10JLL m suggested elsewhere (Hoshide et al., 1988).
The factor Mo is found to exist within the range from 0.51 to 0.78 by the
observation in another static strength test of the same material. Con-
sequently, the estimation was made for the three cases of Afo=0.4, 0.6 and
0.8, which cover the observed values. Figure 6 shows that the experimental
result exists between two extreme distributions for Mo=0.A and 0.8.

ACKNOWLEDGMENTS

The authors are much indebted to Otake Ceram Co., Ltd., for preparing
alumina specimens. This work was partly supported by the Grand-in-Aid for
Scientific Research (No.02805013) from the Ministry of Education, Japan.

REFERENCES

Hamanaka,J., H.Ezumi, A.Suzuki and S.Sugiyama (1990). Proof testing of

ceramic components (2nd Report, Fatigue fracture strength after proof
testing). Trans,Japan Soc.Mech.EngrfSer.A, 56, 462-468.
Hoshide,T., H.Furuya, Y.Nagase and T.Yamada (1984). Fracture mechanics ap-
proach to evaluation of strength in sintered silicon nitride. Int.J.
Fract., 26, 229-239.
Hoshide,T., T.Ohara and T.Yamada (1988). Fatigue crack growth from indenta-
tion flaw in ceramics. Int.J.Fract*, .37, 47-59.
Hoshide,T., N.Sato and T.Inoue (1990). Fatigue properties of ceramics after
proof testing (1st Report, Theoretical analysis). Trans, Japan Soc.
Mech.EngrtSer.A, 56, 212-219.
Hoshide,T., N.Sato, T.Ohara and T.Inoue (1990). Fatigue properties of
ceramics after proof testing (2nd Report, Experimental study). Trans,
Japan Soc.Mech.EngrtSer.A, 56, 220-223.
Ito,S., Y.Yamauchi, M.Ito and S.Sakai (1983). Bending cyclic fatigue test
of pre-loaded ceramics. Proc, 26th Japan Congr,Mater,Res., 270-274.
Kitazumi,J., Y.Taniguchi, T.Hoshide and T.Yamada (1989). Characteristics of
strength and their relations to flaw size distribution in several ceramic
materials(Part 1:Static strength). J,Soc.Mater.Sci,,Japan, 38, 1254-1260.
Yamada,T., T.Hoshide and H.Furuya (1984). Static and cyclic fatigue
strengths of sintered silicon nitride. J.Soc. Mater.Sci.,Japan, 33, 28-33.
Yamauchi,Y., S.Sakai, M.Ito and S.Ito (1984). Bending cyclic fatigue test
of pre-loaded ceramics (II ) (Effects of load condition on fatigue
strength). Proc. 27th Japan Congr.Mater.Res., 235-240.
WS4b3

STATIC AND FATIGUE STRENGTH AND THEIR RELATIONS TO FLAW

SIZE DISTRIBUTION IN CERAMICS

JUNICHI KITAZUMIt, YOSHIFUMI TANIGUCHIt,

TOSHIHIKO HOSHIDE} AND TOSHIRO YAMADA§

tDepartment of Mechanical Engineering, Niihama National

College of Technology, 7-1 Yagumo-cho, Niihama-city,
Ehime 792, Japan, {Department of Mechanical Engineering,
Kyoto University, Yoshida-honmachi, Sakyo-ku, Kyoto 606,
Japan, §Department of Mechanical Engineering, Professor
Emeritus, Kyoto University, Yoshida-honmachi, Sakyo-ku,
Kyoto 606, Japan ( Present address : 5-2 Tokutsune-cho,
Niihama-city, Ehime 792, Japan )

ABSTRACT

In order to study the characteristics of strength of ceramics, the constant loading

rate test and the cyclic loading test were carried out in an ambient atmosphere,
with a beam specimen and a ring specimen of ceramics. In the case of constant
loading rate condition, the fracture stress was correlated with the equivalent
crack length. The results showed that fracture for small inherent flaws occurred
at lower stress than the predicted by the linear fracture mechanics concept. The
tendency in the relation was explained by the modification that a material constant
should be added to the original equivalent crack length. The distribution of
fatigue life was investigated experimentally, and the S-N curves were predicted by
using the crack growth equation under cyclic loading, and assuming that the
distribution of flaw sizes of specimens under cyclic loading was equal to that of
the specimens used in constant loading rate test.

KEYWORDS

Ceramics; static strength; cyclic fatigue; equivalent crack length; crack growth;
life prediction; S-N curve.

INTRODUCTION

In the application of ceramic materials to engineering structures, the reliability

of materials should be guaranteed against various loading systems, which are
expected to be subjected to their components in service. It is important to
characterize the strength of materials against various loads to establish allowable
stress for component design. A large dispersion encountered in fracture strength
under various conditions is considered to be ascribed to flaw-sensitivity
associated with the brittleness of the material. Therefore, to establish allowable
stress for component design, the estimation of strength must be carried out
based on the relation between strength and natural flaws.

In this study, especially, the subjects on the loading modes of static and cyclic
type in an ambient atmosphere were investigated.
697
698
In static loadings, the dispersion in strength of ceramics is considered to reflect
the distribution of pre-existing flaws. Therefore, in predicting the distribution
of strength, the criterion of fracture must be clarified. Several investigations
(Evans et.al., 1970, Henshall et.al., 1974, Mecholsky et.al., 1977, Bansal et.al.,
1978, Kawai et.al., 1982) were carried out from the viewpoint of fracture
toughness. However, it is considered that the condition for fracture initiation
does not obey the Kic criterion; fracture occurs when Ki evaluated for the flaw
reaches Kic. Therefore, it is necessary to investigate a problem associated with
the applicability of fracture mechanics to very small flaws. In cyclic loadings,
a large dispersion is observed in fatigue life of smooth specimens, Therefore,
it is important to characterize the fatigue strength, and to estimate the endurance
limit of materials on the basis of the distribution of flaws for fatigue design.
So, first in this paper, fracture tests under constant loading rate for specimens
of a beam type and a ring type and cyclic loading for the beam type were
performed. Then, the problems mentioned above were discussed on the basis of
experimental results.

EXPERIMENTAL PROCEDURE

Materials and Specimens

The material used was a sintered silicon nitride (Si 3 N 4 ), produced by NGK Spark
Plug Co. Ltd. The density is 3.26 g/cm3 and Young's modulus is 330 GPa.

The fracture toughness, Kic of material was obtained through the controlled surface
flaw method. The indented specimens were annealed at 800*0 for 2 hr in vacuum and
cooled in a furnace. K r c for flaws larger than 300 fim in total length is 5.7 MPa/m.

Two types of specimen were used. One of them was a beam type ( 4 X 5 X 2 5 mm), and
another was a ring type (inner diameter is 19.1 mm, outer diameter is 29.1 mm and
thickness is 5 mm). Each side of specimens was ground with 200-grit diamond wheels.

Static Fracture Test

All fracture tests were carried out by using a closed-loop servo-hydraulic testing
machine. The test for beam specimen was 3-point bending type, and the stress rate
was controlled to be 100 MPa/sec at the point subjected to the maximum nominal
stress. The span length in 3-point bending was 20 mm. The compressive load was
applied to ring specimen along the diametrical direction. The maximum tensile
stress is generated at the two point of the inner surface (Ripperger et.al., 1947),
and the rate of maximum stress was also fixed to be 100 MPa/sec.

Cyclic Fatigue Test

The fatigue tests under 3-point bending were conducted in the same servo-hydraulic
machine. The cyclic sinusoidal load was applied to the specimen at 40 Hz, and the
ratio of the minimum tensile stress subjected to the specimens against the maximum,
R, was controlled to be 0.05. Ten specimens were employed at each stress level.

EXPERIMENTAL RESULTS AND DISCUSSION

Static Strength
 699
Twenty specimens were employed in 3-point bending test. The mean strength is 843
MPa and the standard deviation is 92 MPa. The relation between the fracture
strength a f and the failure probability Pf is approximated by Weibull distribution.

P f =l-exp[-(o- f /876) 9 - 3 0 ] (1)

In 3-point bending tests, the fracture position often deviate from the position of
maximum tensile stress. The true fracture stress distribution (stress at the
fractured location) is described by

Pf=l-exp[-(af/812)6-47] (2)

In ring compression test, nineteen specimens were used. The mean strength is 800
MPa and the standard deviation is 82 MPa. The strength distribution is described by

Pf = l - e x p [ - ( a f / 8 3 7 ) 1 0 - 3 ] (3)

The coefficients of correlation on eq. (1) and (2) are 0.97 and 0.99, respectively.
In 3-point bending tests, when the data were correlated with the true fracture
stress, better fitness for the two parameter Weibull distribution was found rather
than the maximum nominal stress. The effect of specimen geometry on the strength
was small in this study.

Relation between Strength and Inherent Flaw

It is considered that fracture of ceramics initiates from pre-existing flaws, and

that the dispersion in strength of ceramics reflects the distribution of such flaws
related to the surrounding stress states.

The stress intensity factor (SIF), K for a flaw usually expressed in the following
form.

K=a/Ta-F0 (4)

where a is a representative applied stress, a is a representative size of the flaw,

and F 0 is a magnification factor given by the boundary conditions (Hoshide et.al.,
1984, Yamada et.al., 1984). The critical SIF, Kc, for the flaw identified as the
fracture-initiating origins, is obtained as the range of the maximum value of SIF
evaluated for a circumscribed ( semi- or quarter- ) circle and inscribed ( semi- or
quarter- ) circle for the shape of flaw.

If the equivalent crack length a eq is defined by

a e q = a - F 0 2 = (Kc/a)77r (5)

then the relation between the equivalent crack length and the fracture strength a f
is given as indicated in Fig. 1. The value of a e q for inherent flaws are presented
with the range obtained through the last relation in eq.(5) by using the range of
corresponding K c mentioned previously. The solid line in Fig. 1 shows the relation
under the Kic criterion. It is found that fracture from smaller inherent flaws
occurs at a lower stress than predicted by the Kic criterion. Similar results have
been reported by several investigators (Singh et.al., 1979, Miyata et.al., 1986).
Then, correcting the original crack length, the relation between the fracture
stress and the crack length is expressed in the following equation.

c7f=Kic/V n (ae q +ae q o)=Ko/Kaeq+aeqo) (K 0 =Kic/r5t) (6)

700
where, a eq o is the added material constant to the original equivalent crack length.
The dotted line in Fig. 1 shows the relation in eq.(6), where a e q o is equal 10 fim.
Eq.(6) explains the relation between the fracture stress and the crack length from
the small inherent flaw to the large artificial flaw.

£1000
1 T 1 ! II 1 | \l ' i 1 T I II I
H
T
s 3N4 M
I 900
800 " ^ g g g g-\T^ *-o- 4

-* 700" *nNx -
^ 600
" N
\ \
\
1
5 500
£ 400
Inherent flaw
A A Subsurface flaw \\ H

0 Corner flaw \«v j

x

J
_ D Surface flaw Open n a r k s : \
^ 300 Artificial flaw beam specimens ^ I
u ■ Surface flaw H a l f o p e n m ark s :

£■ 200 i i 1 i >i i 1 i i
ring specimens
i M i l l 1 1 1
|
5 10 50 100 500
Equivalent crack length 2 a e q , urn

Fig. 1. Relation between equivalent crack length and

fracture stress in Si 3 N 4 .

Cyclic Fatigue Strength

101 ioz 10
Number of cycles Nf

Fig. 2. Relation between stress and fatigue life of

Si 3 N 4 in cyclic fatigue test under 3-point
bending.

The relations between applied maximum stress and fatigue life are plotted in Fig. 2.
The marks plotted at N f = l mean the data for the specimens fractured during the
first time. And the range of the dispersion of the static strength under constant
loading rate is also shown at N f = l . At 400 MPa of maximum stress, all of 10
specimens did not fractured at 10 7 cycles. Then, it is considered that the above
value of stress is the endurance limit of the material truncated at 10 7 cycles.
 701
Prediction of Cyclic Fatigue Life

A large dispersion was observed in the fatigue life of the smooth specimens, which
depends heavily on the flaw size in the specimens. The dispersion in the fatigue
life may be ascribed to the dispersion of inherent flaw sizes. However, it is
difficult to measure the inherent flaw size of fracture origin in advance.
Therefore, supposing that the distribution of the flaw sizes of specimens in the
fatigue tests is equal to that of the specimens in the static tests, the prediction
of fatigue life is discussed on the basis of the crack growth equation.

Assuming that the fatigue process might be identical to the process of crack
propagation from the initial flaw, the crack growth equation would be usually the
following equation.

daeq/dN=Co*Km (7)

In eq. (7), K m a x = a m a x ^ n (a e q +a e q 0 ,) as a similar form to eq. (6), and n and c 0

depend on material and testing conditions. Integration of eq. (7) from the initial
crack length a cq i to the final crack length a eq f, i.e.

Nf = {2/c 0 (n-2) K n/2 a m a x n } { ( a e q i + a e q o ) (2"n)/ 2 - ( a e q f + a e q 0 ) {2~n) /2) (8)

Assuming that the relation between a eq f and crmax is given by eq. (6), and
substituting ( a e q f + a e q 0 ) 1 / 2 = K o / c 7 m a x into eq. (8), the fatigue life N f is found
by the following equation.

Nf = { 2 / c o ( n - 2 ) 7 r n / 2 a m a x " } { ( a e q i + a e q o ) ( 2 - n ) / 2 - ( K o / a m a x ) 2 - " } (9)

The distribution of the flaw sizes of specimens in the static tests is described by

F a (ae q i ) = l - e x p [ - { ( K o / a 0 ) 2 / ( a e q i + a e q o ) } m / 2 ] (10)
where, m and d o are the shape and scale parameters in Weibull distribution of true
stress in 3-point bending tests, respectively. In cyclic fatigue tests, from eq. (9)
the initial flaw size of specimens is shown by the following equations.

aeqi=[NfcTmaxnCo(n-2)^:n/2/2+(Ko/amax)2-n]2/(2-n)-aeqo for N f > l

} (ID
aeqi=(Ko/c7max)2—aeq0 for N f = l

99 — i — l—l—1 1 \ \ 11 1 1 «—r-r-r
S13N4 ^H
- 70
"S X 50 J
.o H
£ -30 -|
°- ■& H
5 5 10
«"- 5
/ °
yC O
H

-+

E ^F.*«PWS&>"*]
3 i 1 1 1 i l 1 1 1 1 1 1 1 1L,li_

10"^ 10 l
Half equivalent crack length aeqi^.ijm-1-

Fig. 3. Distribution of equivalent crack length for

Si3N4.
702
The flaw size distribution of specimens in fatigue tests can be predicted by
eq.(11) with the experimental data, amax and N f . It is considered that the initial
flaw distribution of specimens in fatigue test is essentially equal to that in the
flaw distribution of specimens in fatigue test is essentially equal to that in the
static test. Therefore, the values of n and c 0 were determined, so that the
difference in absolute value between the both flaw size distributions is small.
The values of n and c 0 are 28, 0.55X10" 1 0 9 , respectively, where stress is in MPa
and crack length is in {im. In Fig. 3, the marks show the distribution of initial
flaw sizes in fatigue test, and the solid line is the flaw size distribution in
static test by eq.(10). The solid lines in Fig. 2 are the S-N curves with different
sizes of initial crack length predicted by eq. (9), using the above-mentioned values
of n and c0. It seemed that the endurance limit truncated at 10 7 cycles would exist
at 400 MPa of maximum stress. Therefore, the S-N curves with flaw larger than 30
fim in equivalent crack length were depicted horizontally at 10 7 cycles.

CONCLUSION

The strengths of ceramics for static and cyclic loads were investigated with
specimens of a sintered silicon nitride .

The fracture for small inherent flaws occurs at a lower stress than the predicted
by the linear fracture mechanics concept. The relation between the strength and the
flaw size would be explained by the modification that a material constant was
added to the original equivalent crack length. In the cyclic fatigue tests, the
dispersion in fatigue life of smooth specimens should be explained from the
dispersion of inherent flaw sizes in specimens. Assuming that the distribution
of flaw sizes of specimens in the fatigue test was equal to the distribution in the
static test, S-N curves were predicted on the basis of the crack growth equation.
It is considered that the tendency in the distribution of fatigue life would be
explained by this prediction method.

REFERENCES

Evans, A.G. and Davidge. (1970). The strength and oxidation of reaction-sintered
silicon nitride. J. Mater. Sci., 5, 314-325.
Henshall, J.L., Rowel iffe, D.J. and Edington, J.W. (1974). Fracture parameters in
refel silicon carbide. J. Mater. Sci., 9, 1559-1561.
Mecholsky, J.J., Jr., Feriman, S.W. and Rice, R.W. (1977). Effect of griding on
flaw geometry and fracture of glass. J. Am. Ceram. Soc., 60, 114-117.
Bansal, G.K. and Duckworth, W.H. (1978T! Effects of" specimen size on ceramic
strengths. Frac. Mech. Ceram., 3, 189-204.
Kawai, M. and Abe, H. (1982). Strength distribution of sintered silicon nitride.
Reports of Research Laboratory of Asahi Glass Co. Ltd., 32, 25-36.
Ripperger, E. A. and Davids, N. (1947). Critical stresses in a circular ring. Tran.
ASCE, 112, 619-635.
Hoshide, T., Furuya, H., Nagase, Y. and Yamada, T. (1984). Fracture mechanics
approach to evaluation of strength in sintered silicon nitride. Inter. J. Frac.,
26, 229-239.
Yamada, T., Hoshide, T. and Furuya, H. (1984). Static and cyclic fatigue strength
of sintered silicon nitride. J. Soc. Mater. Sci. Japan., 33, 28-33.
Singh, J.P., Virkar, A.V., Shetty, D.K. and Gordon, R.S. (1979). Strength-grain
size relations in poIyerystalline ceramics. J. Am. Ceram. Soc., 62, 179-183.
Miyata, H., Nakakado, K. and Kimoto, H. (1986). Effect of micro-damage on fracture
strength of structural ceramics. The Japanese Society for Strength and Fracture
of Materials., 21, 45-59.
WS4b4

FRACTURE STRENGTH OF SINTERED-SioN, UNDER HIGH

TEMPERATURE AND UNIFIED ESTIMATION METHOD KITH
CONSIDERING TEMPERATURE-DEPENDENCE

H.HIRATA, K.IMAI and N.OKABE

Heavy Apparatus Engineering Laboratory Toshiba Corporation

1-9 Suehiro-cho,tsuruii-ku,Yokohaia,230,Japan

ABSTRACT

The teiperature dependence of sintered Si3N* was investigated under

teiperature range above lOOOt up to 1300t) on the oasis of unified estimation
■ethod, which are proposed for the evaluation of ceraiic strength
properties. The normalized fracture strength can be unificationally
expressed by a fonula with three paraieters Cfr, o2^, n) and activation
energy Q. The teiperature dependence of fracture strength are expressed well
by Arrhenius's fonula. The strength shows the distribution of Weibull with
two paraieters. Consequentially if considering effective voluie V e ff and
effective hold tiie teff, either fracture strength or fracture life can be
probabilistically estiiated under the teiperature range above 100(fc up to
1300C.

KEYWORDS

unified estiiation lethod, Si3N4, Arrhenius's fonula, Weibull distribution

INTRODUCTION

The structural ceraiics such as silicon nitride and silicon carbide are
recognized as new structural laterials with high perfonance for their high
registance to heat, corrosion and wear, as well as their light weight. They
are expected to find the wide range of application in the field of various
■achine and apparatus industries. On the other hand, the strength of these
ceraiic laterials are distributed over very wide range, for these laterials
are brittle laterials containning a large nuiber of possible defects. For
application of ceraiics to the structural coiponents, the strength of these
■aterials has been investigated and evaluated by iany researchers. Lately,
advanced lethods for testing and evaluating ceraiic strength have been
developed(T.Tanaka et al.,1988a,b,1989). For purpose to apply to the
reliability design, the authers also proposed a unified estiiation lethod
based on fracture lechanics and the Weibull's statistical theory (N. Okabe et
al. ,1988,1989,1990).

In this paper, we investigated the teiperature dependence of sintered Si 3 N 4

703
704
under temperature range above 1000% up to 1300% on the basis of unified
estimation method. As for experiments, we carried out fast-fracture, cyclic
fatigue and static fatigue tests by means of 3-point bending at each
temperature. The test data obtained at each temperature were unificationally
evaluated by taking the effective volume and effective hold time into
consideratins. To analyze the temperature dependence of fracture strength,
the normalized fracture strength evaluated by the unified estimation
method at each temperature were expressed by a formula of the activation
process. And we studied on the possibility of the unified estimation method
covering temperature dependece of fracture strength.

EXPERIMENTAL PROCEDURES

The materials used in this study were sintered silicon nitride (S-Si3N4)
containing AI2O3 and Y2O3 as the sintering additive. The specimens of rec-
tangular bar type, the dimensions of which were 3*4*40mm were, made by
grinding. The surface roughness of the obtained specimens was not more than
0.8 micrometers. The fast fracture, cyclic fatigue and static fatigue tests
were conducted under 3-point bending with the span length of 30mm at 1000,
1100, 1200 and 1300% in air. The fast fracture tests were carried out at
cross head speed of 0.05, 0.1, 0.5 and lmm/min. A cyclic fatigue tests were
performed at a cyclic frequency of 10Hz and a stress ratio of 0.5. A static
fatigue tests was carried out with the bending load kept constant.

RESULTS AND DISCUSSION

Unified Estimasion Method

The data analysis based on the unified estimation method proposed by the
author et al. was described below. The effective volume, v e f f , and the
effective stress hold time, teff, are
V<rf=Jv(^/^«.x)"dV (1)

where tn is the time until fracture in the case of fast-fracture and is the
period time in the case of cyclic fatigue, all data(tff, t f ), (0^, t c ) , (tf*. Nj)
obtained by kinds of tests were converted into the normalized strength in
the case of Veff=lmm3 and N f t ef |=lsec by the following Eq. (3),

where n f is the inverse of crack growth rate index n. Next, assuming two
parameter Weibull distribution expressed as

Pf*1-exp{-(of,/ff0)m} <4>
the statistical analysis against Of were done by using Maximam likelihood
method ,and

£<, = {(i/w l !*' <I ty /fi

(5)
■ -k/2<in(tf fl /a 0 )H(7 fI /3<>)*-i}
where k is sample size. The calculation from Eq. (1) to Eq. (5) were repeated
until "m/io and n/nQ converge nearly to unity. Also two Weibull distribution
 705
paraieter, *■, 6^, and the constants of strength properties, n*, n, can be
estiiated so as to satisfy the fracture lechanisi at the same tiie. Finally
the unified estiiation equation can be given by the expression

af(N,t«„)n'=ffo V ln(1-Pf)-VV.„ (6)

where 'I and <?Q
^y are the
— estiiated.« values,of Vi ■ and ft*, respectively. This
Eq. (6) can
can be applied for detenining pre probabilistically the allowable
stress, o"
w Q, or guarantee life, N 0 , by point estiiation.
a'

Unified Evaluation of Fracture Strength under Very High Teiperature

Figure. 1 ( a ) - F i g . 1(d) show the d i a g r a i of delayed f r a c t u r e s t r e n g t h
p r o p e r t i e s e v a l u a t e d by the u n i f i e d e s t i i a t i o n l e t h o d , under t h e
teiperatures 1000, 1100, 1200 and 1300°C. Here, All fracture strength data
obtained by the 3-point bending t e s t were converted into the n o n a l i z e d
strength 6*f in the case of V e f f = l n 3 by the following Eq. (7).

#f=tf/V«, (7)
And the delayed fracture strength properties were shown by the relation
between o f and cuiulative effective hold tiie N f t e f f . The solid line in
these figures were estiiated by Eq. (6) froi the paraieters obtained by the
unified estiiation lethod. Fracture strength tends to deteriorate at each of
the teiperatures, which can be explained by Eq. (6). That is, even if under
very high teiperature, fast fracture, cyclic fatigue fracture and static
fatigue fracture can be unificationally estiiated as delayed fracture under
the relation between o f and N f t e f f . Figure. 2 shows distribution of
nonalized fracture strength <ff given by Eq. (3) at 1000t(a) and 1300t(b) for
exaiple by Weibull plot diagrai.

1000°C

V fast fracture
V cycl ic f a t i g u e
T static fatigue V e f f = 1mm 5
IIIU IIIU IIIU iiilii liiiJ i nliiii i i illJ I I
<o IBB
- 1 8 1 2 3 4 5
IB IB IB IB IB 18 IB IB
Effective hold t i m e teff

CL 1BBB
10 = 1200°C \ T0 = 1300°C
*ifl8 u3y
>.
^ ^▼ ^r * " ' T'
^ i

50

1 m m5 J
e ff = 1 m m
v =
ef f v

' "Ul - J - U tn —UU Ul — U l

I llllUI llllllll I II 18

18
_I_U Ul
u u uu

(c) Effective hold t i m e t0 (d) Effective hold t i m e teff

Fig.1 Data for various kinds of bending fracture strength
tests at lOOOt,1200t and 1300t, and unified
estiiation of these fracture strength properties
706
The solid line indicates results of the statistical analysis of the two
parameters Weibull distribution by using the Maxiiai likelihood lethod. The
results seem to agree well with distribution of the normalized fracture
strength. That is, the probability of failure can be approxiiated well by
the two parameters Weibull distribution. The unified estimation was based on
the assumption that all fracture is caused by crack growth froi an initial
defect. As shown Fig. 3(a), the lirror, list and hackle regions were observed
surrounding the fracture initiation site in rooi teiperature fracture tests.
On the other hand, aliost all of licrofractograph in high teiperature
fracture tests did not show lirror, list and hackle. Under very high
teiperature lore fractures seem to originate probably in the loosened grain
boundaries and produced voids rather than in an initial defects. The
application of the unified estiiation to such fracture lechanisi was exam-
ined in this paper. This exaiination has led to the conclusion that the very
high teiperature fracture strength can be unificationlly estimated as well
as the rooi teiperature fracture strength caused by crack growth froi an
initial defect.

Fig.2 Weibull distribution of standarduzed strength based

on unified estiiation under 100(fC(a) and 1300t(b)

(a) Room temperature i _j (b) High temperature L

Fig.3 Fracture surface near origin of crack growth

Teiperature dependence of fracture strength

The teiperature dependence of fracture strength was investigated under very

high teiperature. Fig.4 shows Arrhenius plots of norialized strength 5 %
obtained by Eq. (3), against testing teiperature TQ, indicating that the
strength is lowered considerably with an increase in teiperature. The
norialized strength o^ was approxiiated using the expression for the
activation process as follows.
 707

= igexpC- d/{k(Te+273)}] (8)

where, Q*:Activation energy, k :Boltziann constant,
TQ:testing teiperature, DQ:strength constant

The solid line in this figure shows the value calculated by Eq. (8). If
considering not only the effective voluie v e fx and effective hold tiie
N f t e f f but also the teiperature dependence of fracture strength, the
fracture strength, under very high teiperature above 1000C, can convert into
the norialized strength <?f* in the case of lOOCfc by the unified estiiation
■ethod as follows.

7 ? - crf(Nft.ff)nfexp[(dhO{ Te+273
1 1 }]
1273 (9)
Teiperature dependence of the crack growth rate index n, which was inverse
of nf, was evaluated by following Eq. (10).

n(T)=n 1 O oo + ^n(T e -1000) (10)

Fig. 5 shows the distribution of the norialized strength, converted by

Eq. (9), by weibull plot diagrai. The distribution was eqivalent to the two
paraieter Weibull distribution. Here, the analysis for unified estiiation
requires repeated calculation.

If considering effectve voluie Y e ^ and effective hold tiie te^t fracture

strength can be probabilistically estiiated under arbitrary teiperature T Q
above 1000t up to 1300t by following Eq. (11).

tffexpL ^k>\+m 1273 Ml Veff '

Then, fracture strength at each of the temperatures was estiiated using
paraieters obtained through unified estiiation on the basis of all testing
data under very high teiperature. The broken line in Fig. 1(a)-Fig.1 (d)
indicate the estiiated fracture strength value, which indicates strength
levels and the tendency of strength reduction in the teiperature range froi
1000*C to 1200t. At 13001C, however, the estiiated values seei to depart
considarably froi approximated ones. But they correspond well to all testing
data in a certain range of scatter.

1000
Q_

L """"""--I Q
I*
500
r\|
DO
i

C
<D
i

1
i

N
Veff = 1mm5
"(O teff=1sec
E
i i i i l
o 100
j

z: 800 1000 1500

Temperature Ta (°C)
Fig.4 Teiperature dependence of norialized strength bsed
on unified estiiation lethod
708
99.9 L
^99.0
I
~90.0
oT
£
1
:

a? 50.0

° 10.0 ■ /
V e f f= 1 mm5
t e f f = 1sec
1 L _J L_
' 200 500 1000 2000 3000
Normalized strength ^(MPa)
Fig.5 Weibull distribution of normalized strength based on
unified estimation method within temperature from
lOOOt up to 130dt

CONCLUSIONS

For purpose to clarify temperature dependence above 1000C of fracture

strength properties of silicon nitride ceramics, we carried out fast-
fracture, cyclic fatigue and static fatigue tests by means of 3-point
bending at 100(fC, llOrffc, 1200t and 130dt. On the basis of unified estimation
method, which we proposed for the evaluation of ceramic strength property,
we investigated temperature dependence of fracture strength of sintered
Si 3 N 4 under temperature range above lOOdt up to 130dt.

The results obtained are summarized as follows. The normalized fracture

strength, which were measured by three kinds of test, can be unificationally
expressed by a formula with three parameters tfT, 6n, n) and activation
energy Q. The value of n, the inverse of which is the index in formula:
da/dt=CKn of crack growth rate, increases with elevating temperature. Also
it is larger than twice compared with that below lOOOt. The temperature
dependence of fracture strength are expressed well by Arrhenius's formula.
The strength shows the distribution of Weibull with two-parameters.
Consequentially if considering effective volume V e f f and effective hold time
t e j|, either fracture strength or fracture life can be probabilistically
estimated under arbitrary temperatue T n above lOOCfC up to 130(fc.

REFERENCES

T.Tanaka,N.0kabe and A.Sakaida, (1988).Tensile Strength of S-Si 3 N 4 at Room

and High Temperature,Proc.31st Japan Congress Material Reserch,121-126
T.Tanaka,N.0kabe,A.Sakakida and H.Nakayarna,(1988). Relationship of Tensile
Fracture Strength and Inherent Defects, J.Soc.of Mater.Soc.,22,67-73
T.Tanaka.N.Okabe,A.Sakakida and H.Nakayarna, (1989). Fracture Toughness Test
of S-Si 3 N 4 at Room and High Temperature, J.Soc.of Mater.Soc., 3JL 261-267
N.0kabe,T.Yano,H.Hirata and M.Muramatsu, (1988). Impact Fracture Strength of
Ceramics under High Temperature, Proc. JSME,&Mz2., 217-222
N.0kabe,H.Hirata,M.Muramatsu and S.Hamada, (1989). Fracture Strength and
Unified Estimation Method fo Ceramics, J.Soc.of Mater. Soc. ,31,783-788
N.0kabe,H.Hirata and M.Muramatsu, (1990). Study on Application of Unified
Estimation for Ceramics Strength to Reliability-Design, J.Soc.of Mater.
Soc.,3&,393-399
WS4b5
PROBABILISTIC EVALUATION OF STRENGTH DAMAGE OF CERAMICS
DUE TO THERMAL SHOCK STRESS

T. SAKUMA? N. OKABE, U. IWATA.

• •• •
T. MIZUKAMI and H. TAKAKU

• Central Reserch Institute of Electric Power Industry,

11-1, Iwato Kita, 2-Chome, Komae-shi, Tokyo 201, Japan
•• Heavy Apparatus Engineering Laboratory, Toshiba Corporation,
1-9, Suehiro-cho, Tsurumi-ku, Yokohama 230, Japan
••* Tokyo Institute of Technology, 2-12-1,Ookayama.Meguro-ku,
Tokyo 153, Japan

ABSTRACT

To make a reliability design in ceramic application, the probabiistic

evaluation method of retained strength after the thermal shock is proposed,
applying the unified strength evaluation method. The probability of
the occurrence of cracks is predicted theoritically and compared with the
results of the thermal shock tests using sintered silicon carbide as
specimens and liquid sodium as a quenching medium.

KEYWORDS

Ceramics; Thermal Shock; Probabilistic Analysis; Sintered Sillicon Carbide;

Liquid Sodium;Unified strength evaluation method;

INTRODUCTION

Structural ceramics have superior qualities of heat and abrasion

resistances, and their practical applications are widely expected. Ceramic
fracture strength is subjected to loading conditions such as unloading or
loading stress rate and stress hold time. Different fracture strength is
also caused by the existing probability of initial flaws. Authors.
therefore, have proposed the unified strength evalutation method which has
obtained the ceramic characteristics (Okabe et al.,1989,1990) and have
proposed the thermal shock testing method by quenching in liquid (Sakuma et
al.,1990, Iwata et al,.1990). Authors, in this paper, propose the
probabiistic evaluation method of retained strength after the thermal shock
applying the unified strength evaluation method and estimate the

709
710
probability of the occurrence of cracks. The reduction of strength by the
thermal shock is due to the thermal stresses caused by rapid temperature
changes. The thermal stress theoretically analyzed regarding a cilindrical
body of infinite height(Jaeger,1945),finite height(Karlelar,1971). However,
these studies are not practical in the thermal shock. Furthermorer, studies
are very few regarding the cooling rate, i.e., the non-steady heat transfer
coefficient. Therefore, authors obtained the non-steady heat transfer
coefficients by experiments and thermal stresses are calculated by the
numerical analyses.

EVALUATION OF STRENGTH DAMAGE AFTER THERMAL SHOCK

Unified Strength Evaluation Method

Fracture strength of ceramics is subjected to a slow crack growth

rate from an initial flaw with the size of a expressed as eq.(l).

da ,
= CKmax" = C(0cr/^a> (1)
dt
Distribution of initial flaw with the size of ,a; , is assumed with the
Weibull modulus, m, as eq.(2).

F(ai)=exp{-(a- )-"'2> (2)

a0
From eq.(l) and eq.(2), the nonfracture probability,R, , with,a, ,as a
starting point of fracture can be expressed as eq.(3),
R; ={-b0 (a-,m,xnUtt ) n 'tn - 2 ' } (3)
where n is the crack growth rate index.
Suppose that the values of n is generally 20 - 100, applying the weakest
link theory , the fracture probability, Pf , of the ceramic component,
becomes as eq.(4),

(7m a x t « f r ' ' n V 6 f r > ' m

P, =l-exp{-( )•} (4)
(Jo

where cr0 is the strength constant, and Vt t t and te t t are , as expressed by

eq.(5), the effective volume to be determined by the load stress
distribution and the effective stress hold time to be determined by the
change of load stress with time respectively.

f a fto a
Verr= ( )"dv t.rr= ( )"dt (5)
J V a* a x • Jo (7m ax

Therefore, the fracture strength characteristics of ceramics are given by

eq.(6) from which it is observed that the value is subjected to Ve fr a n d
t e rr , a n d they a r e s c a t t e r e d a c c o r d i n g to t h e W e i b u l l d i s t r i b u t i o n .

err tef r > ' " V. r t > "" =(7o {In (1-Pr )-» }> '■ (6)
 711
Analysis of Strength Damage after Thermal Shock

Considering the maximum principal stresses of thermal stresses generated

by the thermal shock, the effective stress hold time te t t is obtained
according to eq.(5) based on the change in load stress with time cr«ax(t),
and the effective volume V e t r is obtained according to eq. (5) based on the
maximum principal stresses distribution cr»a x (r, 6,z) . Thus, the reduction of
strength due to damage, ACT, is given by eq.(7),

Aff=ff.axt,f f 1 / n V , f f ^ » (7)
where the effective volume Ve r r is obtained by eq. (8),

V,,, = f 2 (*—)-dV (8)

JV ' "» aiax
where a, is the principal stress, and tp=l for cr>0, and «p=0 for cr<0.
Therefore, the retained strength of ceramics after thermal shock CTR is
expressed as eq.(9).
n
(TRtef f l ' " V f tf r » ' » = C 7 o { l n ( l - P f ) - 1 } l ' ■ -am . x U t f ' ' vj f f»'" (9)
Furthermore, the probability of crack occurrence at the time of thermal
shock is when CTR =0 according to eq. (9). Therefore, the relation between
the thermal shock stress crmax and the fracture probability Pr at the time
of the thermal shock is obtained by eq.(10).

Pr=l-exp{-( )■ } (10)

EXPERIMENTS AND ANALYSES

Thermal Shock Test

To confirm the validity of above evaluation, the thermal shock test is

made. As the quenching medium, liquid sodium and as the specimen, sintered
silicon carbide were used. Mechanical characteristics of sintered silicon
carbide are shown in Table 1. The geometric figure of the specimen is a
cylindrical body with conical nose which does not bring ambient gas in as
propsed previously (Iwata et al.,1990) . Temperature of specimen was
measured by thermocouples which were installed in the dummy similar to the
specimen. A specimen was dropped fixed to the supporting holder. Fig.l
shows the correlation between the percentagewise crack occurrence ratio and
quenching temperature differences.

Table 1 Mechanical characteristics of SiC.

Density (g/cm3) 3.20

Bending strength(3-point) (MPa) 539
Yong's modulus (GPa) 391 (RT-773K)
Poisson's ratio c 0.17 RT-773K)
Thermal expansion coeff. (10-J/K) 3.67 (320-793K)
Fracture toughness (MPa-m1'*) 4.6
712
100 -1 1 P-V j
*e
o O D*5 mm / / ' O
W
— A D=7.5 mm
D D*10 mm /
/
f
' / i

<
« 50 / ' i
1 -\
& t
o
z
- / -\
w i A
o I
--DA—-A O—O' _
a
w ok> i i i
100 200 300
QUENCHING TEMP. DIFF.. AT ' C
Fig.l Percentagewise distributions of specimen cracked.

Welbull Distrbutlon

Fig. 2 shows Welbull plots of strengths measured In four point bending of

each specimen before quenching. The effective volume of the specimen Ve rr
was obtained by eq.(ll) and effective stress hold time t«ff was obtained by
the curve of the bending load with time, and fracture strength was
normalized in accordance with eq.(12) under conditions that V ef f=l mm3 and
t eff =l sec. Then, the Weibull plot of O mark in Fig.2 was obtained using
the mean rank method.

Vet f (1 + L2/Li m) r(m/2 + l/2) T(3/2)

(11)
V0 w(m+l)(m+2) r(m/2+l)

at =afUf,' / "V ef f' '" (12)

Solid line in Fig.2 is the strength distribution estimated upon obtained
Weibull modulus m and strength constant using the least square method.
Statistical strength parameters are shown in Table 2.

5 103
FRACTURE STRESS MPa
Fig.2 Weibull plots of strengths before quenting.
Table 2 Statistic strength properties parameters.

parameters
n Co
7.2 37.2 473 MPa
 713

Non-steady Thermal Stresses at the time of Thermal Shock

Non-steady thermal stresses have been obtained numerically by the finite

element method, applying the geometric figure of the specimen of the
thermal shock with supporting holder. Mesh division is 9 nodal points,
element number is 1363 and node number is 4490. The analysis has been made
only during falling through liquid sodium. The time when the tip of the
specimen reached liquid surface has been set at 0, and the analysis of non-
steady thermal conduction has been made during the time until the specimen
has stopped at a given position in liquid. The maximum thermal stresses
have been obtained in reration to the Bi number calculated using the non-
steady heat transfer coefficients obtained by experiments.

EVALUATION OF THE PROBABILITY OF CRACK OCCURRENCE

The probability of the crack occurrence at the time of the thermal shock is
obtained according to eq.(ll). Here, the maximum thermal stresses, the
effective volumes and the effective stress hold times are calculated in
relation to quenching temperature difference, AT, by the results of
numerical analyses. The percentagewise crack occurrence ratio shown in
Fig. 2 has been Weibull plotted in relation to AT. applying the mean rank
method. The result is shown in Fig.3. Solid lines in Fig.3 are the results
of the evaluation of the probability of crack occurrence against each
dimension of the specimen. From this result, it can be concluded that the
evaluation method of the crack occurrence probability, which is under
proposal in this paper, almost satisfies experimental results. Furthermore,
it is possible to evaluate the retained strength after the thermal shock
applying eq.(10).

99
* 90 O D = 5 mm
Q A D=7.5mm
r W
o u
D D=10 mm
oo
HO
M
M § 10
< M
CQ O
O CU

10 50 100 500
QUENCHING TEMP. D I F F . , AT 'C
Fig.3 P r o b a b i l i t y of c r a c k o c c u r r e n c e .
714

CONCLUSIONS

In evaluation of the thermal shock resistance, it is essential to

accurately estimate the thermal stresses. And, it is also necessary to make
the probabilistic evaluation of material strengths. From these points of
view, in this paper, based on the thermal shock experiments using the
specimen of sintered silicon carbide and making analyses of damages due to
the thermal shock applying the unified strength evaluation method, the
proposal has been made on the evaluation method of probability of the crack
occurrence at the time of the thermal shock.

ACKNOWLEDGEMENT

It is added here that this study has been entrusted by Japan Power
Engineering and Inspection Corporation (JAPEIC) upon requests by Agency of
Industrial Science and Technology, Ministry of International Trade and
Industry.

REFERENCES

Iwata.U..T.Sakuma and H.Takaku.(1990). Thermal Shock Resistance of

Ceramics: Critical Quenching Temperature Difference by Quenching in
Liquid Sodium. J. Soc. of Mech. Eng., 907-1, 9-10.
Iwata.U..T.Sakuma,H.Takaku and T.Mizukami.(1990). Thermal Shock Resistance
of Ceramics: Influence of Gas Brought In on Critical Quenching
Temperature Difference. Proc. of J. Soc. of Mater. Soc, 89-90.
Jaeger,J.C. (1945). On Thermal Stresses in Circular Cylinders. Phil. Mag.,
36, 418-428.
Karlekar, B.V. (1971). Nonstationary Quasi-Static Thermal Displacements and
Thermal Stresses in a Cylindrical Body of Finite Height Subject to
Convective Heat Losses. ASME,834-838.
Okabe,N.,H. Hirata, M. Muramatsu and S. Hamada.(1989). Fracture Strength
and Unified Estimation Method of Ceramics. J. Soc. of Mater. Soc., 37,
783-788.
Okabe,N.(1990). Unified Estimation for Ceramic Strength and Reliability
Design. Science of Machine. 42, 39-44.
Sakuma,T.,U.Iwata and H.Takaku.(1990). Thermal Shock Resistance of Ceramics
: A Novel Quench Test Technique. J. Soc. of Mech. Eng.. 907-1. 7-8.
Sakuma,T.,U.Iwata and H.Takaku.(1990). Thermal Shock Resistance of Ceramics
: Thermal Shock Testing based on A Novel Quench Technique.
J. Soc. of Mech. Eng.. 900-50. 365-370.
WS4b6

FRACTURE BEHAVIOR OF SiC FIBER/Si3N4 COMPOSITE

K. UENO, S. KOSE and M. KINOSHITA

Government Industrial Research Institute, Osaka

Midorigaoka 1-8-31, Ikeda, Osaka 563 Japan

Abstract

Silicon n i t r i d e m a t r i x CMC ( C e r a m i c Matrix C o m p o s i t e ) with 5 vol%

chemically vapor deposited SiC fiber has been fabricated by vacuum hot-
pressing at 1400 - 1500 °C. By using MgO and MgF2 mixture as a sintering
a d d i t i v e s , c o m p o s i t e s having 95 % r e l a t i v e d e n s i t y was s u c c e s s f u l l y
f a b r i c a t e d at 1500 ° C , r a t h e r lower t e m p e r a t u r e than t h a t for ordinal
sintering of silicon nitride. The composite showed not brittle and non-
linear fracture behavior with consuming extraordinary big fracture energy (
70000 - 80000 J / m 2 ). The composite had ultimate flexural strength of 590
MPa and fracture toughness of about 15 MPa/m. Much amount of fiber pull-out
was o b s e r v e d . The p u l l - o u t happened due to slipping of not only at
fiber/matrix interface but also at the interface between core carbon fiber
and SiC sheath.

Introduction

Ceramic matrix composite, CMC, with inorganic fiber is expected to realize

higher fracture toughness such like over 15 MPa/m, which we cannot expect for
monolithic ceramics. Therefore, the composite is studied very earnestly
today. As a reinforcing fiber, chemically vapor deposited SiC yarn with high
s t r e n g t h has high p o t e n t i a l b e c a u s e of i t s good r e s i s t i v i t y a g a i n s t high
temperatures during matrix fabrication.

This paper discussed the fabrication of CVD SiC fiber reinforced Si3N4 matrix
composite and its mechanical behavior. To obtain good mechanical properties,
it is necessary to minimize the fiber degradation. Therefore, reaction-
bonded silicon n i t r i d e is chosen as t h e m a t r i x b e c a u s e of i t s lower
715
716
p r o c e s s i n g t e m p e r a t u r e ( ~ 1 4 0 0 ° C ) . Corbin e t . al. f a b r i c a t e d SiC
monofilament/RBSN composite with up to ca. 5 0 - 6 0 vol% fiber ( Corbin et.al.
1985). The composite showed work-of-fracture of 94500 J/m 2 and maximum
flexural strength of 755 MPa. On the other hand, Shetty et. al. has been
fabricated unidirectional SiC monofilament-reinforced Si3N4 matrix CMC by
hot-pressing at 1750°C ( Shetty et.al. 1985). The composite with up to 44
vol% fiber showed average crack-growth-resistance, commonly referred to as
work-of-fracture of 8150 J/m 2 and fracture toughness of 7.2 MPa^m measured by
SENB method. Comparing these works, it is obvious that high processing
temperature degrades the toughness significantly.
It is well known, however, that reaction-bonded silicon nitride has a porous
microstructure. Therefore, when the RBSN matrix composite is placed at high
temperature with air during its operation, SiC monofilament and especially
its carbon coating if used will be attacked by oxidation even in the inner
part of composite body. In this paper, almost full dense body of silicon
nitride matrix was fabricated by hot-pressing, but the processing temperature
was lowered by using mixture of MgO and MgF2 as sintering aide in order to
clear of the fiber degradation problem. The e f f e c t of fabrication
conditions on the composite mechanical properties was studied, and its
mechanical behavior was evaluated on the basis of fracture surface
observations.

Experimental

Composite fabrication

The composite was fabricated by hot-pressing of a stack of SiC fiber sheet

and matrix silicon nitride sheet placed alternately, as shown in Fig. 1. The
SiC fibers used in this study were carbon-coated SCS-6 fibers obtained from
Textron Materials Division Lowell, Massachusetts. The unidirectionally
arranged SiC mat was prepared by putting the shortly cut fibers on a die
having shallow ( about 100 jim depth ) grooves with a distance of 500 jim.

As sintering additives, MgO, Y2O3, and AI2O3 are normally used. In this
study, it is necessary to sinter the silicon nitride matrix at lowest
temperature as possible. Oswald, Riley and Brook reported that the
sintering of silicon nitride was a c c e l e r a t e d by using a fluoride flux (
Oswald et.al. 1987). They used equimolar mixture of MgO and MgF2 and
obtained a full-dense silicon nitride by sintering at 1450°C. Silicon
nitride, labeled as SN-E-10 from UBE KOUSAN Co., was doped with 3.5 wt% MgO
( Iwatani Chemical Industry Co., MTK-30, purity: >99.9 %, average diameter:
0.25 urn) and 3.5 wt% MgF2 ( Morita Chemical Co., Guaranteed grade ) by ball-
milling. Silicon nitride mat was prepared by filtering the slurry with
organic binders such as polyvinylbutyral and a softening agent such as
dibutylphthalate.
 717

Si3N4<
SiC mat,

Fig. 1 Sheet stacking method for

fabrication of SiC fiber/silicon nitride
Fig. 2 Typical cross section of 5 vol%
composite.
SiC fiber/silicon nitride composite.
500 jam.

Hot-pressing was carried out under vacuum atmosphere. The sample having the
size of 10 mm x 50 mm x 5 mm and containing 6 mats of SiC fiber within the
thickness of 5 mm, was sintered at 1400°C to 1500°C for 15 min to 45 min
under 20 MPa with a BN-coated graphite die. The fiber volume was ca. 5 %.

Specimen Preparation

The composite was polished on its surface to remove out the surface layer.
For three-point bending tests, typical specimen dimensions were 10 mm x 50 mm
x 3.5 mm. The lower span was 20 mm, then L/h was 5.7. Bending tests were
carried out at a constant cross-head speed of 0.05 mm/min. Fracture
toughness was measured by SENB ( Single Edged Notched Beam ) method with a
specimen having typical dimension of 10 mm x 50 mm x 5.4 mm and containing 10
layer of SiC mat. Notch was introduced by a diamond wheel with 0.1 mm
thickness to the depth of 1.3 mm. Three specimens were measured for the
composite sintered at 1500 °C for 30 min.

RESULTS

Microstructure and density

Fig. 2 shows a typical cross section of the composite. SiC monofilaments

were placed with a constant fiber-to-fiber distance of about 500 pm. Fig. 3
shows a relationship between relative density and sintering conditions. The
relative density of the composite increased with increasing of sintering time
and temperature. When sintered at 1500 °C, relative density attained to 96
% within 30 min. By X-ray diffractometry, it was revealed that the matrix
was composed of 86 % alpha-type silicon nitride and 14 % beta-type silicon
nitride.
718
Mechanical Properties

Fig. 4 shows''a typical load-displacement curve for the composite in three-

point bending test. The curve composed of two distinct region, that is,
linear and non-linear region, as already reported by Bhatt(1986). Up to 200
~ 300 MPa, load increases proportionally with increasing of the displacement.
In almost specimens, there is slight increase in the slope, and after that,
immediately load downs by fracture. The second non-linear region begins
after this first matrix cracking, showing stepwise increasing of load with
multiple cracking of the matrix, up to ultimate fracture. Increase in the
slope before first matrix cracking in linear region, that is, the compliance
decrease, is considered that the load was applied mainly by SiC fiber which
has higher elastic modulus than that of the matrix silicon nitride.

Fig. 5 shows an effect of hot-pressing temperature on ultimate flexural

strength of the composites sintered for 30 min. The ultimate flexural
strength increased with increasing of the sintering temperature. Maximum
strength was 590 MPa for the composite sintered at 1500 °C for 30 min. Same
tendency was observed for an effect of hot-pressing temperature on first
matrix cracking stress as shown in Fig. 6. The bending strain for first
matrix cracking point, calculated by the cross-head displacement did not
changed as shown in Fig. 6. As described above, at first matrix cracking,
first SiC layer from tensile plane fractured with the matrix beneath the
fiber layer, therefore, the first matrix cracking strain is considered to be
dominated by the maximum stain to fracture of SiC fiber. This is coincidents
with the fact that the strain is constant in spite of the different sintering
temperature.

15 30 45
Hot-pressing time/min

Fig. 3 Relationship between hot-pressing Fig. 4 Typical load-deflection behavior

temperature and relative density. i n three-point bend test.
 719
As shown in Fig. 4, the c o m p o s i t e fractures not in b r i t t l e manner but
noncatastrophically, s o m e t i m e s called as "graceful fracture". During
sequential fiber layer and the matrix layer fracture, huge amount of energy
was consumed. Work-of-fracture was calculated by the load-displacement
curves and tabulated in Table 1. The average value, 78000 J/m 2 is slightly
smaller than the value, 94500 J/m 2 , reported by Corbin et. al., but far
greater than that of normal silicon nitride, 16~70 J/m 2 . It is notable that
their composite had the fiber volume fraction of 50 ~ 60 %, but our composite
is reinforced with only 5 volume % fiber. In Table 1, fracture toughness
was also shown. The average value was 15 MPa/m, which is rather higher than
the value for normal silicon nitride, 6—8 MPa/m. It is observed that
fracture from induced notch ran in the matrix silicon nitride but then was
stopped by SiC layer. That is, SiC layer works well as a so-called "crack
arrester".

Fig. 7 shows the fracture surfaces of the composite observed by SEM. On the
fracture surface, there happens many fiber pull-out. Remarkable point was
the matrix cracking. That is, it seems that there is no distinct main
crack , and the matrix silicon nitride was crashed to smaller fragments.
Such crashing of the matrix during bending means that a certain amount of SiC
fiber had carried the load even in the region behind crack front, and the
matrix surrounded by such fibers was subjected to very complicated stress
state including shearing component.

It was also observed that fiber pull-out happened in two ways, that is, one is
normal pull-out of SiC fiber from the matrix silicon nitride , and another is
pull-out of carbon core fiber from SiC fiber, leaving SiC sheath. It is
considered that these multiple fiber pull-out and the matrix crashing
contributed to observed huge energy for fracture.

| 400

«
2
600
<7> 3 0 0 \-
en
c
0/ 500 I 2001-

400 2
(A
CQ

IE

300
1400 1450 1500 1400 1450 1500
Hot-pressing Temp/'C Hot - pressing Temp / °C

Fig. 5 Effect 6f hot-pressing temperature Fig. 6 Effect of hot-pressing temperature

on ultimate flexural strength. on first matrix cracking stress and
bending strain.
720
Table 1. Some mechanical properties of SiC fiber/ Si3N4»

3-point flexural strength 590 MPa

First matrix cracking stress 200 ~ 300 MPa
Work-of-fracture 78000 J/m 2
Fracture toughness ( SENB ) 15 MPa/m

Fig. 7 Fracture surface of SiC fiber /

silicon nitride composite.

REFERENCES

N.D. Corbin, G.A. Rossetti, Jr. and S.D. Hartline (1985), Microstructure
/ Property Relationships for SiC Filament- Reinforced RBSN. Ceramic Eng.
Sci. Proc, (>, 958- 968.
D.K. Shetty, M.R. Pascucci, B.C. Mutsuddy and R.R. Wills (1985), SiC
Monofilament-Reinforced Si3N4 Matrix Composite. Ceramic Eng. Sci. Proc,
j>, 632- 645.
R.T. Bhatt(1986), Mechanical Properties of SiC Fiber-Reinforced Reaction-
Bonded Si3N4 Composite. In: Tailoring Multiphase and Composite Ceramics
(R.E. Tressler, G.L. Messing, C.G. Pantano, and R.E. Newnham Ed.), pp.
675-686.
J.R. Oswald, F.L. Riley and R.J. Brook(1987), Accelerated Densification
of Silicon Nitride Using a Fluoride Flux. Br. Ceram. Tran. J., 86, 81-
84.
WS5a1

Round-Robin Comparison of Data Evaluation Models for

Fatigue Properties of Metallic Materials

K. KANAZAWA. Y. MONMA and S. NISHIJIMA

National Research Institute for Metals,

2-3-12 Nakameguro. Meguro-ku Tokyo, 153 Japan.

ABSTRACT

An i n t e r l a b o r a t o r y c o m p a r i s o n of fatigue data e v a l u a t i o n m e t h o d s used in

m a t e r i a l s data systems was carried out. This paper presents the major find-
ings from the round-robin tests of the evaluation for h i g h - c y c l e fatigue S-N
data and f a t i g u e crack g r o w t h d a t a . The topics examined are the choice of
dependent-independent variable, the treatment of run-outs,the determination of
endurance limit, and weighting technique in computation of nonlinear model.

KEYWORDS

H i g h - c y c l e f a t i g u e ; S-N curve; f a t i g u e crack growth; m a t e r i a l s database;

statistical procedure; fatigue strength and life.

INTRODUCTION

The importance of data evaluation in the use with factual materials databases
has been pointed our in a VAMAS (Versailles Project on Advanced Materials and
Standards) report(edited by Krockel et al., 1987). The i n t e r p o l a t i o n and ex-
t r a p o l a t i o n of the accessed data are one of essential r e q u i r e m e n t s in the
materials data system. As a results the user often rely on the data evalua-
tion methods and models as implemented in the materials databases.

However, the levels of analytical or modeling methods for the evaluation of

materials property data differ considerably from almost standardized to still
e x p l o r a t o r y d e p e n d i n g on the materials classes, properties and the expertise
of the analyzer.

In view of determining potential problems and seeking the ways to solve them,
a r o u n d - r o b i n type c o m p a r i s o n was carried out on the bases on selected com-
monly used methods of data a n a l y s i s for m a t e r i a l s p r o p e r t i e s as one of ac-
tivities of VAMAS TWA (Technical Working Area) 10. Using the same data sets,
the participants were asked to submit the results of the c o m p u t e r i z e d data
a n a l y s e s carried out on their own system, to the National Research Institute

3
4
for Metals (NRIM) in Tokyo.

The present paper is intended to summarize the findings from comparison of the
numerical results submitted by the international experts. Only results for
fatigue properties are dealt in this paper as m a t e r i a l s p r o p e r t i e s . Creep
properties as well as fatigue properties were chosen for this round-robin test
at the same time, which results were described in VAMAS reports (Nishijima _e_i
_aJL.,1990; Monma et al., 1990)

MATERIALS PROPERTIES DATA DISTRIBUTED

Fatigue properties of engineering steels and alloys were chosen as the common
data for this round-robin test, for which well-established analytical methods
are available and widely used in many materials databases. The primary source
of information on the data used are the Fatigue Data Sheet series published by
NRIM (1978, 1980, 1981). The numerical values of data were sent to all par-
ticipants in machine readable format.

Table 1 lists the type of materials for which the data was distributed to the
participants. Except for the welded joint, the data sets include both "well-
behaved" and "ill-natured" ones with w h i c h a t y p i c a l user or m a t e r i a l s
databases would usually be faced. The well-behaved data sets represent typi-
cal behavior of materials properties and would easily be curve fitted to con-
ventional data evaluation models, while the evaluation of ill-natured data are
considered to be difficult due to the unusual behavior.

Table 2 summarizes the kind of materials properties and the possible combina-
tion of p r o p e r t i e s and materials. The choice of the combinations was left to
the participants.

Table 1. Materials for round-robin comparison of data

evaluation models.

Spcif:ication No. of data sets

1 2
Material type Data source
J IS* UNS* (Heat Id.)
S45C G10450 Carbon steel 2 (CB.CC) FDS/No. 3 U 9 7 8 ) * 3
SNCM439 G43400 Low alloy steel 2 (LA,LI) FDS/No. 2 5 Ü 9 8 1 ) * 3
Carbon steel, 49
SM50B K12000 3 (MB.WM.HAZ) FDS/No. 21(1980)
welded joint
*1: Japanese Industrial Standard, *2: Unified Numbering System by SAE/ASTM,
*3: National Research Institute for Metals (1978, 1981, 1980)

Table 2. Materials properties and possible combination of

comparison of data evaluation models.

Materials
Properties Numerical values
S45C SNCM439 SM50B

High-cycle fatigue
Stress amplitude(S),
Cycles to failure(N)
o O
Stress intensity factor(AK),
Fatigue crack growth
Growth rate(da/dn) o
 5
REPORTING

Each participant was asked to use the most representative m e t h o d s that could
be found in the application modules in their materials databases and to submit
the results of data evaluation, if possible, entirely in machine readable form
on a floppy disk as well as the printouts.

A typical report contained the following items:

1) Data set, indicating the property and the material
2) Data evaluation models and methods
3) Materials constant(s) and the regression coefficients computed
4) Standard error of estimate and coefficient of determination indicating the
dependent variable.

The initial call for the round-robin work was sent through the contact persons
of VAMAS TWA 10. In response to the call for the r o u n d - r o b i n in May 1988,
about 20 people expressed their interest to join the cooperative work. The
data package on a floppy disk was sent out in July 1988. The reports on the
data analysis were collected by the end of March 1989.

METHODS/MODELS USED

There are a variety of analytical models for data evaluation that can be used
in computerized materials data system. In almost every case, the numerical
values of materials data are statistically fitted to the model equation by use
of least squares regression procedures. The effectiveness of computed curves
can be judged from engineering point of view.

Tables 3 and 4 summarizes various methods for evaluating the materials data
reported in this interlaboratory comparison. The number and complexity of the
methods vary according to the kind of property data. Although the parameters

Table 3. Summary of data evaluation models used for

high-cycle fatigue data.

S: Stress amplitude in MPa, N: Number of cycles to failure,

NE and S E : Number of cycles and stress amplitude at the point of inflection

Model Regression Model

Model Type Remarks
Code Equation X Y
Cl Semi-log s log(N)
C3 Linear log(N) Run-outs excluded
C2 Log-log log(S) log(N)
Y=aX+iS
C4 Linear log(N) log(S)
Log-log linear •1
C5 & asymptotic
log(N) log(S-b)

C6 log(N) log(S) Maximum likelihood* 2

Y=aX+yS
C7 log(S) log(N) Staircase method
Log-log (X <log(N E ))
Simultaneous
bilinear Y=Yo
C8 /v\ i /xi w log(N) log(S)
regression and x o
(X> lOg(NE)) nu·* i · *3
Probit analysis
*1: Soya et al.. 1986, *2: Spindel et al.. 1979, *3: Nishijima et a h , 1985
6
in the mode equation are usually determined by a statistical procedure, the
results of the evaluation are greatly affected by the choice of the dependent-
independent variables.

It is noted that iterative computation is often only way to get best fit
parameters to the model equation, as they are nonlinear and cannot be treated
by the conventional analytical procedures. Another aspect of data analysis is
the treatment of "run-outs", or the data points from discontinued test. Since
most of the materials data examined in the round-robin test are failure lives
by the materials testing, they inevitably contain such data points.

COMPARISON OF RESULTS

As shown above we have collected the results generated by a variety of data

evaluation methods. First we will inspect general aspects of the evaluated
results by typical methods and models, looking at some key values from the
regression curves. Then comparisons will be made for the computed values from
two standpoints: life and strength.

High-Cycle Fatigue Data

Five reports from 2 countries were submitted for the high-cycle data. Ex-
amples of the result for high-cycle fatigue data analysis is shown in Fig. 1.
Note that the right arrows indicate the run-out test data. It is important to
note how to treat the run-outs in the course of fatigue data evaluation. Be-
cause the conventional regression procedures do not pay proper attention to
them. The methods used are classified roughly into three groups:

1) exclusion of the run-outs

2) inclusion of the run-outs as failed
3) inclusion of the run-outs with a statistical procedure such as the Probit
method

Another interesting aspect of the fatigue data analysis is the variety of

choice for objective (dependent) variables to be expressed by a function of
explanatory (independent) variables. In engineering applications, it is in
fact a common practice to assume the fatigue strength as the criterion to be
explained with a function of the fatigue life. It is also noted that the
results of evaluation depend on such factors as the model itself, the

Table 4. Summary of data evaluation models for fatigue

crack growth data.
Model equation: Y = a X + ^ , da/dn: Crack growth rate in m/cycle,
Δ Κ : Renge of stress intensitu factor in MPav^m

Model Variabl e
Model Type Remarks
Code X Y
Dl Log-log linear log(da/dn) log(AK) Low da/dn data excluded
D2 Log-log bilinear log(AK) log(da/dn) Two segements
D3 Log-log linear *1
log(da/dn+A) log(AK)
D4 & asymptotic Weighting of data points
*1: Soya etal., 1986, *2: Ohta etal.. 1986
 7

VAMAS Round-Robin, Fatigue S-N, Heat CB of S45C

1 1 1 1 1 1 1
550
1 1 1— 1

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o CB

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n = 19
350 J 1 1 1
10 10 10 10 10
Number of Cycles to Failure

(a) S-N c u r v e s f o r w e l l - b e h a v e d d a t a s e t

VAMAS Round-Robin, Fatigue S-N, Heat CC of S45C

Π5ξ
550
1 1— — C3-P14 o CC
— C4-P05
— C4-P14
Γ500 — C5-P14
— C6-P13
— C7-P01
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O N C | > ^ ^ — C8-P04
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10 10 10 10 10°
Number of Cycles to Failure
(b) S-N c u r v e s f o r i l l - n a t u r e d d a t a s e t

Fig. 1. Comparison of fatigue S-N curves for data sets

of carbon steel.

choice of variable including the t r a n s f o r m a t i o n (log-log or s e m i - l o g ) , the

treatment of run-out data.

T h e r e are two a s p e c t s in the c o m p a r i s o n of the materials reliability data.

One is to compare the evaluated strength for specified lives for v a r i o u s a p -
plications. T h e p r e d i c t e d strength v a l u e s can be used for e s t a b l i s h i n g
materials performance data such as the maximum allowable s t r e s s e s in d e s i g n -
ing. T h e other is to d e t e r m i n e the life for specified test conditions for
comparison as in the ordinary materials testing. A typical situation is that
the former is important for structural design, the latter is indispensable for
the materials life prediction.
8
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CB CC ._., CB CC
490 - 500
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1 410 420 O
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10 5 6
10 10 7 400'
w
105 106 107
480 430 415 520 450430
Stress amplitude (MPa) No. of cycles to failure
(a) P r e d i c t e d f a t i g u e lives (b) P r e d i c t e d f a t i g u e strength

Fig. 2. C o m p a r i s o n of p r e d i c t e d f a t i g u e lives and f a t i g u e

s t r e n g t h for specified test c o n d i t i o n s for data
sets for carbon steel.

Fig. 2 c o m p a r e s the p r e d i c t e d l i v e s a n d p r e d i c t e d f a t i g u e s t r e n g t h b y d i f -
ferent e v a l u a t i o n m o d e l s in h i g h - c y c l e f a t i g u e for s p e c i f i e d test c o n d i t i o n s .
A p p a r e n t l y t h e scatter is m o r e p r o n o u n c e d in longer life region w h e r e t h e p r e -
d i c t i o n is p r a c t i c a l l y m o r e i m p o r t a n t . In p a r t i c u l a r , t h e e s t i m a t e o f
f a t i g u e life near t h e f a t i g u e limit is s t r o n g l y d e p e n d e n t o n t h e e v a l u a t i o n
m e t h o d s . It should b e noted that the treatment of run-out data p o i n t s a f f e c t s
very much t h e e s t i m a t e d r e s u l t s . T h e r a n g e o f v a r i a t i o n ( m a x / m i n ) is t y p i -
cally 20 for t h e e s t i m a t e d lives by v a r i o u s m e t h o d s . If we c o m p a r e the same
r e s u l t s in terms of the strength, however, the scatter seems r e l a t i v e l y small,
and t h e range of v a r i a t i o n s typically less than a few percent.

In d e s i g n i n g the m a c h i n e s t r u c t u r e by r e f e r e n c e of the f a t i g u e endurance, o b -

viously the analyses including t h e e n d u r a n c e limit would superior. On the
o t h e r h a n d , it is n e c e s s a r y to e x t r a p o l a t e the r e s u l t s of failed d a t a p o i n t s
only, when the M i n e r ' s rule is applied to e s t i m a t e the f a t i g u e life under r a n -
dom loading. This treatment o f data y i e l d s rather c o n s e r v a t i v e e s t i m a t i o n o f
the f a t i g u e life.

The m o d e l s with h o r i z o n t a l part h a s c e r t a i n a d v a n t a g e b e c a u s e it c a n i n c o r -

p o r a t e r u n - o u t s properly. T h e r e a r e several v a r i a t i o n s to d e t e r m i n e t h e k n e e
point ( e n d u r a n c e l i m i t ) . It is known that s o m e t i m e s the s t a i r c a s e m e t h o d d o e s
not u s e a n y d a t a p o i n t s a v a i l a b l e f o r the a n a l y s i s . The relative merits of
these m e t h o d s a r e not clear. F u r t h e r d i s c u s s i o n s by e x p e r t s a r e n e c e s s a r y in
o r d e r to c l a r i f y t h e v a l i d p r o c e d u r e f o r t h e d e t e r m i n a t i o n o f t h e f a t i g u e
limit.

F a t i g u e Crack G r o w t h Data

T h e r e a r e 4 r e p o r t s from 2 c o u n t r i e s . T h e m e t h o d s c a n b e c l a s s i f i e d into t w o
g r o u p s : o n e e x c l u d i n g lower da/dn data points near the threshold and the o t h e r
including them. It is o b v i o u s that the former m e t h o d cannot give t h e
 9

VAMAS Round-Robin, Fatigue Crack Growth, SM50B Base Metal

10 o BM
^ Λ
BM
^10 1 n = 100 H
o
>> -
4>1U
e — H
210
on — H
%m
o
l·- -]
vio H
— 01-P14
o — D2-P15
«?
t_ " Mn — D3-P14 1
«1Ü r- D4-P15
D4-P04 !
10
10 15 20 30 50 70 100
Range of Stress Intensity Factor (MPa/m)
Fig. 3. Comparison of curve fitting on fatigue crack growth
data of base metal of carbon steel.

threshold value. Fig. 3 shows comparison of e v a l u a t i o n m o d e l s for f a t i g u e

crack growth data for base metal. It should be noted that the difference of
r e s u l t s by d i f f e r e n t data e v a l u a t i o n m o d e l s is rather small in this case.
This is p r o b a b l y d u e to the fact that the data provided were considerably
thick and fairly well-balanced.

The general trend of difference in p r e d i c t e d v a l u e s by d i f f e r e n t e v a l u a t i o n

models is very similar to that S-N analyses shown in Fig. 2. More differences
are recognized in predicted growth rate (da/dn) than in p r e d i c t e d stress in-
tensity factor ( Δ K ) .

G e n e r a l l y the data point near the threshold levels (low Δ Κ region) are less
than those in higher da/dn region. T h e r e f o r e , w e i g h t i n g of low da/dn data
points is very significant technique in the case when the data has a threshold
point and/or the sample size is small.

CONCLUSIONS

It was confirmed that some data evaluation models and methods are well estab-
lished, w h i l e o t h e r s are p r e m a t u r e . Fairly common and agreed m o d e l s and
m e t h o d s of data e v a l u a t i o n are a v a i l a b l e for s p e c i f i c a r e a of m a t e r i a l s
p r o p e r t i e s , but the r e s u l t s of e v a l u a t i o n cannot be unique due to the dif-
ference in the implementation of the method in practice. In addition to the
r e l i a b i l i t y and a c c u r a c y of the raw data, the c h o i c e of proper m o d e l s and
m e t h o d s of data e v a l u a t i o n would govern the very e x i s t e n c e of a f a c t u a l
material database. T h e k n o w l e d g e and e x p e r i e n c e of valid data e v a l u a t i o n
methods could be shared, if we build an inventory of data e v a l u a t i o n m e t h o d s
and models commonly used in computerized materials data systems.

Specified conclusions for each properties are as follows:

High-cycle fatigue S-N properties;

1) The treatment of run-out data points affects very much on the results of
data evaluation for fatigue S-N curve.
10
2) When the data show ill-natured behavior, more pronounced difference in data
evaluation appears in the results by various methods.
3) The difference in estimated values is very large in life, but rather small
in strength.
4) The choice of independent-dependent variable also affects the results of
data evaluation.
5) For the data analysis of fatigue data with run-outs, a common understanding
for the need of highly mathematical procedure such as the maximum likelihood
method has been obtained.
6) No agreement how to determine the fatigue endurance limits from the data
with run-outs has been reached. Further discussions by specialist should be
followed.

Fatigue crack growth properties;

1) The raw data provided were fairly well-balanced, and the resulting curves
by various evaluation methods were almost identical.
2) A model for fatigue crack growth rate needs to incorporate the nonlinear
calculation with proper weighting of data points in lowei growth rate
region.
3) The computing times are dependent to the initial value of parameters to be
determined, when the computation is made by for the nonlinear models.

REFERENCES

Krockel. H., K.Reynard and J.Rumble (1987). Factual Materials Databanks — The
Need for Standards — . VAMAS TWA 10 Report.
Monma.Y., K.Kanazawa and S.Nishijima (1990). Computational Models for Creep
and Fatigue Data Analysis. VAMAS TWA 10 Report.
National Research Institute for Metals, Japan (1978). NRIM Fatigue Data Sheet,
No.3, Data Sheets on Fatigue Properties of S45C (0. 45C) Steel for Machine
Structural Use.
National Research Institute for Metals, Japan (1980). NRIM Fatigue Data Sheet,
No.21, Data Sheets on Fatigue Crack Propagation Properties for Butt Welded
Joints of SM50B Rolled Steel for Welded Structure — Effect of Welding
Procedure — .
National Research Institute for Metals, Japan (1981). NRIM Fatigue Data Sheet,
No. 25, Data Sheets on Fatigue Properties of SNCM439 (0.39C-1.8Ni-0.8Cr-
0.2Mo) Steel for Machine Structural Use.
Nishijima, S. and A. Ishii (1985). Parametric Representation and Analyses of
S-N Data by Bi-Linear Curve Fitting. J. Soc. Mat. Sei. Japan, 34, 340-346.
Nishijima, S. , Y. Monma and K.Kanazawa (1990). Significance of Data Evaluation
Models in Material Databases. VAMAS TWA 10 Report.
Ohta, S., I. Soya, S.Nishijima and M.Kosuge (1986). Statistical Evaluation of
Fatigue Crack Propagation Properties Including Threshold Stress Intensity
Factor. Eng. Fracture Mech, U, 789-802.
Soya, I., H. Yokota, Y. Tanaka and H. Ouchi (1986). Development of Fatigue
Property Data Base System. Seitetsu Kenkyu, No. 322, 52-62.
Spindel,J.E. and E.Haibach (1979). Some Consideration in the Statistical
Determination of the Shape of S-N-Curve. In: ASTM STP 744, Statistical
Analysis of Fatigue Data ( Little and Ekvall, ed.), pp.30-31. ASTM,
Philadelphia.
WS5a2
ON THE CONSTRUCTION AND THE ANALYSES
OF THE NEW METALLIC MATERIALS DATABASE

Τ. ΤΑΝΑΚΑ*, Μ. JONO**, Η. ΝΑΚΑΥΑΜΑ***,

Η. MAKIURA**** and Υ. ΜΙΥΑΙ*****

* Faculty of Science and Engng., Ritsumeikan University,

Kita-ku, Kyoto, 603, JAPAN.
** Faculty of Engineering, Osaka University, Suita, Osaka,
565,Japan.
*** Faculty of Junior College of automobile Industry, Osaka
Sangyo University, Nakagaito, Daito, Osaka, 574, Japan.
**** New Material Center, The Foundation of Osaka Science
and Technology Center, Utsubo-honmachi, Nishi-ku,
Osaka, 550, Japan.
***** Faculty of Engng., Osaka Sangyo University, Nakagaito,
Daito, Osaka, 574, Japan.

ABSTRACT

The construction of material databases is now becoming a worldwide trend, and

various attempts are being made toward this goal. The New Material Center of
Osaka Science and Technology Center(NMC) is now constructing the New Metallic
Materials Database. The present paper describes the aim, the present state of this
database construction and some examples of analyses of this database.

KEYWORDS

Database; new metallic materials; heat resisting alloy; powder metallurgy alloy;
shape memory alloy.

INTRODUCTION

Main role of the database for traditional materials is to contribute toward the
establishment of reliability design standard. For example, JSMS Database of
Fatigue Strength of Metallic Materials was published at 1982 from such a point of
view, and many efforts have been paid to the analysis of this database (Tanaka,
1990). The database for new metallic materials has one more important role; to
offer the information to optimize the processing technique for new materials under
research and development (R&D). At present, many sorts of new materials with
peculiar function are developed vigorously, but the knowledge on their long-term
durability and reliability are scarcely systematized yet. If there exists any large scale
database for new materials under R&D, the developer may pick up fruitful
information from this database.

In order to overcome such a situation of new material development, NMC began to

construct New Metallic Materials Database at 1986. Among many sorts of new
metallic materials, three sorts of materials; heat resisting alloy, powder metallurgy
(P/M) alloy and shape memory alloy, are selected as targets by considering their
wide spreading in engineering markets.
11
12

Material 1 Material 2 Material 3

f
:ι TB. I
Series 0001
^ ■———■ Ι ι — - τ κ ^
Fabrication
ation Λ f Fabrication^ \
Series 0002 process
ss 1 J I process 2J Series
v 0004

Λ^ττ 5f Heat-treatment
S L 2)
f Heat-treatment "Π Λ . ΑΑΛΛ /
> τη-, ' Series 0003 7

J W ■ , -=5l 1
Characteristics 1 | [Characteristics 2] | Characteristics 11 [characteristicsTI [Characteristics 3

Fig. 1. Concept of experimental series.

CONSTRUCTION OF THE DATABASE

Logic to construct the present database is as follows; technical papers on new
metallic materials are picked up from reference lists offered by on-line service from
JICST (Japan Information Center of Science and Technology), then data are written
on the database sheets in the form of numeral and letter by hands of task force of
the NMC committee, and finally these data on the database sheets are coding-
treated to input the memory of computer as database files together with a
fundamental software to analyze the database. This database system at this stage
can be treated with a personal computer with a memory size of about 20 Mbites.

Database sheets have to possess logical story to avoid confusion, and to facilitate
computer aided analysis of the database. In our database construction, therefore, a
concept of experimental series is used as a tool to link the multi-layer database files
reasonably and logically as illustrated in Fig. 1. This figure indicated that data in
one series consist of the fundamental data concerning to material conditions
(material, fabrication process and heat-treatment.) and the characteristic data
indispensable to respective new materials. A part of entry items for the database is
listed in Table 1. Characteristics data items are selected as representative ones for
respective materials, and Fig. 2 shows an example of printed list of the database for
the case of P/M alloys.

As mentioned above, together with these numerous fact data, this database system
has some tools to analyze material properties, which enable us to evaluate the
physical and/or mechanical properties of three sorts of new metallic materials by
opening the window of analyzing tools and by answering questions displayed on
CRT. Some of these results will be introduced in the following chapter.

ANALYSIS OF THE DATABASE

Heet Resisting AllQy

By searching the sub-domain of this database where the data of heat resisting
alloys are stored, at first, we can obtain the information on material sorts and the
experimental series as shown in Table 2. Table 2 indicates that, at present, data of
744 series for heat resisting alloys are compiled in this database, and furthermore,
 13
Table 1. Example of entry items compiled in the database.
Heat resisting Powder metallurgy Shape memory
alloy alloy alloy
Record Record Record
Record name Record name Record name
key key key i
co AU Author(s) AU Author(s) AU Author(s)
OB TL Title TL Title TL Title
~° JN Journal JN Journal JN Journal
iS VN Vol. & No. VN Vol. & No. VN Vol. & No.
S SE Series SE Series SE Series
E EM Raw material (1) M1 Powder RM Raw material
■§ RC Raw material (2) M2 Powder size distribution (1) A1 Chemical (atm%)
E1
i (2)
Chemical (atm%) M3 W1 composition (wt%)
£ E2 composition (wt%) RM Raw material MM Melting method
HT Heat-treatment & grain size E1 Chemical (1) PM Powdering method
E2 composition (2) WK Working method
Physical properties MX Powder Mixing HT Heat-treatment & grain size
S OT
ST
«
■o TS
Specimen (strength)
Fracture strength
MP
PC
Sintering process
Packing conditions B1 Physical properties (1)
£ HD Hardness SC Sintering conditions B2 Physical properties (2)
w iM Impact value HT Heat-treatment B3 Physical properties (3)
'S FS Specimen (toughness) after sintering MS Specimen (Transformation
tS FT Fracture toughness VD Density temperature)
2 CS Specimen (creep) FD hardness T1 Transformation temperature
j? CD Creep test results B1 Physical properties (1) ST Specimen (strength)
ü HS Specimen (fatigue) B2 Physical properties (2) TS Fracture strength
HM Fatigue test results PT Specimen (Superplasiticity) HD Hardness

(To be continued)

000010 P990 0001 0010 AU S.0KI

000020 P990 0001 0015 TL FRACTURE BEHAVIOR OF SINTERED CARBON STEELS
000030 P990 0001 0020 JN J.JAPAN SOC. POWDER AND POWDER METALLURGY
000040 P990 0001 0025 VN 30 8 316- 3201983
000050 P990 0001 0030 KW ATOMIZED IRON POWDER,GRAPHITE POWDER,
000060 P990 0001 0040 SE 00020003
000070 P990 0001 0050 RM FE FE-C
000100 P990 0001 0055 LI 1 FE
000110 P990 0001 0057 L2 2 C
000280 P990 0001 0058 Zl C-ELEMENT IS NATURAL GRAPHITE POWDER OF PURITY OF 99.5% AND WH
000290 P990 0001 0059 Z2 OSE MEAN PARTICLE SIZE IS 6.0 MICRO-METER
000130 P990 0001 0065 Nl 105 VM
000190 P990 0001 0070 El 1WFEBAL C 0006 P 0008 S 0013 MN 020
000200 P990 0001 0072 E2 2W CBAL

Fig. 2. Example of printed list (P/M alloys).

gives the substantial information such that Ni-base superalloys are most vigorously
researched and developed among many heat resisting alloys.

Then, by selecting appropriate data items from information lists displayed on CRT,
we can obtain physical and/or mechanical information easily and quickly. One
example is shown in Fig. 3, which is a hard copy of CRT image. Furthermore,
according to individual investigator's demand, they can analyze the database by
making a compact data file from the large scale database as introduced in the
following section.
14
Table 2. Number of series in the database for heat resisting alloys.

Materials classification No. of

series -.,..., Onntont? o f M« -base superalloy
ALLY454 1 MAR-M series 30
Low alloy heat resisting steel 39
ASTROLOY 5 MERL76 1
Ferritic Stainless steel 4 FSX414 6 MXON 1
Austenitic Stainless steel 29 HASTELLOY 95 NC14K8 12
Fe - Ni-base superalloy 35 HAYN ES series 2 NiCr80-20 1
Co-base superalloy 10 IN-100 10 NIMONIC series,33
Dispersion hardening alloy 11 IN-600 series 35 RENE series 15
1 IN-700 series 88 TMS series 5
Unidirectinally solidificated alloy
IN-939 18 UDIMET700 15
Ni-base superalloy 594 IN-X750 9 19-9D 1
Single crystal alloy 17 IN-MA series 22 Others 189
Others 4 Total 594
Total 744
Creep rupture curve
Stress(MPa)
350 η
Mater i al: Number of Series
300 H SUS316H Austenitic ST [ 5]
Series number
250 H Alloy800 Temperature T2900010
( 923) ±25K T2900015
200-j T9800220
T9920001
150 T9920005
SUS304K .:
100·
5 0 - i iinun i iinun ι ilium ι iiiimi ι iiiimi
1.0 10 100 1000 10000100000
Time(ks)
Material:SUS304 Scrol1 down
Series No.:T2900010 1
Creep data: [Number of data 5] Scrol1 up
Temeprature(k) Stress(MPa) Rupture time(ks) Elongation(^) T
923 176 6.800E+01
923 166 1.450E+02
There are more data. To see it Hit CR. KEY IN

Fig. 3. Creep rupture curves for austenitic stainless steels.

Powder Metallurgy Allov

As an example of the database analysis, static strength distributions are shown in

Fig. 4 for nine sorts of Fe-base P/M alloys together with the statistical table, and
static strength taken on the abscissa means tensile fracture strength excepting the
case of Fe-B-Mo P/M alloy. This figure gives the information as follows: (1) Addition
of P which spheres the pores distributed in P/M alloys increases the strength. (2)
Addition of other elements such as C, Ni, and Cu increases both the mean and the
scatter of the strength. And (3) Fe-Si-Ni-C P/M alloy shows the excellent static
properties. Through such an analysis on statistical properties and by looking into
the material conditions for the data points distributed at low strength range, we may
get valuable knowledge on the optimization of processing technique.

As another example of database analysis, fatigue strength distribution in rotating

bending fatigue are shown in Fig.5, where the applied stress is normalized by the
 15

Fig. 4. Static strength distribution of Fe-base P/M alloys.

Fig. 5. Fatigue strength distribution of Fe-base P/M alloys.

monotonic tensile strength. At first, when compared with the fatigue strength
distribution of ingot metallurgy (l/M) alloys, it is recognized that the σ 3 /σβ-Ν
relationship much differs depending on additive elements. Then, the background
data stored as fundamental data indicate that classification of S-N curves of Fe P/M
alloy, plotted by open circles, into two groups is due to the difference in the density.
16
60
(0
z • Ti-Ni alloys
50 O Ti alloys
Δ Cu-Zn-AI alloys
40 ■ Cu-Zn-Ni alloys
□ Cu alloys

nφ 30 L
E
3
20 [A

10

ιι,Ι,Ι I I I II I I H
100 200 300 400
Transformation temperature T M (K)
Fig. 6. Distribution of transformation temperature
of shape memory alloys.

Shape Memory Aliov

Figure 6 shows a distribution of transformation temperature, T M , for five sorts of

shape memory alloys. This gives a information on a overview of shape memory
alloys under R&D, and indicates that R&D of shape memory alloys are focused
mainly on two types of alloys; Ti-Ni and Cu-Zn-AI alloys, and the transformation
temperature for Ti-Ni alloy is concentrated near the room temperature. One of the
major characteristics of shape memory alloy is the transformation temperature TM-
Therefore, the database of shape memory alloys must include the information on
factors which affect the TM comprehensively. All of the indispensable factors can be
recorded in our database sheet. And, we can investigate easily on CRT which is a
predominant factor to control the TM by searching appropriate data items and taking
a correlation with the TM as introduced in the section of heat resisting alloy.

CONCLUDING REMARKS

In order to optimize the processing technique, and furthermore to establish the

appropriate characteristic evaluation method, the database may play a role as a key
tool. However, as a common problem for new materials, there are insufficient
published data on their long-term durability, which are indispensable to establish a
valid design standard. Especially from such a point of view, many efforts must be
paid to accomplish a high performance database.

REFERENCES

Tanaka T. (1990). Fatigue strength database of metallic materials and its statistical
analysis. Proceedings of FATIGUE 90. Vol. I. 3-12.
WS5a3

DEVELOPMENT OF PERSONAL-COMPUTER DATABASE

SYSTEM OF FATIGUE STRENGTH

JI-HO SONG, YOUN-YOUNG EARMME, JUN-HYUB PARK,

DONG-HO YOUN, BONG-HAK YOON and JONG-MIN HA

Department of Mechanical Engineering, Korea Advanced Institute of

Science and Technology, P.O. BOX 150, Cheongryang, Seoul, 130-
650, Korea

ABSTRACT

A relational fatigue strength database system was developed on personal computer. The
relational database management system FoxPro Ver 1.0 was used, which is compatible with,
and runs much faster than dBASE IV. The database system developed contains 545 S-N and
311 ε-Ν curves. In addition, 280 fracture toughness data which are valid K K data according to
ASTM standard are contained. Several application programs were also developed. Using the
fatigue strength database system, approximation methods of ε-Ν and S-N curves from material
mechanical properties data were discussed.

KEYWORDS

Relational database system; fatigue strength; ε-Ν data; S-N data; K c data; approximation of ε-
N curve; Manson's universal slope method; Mitchell's method.

INTRODUCTION

The importance of collection and utilization of fatigue test data has been well recognized and
several useful data books of material fatigue strength have been published(e.g., JSME,
1961(1982), 1965, 1974, 1983). In the recent, the development and implementation of fatigue
strength database systems in a computer-based environment is a matter of concern.

In this work, a relational fatigue strength database system for personal computer was
developed, utilizing two kinds of databooks published in Japan(JSMS, 1982; JSME, 1983).
Using the database system developed, methods of ε-Ν and S-N curves from material
mechanical properties data were discussed.
17
18

RELATIONAL FATIGUE STRENGTH DATABASE

Since the relational database model has several advantages in designing, using and querying,
this model was chosen in the database design. Fatigue strength database was developed using
the relational database mangement system FoxPro Ver 1.0 which is compatible with, and runs
much faster than dBASE IV.

Details of Datahase

Datacode A datacode was used to denote main character of the data. The datacode with serial
number becomes primary key representing a set of fatigue strength data.

Relation Scheme Fatigue strength database is composed of 16 components or entities as can be

seen in the E-R(entity-relationship) diagram shown in Fig. 1.

Programs Five kinds of application programs, namely, appending, deleting, updating, system
application and analyzing programs, were developed. By using the system application program,
graphical data can be read directly through a digitizer.

1 N

Fig. 1 E-R (entity-relationship) diagram

 19

Data Sources

High-cycle fatigue S-N numerical data in the databook published by the Society of Materials
Science, Japan(JSMS, 1982) and low-cycle fatigue ε-Ν graphical data in the databook
published by Japan Society of Mechanical Engineers(JSME, 1983) were utilized. 545 S-N
curves data and 311 ε-Ν curves data are contained in the database. Besides, fracture toughness
data were collected from journal articles, referring the papers on the sources of fracture
toughness data(Hudson and Seward, 1978,1982, 1989; Chambers and Sinclair, 1986; Assaad
and Sinclair, 1988). 280 valid K c data according to ASTM standard were contained in the
database.

APPLICATIONS

The database system is expected successfully used for obtaining fundamental fatigue strength
data of materials in fatigue analysis or fatigue life predictions, and for materials selection at
design stage. There are offen practical needs to estimate fundamental fatigue properties such as
fatigue limit, S-N or ε-Ν curve, with a limited amount of materials properties data. Here,
utilizing the database, approximation methods of ε-Ν and S-N curves were discussed.

Approximation of ε-Ν Curve under Axial Loading

Among various approximation methods, Manson's universal slopes method(1965) and

Mitchell's method(1979) have been relatively well utilized for their simplicity. Manson's
universal slopes method is expressed as

A8 t =A8 e +Ae p =C e N f ^C p N f c =3.5(a u /E)N f - 012 +8 f 0 - 6 N f · 0 · 6 (1)

where Δε^ Δεβ and Δερ denote total, elastic and plastic strain ranges, respectively, au is the
monotonic tensile strength, E{ is the fracture ductility and N f is the number of cycles to failure.
Mitchell's approximation method is as follows;

A8t/2=A8e/2+Aep/2=(o;/E)(2Nf)b+8;Nfc (2)
G^ u +345(MPa), b=-(l/6)log[2a f /a]
8^=8,, C=-0.6

where G{ is the fatigue strength coefficient and 8f' is the fatigue ductility coefficient.

Figure 2 shows the results of life predictions by two methods for various steels. Except for cast
steels, Manson's method provides excellent prediction results so that most of all data are within
factor of five scatterband, while Mitchell's method gives non-conservative estimate. For cast
steels, both methods give over-conservative predictions.

The prediction results for aluminium alloys are shown in Fig. 3. Both methods give good
results, except mat Mitchell's method is apt to give non-conservative predictions for the fatigue
life range longer than 104 cycles.
20

10 3 10 D B «;
■ O Carbon steel 3 : 0 Carbon steel s£
' D Alloy steel ~*5ί -Π Alloy steel ^ / M R
10 4 :ΔStainless steel . ^ H » 10 4 rAStainless steel °JäfflBP
z :<>Cast steel jytPf :OCast steel ^ S H S e ·
3
·2ιο . Μ Γ 0 4 A |io3
wisp *
o ·4
0 ♦*
e
|io
0)
*" * Λ I
a< 10
cu 10 k
■ y^ o
/^ · I l l l l l l 1 ■■■■■II
I 11. l l l l l l 11 l l l l l l / ! _ ! ._ l l . l lLl 1 1.1111.
1 1 1 1 1 . .I . . . . . . . . 1. .

I 10 10 2 10 3 10 4 10 5 1 10 10 2 10 3 10 4 10 3
Cycles to failure, Nf Cycles to failure, Nf
a) Manson's method b) Mitchell's m e t h o d

Fig. 2 Comparison of experimental data with ε-Ν life predictions by Manson's universal
slopes method and Mitchell's method for various steels under axial loading.

10 102 10 3 10 4 10 5 10 6 10 102 10 3 10 4 10 5 10 6
Cycles to failure, Nf Cycles to failure, Nf
a) Manson's m e t h o d b) Mitchell's m e t h o d

Fig. 3 Comparison of experimental data with ε-Ν life predictions by Manson's universal
slopes method and Mitchell's method for aluminium alloys under axial loading.

Approximation of S-N curves

As most of all the ε-Ν data collected from the JSME databook(1983) are confined within the
fatigue life range shorter than 105 cycles, life predictions for high-cycle fatigue were performed
using the S-N data from the JSMS databook(1982). Figure 4 shows the results of S-N life
predictions for steels under axial loading. While Mitchell's method gives significantly non-
conservative results, Manson's method provides reasonable results. However, the data scatter is
 21

10 ,β
ιο·
10*
2
10'
• 41- 10'

τ> 10»
α>
*J
10 4
ο
Ό 10*
<υ
10a

10
1 . I I III!
I H UM I HUM I I IM
10 10 '10 '10 *10 '10 "10 '10 '10 *10 " 1 10 10 f 10 310 410 '10 *10 710 e10 10 ,0

Cycles to failure, Nf Cycles to f a i l u r e , N f

a) Manson's method b) Mitchell's method

Fig. 4 Comparison of experimental data with S-N life predictions by Manson's universal
slopes method and Mitchell's method for steels under axial loading.

10 10 *10 J10 410 s10 *10 710 '10 10 10 10 10 *10 '10 Ί 0 »10 '10 710 "10 10 10
Cycles to failure, Nf Cycles to failure, Nf
a) Manson's m e t h o d b) Mitchell's m e t h o d
Fig. 5 Comparison of experimental data with S-N life predictions by Manson's universal
slopes method and Mitchell's method for aluminium alloys under axial loading.

considerably larger compared with ε-Ν life predictions. The results for aluminium alloys under
axial loading are shown in Fig. 5. Similar trend is found, the data scatter is significantly large.
Figure 6 shows the results for steels under rotating bending. For rotating bending, Mitchell's
method gives reasonable predictions, while the results by Manson's method are over-
conservative.

It may be concluded from these results mat Manson's universal slopes method provides good
approximation of ε-Ν curve under axial loading, and S-N curves under rotating bending are
well approximated by Mitchell's method. However, the predictions of high-cycle fatigue life by
22

1 10 10 2 10 3 10 4 10 *10 '10 7 10 g 10 *10 ,β

10 10 2 10 3 10 4 10 *10 ' 1 0 710 *10 *10 ,0

Cycles to failure, Nf Cycles to failure, Nf

a) Manson's method b) Mitchell's method
Fig. 6 Comparison of experimental data with S-N life predictions by Manson's universal
slopes method and Mitchell's method for various steels under rotating bending.

these methods may be practically meaningless, because of very large scatter. Studies are now
being carried out to improve the precision of life predictions, and to investigate characteristics
of fatigue properties. Besides, fracture toughness data will be analyzed.

CONCLUDING REMARKS

A relational fatigue strength database system for personal computer was developed. Using the
database, approximation method of ε-Ν and S-N curves from material mechanical properties
data were discussed. Approximated ε-Ν curves by Manson's universal slopes method provide
reasonable predictions of low-cycle fatigue life. However, predictions of high-cycle fatigue life
by approximated S-N curves are not satisfactory due to poor precision. A study is necessary to
improve the precision of S-N curve approximation.

REFERENCES

Assaad, A. T. and G. B. Sinclair(1988). Further remark on obtaining fracture toughness values

from the literature, Int. J. Fract., M, R47-R60.
Chambers, A.E. and G. B. Sinclair(1986). On obtaining fracture toughness values from the
literature, Int. J. Fract., 2Q, Rl 1-R15.
Hudson, C. M. and S. K. Seward(1978, 1982, 1989). A compendium of sources of fracture
toughness and fatigue crack growth data for metallic alloy-part I, II, III.
Int. J. Fract, 14, R151-R184,2ü, R59-R117,2£, R43-R63.
JSME(1961(1982), 1965, 1974, 1983). JSME Data Book: Fatigue of Metals. I(2nd edition),
II, III, IV. Japan Society of Mechanical Engineers, Tokyo.
JSMS(1982). Data Book on Fatigue Strength of Metallic Materials, Vols. 1, 2, 3. The Society
of Materials Science, Japan, Kyoto.
Manson, S. S.(1965). Fatigue: A complex subject-some simple approximations, Exp. Mech., 5,
193-226.
Mitchell, M. R.(1979). Fundamentals of mordern fatigue analysis for design. In: Fatigue and
Microstructure. pp. 385-437. ASM, Metals Park, Ohio.
WS5b1 PROBABILISTIC MODEL AND COMPUTER SIMULATION
ON SMALL FATIGUE CRACK PROPAGATION OF METALLIC MATERIALS

T. SAKAI*, K. TOKAJI** and T. OGAWA**

* Faculty of Science and Engineering, Ritsumeikan University,

Kita-ku, Kyoto, 603 Japan
**· Faculty of Engineering, Gifu University,
Yanagido, Gifu, 501-11 Japan

ABSTRACT

The statistical aspect of small fatigue crack propagation is first reviewed

for various kinds of metals. A probabilistic model is constructed on the
propagation behavior of such small cracks by considering crystallographic
conditions of the material. Based on this model, the crack propagation
behavior was simulated with the aid of Monte Carlo technique.

KEYWORDS

Fatigue crack; crack propagation; probabilistic model; simulation; metal

INTRODUCTION

Crack propagation behavior in the early stage plays an important role to

determine the fatigue life of metallic materials, since the propagation
process of small surface cracks occupies the predominant part of the total
fatigue life. These small cracks usually indicate the growth rates markedly
higher than those for large cracks which are characterized by Paris' law[l].
Another typical property of such small cracks is to indicate a large scatter
of growth rates and a distinct fluctuation of the crack propagation path
being affected by microstructural conditions.

In this study, a series of experimental results on small crack propagation

is first reviewed briefly. Then, a probabilistic model is constructed on
the propagation behavior of such small cracks by combining distribution
characteristics of the grain size, Schmid factor of each grain and
misorientation at grain boundaries. Based on this model, the crack
propagation behavior is simulated with aid of Monte Carlo technique. The
results are finally compared with the experimental aspect on the complicated
propagation behavior of small surface cracks.

EXPERIMENTAL ASPECT ON PROPAGATION BEHAVIOR OF SMALL SURFACE CRACKS

Microscopic Observation of Small Surface Cracks

The authors have reported many microscopic photographs of small cracks for a
wide range of metallic materials[2-4]. Figure 1 shows an example of such
small cracks caused on titanium specimen surface under rotating bending. The
fatigue crack initially took place with a definite length(2c=74pm), and it

23
24

1.0 0.8 0.6 0.4 0.2 0 0.2 0.4 0.6 0.8 1.0
Fig.l. Small fatigue crack on titanium Surface crack length c mm
specimen F i g . 2 . Crack growth r a t e v s . c r a c k l e n g t h

propagated through marked refractions in subsequent cyclic loading. This

fluctuation of the crack path was distinct in the early stage of the
propagation.

Microscopic Variation of Crack Growth Rates

Variation of the crack growth rate on a titanium specimen(Fig.l) is shown in

Fig.2. When the crack size is below a definite size, the marked variation is
observed in the growth rate. The main turget of this study is the
statistical variation of the crack growth behavior for small cracks within
the critical size. In Fig.2, the crack growth rate indicates sharp
decreasings at several stages in the crack propagation as shown by arrows.
The distance between adjacent arrows well corresponds to the grain size of
this material.

Crack Growth Rate versus Stress Intensity Factor

The authors have observed crack propagation behavior for ten of titanium
0 2c<400pm
Microscructurally small crack
Pure titanium (TB35C)
Rotating bending (R=-l)
σ=250 MPa (10 specimens)

(a) Surface grains and small crack

G.B. : Grain boundary

-δ„-. _ δ 2 — * - ό , - * - δ 3- * * - δ 5 - *
Crack prop, path

Schmid factor λ4 λ2 λ0 λ3 λ5
Crack growth rate * y*3 *
2 3 4 5 10 20 30 50 Misorientation θ6 θ4 υ2 "5

Maximum stress intensity factor (b) Notation of grain size, Schmid factor,
Kmax MPa*fii crack growth rate and misorientation

Fig.3. da/dN vs. Kmax Fig.4. Surface grains and definition of variables
 25
specimens under rotating bending by means of the previous method.
Relationships between the crack growth rate and maximum stress intensity
factor are plotted altogether in Fig.3. The marked variation is found in
the low region of Kmax. The crack length on the specimen surface is denoted
by 2c, whereas a is the crack depth. Sharp decreasings of the crack growth
rate in Fig.2 correspond to those in Fig.3.

The general trend of the crack propagation behavior in Fig.3 is summarized

as follows; The crack propagation is repeatedly prevented by grain
boundaries and, therefore, the growth rate is often decreased in small
cracks with Kmax<4MPav"m approximately. However, if the crack length exceeds
the critical size, the growth rate comes close to that in the growth law for
large cracks and the variation of the growth rate is rapidly reduced.

PROBABILISTIC MODEL ON PROPAGATION BEHAVIOR OF SMALL CRACKS

The common feature of the small crack propagation for metallic materials is
summarized as follows together with original properties of such crystalline
materials;
(1) The grain size has a statistical distribution.
(2) The crystalline orientation of each grain has a statistical
distribution.
(3) The fatigue crack initially takes place with a definite length.
(4) The crack growth rate in each grain is affected by the crystalline
orientation.
(5) As crack length is within a critical size, the crack propagation is
markedly prevented by grain boundaries and sharp decreasings are repeatedly
caused in the da/dN-Kmax relationship, but the average rate is almost
constant regardless of the crack extension.
(6) If crack length exceeds the critical size, the crack growth tends to
Paris' law for large cracks and the variation of the rate is reduced
distinctly.

Based on the above general aspect on the material itself and the small crack
propagation, a probabilistic model is constructed on the complicated
propagation behavior of small surface cracks under cyclic loading. As
illustrated in Fig.4, a fatigue crack is caused with the initial length of
2CQ in the grain of No.O, and it grows gradually through several grains
repeating refractions at grain boundaries. For the sake of simplicity, the
crack propagation behavior is projected to the horizontal axis as shown in
Fig.4(b). The grain size is denoted by $, the Schmid factor of each grain
by X , the crack growth rate of each grain by v* and the misorientation at
grain boundaries by Q, respectively.

Now, the concrete model and discussions are focussed to titanium specimens
in this study, since experimental results are most furnished for this
material. According to the earlier work[4], distribution characteristics of
the grain size are well approximated by a log-normal distribution.

It is well known that the feasibility of crack initiation depends on the

resolved shear stress on the primary slip system of the individual grain.
The crack propagation is also governed by the slip system when the crack
size is within several grains. Thus, the feasibility of crack growth is
strongly affected by the crystalline orientation of each grain. Schmid
factor X is the most convenient variable to represent the feasibility or
resistance of the crack growth. The larger the Schmid factor X is, the
higher the resolved shear stress r becomes. Accordingly, it is supposed
26
that the growth r a t e becomes high as the grain has a high value of Schmid
factor. Thus the following expression can be assumed between the growth
rate and Schmid factor in each grain;
υ*. = αλ + β (1)
where parameters are fixed to a=0.004 and β=0 as a reasonable example.

Schmid factor has the upper and lower bounds Xu and λ£. In such a case,
Beta-distribution i s preferably accepted to represent the s t a t i s t i c a l
distribution, since this distribution has a wide applicability depending on
the parameter values. The probability density function is given by
s-1 t-1
( λ λ
f(X)= " ^" ( ^ " λ )
, [λΖΐλ£λ„] (2)
au-H) s(s3t)
where B(s,t) is the Beta-function defined by

B(sJt) = f1 xS~1(l-x)t"1dx (3)

0
Since titanium has a hep structure, the number of active slip systems is
less than those in bec and fee metals. Consequently, it is expected that
the Schmid factor for the active slip system yields in a wide range of
0<λ<0.5. From this point of view, the upper and lower bounds are put as
Xu=0.5 and λ£=0. Moreover, parameters in Beta-distribution are put as
s=t=l, where Eq.(2) gives a uniform distribution in the domain of [λ£,λ^].
If Schmid factor of a grain is provided by Monte Carlo technique, one can
obtain the crack growth rate of the grain through the above procedure.

Crack propagation is prevented by grain boundaries as mentioned previously.

The preventive effect is supposed to depend on the misorientation of the
adjacent grains. By introducing the coefficient of ξ 0 , the preventive
effect is here formulated as follows;

?=? 0 e" n r («)

where r is the distance from grain boundary to the crack tip. Then the
actual growth rate in any site inside a grain is given by

y=v*-C 0 <T nr (5)

The preventive effect is illustrated in Fig.5. If the crack ceases to grow
at a boundary, it must be ξο=ν*. On the contrary, when the boundary is
disappeared(6=0), it must be ξο=0. The simplest expression to satisfy this
aspect is
λ

So = F " e ' (Θ
Ζ < Θ < Θ "> (6)
Distribution c h a r a c t e r i s t i c s of the misorientation are also formulated by
the Beta-distribution in the range of 0<θ<π/2. The lower and upper bounds
are put as θ£=0 and θ ^ π / 2 . Finally, i t i s supposed that the crack growth
rate is recovered following Eq.(5) after the crack tip goes ahead across the
grain boundary.

Based on the above procedure, one can simulate the crack propagation
behavior of small surface cracks. If crack length exceeds the c r i t i c a l
size, i t is assumed that the crack growth is characterized by the following
Paris' law for large cracks;
V (7)
=%= CaK)m
 27
(START)

I Setting of parameters
ξο
(a)
Generation of
i=Co^n" ί(Ι).λ(Ί),θ(Ι)

Crack growth in right hand side

h\ y(i)-v*(i)-Co'(De"nr
\ ^ äor(l)mtN-v(l)
Γ cr(I)=e0+Acr(I)

0
— t-
5
— ^ .
10 15 20 Cr ack
X
growth in left hand side
Distance to/from grain boundary r(ura) U(I)-U*(I)- 5o(D e-nr
Δσ^(Ι)=ΔΛ/·ΐ)(I)
cz(I)-c0+Ac Z<D
(b) nr
y = y *-c o e -
Total crack length and SIF

c(I) . Co+ Mi)p(i)

U *i:
\/ / ^ —
> ^
K(i)»o/i?(T)-F(i)
*** Π- 1
Output of numerical results
y(I),cr(I),Cj(I),c(I),X(I)
' 1
Graphical plot of results
y(I) versus c(I)
1 L 1 |
V(I) versus Δλ
0 5 10 15 20
Distance to/frora grain boundary r(um)

Fig.5. Crack growth preventive effect

Fig.6. Flow-chart of simulation
The statistical variation of this macroscopic crack propagation law has been
investigated by many researchers[5-7], but such a variation is not discussed
in the present study.

COMPUTER SIMULATION OF CRACK PROPAGATION BEHAVIOR

Figure 6 indicates the flow-chart of the computer simulation on the crack

propagation behavior of small surface cracks. On titanium specimens,
concrete values of the parameters required in the simulation are all
provided in the previous section. By means of Monte Carlo technique, the
crack propagation behavior was repeatedly simulated ten times. Three typical
examples of dc/dN-c relationships obtained are shown in Fig.7. Nps
indicated in the figure is the crack propagation life during the initial
crack(2e0) grows to the critical length of 400um. In Fig.7, the growth rate
repeatedly indicates sharp decreasings at several sites which corresponds to
grain boundaries. Overall trend of this crack propagation behavior is in
good agreement with that in the central region of Fig.2.

All of da/dN-Kmax relationships obtained are plotted in Fig.8. The

individual crack propagates repeating the sharp decreasing and recovering of
the growth rate at grain boundaries. In the present simulation, the growth
rate is supposed to converge upon the crack propagation law of large cracks
at Kmax=5MPavTn as crack length exceeds the critical length (2c=400μm).
Small cracks are sometimes classified into microstructurally small crack and
mechanically small crack[2-4,8]. From the result of Fig.8, it is expected
that the transient period from microstructurally small crack to the large
crack which is governed by the Paris* law[l] gives the mechanically small
crack.
28
Simulated for titanium Simulated for titanium
Rotating bending(R"-l) - 0 - Nps»l.43x10 s Rotating bending(R«=-l)
o-250MPa (10 Specimens) - 0 - Nps-1.57x10 s o=250MPa (10 Specimens)
- ♦ - Nps-1.78x10 s
Crack growth law
for large crack
Crack t i p 2 Crack t i p 1
■o\*-

Γ 1

1 J 1 1 1 1
0.2 o.i o fO.l
Φ 10"
Crack length mm
Fig.7. Crack growth r a t e vs. crack length

CONCLUSIONS

The c h a r a c t e r i s t i c f e a t u r e on t h e p r o p a g a - <j
t i o n b e h a v i o r of s m a l l s u r f a c e c r a c k s was £
f i r s t r e v i e w e d on a w i d e r a n g e of m e t a l l i c icr J_ J I I I 1 I
materials. A p r o b a b i l i s t i c m o d e l of t h e Maximum stress intensity factor
c r a c k p r o p a g a t i o n was t h e n c o n s t r u c t e d by Kmax MPa /m~
c o m b i n i n g s t a t i s t i c a l d i s t r i b u t i o n s of t h e Fig.8. da/dN vs. Kmax
g r a i n s i z e , Schmid f a c t o r of each g r a i n and
m i s o r i e n t a t i o n a t g r a i n b o u n d a r i e s . Based on
t h i s model, computer s i m u l a t i o n s were r e p e a t e d l y performed on s m a l l c r a c k
g r o w t h of t i t a n i u m s p e c i m e n s . O v e r a l l t r e n d of t h e c r a c k p r o p a g a t i o n
b e h a v i o r o b t a i n e d was i n good a g r e e m e n t w i t h t h e e x p e r i m e n t a l b e h a v i o r of
small crack propagation.

REFERENCES

1) Paris,P.C. and F.Erdogan(1963). A critical analysis of crack propagation

laws. Trans. ASME. Ser.D, 85, 528-534.
2) Tokaji,K., T.Ogawa, Y.Harada and Z.Ando(1986). Limitations of linear
elastic fracture mechanics in respect of small fatigue cracks and
microstructure. Fatigue Fract. Engng. Mater. Struct., 9, 1-14.
3) TokajijK., T.Ogawa and Y.Harada(1987). Evaluation . on limitation of
linear elastic fracture mechanics for small fatigue crack growth. Fatigue
Fract. Engng. Mater. Struct., 10, 281-289.
4) Tokaji,K., T.Ogawa, Y.Kameyama and Y.Kato(1990). Small fatigue crack
growth behaviour and its statistical properties in a pure titanium. Proc.
Int. Conf. Fatigue 90, Vol.2, 1091-1096.
5) Sakai,T. and T.Tanaka(1979). Statistical study on distribution charac-
teristics of fatigue crack propagation life of metallic materials. J. Soc.
Mat. Sei., Japan, 28, 880-886.
6) Ichikawa,M., T.Takura and S.Tanaka(1982). Statistical investigation of
fatigue life by separating crack initiation and propagation lives. J. Soc.
Mat. Sei., Japan, 31, 697-702.
7) Ichikawa,M., S.Akita, T.Takamatsu, T.Matsumura, T.Sato and S.Nishijima
(1988). Reliability engineering approach to fatigue crack growth rate using
DC electrical potential method. J. Soc. Mat. Sei., 37, 1010-1016.
8) Tanaka,K.(1988). Mechanics approach to small fatigue crack propagation.
Trans. Japan Soc. Mech. Engrs., 54, 1-7.
WS5b2

CRACK INITIATION FATIGUE LIFE AND SIZE EFFECT EVALUATION

OF NOTCHED STRUCTURES BY USE OF MATERIALS DATA

Chr. Boiler
Messerschmitt-Bölkow-Blohm GmbH, Aircraft Division
Postfach 80 11 60, D-8000 München 80, Germany

T. Seeger
Technische Hochschule Darmstadt, Fachgebiet Werkstoffmechanik
Petersenstr. 13, D-6100 Darmstadt, Germany

ABSTRACT
The influence of specimen or notch size on fatigue life can be
well accounted for within procedures based on material's data
(Local Strain Approach), which is discussed and validated.

KEYWORDS
Fatigue life evaluation, Local Strain Approach, notch size, Kf

INTRODUCTION
Numerical procedures increasingly help to optimize structures'
fatigue behaviour and to reduce cost-driving experiments. In
combination with Finite Element Analysis (FEA) Local Strain
Approach has become an interesting procedure for fatigue life
evaluation, which simply reguires experimental effort in eva-
luating materials data for cyclic loading. How to account for
the effect of notch and/or specimen size within Local Strain
Approach will be explained in the following.

LOCAL STRAIN APPROACH

The Local Strain Approach initiated by Manson (1953) and Coffin
(1954) starts from the idea, that materials mechanical beha-
viour in a notch can be transferred to an unnotched specimen,
when notch root and unnotched specimen are under the same
loading condition. To evaluate fatigue life this requires (1) a
stress concentration factor Kt , (2) a load notch strain rela-
tionship, (3) material's stress-strain relationship for cyclic
loading and (4) material's fatigue life relationship (Fig. 1 ) .

29
30

Kt may be taken from

Local Strain Approach handbooks (e.g. Peter-
son, 1974) or evaluated
by FEA. FEA may also be
used to evaluate the
load notch strain rela-
tionship which relates
loads to notch stresses
and strains. Possible is
also Neuber's (1961)
relationship (Neuber's
rule) written ace. to
Seeger and Heuler (1980)
Fig. 1 as follows:

σ · ε = (S-Kt)2/E · (e*-E)/S* (1) ε = f(o) (2)

Eq. (1) is applied in relation with material's elastic-plastic

stress-strain behaviour (eq.(2)). σ and ε are local stresses
and strains, S a nominal stress related to Kt , E Young's
modulus, S*=S-Kt/KP a special nominal stress identical to yield
stress when S reaches the state of full plastification, e* a
special nominal strain related to S* according to eq. (2) and
Kp the ratio between load at full plastification to load at
initiation of plasticity. If full plastification is not rea-
ched, which is very usual, e*·E/S* becomes unity.

Material's σ-ε and fatigue-life relationship can be obtained

either from tests or materials data collections (e.g. Boiler
and Seeger, 1987, Bäumel jr. and Seeger, 1990).

Eqs. (1) and (2) allow to describe the σ-ε-path in the notch
for elastic-plastic material. Considering material's memory be-
haviour closed hysteresis loops are obtained, where each is de-
fined as a damage event and characterized by Smith's et al_..,
(1970) parameter

PSWT = ( (Oa+Om)· ε β · E ) 1 /2 (3)

Index a characterizes the amplitude and om mean stress.

Material's fatigue-life relationship can be described by a
PswT-life curve using Manson's (1965) constants leading to

PSWT = (Of'2· (2N) 2b + E·Of» · εί' · (2N)b +c

) * / 2 > PSWT,E (4a)

with Ρ8νντ,Ε=Ε·εβ,βΐ,Ε·(1 + ε 9 , Ρ ι,Ε/ε 3 ,βΐ,Ε) 1 / 2 (4b)

or a bilinear relationship in log-log scale being
N = 2· 10* · (PSWT/PSWT . κ )'k» (5)

for PSWT £ PSWT.E. Within eqs. (4) and (5) N are cycles to
failure, Of ', b, εΐ' and c constants, ea,ei and ε3,Ρι is
elastic and plastic strain, PSWT,K the PSWT value at a fatigue
life of 2*106 cycles and kP the slope of the line. The index E
indicates the respective value for fatigue endurance limit.
 31
By use of eg. (4) or (5) and Paimgren-Miner's damage accumula-
tion rule fatigue life of a randomly loaded notch is obtained.

NOTCH SIZE EFFECT

A notch is mainly characterized by Kt. . This assumes elastic and
homogeneous material behaviour and uniaxial stresses and
strains. With real materials these assumptions may not be valid
anymore. Experiments show that fatigue strength is reduced with
increasing notch size. This size effect can be accounted for by
use of a notch fatigue factor Kf instead of Kt where Kf is de-
fined for the endurance limit as stress of an unnotched
specimen to nominal stress of a notched specimen. Kf-procedures
have been proposed by Stieler (1954), Neuber (1968), Peterson
(1974) and others. They explain size effect by the stress
gradient in a notch which cannot follow the theoretically
calculated stress gradient because of increasing influence of
microstructure (grains and grain boundaries) with decreasing
notch size. Kloos (1976) categorized this type of size effect
which has become part of design standards and handbooks as the
stress gradient related size effect.

Weibull (1951), Kuguel (1961), Böhm (1980), Boiler (1988) and

others explain size effect by the idea that crack initiating
failures are randomly distributed in the material. This random
distribution is one of the reasons for scatter in materials'
properties. If notch or specimen size is decreased, the proba-
bility of occurence of the severest failure within the
material decreases and therefore increase notch or specimen
strength. Importance of this difference in strength increases
with decreasing probability of survival. This has been catego-
rized as statistical size effect (Kloos, 1976).

Often Weibull's (1951) 2-parameter probability distribution

P = 1 - exp[ -m· (L)M (6)

is applied with P being probability of failure, L strength and

k and m constants. If k and m are valid for a specimen of size
Mi probability of survival of an n = M2/Mi times bigger
specimen of size M2 is

1 - P2 = (1 - Pi ) n (7)
Inserting eg. (6) into eg. (7) leads to P of specimen 2
P2 = 1 - (1 - Pi) n = 1 - exp[ -m· (M2/Mi)· (L)k ] (8)
When Pi eguals P2 egs. (6) and (8) are egual resulting in
Li / L 2 = (M2/Mi)1/k (9)

As cracks usually initiate from specimens' surface specimen

sizes Mi and M2 are defined as specimens' highly stressed
surfaces Ai and A2. Böhm (1980) proposed the following eguation
for evaluating the highly stressed surface of notches
32
L(x,y,z)
AH s = ( ) k dA (10)
Lm a x
As

L(x,y,z) is stress σ on each point of the surface, Lmax the

maximum stress on the surface, As the specimen's surface and
AHS the specimen's highly stressed surface. The integration may
be performed analytically or by FEA (Böhm, 1980, Boiler, 1988).

Instead of σ PSWT can be selected for L

in eq. (6) and (8)-(10) (Boiler, 1988).
As the distribution of PSWT follows the
distribution of σ for completely elastic
material (Fig. 2) and k does not show
significant difference for σ and PSWT it
is of minor importance of either using σ
or PSWT in these equations.

k is either evaluated from experiments

performed on one load level (Böhm, 1980)
or by moving test results parallel to
Fig. 2 the fatigue-life-curve to a defined fa-
tigue life Ni (Boiler, 1988) (Fig. 3 ) .

If PSWT and the respective highly stressed surfaces are

selected in eq. (9) this leads to
PSWT, 2 AH £
log PSWT T ΙηΙηφ τ = ( .) 1 / k (11)
Ps WT ,1 AH ί

For evaluating fatigue

notch size effect by Local
Strain Approach the follo-
N| logN wing is required:
Fig. I" (PSWT)

1. calculate size AHS,N of the notch by use of eq. (10)

2. evaluate the PSWT-life-curve of an unnotched specimen
with size AHS,N using eq. (11). This is performed by
shifting the PSWT-life curve of an unnotched specimen with
a size AHS,U by a factor of (AHS, U / A H S , N ) 1 / k .

This PSWT-life curve for an unnotched specimen with size A H S , N

can then be used to evaluate the fatigue life of the notch.

When Kf is used in eq. (1) instead of Kt no shift of material's

PSWT-life curve is required.

EXAMPLES
A procedure based on stress gradient related size effect
(Stieler, 1954) is compared to a procedure based on statistical
size effect (Boiler, 1988) for fatigue life evaluation for the
following two different types of specimen:

a) Centerholed plates of structural steel StE460 (DIN spec.)

loaded under push-pull constant and random amplitude load
 33
sequences (Gaussian
sequence with 5· 105

^φ^Η
D W L T
[mm] [mm] [mm] [mm] cycles and TWIST).

ψ
51,6 258 450 7,5
16,0 80 500 10,0 b) Circumferentially not-
15,6 78 300 7,5
15,6 78 300 2,25
ched round bars of
8,0 40 280 5,0 steel 30CrNiMo8 loaded
5,2 40 150 2,25
4,0 20 240 4,0 under push-pull and ro-
2,0 10 220 2,0 tating bending constant
amplitude loading.

The origin of the expe-

Fig. 4a riments is mentioned by
Boiler (1988).

Figure 5 illustrates the result

for StE460 when strength ratio
is plotted versus size ratio
ace. to eq. (11). Compared to
the experiments no significant
difference is obtained with the
two procedures considered.

The specimen size tested for

30CrNiMo8 varies by a factor of
nearly 104 in size of highly
stressed surface. Each data
ROTATIN G BENDIN G
point represents the mean value
PUSH-PUL L o
of several tests. No influence
[mm] [nun] [mm]
[mm]
of loading condition or Kt can
*{
(mm) [nun] [mm] [mm] 3 0 1,
10 5 8 0,
47,5 be recognized. Only specimen
ύ 20 80 149,6 and/or notch size is signifi-
2 θ ! β3
9 , 64
2 8 , 93 4 ^ 05
0 ,6 6 ,8
2 0 , 39
3 8 , 51
2 7 , 59
52,1
1,2
3,6 cant. This is well described by
s'.o 3 8 , 57 5 3 , 57
6 . 96 1 0 , 96 8 ,9 1
8 0 4,
0 0 8, 1 3 6 4*
14 ,'2
17,8
the statistical size effect. The
0 . 55 3 β ' , 72
5 9 . 20
32,8
6 0 , 27
β ! οο
11,0
17,0
0 ,1 10 16
32
3,θ1
6,0
application of procedures based
1 . 15 1 2 6 , 00 23,0
0 .8
35
80 34 1 2 8 , 43
10,5
24,0 on stress gradient related size
1 0 0 , 43
effect leads to a relation to Kt
and an increase in unconserva-
Fig. 4b tive prediction with increasing
specimen and/or notch size, the
latter being based on the assumption Kf <, Kt .

Fig. 5 Fig. 6
34
CONCLUSION
The reasons for stress gradient related size effect procedures
being not satisfactory is because (1) notch size of experiments
leading to this procedure varied less than a factor 10 (statis-
tical aspect was not obvious), (2) the procedure cannot differ-
entiate between specimens with same notch radius but different
cross-section areas and (3) the effect of notch-plasticity is
interpreted as size effect. Stress gradient related size effect
still needs experimental verification. Its importance to struc-
tural steels is minor compared to the statistical size effect.

REFERENCES
Bäumel, A. jr., T. Seeger (1990). Materials Data for Cyclic
Loading. Supplement 1, Elsevier, Amsterdam
Böhm, J. (1980). Zur Vorhersage von Dauerschwingfestigkeiten
ungekerbter und gekerbter Bauteile unter Berücksichtigung
des statistischen Größeneinflusses. Ph.D. Thesis, München
Boiler, Chr., T. Seeger (1987). Materials Data for Cyclic Lpac[-
ing. Vol. A-E, Elsevier, Amsterdam
Boiler, Chr. (1988) . Der Einfluß von Probengröße und ObjerfJ^cJi-
enrauhigkeit auf Lebensdauerabschätzungen bei Betrachtung der
örtlichen Beanspruchungen. Heft 46,Veröffentl. d. Inst. f.
Stahlbau u. Werkstoffmechanik, TH Darmstadt
Coffin, L.F. jr. (1954). A Study of the Effects of Thermal
Stresses on a Ductile Metal. Trans. ASME, Vol. 76, 931 - 950
Kloos, K.-H. (1976). Einfluß des Oberflächenzustandes und der
Probengröße auf die Schwingtestigkeitseigenschaften.
VDI-Bericht 268, 6 3 - 7 6
Kuguel, R. (1961). A Relation Between Theoretical Stress Con-
centration Factor and Fatigue Notch Factor Deduced from the
Concept of Highly Stressed Volume. Proc. ASTM, Vol. 61, 732 -
748
Manson, S.S. (1953). Behaviour of Materials Under Conditions of
Thermal Stress. NACA TN-2933
Manson, S.S. (1965). Fatigue: A Complex Subject - Some Simple
Approximations. Experimental Mechanics, V o J U 5 , 7, 193 - 226
Neuber, H. (1961). Theory of Stress Concentration for Shear-
Strained Prismatical Bodies with Arbitrary Nonlinear
Stress-Strain Law. Trans. ASME, J. Appl. Mech. , 2j8, 544- 550
Neuber, H. (1968). über die Berücksichtigung der Spannungskon-
zentration bei Festigkeitsberechnungen. Konstruktion,, 2_0, 7,
245 - 251
Peterson, R.E. (1974). Stress Concentration Factors. J. Wiley &
Sons, New York
Seeger, T., P. Heuler (1980). Generalized Application of
Neuberfs Rule. J. of Test. & Eval., Vol. 3, 4, 199 - 204
Smith, K.N., P. Watson, T.H. Topper (1970). A Stress-Strain
Function for the Fatigue of Metals. J. of Materials, JMLSA,
Vol. 5, No. 4, 767 - 778
Stieler, M. (1954). Untersuchungen über die Dauerschwingfestig-
keit metallischer Bauteile bei Raumtemperatur. Ph.D. Thesis,
Stuttgart
Weibull, W. (1951). A Statistical Distribution Function of Wide
Applicability. J. of Appl. Mech., 18, No. 3, 293 - 297
WS5b3

QUANTITATIVE ANALYSIS OF DEFORMATION NEAR FATIGUE

CRACK TIP USING IMAGE PROCESSING TECHNIQUE

M.JONO and A.SUGETA

Department of Mechanical Engineering, Osaka University,

Yamadaoka, Suita, Osaka, Japan

ABSTRACT

Fatigue crack growth tests were carried out on 3% silicon iron and direct,
real time observation of crack growth behavior was made. Correlation between
crack growth rate and crack tip opening displacement was investigated and
quantitative analysis of crack opening displacement and deformation behavior
near crack tip was made by using a newly developed image processing
technique.

KEYWORDS

Fatigue crack growth; Direct observation; Computer image processing; Near

crack tip deformation; Crack opening displacement.

INTRODUCTION

Since the fatigue crack growth phenomenon is considered to be intrinsically

localized, microscopical direct observation is an effective technique to
understand the fatigue crack growth mechanism and a fairly large number cf
microscopic studies have been made(for example; Laird and Smith, 1962;
Pelloux, 1969; Neumann, 1974). In the early work, present author and others
have designed a servo-hydraulic fatigue loading facility operating in a
scanning electron microscope (SEM), and have conducted fatigue crack growth
tests to elucidate the fatigue crack growth mechanism(Kikukawa et al.. 1979;
Kikukawa et_al., 1982; Jono and Sugeta., 1988,1990).

In this study, a micro-computer aided image sampling system and image

processing technique were developed. And the crack opening displacement and
deformation behavior near crack tip under constant amplitude and repeated
two-step fatigue loading were quantitatively analyzed and correlation be-
tween crack growth rate and crack tip opening displacement was investigated.

FATIGUE TESTING AND IMAGE SAMPLING SYSTEM

The block diagram of fatigue testing system is shown in Fig.l. The servo-
hydraulic fatigue loading facility operating in an SEM is controlled by a
micro-computer(NEC PC9801-VM2). The computer image processing and data
35
36

Fatigue testing apparatus

Fatigue loading facility SEM

Servo Load |Displacement| Secondary Scanning! Sweep
valve signal signl electron signal signal
signal
^ ^
Subtraction Differential
Servo ampTl circuit circuit
T — * » i
1 Mixing circuit j
I D/A converter nDMA type A/D3converter k-
ψ
T
C.P.U. Main memory C.P.U. Main memory 640 Kbytes
PC-9801VM2 348 Kbytes PC-9801VX4 Bank memory 4 Mbytes

Fig.l Block diagram of fatigue testing system.

Superposition of Two SEM Images

Calculation of Correspondence
between Two SEM Images by
Using SSDA Method
ΙΠ
Measurement of Displacement
between Corresponding Points
Calculation of Displacement
Distribution

Fig.2 Configuration and crystal- Fig.3 Flow chart of

lographic orientation of crack analysis
test specimen. procedure.

sampling systems are composed of a micro-computer (NEC PC9801, memory

capacity is 4 Mbytes) and a high-speed direct memory access (DMA) type A/D
converter(ELMEC EC-2390). The secondary electron signal of the SEM was
directly transferred to the main memory of the micro-computer through DMA
type A/D converter with digitizing rate of 5 ysec per point to make it
possible to sample the successive ten flames of SEM image data under fatigue
loading of 1 Hz. The sampling cycle was found to not always synchronize
with the scanning signal of the SEM , so the restructure of SEM images from
the continuously sampled secondary electron signal data was made by
detecting the starting points of sweep and scanning signals of the SEM.

Fatigue crack growth tests were performed on a grain oriented 3% silicon

iron under constant and repeated two-step loadings. The specimens
configuration of which was shown in Fig.2 with crystallographic orientations
were mechanically polished with emery papers and finally electro-polished.
Fine magnesium oxides were scattered on a surface of the specimen as
location markers and then the surface was gold coated to enhance the
resolution in SEM images.

IMAGE PROCESSING TECHNIQUE

Figure 3 shows the flow chart of fatigue crack analysis with the aid of
 37

# I
ife»^ -.-
^Mfcfc^
- · · c^ £
i^T *
iLr'· :' Λ
^ ^ f^c" ^
H^ -ί---- bO
^^■^
^ ^ " t a -
^
^ ^ Ί ■^^
- ΐ ^ · . ι=:
- ? * . ·-·
-σ
^^■h^
'*%■
^ -
-.-
.
^
ο
-3

2 μ. m
\ Ψ
—
Fig.4 Example of SEM Fig.6 SEM image processed
photograph of by thresholding.
fatigue crack.

Specimen surface JiS?

Crack
CODy= COD cos9
CODx=CODsin9

30 100 150 200 250

Brightness

Fig.5 Brightness distribu- Fig.7 Definition of crack

tion of SEM photograph. opening displacement.

image processing technique. Firstly, crack region is detected by

thresholding. The example of SEM photograph of fatigue crack is shown in
Fig.4. Figure 5 shows the brightness distribution of the SEM photograph
indicating that the region with low brightness value corresponds to fatigue
crack and that with high brightness to magnesium oxides, and mid-region
shows the test specimen surface. Since the brightness distribution of crack
overlaped with that of the test specimen surface, it was difficult to sepa-
rate crack region from specimen surface region, clearly. So, crack region
was recognized as the largest region among the detected regions by
thresholding using the optimum threshold value. The SEM image processed by
thresholding is shown in Fig. 6. Secondly, crack region was divided to small
regions at crack deflection points and principal axis of inertia of each
region was calculated. Center line of fatigue crack was obtained by
connecting the each principal axes of crack regions.

EXPERIMENT RESULTS AND DISCUSSION

Crack opening displacement(COD) is defined as the opening displacement in

perpendicular direction to crack center line as shown in Fig.7. Figure 8(a)
and (b) show examples of COD measurements where are shown fatigue cracks in
the middle, and the measured COD values are shown in the bottom of each
figure, respectively. The COD gradually decreased with approaching to the
crack tip and the abrupt change of COD near crack tip was observed. Crack
tip opening displacement(CTOD) was defined as the COD at the location where
the abrupt change of COD occurred. And also the microscopic crack growth
38

(a) CTOD = 1 5 ( p i x e l ) = 0 . 5 1 ( # m ) (b) CTOD = 3 0 ( p i x e l ) = 1.02(//m)

0 m i c (CTOD) = 21. 3(degree) <9mic (CTOD) = 31. 1 (degree)

F i g . 8 Examples o f COD measurement.

10"'
r
0
o FT=0.0 o
O R=0
Δ R = 0.1
r
I J
-tf
— o· i Δ
10 Δ R=0.1
-^ιο 7 $
20 E A)
6.

ε
30
oo
2ß
CD 40 o — o 10'
0 o ca
o-c * o o CP
50
GO I
ODC) 0
II
6
1°
9 8 7
10" 10" 10~ -9L 11
(da/dn)mj C m/cycle io~8 io7 10 6 10"5
CTODy m
Fig.9 Relationship between
crack growth rate and Fig.10 Relationship between
crack growth direction CTODy and crack
angle. growth rate.
direction, Qm±c » w a s calculated as an inclination angle of the crack center
line in crack tip region to perpendicular direction of loading axis.
Measured values of CTOD and 6 m i c are shown below the figures.
Figure 9 shows the relationship between microscopic growth rate, (da/dn)mic,
and microscopic growth direction 0 m i C ,of fatigue cracks. Figure 10 shows
the relationship between the vertical component of CTOD, CTODy, and the
perpendicular component of microscopic growth rate to the loading axis. CTOD
and 9 m i c were measured on the SEM photographs and also measured by using
the image processing technique. It was found that there existed strong
dependence of crack growth direction on crack growth rate. At the growth
rate above about 2X10"7 m/cycle, 6 m i C almost equals to zero indicating that
two preferential slip directions of the material operated to almost
identical extent simultaneously, and fatigue crack grew in near Mode I.
However, microscopic crack growth direction angle increases with decrease of
crack growth rate and coincides with the preferential slip direction at the
growth rate below 10~8m/cycle. A good correlation was also found between
crack growth rate and CTOD, and the ratio of growth increment to CTODy in
the range of growth rate from IO"8to 2X10"7m/cycle was about one-tenth.
 39

Detection of Crack Region

1
1 Judgement of Crack 1
3eflection 1
i
| Determination of Crack Center Line |
1
| Measurement of COD |
1
| Measurement of CTOD |

Fig.11 Flow chart of

deformation analysis
procedure.

(c) Superposition of two

Fig.13 Displacement distri- SEM images.
bution around the Fig.12 Deformation behavior
fatigue crack tip. near the crack tip.

Although this ratio is small compared to that of Mode I crack where 0.5 -
0.6 was observed in experimental measurement(Kikukawa et al.. 1979), the
vertical component of CTOD was suggested to be a gorverning parameter of
crack growth even in the mixed mode fatigue cracks. Moreover, in the
growth rate region below 10" 8 m/cycle considerable decrease of the ratio of
crack growth increment to CTOD was found with decrease of crack growth rate.

It was tried to analize the deformation near fatigue crack tip by

superposition and comparing two SEM images sampled at a minimum load and at
a succesive maximum load. Figure 11 shows the flow chart of near crack tip
deformation analysis procedure. The superposition was made by corresponding
magnesium oxides located in the region ahead of crack tip of two SEM images,
since it was reported that little slip deformation occurred ahead the crack
tip for Mode I cracks(Kikukawa et al.,1979). Calculation of correspondences
between two SEM images was carried out by using Sequential Similarity
Detection Algorithm (SSDA) method(Komai and Kikuchi, 1985). A SEM image was
divided into 300 window areas and a corresponding area to each window area
was searched on the other SEM image. Displacement is quantified by measur-
40
ing a shift distance between the coressponding area. The results of defor-
mation analysis is shown in Fig. 12. Figure 12(a) and (b) show the SEM
photographs sampled at the minimum and maximum load, respectively. In Fig.
12(c), square symbols represent center of window areas in the SEM image
sampled at the minimum load(Fig.12(b)) and circular symbols show center of
coressponding areas in the SEM image sampled at the maximum load. In order
to obtain continuous displacement distribution around the crack tip, spline
function with two variables was fitted to the discrete displacement
distribution as shown in Fig.12, and the calculated results are shown in
Fig.13. It was found that displacement occurred almost uniformly behind the
crack tip and decreased near creek tip region, and there occurred little
deformation ahead of the crack tip. Kikukawa et al.(1979) reported that
deformation began to occur at the apex of crack tip along the slip lines for
Mode I fatigue cracks. In this example, however, deformation was also
observed in the region in front of slip lines, which passed through the
crack tip, shown by dashed line in Figs.12 and 13. The deformation direction
in the region behind crack tip was found to be approximately 55 degree,
which coincides with the slip direction of the material.

CONCLUSIONS

Direct, real time observations of fatigue crack growth behavior were made by
using image processing technique. Main results obtained are summarized as
follows;
There existed a good correlation between crack growth rate and crack tip
opening displacement,CTOD, and CTOD was found to be a governing parameter of
fatigue crack growth rates. And also,it was found that microscopic crack
growth direction was closely related with crack growth rates. Moreover, the
usefullness of the newly developed image processing technique in a
quantitative analysis of crack opening displacement and deformation behavior
near crack tip was confirmed.

REFERENCES

Jono,M. and A. Sugeta (1988). In-situ observations of growing fatigue crack

by field emission type scanning electron microscope. Proc. VI Int. Congr.
Exp. Mech., 801-806.
Jono,M. and A. Sugeta (1990). Direct observation of growing fatigue crack by
field emission type scanning electron microscope and developement of
computer image processing technique. Proc. Fatigue*90, 1211-1216.
Kikukawa,M., M. Jono and M. Adachi (1979). Direct observation and mechanism
of fatigue crack propagation. ASTM STP 675. 234-253.
Kikukawa,M., M. Jono, M. Iwahashi, A. Ichikawa and N. Uesugi (1982). Fatigue
testing apparatus assembled in a field- emission type scanning electron
microscope and direct observation of fatigue crack propagation. J.Soc.
Mat. Sei., 31, 669-674.
Komai.K. and J. Kikuchi (1985). 3-dimensional image analysis of fatigue
fracture surface. J. Soc. Mat. Sei., 34, 648-652.
Laird,C and G.C. Smith (1962). Crack propagation in high stress fatigue.
Phil. Mag., 7, 847-857.
Neumann,P.(1974). New experiments concerning the slip processes at propa-
gating fatigue cracks. Acta Meta., 22, 1157-1165.
Pelloux,R.M.N.(1969). Mechanisms of formation of ductile fatigue striations.
Trans. ASM, 62, 281-284.
WS5b4

FATIGUE DAMAGE ESTIMATED ON ENERGY DISSIPATIVE ANALYSIS

Tung Xiaoyan

Aircraft Engng. Dept., Northwestern Polytechnical University

ΧΓAn, Shannxi, 710072, P.R. China

Wang Dcjun Xu Hao Lee Yuejun

Dept. Π of Mech. Engng., Northeast University of Technology

Shenyang, Liaoning, 110006, P.R. China

ABSTRACT

Consider the irrecoverable energy dissipation in fatigue damage process and take the cy-
cle-dependence into account, a fatigue damage model has been proposed. Comparisons
have been done between the estimated results by this model and several usual ones with
test results.

KEYWORDS

Energy dissipation; Cycle-dependenc; Fatigue damage; Irreversibility.

INTRODUCTION

In classical phenomenological fatigue damage theories, many significant investigations

have been done on the selections of fatigue damage parameters( Kitagawa,Plumtree,
1990), in order to describe the phenomena in fatigue damage process based on the exper-
iment data. In summary, the usual fatigue damage parameters, which were determined by
the algebraic combinative terms of elastic and plastic strain and stress, can be considered
as the quantities of displacement or force and power during defoming process of metals,
the usual fatigue damage parameters. Then the problem we may meet is how to define a
fatigue damage parameter with clear physical implication.
Since fatigue phenomena were known, fatigue damage have been considered to be an
irrecoverable energy dissipative process( High, 1928 ). With this concept, the well-known
Miners law was derived by the hypothesis that energy dissipation of fatigue damage is
conservation Miner, 1945 ). Furthermore, widely investigations have been done on plas-
tic strain energy dissipation in fatigue damage ( Morrow et al., 1965) ( Eyllin etal., 1985).
Meanwhile many valuable results have been achieved. With the development of the
infrared thermographic technology( Harig et al., 1986 ), the problems how to describe

41
42
completely the energy dissipation of fatigue damage have been raised. Simultaneously,
the davantages on energy dissipation of fatigue damage have been applied to predicting
fatigue life ( Kliman, 1985 ) and estimating and simulating local stress-strain responses(
Glinka, 1985; Boisserie, 1983 ).
In this paper, a fatigue damage model based on energy dissipation analysis of fatigue
damage has been proposed. In order to obtain a satisfied fatigue damage model, the
cyclic properties of energy dissipation of fatigue damage have been discussed according
to the irrecoverable thermodynamics.

FATIGUE DAMAGE FUNCTION ON ENERGY DISSIPATION

In usual fatigue damage models, although some were defined as the function of hysteresis
energy, the irreversibility of fatigue damage hasn't been really taken into account( Tung
et al.,.1989 ) From the view point of that fatigue damage is an irrecoverable energy
dissipative process, the energy dissipation of metals in forms of heat or nonpropogating
cracks or defects will be occurred during fatigue damage process and there exist the ef-
fects of Inelastic and microplastic strain energy on fatigue damage in the period of cyclic
loading, therefore it is not an integrate definition on fatigue damage. From the correla-
tion of cyclic mechanical and heat energy dissipation in fatigue damage process, it can be
concluded that the past cyclic fatigue damage is larger than the current one under the
same condition, because of affecting of cycle-dependence on fatigue damage( Tung et
al.,.1990)

IRRECOVERABLE ENERGY DISSIPATION IN FATIGUE

According to the energy dissipative structure proposed by Tung ( Tung et al.,.1990 ) , it

can be concluded that the energy dissipation of metals under cyclic loading is mainly con-
sisted of mechanical and heat ones. In order to study fatigue damage, this paper has inte-
grated the relations of the cycle-dependence of fatigue damage with mechanical and heat
energy dissipation, on the basis of the test results ( Tung et al.,.1991 ) and on the
numerically analyzing results by thermodynamics (Tung et al.,.1990 )

Mechanical energy dissipation in fatigue

Mechanical energy dissipation interested in this paper includes cyclic hysteresis energy
and total absorbed energy to failure. In fatigue tests of metals under full-reversed con-
stant controlled strain, the changes of cyclic hysteresis energy of metals with numbers of
cycles aren't apparent( Eyllin, 1895; Tung et al.,1989 ), but it isn't a general phenomenon,
for some metals, such as alloy 40CrNiMoA with Masing property, the cyclic hysteresis
energy changes with numbers of cycles and the controlled strain levels. When the control-
led strain ea < ε0, the changing ranges of cyclic hysteresis energy with numbers of cycles is
very large, conversely, when e a >e 0 , its change is small that it can be neglected.
From the recently experimental relation of cyclic hysteresis energy versus numbers of cy-
cles of alloy 40CrNiMoA, it can be found that cyclic hysteresis energy changes with
numbers of cycles, its changing rate is also associated with the controlled strain levels.
According to these facts, we can assume the cyclic hysteresis energy following the form:
AWp=AWpo(N)ß' (1)
Where: Δ Ψ ρ ο , β' are internal variances which are relative tothe controlled strain levels
and cyclic properties, N is numbers of cycles. Here we hypothesize the parameters Δ
W po and β' to follow the forms:
AW ^ = AW Je*'*"
ß'Jß/^-'*' (2)
 43
Where: A W p / , α,, β' and βλ are all material constants, function g(x) means: g(x) = 0
for x < 0 ; g(x) = x for x > 0 . ε0 is material constant associated with cyclic stability of
micro structure of metals, 8ais controlled strain level.
By the comparison of the experimentally measured results of total absorbed energy to
failure with cyclic hysteresis energy, we can find that the theoretical and test results are
quite different, the largest deviation is about 35%. As mentioning below, the conclusion
will be also verified by the results of numerical analysis of heat energy dissipation. This
shows that when the mechanical energy is transformed into the heat plane during fatigue
damage process, part of the energy will be dissipated simultaneously in the way of heat
exchanges with environment.

Heat Energy Dissipation In Fatigue

As we know that local cyclic hysteresis energy almost couldn't be estimated based on the
classical theory of mechanics of solid material, Moreover, it is difficult to learn how fa-
tigue damage is nucleated in a cycle in terms of cyclic hysteresis energy.
According to the numerical analysis of heat energy dissipation, we find that heat energy
dissipation changes with numbers of cycles. By means of introducing the concept of effi-
cient energy dissipative rate η, ie: the ratio of average cyclic stored energy Q r 5 t o cyclic
hysteresis energy Δ W p , the relation of efficient energy dissipative rate η with cycleratio β
(N / Nf) can be obtained as following form:
QTS
* = ^T=miß + m2 (3>
P

Where: m, and m 2 are material constants.

According to the analysis of heat energy dissipation of fatigue damage, we can also find
out the cyclic changes of heat energy dissipation of metals are associated with the control-
led strain levels, under the same cycle ratio, the higher the controlled strain levels are, the
larger its heat energy are dissipated( Tung et al., 1990 ). This indicates that fatigue dam-
age is associated with controlled strain levels. In the light of the relation of the deviation
of cyclic heat energy dissipation to controlled strain levels, the change of micro structure
of metals with numbers of cycles can be qualitatively determined. The cyclic changing
properties of microstructure of metals can also be reflected through using heat energy
dissipation as the describing parameter.

FATIGUE DAMAGE MODEL ON ENERGY DISSIPATION

There were two main shortcomings in usual fatigue damage models which are considera-
tion of the irreversibility on fatigue damage and the cycle-dependence of fatigue damage
respectively. Based on the study on mechanical and heat energy dissipation, the fatigue
damage process during cyclic loading has been redescribed as following:
(1) During cyclic loading process, the intrinsic microstructure deformation begins at
some local area and is reduced by the irrecoverable deforming work, then fatigue damage
is nucleated by the local distortion.
(2) The values of fatigue damage is proportional to the efficient energy dissipation
transformed from the deforming work of metals, ie: the cyclic fatigue damage of metals is
proportional to the efficient energy dissipation in the corresponding cycle.
(3) It is assumed the cycle-dependence of fatigue damage can be described by the
cyclic changing rule of cyclic hysteresis energy.
(4) When efficient irrecoverable energy is accumulated to reach itscorresponding to-
tal absorbed energy to failure, fatigue failure occurs, and fatigue damage D = D f .
(5) For convenience of deriving fatigue damage model, we assume that the initial fa-
tigue damage D 0 reduced by the microstructure of metals can be neglected, ie: D 0 = 0.
Acoording to above description on fatigue damage, we have:
44

+
D = JD0 N/Nf->0
(4)
Df N/Nf->\
J J
and
(5)
Where: W^denotes the total absorbed energy to failure. Here we let:

AW
(6)
n
fr
Then:
dD &Wp AW^ ,
= = (Wi/?+M } (7)
^ "'^7 "^T >
Integrating double sides of eqn.(7), we have:
£^W ™ /r-a + 1 B'+\ m
\ m
i
(8)
Where, Wf/ is material constant.

It can be found that ß' is in the range :

, here we assign β'τζβχ.

Now, let us discuss the relationship between this proposed model to the usual models:
(1) Assume that cyclic hysteresis energy isn't associated with controlled strain levels,
ie: ßf = 0, then we have:
D=-j^N1~aß(-^-ß + m2) (9)
From eqn. (9), it can be concluded that the rule of fatigue damage evolution is a
nonlinear function of cycle ratio, it not Inly depends on the cycle ratio, but also associates
with the properties of micro structure of metals.
(2) Furthermore, assume the cyclic heat energy dissipation is constant during cyclic
loading, then η = m 2 , we have:
AW
D—jp-e-Ny'ß-m, (10)
Eqn. (10) are similar to the well-known Halford—Morrow's model, which shows that the
usual fatigue damamge model can be considered as the special forms of this proposed
model.

ANALYSIS AND DISCUSSION ON FATIGUE DAMAGE

In order to compare this proposed model with the usual ones, the fatigue failure test of
double-notched specimens of alloy 40CrNiMoA with the theoretical concentration fac-
tor K t = 2.64 has been performed by using the condensed blocket spectrum( Nelson,
1977). The material constants of alloy 40CrNiMoA in this proposed model are deter-
mined from the cyclic properties of cyclic inelastic responses and cyclic hysteresis energy
and heat energy dissipation based on the fully reversed constant controlled strain fatigue
tests and the measurement of cyclic self-heating process. Table 1 lists the material con-
stants of alloy 40CrNiMoA.
 45
Table. 1
*0 wvv
«1 Pi h m, m2 wv α'
po
0.006 0.011 5.920 0.017 10.880 -0.48 1 533.87 0.327

Fig.l shows the cyclic rules of the evolution of fatigue damage estimated by this proposed
model and Halford-Morrow's one, it is found that the evoluting rule estimated by this
proposed model is nonlinear, with respect of the consideration of the irreversibility of

Fig.l
damage process and the cycle-dependence of fatigue damage, this proposed model is bet-
ter than Halford-Morrow's one.
Utilizing modified Brose's "effective factor Martix" method( Tung et al., 1988) for cyclic
stress strain simulation and equivalent energy analysis for local response estimation(
Tung et al., 1988); finally predicting fatigue lives. A computer program to predict fatigue
life for the notched members subjected to complex loading history has been worked out
in this paper. Fatigue lives have been predicted by the proposed damage model and sev-
eral usual fatigue damage models respectively.
Fig. 2 gives the comparison of fatigue lives predicted by the proposed damage model and
Landgrafs, Smith-Watson-Toppers and Halford-Morrow's models with the experi-
mentally measured results, it is shown that fatigue lives predicted by this proposed model
are better in agreement with the test results than by the others. Its scatter band is of
+15.9%—30.9%, with the decreasing of the maximum load in the loading spectrum, its
predicted fatigue life changes from over the test results into low its. From this figure, we
can also find that fatigue lives predicted by the other models are all over the test results,
their scatter bands are: Halford-Morrow's: +78.4%-+234.2%; Landgrafs:
+7.0%-+l57.6%; Smith-Watson-Topper's: +27.6%-+123.9%.

CONCLUSIONS

With respect of the consideration of the irreversibility of damage process and the
cycle-dependence of fatigue damage, this proposed model is better than Halford-Mor-
row's one.
According to the comparison of fatigue lives predicted by the proposed damage model
and several usual ones with the experimentally measured results, it is shown that fatigue
lives predicted by this proposed model are better in agreement with the test results than
by the others. With the decreasing of the maximum load in the loading spectrum, its pre-
dicted fatigue life changes from over the test results into low its.
46

a kf=2.44
*° / /
£ io3 #
*
•I » ^
cd
UH
Ό
10'
f ^Τ
<υ
o
"α>^ 101 k_ i - i j

VH 10l 102 103 104

Real Fatigue Life (NBL) Real Fatigue Life (NBL)
# — Halford—Morrow Δ — This proposed model
O — Landgraf A — Smith-Watson-Topper
Fig. 2

ACKNOWLEDGEMENT

The authors thank National Nature Science Foundation of China (NSFC) and
Aeronautic and Astronautic Science Foundation of China (AASFC). This work was
supported in part by whose auspices with contracts NSFC No. 19002017 and AASFC
No.90B53167.

REFERENCE

Kitagawa, H. (1990) Proc. of Fatigue^O , Hawii, pp45.

Plum tree, A. (1990) Proc. of Fatigue^O , Hawii, pp65.
Haigh, B.P. (1928) Trans. Faraday Soc. , Vol 24, ppl25.
Miner, M.A. (1945) J.Appl. Phys. Vol 16A, ppl59.
Morrow, J - D . (1965) ASTMSTP378,45.
Eyllin, F (1985) Trans ASME J. Pressure Vessel and Tech. Vol 107, No. 1, ppl 19.
Harig, H. and M. Webber (1986) HTM, Vol 41, No. 5, pp286.
Kliman, V. (1985) Inter. J. Fatigue , Vol 7, No. 1, pp39.
Polak, J. (1983)Maters. Sei. Engng., Vol 61,No. I,ppl95.
Glinka, G. (1985) Engng. Fract. Mechs., Vol 22, No. 5, pp839.
Morz, Z. (1983) Trans ASME J. Engng.Maters and Tech. ,Vol 105, No. 1, ppl 13.
Boisserie, H.T. (1983) Trans ASME J. Engng. Maters and Tech. ,Vol 105, No. I , p p l 5 5 .
Tung, X.Y.; D. J. Wang ang H. Xu (1989) Inter. J. Fatigue (1989) Vol 11, No. 5,pp353.
Tung, X.Y.; D. J. Wang ang H. Xu (1990) Proc. CMRS^O Beijing.
Tung, X.Y.; D. J. Wang ang H. Xu Acta Met. Sinica, (be accepted to publish).
Tung, X.Y.; D. J. Wang ang H. Xu (1991) Acta Met. Sinica, (will be published) Vol 27,
No. 2.
Nelson, D.V. (1977) Fatigue Under Complex Loading, Advanced in Engineering 6,
ppl 65.
Tung, X.Y.; D. J. Wang ang H. Xu (1988) Acta Met. Sinica, (in Chinese), Vol 9, No. 3.,
pp279
Tung, X.Y.; D. J. Wang ang H. Xu (1988) J. of Northeast Univ.,(in Chinese), Vol 9, No.
4,PP354
WS6a1

RECENT EVOLUTION OF GAS TURBINE MATERIALS AND

THE DEVELOPMENT OF MODELS FOR LIFE PREDICTION

M. McLEAN1, B.F. DYSON2 and R.N. GHOSH 3

department of Materials, Imperial College, London SW7 2AZ, UK

2
Division of Materials Metrology, National Physical Laboratory, Teddington, Middx TW11 OLW, UK
3
National Metallurgical Laboratory, Jamshedpur 831007, India

ABSTRACT

Important developments in materials for gas turbines are briefly reviewed. Effective use of such materials
is often limited by incomplete understanding of the material behaviour and deficiencies in representing
the relevant data. An approach to describing the creep behaviour of nickel-base superalloys in terms of
physical models of damage generation is outlined and comparisons of model-base predictions with
experimental data are made. Models for both isotropic and single-crystal superalloys are described.

KEYWORDS

Creep; modelling; superalloys; anisotropy; damage; single-crystal.

INTRODUCTION

The development of the gas turbine over the past fifty years or so has resulted from a combination of
improvements in engineering design, materials performance and manufacturing technology. This industry
has been particularly effective in identifying the materials characteristics limiting the efficiency, reliability
and lifetime of plant, and in promoting developments in materials technology to alleviate these problems
over a relatively short time scale.

The evolution of turbine blading materials for aero-engines has led to an average increase in temperature
capability of about 5 K^ear. Several reviews have detailed the historical development of these materials,
which are largely nickel-base superalloys, from the early y-reinforced wrought alloys (eg Nimonic 80A)
through the cast-alloy versions (IN 100, MarM200) to those with controlled textures and grain
morphologies produced by directional solidification (MarM002). Currently, the most advanced alloys
are designed to be used specifically in the single crystal form where relatively simple chemistries have been
identified (eg CMSX2, SRR99), eliminating the solute additions previously intended to strengthen grain
boundaries. This has decreased the melting range of the superalloys, allowing:

a) higher temperature heat treatments to control the γ' size and morphology more effectively,
b) higher γ' volume fractions to give increased creep strength, and
c) higher incipient melting points that allow increased operating temperatures.

By increasing the stresses and temperatures on turbine blades, there have been consequential demands on
the turbine disc alloys. Here the problem is not so much one of temperature capability, although the
operating temperatures have certainly risen significantly. Rather, because these components are very

49
50

highly stressed, nickel-base materials such as IN718 having high yield strengths have been developed. The
fracture toughness of such materials, which can be fabricated into components by either forging or powder
metallurgy routes, has become increasingly sensitive to the presence of small defects, such as inclusions.
Indeed, the predicted critical defect sizes for turbine disc alloys that are currently being developed
(-15 /xm) are significantly below the resolution of available NDT procedures. It is anticipated that quality
assurance of components produced from such alloys will rely on careful control of the manufacturing
process, rather than by post-production monitoring. There is growing interest both in establishing
appropriate specifications for superclean disc alloys and in developing appropriate procedures for
characterising the level of cleanness in relation to the projected service requirements.

Modern compressors are mostly manufactured from titanium alloys. In aero alloys, in particular, the
weight saving associated with replacement of nickel by titanium-based materials has been of particular
importance. As operating temperatures of gas turbines progressively rise, there are important
implications for the viability of performance of conventional titanium alloys which are unlikely to have
adequate strength at the projected operating temperatures of 750-800°C. It is for this application that
there has been such intense effort in developing structural intermetallics based on the titanium
aluminides, such as the Super «2 system. There remain considerable problems to be solved, particularly
in relation to the fracture toughness of intermetallics.

Most advanced materials have been developed in a semi-empirical manner to achieve certain target
properties, and they have been implemented very quickly and successfully in gas turbine technology.
However, application of these materials has generally preceded a clear understanding of the factors
governing their performance in service conditions. Modern analytical design procedures can only be
effective if there is an appropriate representation of the material properties and this generally is still not
available. This is particularly true in relation to the anisotropic properties of single crystal superalloys.
There is, therefore, considerable scope for improved performance through better design procedures based
on improved descriptions of material performance.

The remainder of this paper will be concerned with developments in the modelling of high temperature
deformation of superalloys for turbine blades, both in isotropic and anisotropic single crystal forms.
Through this, a procedure for representing the highly non-linear deformation behaviour at high
temperature has been established that has considerable advantages for both design purposes and for life
prediction.

MODELLING APPROACH

There have been two broad approaches to representing the shapes of creep curves, which are generally
non-linear in nickel-base superalloys. The first, and apparently most direct, is to describe strain as a
function of stress, temperature and time.

ε = ε(σ,Τ,ί) (1)

This can provide a good empirical description of constant stress and constant load data, but it is not
straightforward to extend the analysis to deal with more complex loading conditions such as multiaxiality
and material anisotropy. Even the prediction of behaviour under changing stresses and/or temperatures
requires additional assumptions to be made before Equation 1 can be used. The second approach
describes the creep rate ε in terms of a series of state variables (Sj, S^...) which represent controlling
aspects of the material structure and couples this with expressions representing the evolution of the state
variables.

e= f(cXShS2....)

έχ = g ^ T ^ S * . . . ) (2)

S 2 = h(a,T,S1,S2....)
 51
Although Equation set 2 is rather more cumbersome, and generally requires numerical analysis, it
provides a formalism that has the potential to relate quite directly to the underlying mechanisms
controlling deformation and fracture. Furthermore it provides a flexible framework that can be extended
to represent more complex loading conditions. The underlying problem is to identify the explicit forms of
the functions represented in Equation set 2 and to develop a formalism to evaluate the appropriate
constants by analysis of an available database.

ISOTROPIC MODEL

Nickel-base superalloys have a common characteristic of many engineering alloys for high temperature
service in that they exhibit creep behaviour that is dominated by a progressively increasing creep rate. The
discipline of continuum damage mechanics (CDM) has been developed by Kachanov (1958) and
subsequent workers to account for this type of behaviour in terms of an empirical representation of a
degradation of the material. This approach has been modified in a series of papers to reflect current
understanding of the physical mechanisms leading to changes in the strain rate; however, the constitutive
equations are framed in terms of engineering measurements rather than of the microstructural features
(eg dislocation density, particle size, cavity density). The early development has been reviewed by Dyson
(1990).

Ashby and Dyson (1984) have reviewed the detailed micromechanisms that can "damage" engineering
materials and lead to tertiary creep. For superalloys with an equiaxed grain structure, the most important
of these can be summarised as follows.

(i) Changes in material microstructure of which the density of mobile dislocations is the most
important. This mechanism derives from the observation of Dyson and McLean (1983) that creep
rate correlates with accumulated plastic strain; the current status of this model has been reviewed by
Dyson (1990).

(ii) Loss of internal load bearing section occurs by the development of cavities. This mechanism has
been considered in detail by Dyson and Gibbons for the case where cavity growth is constrained by
the creep rate of uncavitated material.

(iii) Loss of external section due to geometrical changes that occur during creep.

In addition a representation of primary creep in terms of an increasing internal stress S has been
introduced. Dyson and McLean (1990) have combined the effects of all of these terms to give the
following Equation set 3.

ε = έ|(1 - S)(l + w 3 ) exp (wx + w 2 )

S = HCJ(1 - S) - RS

w j = ηέ (3)

w 3 = C£

The initial creep rate b[ is represented as a function of stress σ and temperature T by the conventional
power law equation,

n
-p (£) <«>
where k[0,a0 are normalising constants; the stress exponent n and the activation energy Q represent the
52
stress and temperature dependences respectively. h[ is modified by changing values of the dimensionless
state variables (S, wj, W2, W3) which have the following origins:

a) S is an internal stress associated with material heterogeneity that increases with a hardening
coefficient H but is limited by material recovery represented by R.

b) wj is due to loss of external section, which for axial creep testing with constant load is related to the
change in testpiece cross-section A, ie wj = n ln(Aj/A) = ηε.

c) W2 is associated with loss of effective internal cross-section due to creep-constrained cavitation and
is sensitive to the fracture strain £f.

d) W3 results from a progressive increase in mobile dislocation density p which increases the creep rate
of Class I solid solution alloys or particle strengthened alloys through the well known Orowan
equation: k = pbv, where b is the Burger's vector and v is the dislocation velocity. In the present
formalism W3 = (p - PJ)/PJ where pj is the initial dislocation density.

Not all of the mechanisms described above will occur in every test condition or for superalloys of every
microstructural form. For example, in constant stress tests wj = 0 and in high ductility materials where
cavitation is not a problem W2 = 0 (eg in directionally solidified superalloys). However, generally the set

of parameters (q, H, R, C, n, ef) completely defines the creep behaviour in terms of Equation set 3.

A procedure, implemented in a software package designated CRISPEN, has been developed to evaluate
the optimum values of the model parameters by analysis of creep curves. The procedure has been
described in some detail by Dyson and McLean (1990). A database of creep curves can, therefore, be
transformed into a database of model parameters from which predictions can be made for arbitrary
loading conditions, including changing stresses and/or temperatures, by interpolation or limited
extrapolation of the model parameter database.

Figure 1 shows a typical example of the optimum fit of the Equation set 3 to a set of creep data. This,
however, is not a good test of the model since many 4-parameter equations, whether empirical or
physically based, can give an equally good fit. Of more importance is the comparison of measured data
with predictions from a limited database. Two comparisons of measurement and prediction are given in
Figures 2 and 3. In Figure 2, a creep curve prediction of the superalloy IN738LC is in close agreement
with the data, particularly when bearing in mind the scatter associated with creep measurements. Figure 3
makes a broader comparison showing the measured and calculated times to achieve strains of 10% for the
single crystal superalloy SRR99 with [100] axial loading. The agreement is, again, within the scatter of the
creep data.

Extension to predict the creep strain associated with cyclic stresses from a constant stress database for
SRR 99 is shown in Figure 4 and this prediction is also close to the measured data.

ANISOTROPIC MODEL

The creep behaviour in single crystal superalloys is sensitive to crystal orientation, and this orientation
dependence has been shown to be dependent on the alloy, stress and temperature (eg MacKay and Maier
(1982), Caron et al. (1988)). The analysis described above has recently been extended by Ghosh et al.
(1990) to account for such crystallographic effects. The principal assumptions of this new analysis which
is based on interpretation of available microstructural studies are as follows.

a) Failure does not occur by development of creep cavities but by a geometrical instability.
Consequently W2 = 0.
 53

SRR99 Single crystal superalloy

Exponential model
750MPa.750*C

1000
Time(h)

Fig. 1. Fit of Equation set 3 to a creep curve for SRR99 tested at

750MPa/750°C

- 1 i ; j -
IN738 LC.directionally solidified
170 M P a . 8 5 0 MPa

Predicted creep behaviour Ί / /

(reference curve 3 0 0 M P a . 8 5 0 e C _ | \ ^ /
□ Experimental data
/a jf
/ G /
/ o /
- / ° /

^^ -
ur*-rrrflOOßß°°^ i _J

Fig. 2. Comparison of measured data for a long term creep test on IN738LC
(170 MPa, 850°C) with predictions made from short term data assuming a
10% uncertainty in extrapolation
54

10000
SRR99. Single crystal superalloy

; iooo
^ '
; loo Ä*r
ί •*r
j 10 κ * ° * ^ • 750eC D900eC
+ 800°C * 950"C
* 850*C O 1000eC
1
1 100 1000
Measured time(h)

Fig. 3. Comparison of measured and calculated creep rupture lives

for all test conditions available for SRR99

Fig. 4. Comparison of the measured creep curve for cyclic stressing of SRR99
with the calculated curve based on a constant stress database
 55

SRR99 4 5 0 Μ Ρα 8 5 0 °C <001> SRR99 3 0 0 M Pa 950°C

D Shear D < ώ3 52 7^>

— E x p e r i m e n t ed 0 < 1 3 4 >
v Tensile
X < 2 3 10>
e x p e r i m e n t al

Fig. 5. Comparison of the fits for tensile and shear Fig. 6. Calculated and measured creep curves
formulations of the model to an experimental for complex orientations of SRR99
creep curve for SRR99 with <001> tensile tested at 300 MPa/950°C
orientation at 450 MPa/850°C

O r i e n t a t i o n change

to reach a strain of 10'

a 5O0-75Oh
SRR99 O 7 5 0 - 1 0 0 0h
X 1000-1200h
Temp 850°C + 1200-1500h
v 1500-1750h
S t r e s s 350MPa Δ 1750-20O0h

|111( <T01> + |001{ <110>

Fig. 7. Predicted rotations for SRR99 with < 1 2 3 > Fig. 8. Calculated anisotropy of creep
tensile orientation tested at 850°C with performance for SRR99 at 400 MPA/
various stresses between 350 and 500 MPa 850°C displayed as contours of time
to achieve 10% strain
56
b) Deformation occurs on two well defined slip systems {111}<101> and {001}<110>. The relative
preponderance of octahedral and cube slip is a function of stress and temperature.

Equation set 3 has been re-expressed in terms of the shear stresses and shear strains associated with the
active slip systems. All the possible shear displacements are summed to account for the tensile strain. If
7 k is the magnitude of the shear strain on the k-th slip system represented by (n^k η^ η^) [b^k b^
b^\ where nj k and bj k are the components of unit vectors defining the slip plane and slip direction
respectively, the resulting displacement gradient component ε^ is given by

e. k _ *yktj.kn.k (5)

The suffixes i,j take values 1, 2 or 3 representing the components along cube axes and £jjk is the
contribution from a single slip system k. If simultaneous slip is possible on N slip systems, then the total
displacement gradient eji is given by the summation

N
£ e
k
ij- Σ ij
k=l

This small displacement, in general, leads to both a strain and rotation of the original tensile axis [t^ t2 tß]
to a new orientation [Tj T2 T3]. This can be represented by the matrix transformations

1+εη ε2\ £31

ε 1+ε ε
12 22 32 (5)
ε ε 1+ε
13 23 33

The axial strain ε is determined from the difference in magnitude of the two orientation vectors

_T-t
(6)

Following the same reasoning used to derive the tensile creep equation, shear creep equations have been
developed for each allowed slip system using a damage parameter w^ that again represents a growth in the
density of mobile dislocations. (Here we ignore primary creep.)

(γ* = 7 i k(l+wk)) (Ό

(w k = jS k 7 k )

ej k , |Sk are the model parameters and there are different values for each slip system.

Ghosh et al (1990) have described in detail how the model parameters are derived from a set of creep
curves for [100] and [111] orientations; this will not be repeated here. Figure 5 shows that the tensile and
shear formulations make identical representations of the creep curve for a [100] orientation which is not
subject to rotations. This is because the calculation for this situation are alternative formulations of the
same model.

Having established a model database in a similar way to that described for the isotropic model, the creep
behaviour for arbitrary crystal orientations can be calculated. Examples of such calculations are shown in
 57
Figure 6. For the particular data analyses for the alloy SRR99, the crystal rotations predicted can be very
sensitive to stress as is shown in Figure 7.

With this procedure, it is now possible to map the predicted creep performance for all possible
orientations either in terms of the strain accumulated in a given time or as the time to reach a specified
strain (Figure 8).

SUMMARY

If design methods incorporating sophisticated computational procedures, such as finite element analyses,
are to be developed then there must be a parallel evolution of methods for representing the relevant
material behaviour in order to make reliable prediction of material life under service conditions. The
above analysis outlines an approach that relates to the creep performance with particular relevance to
superalloys. However, in its present form the work is incomplete since it refers to uniaxial stress
controlled loading although it does not neglect the possibility of environmental interactions, the
important advantage of the approach of relating strain rate to state variables, is that it is possible to
modify the equations to incorporate other features that dominate certain circumstances. The scope of the
present presentation does not allow all of the current developments of this type of model to be
comprehensively reviewed. However, currently in our three laboratories we are addressing a range of
different phenomena that can modify the rate of deformation. These including the following

a) oxidation/corrosion leading to changes in load-bearing section;

b) multi-axial stresss states;

c) generalised loading including stress-control, strain-control, stress relaxation and through-zero

fatigue loading;

d) anisotropic dimensional changes due to anisotropic deformation.

To complement this type of modelling activity, experimental programmes are in progress to allow
validation of some of the predictions.

REFERENCES

Kachanov, L.M. (1958). Izv. Akad. Nauk. SSSR, 26,8,26.

Ashby, M.F. and Dyson, B.F. (1984). Advances in Fracture Research (S.R. Valluri et al., Eds) Pergamon
Press, 1,3.
Ion, J.C., Barbosa, A., Ashby, M.F., Dyson, B.F. and McLean, M. (April 1986). The modelling of creep
for engineering design, DMA A115.
Dyson, B.F. and Gibbons, T.B. (1987). Acta Metall., 35,2355.
McLean, M. (1989). Materials and Engineering Design: The Next Decade (B.F. Dyson and
D.R. Hayhurst, Eds), Institute of Metals, London, 287.
Dyson, B.F. and Osgerby, S. ibid, 373.
Dyson, B.F. and McLean, M. (1983). Acta Metall., 31,17.
Dyson, B.F. (1990). Modelling of Material Behaviour and Design (J.D.Embury and A.W. Thompson,
Eds), TMS, Warrendale, Pa., 59.
Dyson, B.F. and McLean, M. (1990). ISIJ International, 30,10,802.
Barbosa, A., Taylor, N.G., Ashby, M.F., Dyson, B.F. and McLean, M. (1988). Proc. 6th Int. Conf. on
Superalloys, Seven Springs, Pa.
MacKay, R.A. and Maier, R.D. (1982). Metall. Trans., 13A, 1747.
Caron, P., Ohta, Y., Nakagawa, Y.G. and Khan, T. (1988). In Superalloys 1988 (D.N. Duhl et al, Eds.),
Metall. Soc, Warrendale, Pa., 215.
Ghosh, R.N., Curtis, R.V. and McLean, M. (1990). Acta metall. mater., 38,10,1977.
WS6a2

LIFE ANALYSIS OF A GAS TURBINE FAN DISC

Tarun Goswami
Department of Materials Engineering
University of Wollongong
POBox 1144 NSW 2500 AUSTRALIA.

ABSTRACT
A fan disc was analysed for life from various laboratory data. A laboratory testing programme
was planned to generate material data at the representative working conditions of a fan disc.
The life analysis was made within the framework of a safe life design, that determines the life
prior to the onset of a crack. A safe crack propagation life was also analysed by carrying out a
number of crack growth studies over a set of material conditions. A safe life, that includes
initiation and a propagation phases of a crack, has been derived to be 4100 flying hours, based
on this analysis and the limiting conditions.

KEY WORDS

Fan disc, safe life, crack initiation, crack propagation, mission profile, gas turbine, fatigue.

ENmiODUCTION

The operating condition for a military gas turbine engine is very complex. The individual
components are loaded severely in cold and hot section. Hot section components accrue distress
by low cycle fatigue, thermal fatigue and oxidation and are not within the scope of this paper. A
fan disc, which is a cold section component, has been analysed with the assumption that,
operating conditions are near ambient. Figure. 1, shows a gas turbine and fig.2,a fan disc.

Fig. 1. A gas turbine. Fig.2. A fan disc.

59
60

Until recently the design philosophy followed a safe life criterion. There are several aircrafts and
the engines, retired prematurely, following the above concept. These aging aircrafts have a
potential for further usage if returned to service (RTS). The growing economic interests to using
the useful life of these critical components are dealt within the retirement for the cause philosophy
(RFC) (Annis et al,1987).

While following the "RFC, and the damage tolerant design concepts, (Mil. Stand. 1783, 1984),
a component life consists of a safe life prior to the onset of a crack and a safe crack propagation
life. Fan disc analysis was made within the linear elastic regime where, crack growth rate was
correlated with ΔΚ as shown in fig.3. The mechanics of this curve follows a below - threshold
growth, slow propagation and a power law propagation that leads to the unstable crack growth
and failure. The physics and mechanics of the crack growth in the above stages is an area of
current research (Thompson et al,1987).

Macrocrack growth data

| | log ΔΚ
I AK thr for large crocks
AK t h rfor microcrocks

Fig. 4. Crack detection and Component 's

Fig. 3. Phases of crack propagation. return to service or retire.
The 'RTS' requires a reliable crack detection capability and an advance 'non destructive testing'
(NDT) certification. On each inspection, the individual component is examined for a crack. On
crack detection, the severity of the crack is studied with a viable crack growth law statistically and
the component is either 'returned' or 'retired'. Figure 4, shows the inspection interval for
crack growth for a gas turbine component and subsequent return for further usage.

FAN DISC

A fan disc is an important component of a gas turbine mainly because it is susceptible to foreign
body ingestion, such as bird-hits,dust and unspecified particles. The fan disc design requires
complete structural integrity of the disc and blade assembly. The failure of blade and fasteners
such as bolts are designed to be contained however, the energy of a rotating disc is too high to be
contained. Stress analysis for a fan disc was carried out within the linear elastic considerations
with a finite element package, by employing 200 elements in the disc cross section as shown in
fig.5. The design limit of 0.2% proof stress was allowed at the disc hub. Mesh generation and
stress analysis of a fan disc is dealt else where (Goswami, 1991).

EXPERIMENTAL

The following experimental route was planned for a fan disc life analysis.
Table-1. Summary of mechanical properties of a fan disc material
(TI6A14V).
 61

Material Heat treatment 0.2%oys au KIC %el %RA grain

Ti6A14V Mpa Mpa Mpa m 1 / 2 25 mm diaμm
Rolled STOA 1000 1175 80 13 32 8-10
Forged STOA 900 980 75 15 42 15

Table -2. Summary of test programme and parameters.

Testing Material Testing type Relationship Temperature Frequency R ratio Remarks

°C Hz
HCF hot rolled push-pull S-N 26 30 -lto.75 [email protected]
LCF forged push-pull et-Nf 26 0.33 -1
Crack
growth Forged push pull da/dN vs ΔΚ 26 35 0.1
Full
scale Forged spin pit 0-max-0 26-40 183.33 0 fan disc |

RESULTS
High Cvcle Fatigue

The traditional S-N approach to the fatigue analysis of a fan disc was carried out at different R
ratios to imbed mean stress effects of a random profile. The constant life curves were generated
at 10 ,10 5 and 10' cycles and has been dealt else where (Goswami, 1990). The results of the
S-N diagram is shown in fig.6 at varying R ratio of -1 to 0.75 at the R ratio interval of 0.25.

-ΛΖΟΟ -600 £00

Fig. 5. Cross section of a fan disc (not to

the scale). Fig. 6. Constant life diagram.

Low Cycle Fatigue

Several tests were carried out under total strain control conditions. The results of strain range
(Aet) versus cyclic life (Nf) relationship was represented in the Manson-Coffin relationship. A
and B were the elastic and plastic line intercepts and a and b were their slopes respectively

Aet /2 = A (2Nf)a + B (2N f )' (1)

62
Constitutive equation used above extrapolates the life at longer range with lower strain range
combinations. The cyclic stress-strain relationship was represented in the following equation.
Where K,cyclic strength coefficient and n is the strain hardening exponent.

Δσ/2 = K (Δερ) η (2)

Various constants of the above equations are presented in table 4. and in fig.7.
Table.3. Constants in the constitutive equations.

A -a B -b KMpa n Temperature °C
0.0303 0.09 0.8582 0.75 2210 0.14 26 |
Crack Growth
The compact tension specimens of the dimensions {thickness=10,width = 50 and a/W=0.2}
were machined form a disc forging in the rim radial direction to simulate a condition of rim radial
growth. A pair of specimens were studied for a set of heat treatment conditions out lined below.
Table-4. Summary of heat treatment cycles.

Condition Heat Treatment 1

Recrystalization Anneal 1200K/4Hr/cool@50K/hr to 1035 /AC

15%Primary α(15%α ) 1225 K/lHr/AC + 975K/2Hr/AC
50% Primary a. 1145K/2HT/AC+ 975K/2Hr/AC
Beta quench 1310K/30min./WQ+975K/2Hr/AC
Beta Anneal 975K/2Hr/AC
Solution Treatment and age 1225/lHr/WQ+865K/4Hr/AC
[Solution Treatment and overage 1225/1 Hr/WQ+865K/24Hr/AC 1

Crack growth studies were carried out at room temperature at 35 Hz with R ratio of 0.1. The
constant amplitude testing was carried out with the pre-cracking amplitude of ΔΚ, 14 Mpa
m 1/2 , however, the ΔΡ was reduced at a/W ratio = 0.29, sufficiently less than the starting crack
propagation stress intensity range of 18 Mpa m 1/2 . This material exhibited a bilinear crack
growth behaviour, because of structure sensitivity. An effective power law regime for the
crack propagation studies ranged from 18-22 Mpa m 1/2 The stress intensity range was
calculated in accordance with ASTM E 647-81.

ΔΚ= P(2+cc)/BW 1 / 2 (l-a) 3 / 2 [ 0.886+4.6a -13.32a 2 +14.72a 3 -5.6 a 4 ]

where, a = a/W at a/W > 0.2. (3)

Crack growth in terms of caliberation equation of (Saxena et al 1978) was employed for clip
gage data as follows,

a/W= 1.000 - 4.6695 U + 18.460 U 2 - 236.82 U 3 + 1214.9 U 4 - 2143.6U5

where, U = l/{ EB(CMOD)/P} 1/2 + 1 (4)

 63
The cyclic crack growth rate was monitored optically and also by using a clip gauge. Equation
(4) (Saxena et al, 1978), was used to fit the data from the clip gage to get the cyclic crack
growth rate. Figure.8, shows the crack growth rate data with respect to stress intensity range for
various material conditions. The data points were joined by a least square fit method and the
crack growth rate was represented in an effective Paris equation tabulated below for a STOA and
STA condition, other parameters were dealt else where( Goswami, 1991).
1-1. 10 - 2 .

♦* | • ■

J 10-3J
♦
/ ■
E
A STA
E ♦ MA
jr'· ■■' BA
■ ♦ RA
E ♦ total strain *. ■ BD

♦ elastic strain
o plastic strain
10"
10 - 3 . 100
10 10* 10° 10 4 10

cycles to failure Δ K Mpa/n

Fig. 7. Total strain range versus cycles to Fig. 8. Crack growth data for a fan disc
failure. material.
Table 5. Constants of the crack growth law.

Material Heat Treatment c m Remarks |

STOA 9.4 * 10~8 2.6 at the effective power law regime
with AK>23Mpa m 1 / 2 .
STA 6.3* 10"9 3.46 Paris Equation, da/dN = C (AK) m

Component Testing

A fan disc component was rig tested in a spin pit facility as shown in fig,9. The employed
waveform was 0-max-0, that simulates a take-off - landing excursion. The disc was withdrawn
from further testing at 40,60,90 and 100 thousand cycles. A Non Destructive Testing was
carried out to detect a crack however, no crack was found to have initiated. It was concluded that
the disc has reached its life in the initiation stage.

Fig. 9. Spin pit facility. Fig. 10. A candidate mission profile.

64
DISCUSSION

Safe Life.

An exact definition of the onset of a crack for the disc components is much in controversy.
However, there have been approaches dealing with this within the damage mechanics(Chaboche
1987). A paper dealing with the several assumptions for disc initiation life has been carried out
else where (Goswami, 1991).

In order to determine a fan disc life prior to initiation from the above generated data requires the
knowledge of the engine mission profile. A candidate mission profile was generated at the disc
hub as shown in fig. 10. There has been an international effort to standardize the mission profile,
its discretization interms of rig cycles, to device a component testing route for life analysis (Mom
et al, 1985). TURBISTAN has been in use to deal with the mission analysis and is shown in
fig. 11 (Mometal, 1985) »<«n no<« i
nr« tiMM nor«

' CKlKtl HI
i n» M#«I«WUV«···«
! Ml
M I I UI J
I II 1» U « l | i "t 1*1

_
\/4
1 ,_S^— ^-~
wMI —
f
i » M i ir
tnci«<

\f^\

,ν-ΛΑ :«utj» CMJltü C»U'1I ΙΛ*Οΐ"β L I—\r-i j

1
. — UM» )
lind** m ΛΓ (NOIf f 1IIWI00V»«!

Fig. ll.TURBISTAN'mission cycle

(Mometal 1985).
A preliminary analysis of the mission as shown in fig. 10, was carried out for a fan disc
(Goswami, 1989). Specimen and component data were correlated to determine a scaling factor
as shown in fig, 12. Total rig cyclic data were scaled down with the derived scaling factor of 75,
that fixes the limit for safe life of 2600 flying hours. Each mission and severity was assumed
critical with 75 excursions crossing 70% design load limit.
Safe Crack Propagation Life.

Previous study made in this area, (Jones 1972), describes the overloading effects. A crack
relaxation was found for the following 8000 constant amplitude cycles with the application of a
single overload with an overloading factor of 1.2. The random waveform effects of a mission
profile have been incorporated in TURBISTAN program. Fig. 13, shows the modelling of
constant amplitude data in terms of random waveform such as TURBISTAN (Mom et al,1985).
1400 -i da/df (m/flight)
Full Scale data
1300 A
Fv534
1200 H
(Uncracked) Full Scale data
1100 H
Ti6AI4V
1000
900 ■] R=0
800-J
Q. 2 700 A Smooth uniaxial data

600 A
500 A
400 4
10« 10c
Cyclic life
Fig. 13. Modelling of compact specimen
Fig. 12. Component and specimen data data under TURBISTAN profile
correlation. (Mometal 1985).
 65
At the end of the safe lifing, the component was assumed to have initiated a crack of 0.13mm
(Annis et al,1987), though the exact size is in question, we assume an initiation effect causes a
crack of 0.13mm. The component stress intensity factor ranges from 30-35 Mpa m i/ ^bearing
the above assumed crack size the remaining life for the disc component is to grow an initiated
crack to a critical size of 0.8mm. A flight cycle has 5-6 manouevering excursions, together with
a safety factor we arrive at a safe crack propagation life of another 1500 flying hours.

CONCLUSION
A safe lifing was carried out for a gas turbine fan disc with the application of various data
generated in laboratory. 2600 flying hours have been analysed based on safe life design
concepts.

A safe crack propagation life of a fan disc component has been analysed based on the Paris
equation representative of flight by flight cycle that yields 1500 flying hours.
ACKNOWLEDGMENT

The author acknowledges Mr. A. Prasad, Mr. R. Padmanabhan and Dr. K.Ramchandra for all
the support in the Gas Turbine Research Establishment Bangalore India. The support from Prof.
W. J.Plumbridge is highly acknowledged.
REFFERENCES.
Annis,C.G. jr, Mills,M.S, and Harris,J. A. (1987) 'Engine component retirement for the cause
Vol.2, Life assessment -system development report AFWAL -TR -87. 4069.
ASTM E647-1981, 'standard test method for constant load amplitude fatigue crack growth above
10"8m/cycle' Annual book of ASTM standards Part 10. ASTM Philadelphia PA.
Chaboche, J.L. (1987)'Fracture mechanics and damage mechanics complementarity of
approaches' Proc. of Int. Conf. on numerical methods in fracture mechanics. San Antonio
Texas USA.
Goswami,T.(1989) 'Discretization of an engine mission profile in terms of O-max-0 equivalent
cycles'Australian Aeronautical Conference Melbourne.
Goswami, T.(1990) 'Material aspects in the life prediction of gas turbine components' TMS Out
standing student paper in the physical and mechanical metallurgy division.
Goswami,T.(1991) 'Disc initiation life - a few assumptions' Poster session in the 6th IntConf.
Mechanical behaviour of materials Kyoto Japan.
Goswami, T. (1991) 'Fatigue and life prediction of high temperature components'(Ph.D. thesis
at the University of Wollongong)
Military Standard. 1783. U.S. Air Force (1984^ 'Engine Structural integrity programme'.
Mom AJ.A, Evans,W.J, and Ten Have A.A (1985) ' TURBISTAN a standard load sequence
for aircraft engine discs' AGARD CP 393.
PinderaJ.T and Kransowski, B.R, (1984) 'Crack tip modelling' Canadian fracture conference,
Kluwer Acedemic publishers.
Saxena,A, and Hudak SJ.KJr.(1978) 'Review and extension of compliance informations for
common crack growth specimens. Int. Jr. Fracture . 14.
WS6a3
EVALUATION OF METALLURGICAL DEGRADATION
ON GAS TURBINE COMPONENTS

Y.YOSHIOKA, D.SAITO, K.FUKUDA, K.FUJIYAMA, N.OKABE

Heavy Apparatus Engineering Laboratory

Y.ABURATANI
Turbine and New Energy Development Department

Toshiba Corporation
2-4 Suehiro-cho, Tsurumi-ku, Yokohama, 230, Japan

ABSTRACT

To extend the life economically and reliably, the life exhaustion and refur-
bishment concepts in each hot gas path component of gas turbines were estab-
lished. In the natural gas fired base-load operation, creep- and oxidation-
life are primarily determinant to the first-stage buckets. Coating life
should also be taken into consideration to determine the oxidation life and
refurbishment time due to the life less than the mechanical life of the
underlying bucket material.

To the transition pieces, creep deflection is important especially in the

case of the material Hastelloy X as well as it is important to the first-
stage buckets. Metallurgical methods to estimate the mechanical properties
were developed.

KEYWORDS

Gas Turbine; Bucket; Creep; Coating; Refurbishment; Oxidation; Deflection;

IN738LC; Hastelloy X; Degradation; Transition piece

INTRODUCTION

A trend toward use of gas turbines are recently increasing in Japan due to
the quick starting time, shorter installation period, and moreover the high
efficiency as a usage of combined-cycle power plant. In accordance with
the increase of operating experiences, the extension of refurbishment and
replacement life of the hot gas components are being claimed from the users.
That is , in turn, increase of the needs for accurate life-assessment tech-
niques. This paper presents the concepts of the bucket life exhaustion
mechanism and one of the methods to assess the life from the metallurgical
observations which was developed to assess the amount of creep deflection on
transition pieces.

CONCEPT OF THE BUCKETS LIFE EXHAUSTION

67
68
The buckets does not permit a crack, then crack initiation is life-determi-
nant. Figure 1 shows the model of crack initiation mechanism. In the natural
gas fired base load operated machines, creep damage seems to be predominant
rather than fatigue even if creep damage enhanced fatigue crack initiations.
Creep crack initiation life should be, therefore, assessed. Creep cracks
will be started at the onset of tertiary stage of creep in the bucket mate-
rial IN738LC, that is around 0.5% strain or more. At greater than the value,
grain boundary cracks begin to form, but the probability is statistically
the lower region of IN738LC's data scatter band (H.L.Bernstein,1990). When
we assess the bucket life, structural changes should be taken into consider-
ations. The structural changes mean both the reduction in effective cross-
section of the buckets due to oxidation and the degradation of the bucket
material during the operations even though refurbishment heat treatment are
performed.

To prevent the oxidation, first-stage buckets are coated. But the coating
life is shorter than the creep life of the buckets. Recoating is therefore
applied before the underlying material is oxidized. In the coating life,
operating temperature, which is related to the depletion rate of Al content
at the surface, is life-determinant. In mainly lower temperature portions of
the bucket blade, coating layer suffered cracks probably due to less ductil-
ity to endure thermal strain at the stops of normal cycles and the trips.
But the cracks are closed due to the stress of compression applied at the
surface during the operations. Therefore, the hottest portion which is 40 to
50% of the bucket blade length from the tip, is critical for the coating
life.

Fig.l. First-stage coated buckets life exhaustion model

in natural gas fired base load operation.
 69
Coating life is influenced by the operating conditions, fuel and site.
Therefore field experiences of the fleet machine is important. Before con-
suming the coating life and suffering the base metal oxidation, refurbish-
ment of the coating layer are performed to attain the full design life of
the buckets. Subsequent to stripping off the coating and locally attacked
portions, applied are conven- _
tional heat treatment which
consists solutioning and
aging. This treatment seems
not to fully refurbish the
material because the solution
temperature is lower than the
r1 solvus temperature of
IN738LC. The surface of base
metal is also deteriorated,
which influences the degree of
restoration of the material
and coating performance.

Figure 2 illustrates wear-life

consumption and maintenance
time model of the first-stage 0 t1 t2 t5
buckets. To make a maintenance Service hours (h )
optimization schedule gives Fig.2. First-stage buckets wear-life
the buckets maximum life which consumption and maintenance
is closing to the design life. time model.

METALLURGICAL ESTIMATION OF MECHANICAL PROPERTIES

As well as creep strain life is important for the first-stage buckets, creep
deflection is important for the transition pieces which are subjected to
inner panel creep deflection during service. So, development of a creep
crack initiation life estimation method for the first-stage buckets material
IN738LC and a creep deflection estimation method for the transition pieces
material Hastelloy X non-destructively are required. Quantitative evaluation
of microstructure related to the mechanical properties was performed by
using the image analyzer and development of hardness, tensile strength,
yield strength, and creep strength estimation method from the microstructure
of Hastelloy X were established.

TEST PROCEDURE

AMS specified Hastelloy X material (AMS55365) were used. The composition of

the material served are as follows (wt%);
C :0.06 , Si: 0.4 , Mn:0.7 , S:<0.01 , Cr:22.3 , W:0.6 , P:0.01
Corl.O , Fe:17.4 , Nirbalance

After the specified heat-treatments, which were solution-heated at 1150°C

for an hour and then cooled in water, were applied, the materials were aged
at 750°, 800°, 850°, 900°C up to 104 hours in the air. Test samples were ma-
chined out of the materials which were in as-heat-treated and aged condi-
tions and served for microstructural observations, Vickers hardness tests,
tensile tests, and creep rupture tests.

RESULTS
70
Figure 3 shows the behaviors of microstructure during the agings. No precip-
itates except some primary carbides M Ö C were observed in the as-heat-treated
condition. Carbides such as M6C,Mi2C and M23C6, were precipitated

Virgin 850°C/103h 850°C/104h 800°C/104h 900°C/10*h

Fig. 3 Metallurgical changes due to the agings (aging temp./time).

and M12C changed to μ phase

during the agings.The size and 5 |750^C Aging| 1800t Aging[ |850°C Aging| [900οΟ Aging|
number of precipitates in- ?ί ϋ ^ 1000
creased and coverage of the " | 900h
precipitates to the grain = ~ 80ol·-
boundary also increased as !
aging time and
•cT
700
600
temperature > ? 2 400
rffTTI rfTTI m m
increased. 8 1 5 500
0 «· 200
40
Figure 4 shows the behaviors
of mechanical properties at
oas 20l·
0 ΓΗ-. cm. tim
room temperature. Tensile <55• ~ 40
nm
60

strength, 0.2% strength, and «</»^ 200

hardness increased up to 103 ί «ς 250
hours and after then they ■· S■ *§ ~! 200
150l
decreased. The behaviors were 0 1 3 6x10* 0 1 3 610x10 s 0 1 3 6x10 s 0 1 3 610X105 (hours)

similar to those of the pre-

cipitates. The elongation and Fig.4. The behaviors of mechanical properties
reduction of area were at room temperature during the agings.
decreased coincidentally. c
a; |750°C Aging] foot Aging| |850t Aging||9ÖÖ C Aging]

Creep rupture properties at

m Im Iki
BÖ 40
850°C are shown in Fig.5.
Rupture life decreased and the h£L Test condition
850 °C
ductilities and minimum creep 5g 60 [ -,-n J T i J"h J > n 78.5 M Pa
rate increased during the
agings, even though the number E 5g 60 -j-n _m -ΓΤΤΊ
of precipitates increased.
ΓΓΠ ΓΓΠ d d l j=a

^mn fb rh
3 OJ^ 500
%~5 400
K
DISCUSSIONS 300 Test condition
?^ 60 850 °C

Estimation for the hardness,

n Ml HtL 49MPa
<Q 6°
tensile, yield strength, creep F «r © 40 -ΗΊ n a
deflection, and rupture life l ^τπ ,-Π Π ,-ΓΠ
were developed. Hardness, ten- J p g 8:
8
0 3 6X105 0 3 6 10x10s 0 3 10x10s 0 3 6 10x10s (hours)
sile, and yield strength are
closely correlated with preci- Fig.5. The behaviors of creep rupture pro-
pitates which play a role to perties at 850°C during the agings.
 71
interrupt movement of dislocations.
In the results obtained, they were
closely correlated with the number
of precipitates as shown in Fig.6,
7, and 8. The equations are as
follows;

HV = 179.7 + 0.0009433 * N — ( 1 )
TS = 756.2 + 0.001588 * N — ( 2 )
0.2%YS = 292.6 + 0.001279 * N
—-(3)
20000 40000 60000 80000
NrNumber of precipitates per Number of precipitations (i/mm 2 )
unit area ( 1/mm2)
HV:Vickers hardness Fig.6 Correlation between Vickers
TS:Tensile strength (MPa) hardness and number of
YS:Yield strength (MPa) precipitates.

2 900

20000 40000 60000 80000 20000 40000 60000 80000

Number of precipitations d / m m 2 ) Number of precipitations (1/tnm 2)

Fig.7. Correlation between Tensile Fig.8. Correlation between 0.2% yield

strength and number of strength and number of
precipitates. precipitates.

Creep deflection rate are correlated with grain boundary coverage ratio of
precipitates inversely (Matsuo et al., 1987) and the volume fraction of
intragranular precipitates directly. The equations of minimum creep rate at
the test conditions of 850°C/49MPa and 78.5MPa are as follows;

CR(850,8)=(1-θ)[{3.82*109*exp(-250321/RT)}(V-0.306)2+0.439 (4)
CR(850,5)=(1-0)[{8.92*108*exp(-257541/RT)}(V-0.306)2+0.0260 (5)
CR(850,8):Minimum creep rate at test condition of 850°C,78.5MPa
CR(850,5):Minimum creep rate at test condition of 850°C,49MPa
Θ:Grain boundary coverage ratio, T:Absolute temperature (K)
R:Gas constant (J/mol,K), V:Volume fraction (%)

Figure 9 shows the correlations between the actual values and calculated
values. Good correlations between them were obtained.

The creep rupture life were also estimated from the calculated minimum creep
rates by using the Monkham-Grant equation. The equation are as follows;

tr=184.6 * CR-0.2503 (6)

tr:creep rupture life
CR:creep rate (%/h)

The relationships between calculated and measured rupture life are shown in
Fig.10. Rather large scatter band was observed.
72

^+5tr . / 1.4
Test condition Test condition
,+$σ s'
850 c €/78.5MPa
E| · 0 12 " 850°C/49MPa / ' yS "
,'
1.0
D
- s'n

•§2 0.08 | " 5 0.8 - S'

*a

■D &

uX ,-la
α> α> 0.06 °D ^^" 5 σ
Sa
'°
_3 0.04 1m / °
6 0.2 ß ,'
° 0.02 ,'
0.02 0.04 0.06 0.08 0.10 0.12 0.14 0,
0.4 0.8 1.2
Minimum creep rate (%/h) Minimum creep rate (%/h)

Fig. 9. Correlation between calculated and measured minimum creep rate.

200 400 600 800

Rupture life (h)

Fig.10. Correlation between calculated and measured creep rupture lives.

CONCLUSIONS

(1) Creep crack initiation is life-determinant for the first-stage buckets

in the natural-gas-fired base load operated gas turbines. 0.5% creep strain
life assessment method which takes the reduction in effective cross-section
of the bucket blade due to oxidation and the degradation of the material
into account is reguired to assess the bucket life. Coating oxidation life
is also concerned for making a maintenance optimization schedule to have
full design lives of the buckets.

(2) Metallurgical methods to assess the mechanical properties and the creep
life for Hastelloy X were developed. Tensile strength, 0.2% yield strength,
and Vickers hardness were estimated from the number of the precipitates.
Minimum creep rate were estimated from the grain boundary coverage ratio and
volume fraction of the precipitates. Creep rupture life were also estimated
from the calculated minimum creep rate by using the Monkham-Grant equation.

REFERENCES

Henry L Bernstein (1990). Life Assessment & Repair Technology for Combustion
Turbine Hot Section Components. ASM International, 111-118

T.Matsuo, M.Ueki, M.Takeyama, R.Tanaka (1987). Strengthening of nickel-base

Superalloys for nuclear heat exchanger applications. J. Mater. Sei.,22,
1901-1907
WS6a4

CRACK SIMULATION AND LIFE ASSESSMENT OF GAS TURBINE NOZZLES

K.FUJIYAMA, Y.YOSHIOKA, N.OKABE and K.KIMURA

Heavy Apparatus Engineering Laboratory,

Toshiba Corporation,
1-9 Suehiro-cho, Tsurumi-ku, Yokohama, Japan.

ABSTRACT

For the purpose of presuming damage and degradation of used gas

turbine nozzles, hardness tests, low cycle fatigue tests and fatigue
crack propagation tests are conducted on Co-base nozzle superalloy
FSX414 thermal aged up to 10,000 hours. Although hardening occurs
due to thermal aging, there is no significant change in fatigue
properties. The fatigue crack behavior is attributable to crack
propagation morphology and is simulated by fractal geometry model of
dendrite structure and random distribution of initial cracks. The
multiple crack simulation is proved to be a promising technique for
life assessment of nozzles which are used in the crack existing
state after inspection and repairment.

KEYWORDS
Gas turbine nozzle; Life assessment; Simulation; Co-base superalloy;
Fatigue crack; Degradation; Fractal geometry.

INTRODUCTION
Combined-cycle power plant utilizes waste heat of exhaust gas from
gas turbine to generate steam for operating a steam-turbine
generator. As this system offeres more flexible operation and higher
efficiency than conventional steam turbine plant, the commercial
utilization of combined-cycle plant has recently been increasing.
Gas turbine maintenance is one of the most significant points for
assuring the reliability of the combined-cycle plants
(Viswanathan,1989, Ichikawa et aJ. ,1989).
Cracks are often observed in nozzles as shown in Fig.l. These cracks
are caused by thermal stress due to uneven heating and cooling
during start-up, steady state operation and shutdown cycles. The
nozzles are used in the crack existing state after inspection and

73
74

Fig.l. Example of cracks initiated in nozzles.

repairment, according to judgement on the detected cracks.

Therefore, the crack propagation life up to the next inspection
period must be predicted accurately. It is also important in the
life assessment to evaluate the effect of material degradation which
is expected to occur during high temperature exposure. This paper
deals with these problems through the investigation of fatigue crack
morphology and the simulation of the cracks.

EXPERIMENTAL PROCEDURE
The material used is the cobalt base superalloy FSX414. The 20mm
thick plates are manufactured through the investment cast process.
The chemical composition of the material is as follows (wt%);
C:0.25, Si:0.78, Mn:0.70, S:0.008, Ni:10.1, Cr:30.2,
W:6.94, B:0.007, Fe:0.37, Co:bal.
The plates are solution-heated at 1150 C for 4 hours and aged at
982°C for 4 hours. Further thermal aging is conducted using electric
furnace at temperatures 750,800,850 and 900 C, for 1000, 3000 and
10000 hours.
Test specimens are cut from the plates after aging. The low cycle
fatigue specimen is the smooth round bar with 25mm gage length and
10mm diameter in the test section, and the crack propagation
specimen is 1TCT type one in 5mm thickness.
Hardness tests were conducted using a Vickers hardness tester with
294N weight. Low cycle fatigue tests are conducted for the virgin
and the 10000h aged materials at 850 C using an electro-hydrauric
servo fatigue testing machine. The strain ranges are 0.5%, 0.8% and
1%, and the strain rate is 0.25%/s. 30min strain hold tests are also
conducted at 1% strain range. The number of cycles to failure Nf is
determined as the 25% drop of peak stress from the steady state
value. Fatigue crack propagation tests are conducted at 850 C with
3Hz sinusoidal wave and the R-value is 0.1.
 75
EXPERIMENTAL RESULTS
As shown in Fig.2, hardening occurs due to thermal aging. Moreover,
strain induced hardening is observed in the early periods of low
cycle fatigue tests. Figure 3 and Fig.4 indicate that the low cycle
fatigue lives and the fatigue crack propagation rates are both
rather insensitive to the thermal induced hardening. Figure 3 also
shows considerable reduction in fatigue life due to strain hold.
Figure 5 shows crack morphology in the longitudinal section of a
failed low cycle fatigue specimen. Small cracks initiate randomly at
the specimen surface toward the direction perpendicular to loading
axis. The main crack propagates preferably along dendrite boundary
indicating considerable branching.

Fig.5. Observation of crack morphology along the

logitudinal section of a low cycle fatigue
specimen.

DISCUSSION
DENDRITE STRUCTURE AND FATIGUE CRACK SIMULATION
Refering Fig.5 as an example, observation results of low cycle
fatigue cracks with or without hold time are summalized as follows.
(l)The surface cracks initiate randomly either at dendrite core or
at dendrite boundary. The initial crack angle is usually
parpendicular to loading axis.
(2)The main crack propagetes preferably along dendrite boundaries
accompanying branching. The dendrite cores sometimes work as
obstacles for crack propagation.
(3)There are small cracks ahead of the propagating crack front.
These small cracks help advancing main cracks by the coalescence
mechanism.
As indicated in the experimental results, the fatigue properties of
FSX414 are not strongly influenced by thermal aging in spite of the
considerable hardening. This insensitivity may be related to the
dendrite boundary crack propagation because the thermal induced
hardening is supposed to be mainly caused by MooCfi carbide
precipitation in dendrite cores.

To simulate the crack morphologies observed in the low cycle fatigue

damaged specimens, following procedure was executed.
76
400 5x102
FSX414 I FSX414
Vi rgin [ 850°C(R = 0.1)
750 °C aged [ O Vi rgin
> 800°C aged o
\ Δ 8 5 0 ^ , 5000 h aged
850 °C aged
550 E I D 8 5 0 ^ , 10000hagedΔ
900°C aged E
ω
c Δ
■ö
"ö 10 L- Δ
\

I
■ö - Δ

500h

c
q
a?
4->

GO
(Ό
250 a
5000 10000 o
A g i n g hours

Fig.2. Relationship between a

CO
104
hardness and aging O
hours.
5x10 I .... i 1 1 1 1 1

5 10 50
Stress intensity factor range ,
Jk ( MPa /~m~ )
Fig.4. Fatigue crack propagation
properties of virgin and
thermal aged FSX414.
1 0
Γ
FSX414 850 °C
^ S t r a i n hold Continuous
( 50 m i n )
' Δ —C^- Virgin

ω
" A 850°C ,10000h aged

*V
GO
c --·--
03 -j |
- Δ A
C
CO

0.1 . . . I IIMI J —■ ■ i i i t » ! _l 1 1 1 1 II l l 1 I i 1 I i iI

10 10^ 10 5 10 4 10°
Cycles to failure, Nf
Fig.3. Low cycle fatigue properties of
virgin and thermal aged FSX414.
 77
(1)Random dendrite structure of FSX414 is simulated by modifying
"Percolation cluster" (Stauffer,1985).
This is made by follwing sequence;
a)Square lattices are set in 2 dimensional area.
b)Points are dotted with possibility=0.5 using random numbers.
c)Bond the neighboring dots.
d)The bonded paths are treated as dendrite boundaries.
(2)Crack initiates arbitrarily at surface parpendicular to loading
axis with prescribed possibility by random number.
(3)Crack propagates along dendrite boundary. If there is no dendrite
obstacle, the crack propagates parpendicular to loadingr axis. If
this path is not available, crack propagates along 45 inclined
boundary to loading axis. Crack branching occurs when two paths of
45 inclined boundaries are available. If these all paths are
unavailable, the crack is arrested. The arrested crack can grow when
another crack approaches close to the crack tip or no other crack
can propagate.
Figure 6 shows an example of
low cycle fatigue crack
simulation. The dendrite
structure is constructed
well using the method
mentioned above, because
both the model and the real
dendrite structure have
equal value about 1.3 in
fractal dimension. The crack
propagation rate is set
constant in this case. The
crack morphology is quite
similar to real crack as
shown in Fig.5.
A model has been proposed as Fig.6. Simulation of low cycle
to the random distribution fatigue crack of FSX414.
of fracture resistance and (Longitudinal section)
crack driving force at grain
boundaries (Tada et aJ. ,1990). The construction of an exact model
for dendrite boundary failure mechanism is still under study.

LIFE ASSESSMENT METHOD FOR GAS TURBINE NOZZLES

Figure 7 shows life assessment procedure for gas turbine nozzles
including damage tolerant concept and multiple crack simulation.
Initial crack distribution is determined using inspection records
after repair and is used for multiple crack simulation analysis. In
the simulation, if the longest crack size a reaches a critical
size a before next inspection for expected o^e^rating patterns, the
c
nozzle is replaced. If the nozzle is sound, it is used again. This
sequence is repeated until the retirement, updating the crack
distribution model from the informations on each inspection.

Figure 8 shows an example of multiple surface crack simulation.

Initial crack size is assumed uniform but the initiation sites are
randomly distributed with the probability of 0.005 for highly
damaged area in the subject component. The example simulates real
crack morphology as shown in Fig.l. Under the assumption that crack
propagation rate is constant, crack coalescence accererates the
78

Fig.8. Multiple crack simulation

of FSX414 (Crack initiation
probability = 0.005 at highly
stressed zone indicated with the
mark;[~ in the left hand side) .

Fig.7. Life assessment procedure

for gas turbine nozzles.

(l)In spite of thermal induced hardening of FSX414, fatigue

properties are insensitive to thermal aging within the test
condition. These characteristics are attributable to fatigue crack
propagation along dendrite boundaries.
(2)Fatigue crack morphology is simulated by fractal model of
dendrite geometry and random distribution of initial crack.
(3)Multiple crack simulation is a promising technique for assessing
damage tolerant life of gas turbine nozzles.
Further study on the stochastic nature of fatigue cracks and local
failure mechanism is necessary for more practical simulation.

REFERENCES
Viswanathan.R. (1989). Damage Mechanisms and Life Assessment of High-
Temperature Components. ASM International,415-479.
Ichikawa, M. and N. Okabe (1989). Recent Studies on Structural Safety
and Reliability.Current Japanese Materials Reserch (T. Nakagawa,
H. Ishikawa and A. Tsurui, Ed.),5,1-24.
Stauffer, D. (1985). Introduction to Percolation Theory. Taylor &
Francis.
Tada, N., T. Kitamura and R. Ohtani (1990). Monte Carlo Simulation
of Creep-Fatigue Small Cracks Based on a Three-Dimensional Model
of Random Fracture Resistance of Grain boundaries. Trans. JSME,
56-A, 708-714.
WS6a5

CREEP-FATIGUE DAMAGE EVALUATION OF INCONEL 738LC SUPERALLOY

M. SAKANE and M. OHNAMI

Department of Mechanical Engineering, Faculty of Science and Engineering,

Ritsumeikan University
56-1 Tojiin Kita-machi Kita-ku Kyoto, 603, Japan

ABSTRACT

Creep-fatigue damage was evaluated by replication, X-ray, hardness and UT under uniaxial and
multiaxial stress states. Crack monitoring was the most reliable method of detecting creep-fatigue
damage of Inconel 738LC superalloy.

KEYWORDS

Creep-fatigue damage; superalloy; high temperature; multiaxial stress; X-ray.

INTRODUCTION

Creep-fatigue damage evaluation is an urgent problem for the life extension and safety of the high
temperature components, such as nuclear plants and gas turbines. The aim of this study is to
develop an appropriate method of evaluating creep-fatigue damage for nickel base superalloys under
two loadings ; one is the uniaxial loading and the other is the multiaxial loading.

EXPERIMENTAL PROCEDURE

The material tested is Inconel 738LC nickel base superalloy of which chemical composition and
heat treatment is listed in Table 1 (Ibuchi et aL, 1990). Uniaxial push-pull creep-fatigue tests were
carried out using a solid specimen with 10 mm diameter and push-pull/reversed torsion tests were
made using a hollow tube specimen with O.D. 8 mm and I.D. 5 mm. Electric hydraulic uniaxial

Table 1 Chemical composition and heat treatment of the material tested (wt % ) .
c Al Ti Cr Mo W Co B Nb Zr Ni

0.10 3.58 3.40 15.82 1.68 2.90 8.60 0.011 0.87 0.056 Bal.

1393 K X 2 Hrs. Ar gas fan cool.

1116 K x 2 H r s . Air cool.
79
80

IN738LC, T H I 2 3 K , in Ain IN738LC, T - I I 2 3 K , in Ain

10
X 0^)5=0.9% ""
O t h = 0 mi n. • 0.7% th = 0min.
• t h = 1 0 mi n.
3 th= 3 0 m i n .
σ>

σ
JO
(a)
ι2 o
10"
102 103 104 103 0.0 0.2 0.4 0.6 0.8 1.0
Number of cycles to failure Nf Life ratio N/Nf
Fig.l Creep-fatigue lives in push-pull tests.
IN738LC, T=II23K, in Ain
X o Λε=0.9%
IN738LC, T=II23K, in Ain • 0.7% th=IOmin.
E
E
CD o 46 =0.9% o
■σ
• 0.7% th'Omin. D

(D =¥=*:
C
c ■σ
O D
1 l· JO
0)
O (b)
O
o
• O 0l
0.0 0.2 0.4 0.6 0.8 1.0
-Crf
Life ratio N/Nf
0.0 0.2 0.4 0.6 0.8 l.o Fig.2 Change in microvickers hardness
Life ratio N/Nf in (a) no hold-time and (b) 10 min.
Fig.3 Variation of attenuation coefficient hold-time test.
of ultrasonic wave with life ratio.

and push-pull/torsion machines were used for the strain controlled tests at 1123 K in air. Five
damage evaluation methods were applied; microvickers hardness, attenuation coefficient in UT,
misonentation angle, crack length measurement by replica and crack monitoring by a.c. potential
method.

TEST RESULTS AND DISCUSSION

Damage Evaluation in Uniaxial Test

Figure 1 shows low cycle fatigue lives in hold-time and no hold-time tests under push-pull loading.
 81

IN738LC, Τ Η Ι 2 3 Κ , in Αίη IN738LC, Ί Μ Ι 2 3 Κ , in Ain

O G r e i n No. 1 O G r a l n No.
'S • G r a i n No. 2
3 G r a ! n No.3
\ • G r a i n No.
3 G r a i n No.
216=0.9%
trHOmln.
C G r a l n No. 4 C G r a l n No. 6
o
ρ o

ο o
(b)
n| 1 1 1 1
0.2 0.4 0.6 0.8 1.0 1.0
0.0 0.2 0.4 0.6 0.8
Life ratio N/Nf
Life ratio N/Nf
Fig.4 Change in mean misorientation ratio with life ratio
(a) Δε=0.9%, tH=0 min. (b) Δε=0.9%, tH=10 min.

Introduction of 10 min. hold-time reduces the fatigue life to 70 % and that of 30 min. to 50 % in
comparison with no hold-time test. The inelastic strain range is about 10 % of the total strain range
in no hold-time test at the total strain range (Δε) of 0.9 %, so that the deformation behavior of the
material tested here is almost elastic. The percentage of the inelastic strain range increases in
hold-time tests in comparison with no hold-time tests, but it is 20 % in 30 min. hold-time test at
the total strain range of 0.9 %.

Figures 2 (a) and (b) show the variation of the microvickers hardness with cycles in no hold-time
and 10 min. hold-time tests. A slight decrease in hardness with cycles is observed in the latter test
but there exists no change in the former test. In both the tests, the change in hardness with cycles
is very small for the superalloy employed in this research.

Figure 3 shows the variation of the attenuation coefficient obtained in the ultrasonic test, where the
attenuation coefficient defined is the area ratio of the first and second reflections between 5 MHz
and 15 MHz on the spectrum vs. frequency diagram. As well as the former parameter, the
attenuation coefficient also expresses no clear change with life ratio.

Figures 4 (a) and (b) are the variation of the mean misorientation angle for four grains with cycles
in no hold-time and 10 min. hold-time tests. The misorientation angle of a grain shows a
significant increase in both the tests while the other grains do not. Thus, the increase in the
misorientation depends on grain and that the selection of grain is of importance when evaluating the
creep-fatigue damage by the X-ray Laue method.

The three methods sated above are not effective for the creep-fatigue damage evaluation of Inconel
738 superalloy. The reason for the ineffectiveness is considered as follows. Inconel 738 LC
superalloy employed here exhibits no large inelastic deformation, but the above three parameters
mainly measure the accumulation of inelastic strain as the damage and that the three parameters do
not properly evaluate the damage accumulation in creep-fatigue test.

Other than the three parameters, crack extension behavior was measured with replication method.
Figures 5 (a) and (b) represent the main crack extension curves occurred at the grain boundaries in
82
IN738LC, T-II23K, in Ain IN738LC, T = I I 2 3 K , in Ain
10 10
s
o 215=0.9% th 0min. o J6S0.9% thsIOmin.
• 0.5% E • 0.7%
E E
£
σ
σ CVJ
CO

6
s
o
σ (b)
O o
10" 10"1
0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.2 0.4 0.6 0.8 1.0
Life ratio N/Nf Life ratio N/Nf
Fig.5 Crack extension curves measured by replication method.
(a)tH=0 min (b)tH=10 min.

IN738LC, T = I I 2 3 K , in Ain IN738LC, T=II23K, in Ain

101 I 1 I 111 1 1 I I I I l |l 1 1 I I I I 1 _1 10)4 . ' ' M nii| "Ί ' ' M im.
£
O push-pull "
• torsion
- O push-pull "
• torsion J
ib
0>

3
1 t- 10 :
^:^r^— i

(a) (b)

10" i I i ml i i i I i ml
10 2 ■ ■ ■ l i m i , —i—i i 1 i m l 1—i—i_l. i m
10 2 10 3 10 4 10 5 10 2 10 3 10 4 10 5
Number of cycles to failure Nf Number of cycles to failure Nf
Fig.6 Biaxial low cycle fatigue data correlation with
(a)Mises' strain range and (b) Mises' stress range.

no and 10 min. hold-time tests. Crack nucleates in the early stage of life ratio. It appears that the
crack already nucleates less than 20 percent of the fatigue life. After the crack nucleation, the crack
propagates almost at the constant rate in semilogarithmic diagram. The similar crack propagation
behavior has been also confirmed for IN 738LC superalloy (Matsuda et al., 1986). Therefore, for
superalloys like Inconel 738 LC employed here, the monitoring of the surface crack is only the
effective damage evaluation means. The other damage evaluation methods stated above are not
effective since they mainly measure the inelastic strain accumulation.

Damage Evaluation Under Multiaxial Stress State

In the discussion on the damage evaluation under uniaxial stress state, what becomes apparent is the
effective means for the creep-fatigue damage evaluation of superalloys being the crack monitoring.
 83

IN738LC, T=II23K, in Ain IN738LC, T=II23K, in Ain

1.7 2. 1 i
p u s h - -pu 11 t o r s i on
T
O50Hz
ÜJ 3500Hz Lü
\ © 1 KHz
Lü
050Hz
»500Hz
Lü 02KHz ClKHz
©3KHz
• 5KHz ·_ L 03KHz
• 5KHz
1.3 2 1.
(a)
^%^-

£ ^o £
0.9 0.9
0.0 0. 5 1.0 "0.0 0.5
Life ratio N/Nf Life ratio N/Nf
Fig.7 Variation of a.c. potential ratio with life ratio at various
frequencies, (a) push-pull test (b) torsion test

IN738LC, T=II23K, in Ain IN738LC, T H I 2 3 K , in Ain

2. 1 1 Ί— 1 S 1 2. 1 1 1 1 1 1
A f=5KHz
s
f = 5KHz Δ push-pull A ^
Lü
Lü
\ Δ push-pull \ A torsion
A torsion Lü A yT
Lü A
O f = 5 0 0 Hz
A, σ fL· O push-pull J
*" 1. 5 f = 5 0 0 Hz \ 1.5 • torsion Ί

7 Δ Δ°
O push-pull
• torsion J·
T ^^^^%
^X·
£ £^^
£ a* A • • ^ ^ /ΑΔ Δ
5 ^

Ko·—% Γ · · θ
1 i J 1 0.9 I 1 1
0.9 1 i
0 1 2 3 4 0 1 2 3 4 5
Crack density D, mm/mm2 Maximum crack length I, mm
Fig.8 Relationship between a.c. potential Fig.9 Relationship between a.c. potential
ratio and crack density. ratio and maximum crack length.

In this section, we will apply the a. c. potential method to crack monitoring under the biaxial stress
state.

Test material is the same as that used in the uniaxial test, but the shape of the specimen is a hollow
cylinder. Push-pull and reversed torsion tests were made at 1123 K. The a. c. potential method
used was that the a. c. 5 A with the rectangular wave shape at 50 Hz was sent to the specimen and
the voltage increase due to the crack nucleation and extension was monitored. Voltages at various
frequencies from 500 Hz to 5 KHz were determined by analyzing the detected a.c. potential wave
using the fast Fourier transformation (FFT).
84

Figure 6 shows low cycle fatigue lives correlated with (a) Mises' strain and (b) Mises' stress ranges.
The Mises' strain cannot correlate the fatigue data in push-pull and reversed torsion within a factor
of two scatter band. The Mises' stress correlates the fatigue data within a factor of two scatter band.
This trend of the data correlation is quite the reverse to type 304 stainless steel (Sakane et al., 1987).
For type 304 stainless steel, the Mises' strain gives a better correlation than the Mises stress. The
Mises' stress gives rather a poor correlation.

Figures 7 (a) and (b) represent the experimental relation between the potential ratio and fatigue life
ratio in tension and torsion. Potential ratio is the potential normalized by the potential before test.
The potential ratio at 5 KHz increases rapidly in the early stage of life ratio but the increasing rate
becomes small in the final stage. Conversely, the potential ratio at 500 Hz yields no increase in the
early stage but a rapid increase in the final stage, caused by the macro crack extension. The
potential ratio at high frequency is more sensitive to the fatigue damage in the early stage.

In order to examine the relation between the frequency dependence of the potential increase and
crack morphology, the crack density and maximum crack length were measured by replica,
intermitting tests. The relationship between the potential ratio, crack density and maximum crack
length is shown in Figs.8 and 9. In these figures, the test results at 500 Hz and 5 KHz are presented
as a representative value of low and high frequencies. These figures clearly show that the potential
ratio at 500 Hz has a clear correlation with the maximum crack length while that at 5 KHz with the
crack density. Since there exists the skin effect in a. c. potential, the potential at high frequency
detects small cracks more sensitively than that at low frequency. The potential at 500 Hz only
detects macro cracks and that it increases after the macro crack nucleation.

From the above consideration, the fatigue damage of superalloys can be detected accurately by using
the a. c. potential method. The a. c. potential at high frequency more sensitively detects the fatigue
damage in the early stage while that at low frequency the fatigue damage in the final stage. The
physical meaning of a.c. potential at high frequency corresponds with the crack density while that
at how frequency with the maximum crack length.

CONCLUSIONS

(1) Microvickers hardness, attenuation coefficient in UT and misorientation angle are not effective
for the creep-fatigue damage evaluation of the nickel base superalloy. The cause of ineffectiveness
of these means is attributed to the small inelastic deformation of the superalloy. Only the effective
means is the crack monitoring by replication.
(2) A. c. potential method is developed to detect the biaxial fatigue damage. The developed method
is effective for the fatigue damage evaluation. The a.c. potential at high frequency corresponds to
the crack density while that at low frequency with the maximum crack length.

REFERENCES

Ibuchi, H., H. Kimura, M. Sakane, M. Ohnami, M. Muramatsu and K. Fujiyama (1990). Damage
Evaluation of Inconel 738LC Nickel-Base Superalloy in Creep-Fatigue. /. Soc. Mater. Sei.
Japan, Vol.39, pp.522-528.
Matsuda, N., S. Umezawa and T. Terunuma (1986). Small crack Initiation and growth behavior of
IN738LC at low cycle fatigue and thermal fatigue, J. Soc. Mater. Sei. Japan, Vol.35,
pp.810-816.
Sakane, M., M.Ohnami and M. Sawada (1987). Fracture modes and low cycle biaxial fatigue
life at elevated temperature, J Eng. Mater. Tech., Vol.109, pp.236-243.
WS6a6 LIFE PREDICTION - THERMAL FATIGUE FROM
ISOTHERMAL DATA

WJ. Plumbridge and T. Goswami

Department of Materials Engineering
University of Wollongong
PO Box 1144 NSW 2500 AUSTRALIA.

ABSTRACT
Isothermal fatigue (IF) behaviour was generated in a separate paper for a gas turbine blade
material MarM002, and the life prediction was made in terms of generic models
phenomenologically. The isothermal damage mechanisms were studied to develop a Thermo-
mechanical life prediction model.

The empirical modelling of Thermo-Mechanical Fatigue, (TMF), was made in terms of cyclic
stress-strain in a product and hysteretic energy in time dependent form. The TMF lives were
assumed that of isothermal, at the maximum temperature of the TMF cycle. The prediction of In
Phase life was more than the Out of Phase ones and was not expected. The Spanning function,
Taira's empirical model, strain range Partitioned components of a hysteresis loop, were studied.
TMF life was overpredicted by all the above models,however, Taira's empirical model was too
conservative.

INTRODUCTION

A highly stressed gas turbine blade component, requires performance under a hostile
environment. Where in addition to fatigue being predominant, creep and oxidation, compound
the damage kinetics and reduce the fatigue life. Necessarily, this critical component operates
under a varying temperature with respect to loading conditions. Thermal shock and fatigue thus
needs much attention to design a component for such usage.

Isothermal fatigue (IF), behaviour offers a decrease in life with increase in temperature, plastic
strain range and decreasing strain rate. Life also decreases with increasing hold time in the
peak tensile strain for the low alloy steels and the opposite for the Nickel based superalloys. The
microstuctural basis and metallographic studies are documented (Plumbridge et al, 1987 and
Plumbridge, 1987 ), for isothermal behaviour of Mar M 002 and several materials operating at
high temperature. The fracture processes and the deformation mechanisms, have also been dealt
in (Plumbridge et al, 1987, Plumbridge 1987 and Mughrabi, 1985). The life prediction of
Isothermal behaviour within the perspective of phenomenological approaches prove
conservative and often the prediction band falls within 2% of experimental values.

(a) Out of phase (OP) (b) In Phase (IP) (c) Diamond cycle (DC)

Fig.l. Basic thermo-mechanical cycles,

(a) IPcycle, (b) OP Cycle
(c) Diamond shape.

85
86

Basically, TMF constitutes an Ίη-phase' and an 'Out of phase' cycle as shown in fig.l(a-c).
Fig.2, illustrates the thermal cycle for a turbine blade airfoil because of an aircraft flight cycle.
Suction and pressure sides describe different thermal cycles as they are loaded differently. The
trailing edge is hard to cool where as the leading edge has a faster cooling system. The in-phase
(maximum strain at maximum temperature) and out of phase (maximum strain at minimum
temperature) cycles are shown in fig. l(a-c). A TMF cycle for a blade section TL', often
describes a peanut shape as shown in fig.2. A basic TMF analysis was carried out for a high
pressure turbine blade (Goswami,1988) representative of a flight profile. For turbine blade
superalloys, (Bill et al, 1984), the in-phase TMF cyclic lives were found shorter than out of
phase cycles, at high mechanical strain ranges where as, vice-versa with low mechanical strain
ranges.

Acceleration

Deceleration

Pea nut shape TMF loop for a turbine blade

Fig.2. A gas turbine blade and TMF

cycle.

Present study has been undertaken in two steps. Isothermal behaviours have been analysed and
modeled for life (Plumbridge et al 1987 ) in the first part. The second stage considers an
analytical approach to the TMF life prediction from the isothermal data. This mainly considers
TMF lives equivalent to isothermal at the maximum temperature of the TMF cycle at the same
inelastic strain range. The partitioned PC and CP cycles of a hysteresis loop at an intermediate
temperature was considered as a failure characterizing criterion based on the strain range
partitioning technique. The time dependent Ostergren's (Ostergren 1976) and hysteresis energy
models were also analysed. Empirical model proposed by (Taira et al, 1979) for TMF life
prediction was applied to the Mar M 002, isothermal data, which was too conservative. The
damage mechanisms were studied for isothermal behaviour at 750,850 and 1000°C, a
predominating oxidation mechanism was found exists beyond a threshold temperature. A review
of damage mechanisms was carried out for several blade materials such as Mar M 200,Mar M
247,IN 100 and B 1900 Hf under TMF, (Goswami, 1988). In this paper, oxidation as the
most damaging failure criterion for the IF and TMF of these materials at high temperature has
been proposed.

EXPERIMENTAL

Mar-M 002, was characterized, where the specimen design details, test facility for fatigue
testing along with various controls for temperature and strain range measurements were
described in (Ellison et al, 1984). Isothermal fatigue tests were carried out at three different
temperature ranges at 750,850 and 1000°C with the application of dwell sequences in tension and
compression.
 87

Data.

Table 1. Summary of Isothermal behaviour.

Temp.°C A B -a -ß strain rate EMpa -Y

750 0.0161 0.003338 0.115 0.263 0.002 166986 0.378 |
850 0.0130 0.008867 0.109 0.354 0.002 159995 0.469 |
1000 0.0076 0.06286 0.145 0.595 0.002 146004 0.740 1
Table 2. Constants in the analytical model.

m a b Aet % Δείη % AaMpa Δσ mean

0.0005 24350 0.388 0.896 0.076 1496 33

0.0002 8030 0.300 0.946 0.178 1178 156 1
-0.0042 3265 0.333 0.808 0.411 538 69 1
Table 3. Equivalent TMF lives from various models.

Inelastic Δε Δε
ίησί IP cycles AW IPcycles Δε
ίησί
OPCycl< ;AW OP cycles
(a) (b) (c) (d) (e) (f) (g) (h)

0.0002 0.0196 31639 0.014703 46659 0.0892 4082 0.0642 6358

0.0004 0.0852 4343 0.062425 6612 0.4095 520 0.2950 811 |
10.0008 0.1248 2592 0.093623 3824 0.6104 303 0.4397 473
10.001 0.168 1735 0.126031 2558 0.832 199 0.5994 311 1
0.004 1.068 142.5 0.8012 210 5.68 15 4.0922 24

The data from the above table has been analysed by spanning function method of equation 7, to
obtain an intermediate life range as shown in fig.5.

DISCUSSION
Life Prediction
The failure criterion of Ostergren's describes the phasing action for an In Phase/IP' and Out of
Phase, ΌΡ' that considers inelastic strain range and peak tensile stress as a power function of
cyclic lives. The TMF loops were assigned values from the table 1 and 2, for a particular
temperature, strain and stress range. Failure criterion was studied in a time dependent form.
The product term of equation 4 and 5, was studied separately. Also, the hysteretic energy term
was equated to the right hand side of equation.5. All the variables associated with this method
can be established by following the constitutive equations (Appendix. 1). Life prediction was
made at each temperature, stress and inelastic strain range, describing a TMF hysteresis loop.
In and out of phase results were obtained separately with respect to temperature and were
plotted in fig.3. The TMF life assumes IF values at the maximum temperature of a TMF cycle.
Being so, the IP lives were found longer than the OP as shown in fig.4 . Energy terms of the
TMF life prediction as appear in fig.4, exhibits the same behaviour. The expected behaviour in
the TMF, is to have IP life shorter man the OP in the case of blade materials which operate much
beyond 0.5 of material melting temperature. Owing to a large difference in the TMF lives at 750
and 1000° C, spanning function method was applied to determine an intermediate life for
88
temperature range of 750-1000° C. Spanning function method, overpredicts the TMF life as
shown in fig.5. Due to this discrepancies (Taira's et al 1978) empirical model was applied and
the observed behaviour is shown in fig.6. This shows, IP lives shorter than the OP, determined
with a multiplication factor of 8 and 4 on isothermal damage parameter respectively . Further
studies are underway to develop an empirical model, from the damage mechanisms to include
fatigue, creep and oxidation mechanisms separately and in interaction mode.

10° i
a a IP Energy term n IP Energy term
0
D IP Product form Q IP Product term

♦ a
♦ OP product form
£ 10« 4 ♦ OP Product term
♦ OP Energy term ·
o OP Energy term

10 1 T -
100 1000 .0001 .001
Temperature (oC) Inelastic strain range

Fig.3. TMF cycles and the cyclic life Fig.4. TMF life prediction from IF
vs. temperature plot. lower life data.

10 D
o IP Energy term
a IP Product form * ♦ CP
1 0 - -J a

io3 j 103 J

102 J
I ♦
♦
OP Product form
OP Energy term
1
°2] •
□ IP a

1 01

' ""* ■ ■ r-1

■ ■ "Γ 1—r-i
.0001 .001
.0001 .001
Inelastic strain range Inelastic strain range
Fig.5. Spanning function of the TMF Fig.6. Taira's model of TMF life
life fractions and intermediate prediction from IF data.
lives.

Damage Mechanism
At elevated temperature isothermal fatigue, many mechanisms have been found active, such as,
coalescence of secondary cracks with the main crack, formation of a network of voiding, their
linking and subsequent crack advancement, mixed mode of % intergranular and transgranular
crack growth and grain boundary sliding. In the case of TMF, a number of mechanisms in
addition to above have been found to dictate damage evolution. These are environmentally
assisted oxidation mechanisms apart form creep-fatigue. Oxidation of the coating surface
nucleates a crack. Oxidation also occur at the crack tips and the crack faces, as crack advances.
There may also be second phase oxidation. In the case of gas turbine blade materials, there is a
mismatch in the thermal expansion coefficient between the coating and the metal matrix that
concentrate the strains locally and nucleates a crack. It was found in the previous study
(Plumbridge et al,1987), that a crack nucleated from the coating stopped at the metal surface in
certain cases. However, these sites are often the potential sites for crack initiation, which
moves past in the metal matrix. In the case of polycrystal materials such as Mar M 002,Mar M
200,Mar M 247, IN 100 and B 1900 Hf, the oxidation mechanism is found to be active, after a
 89

threshold temperature. This necessarily results in depletion of γ along the crack face. A
mechanistic diagram of such a case can be drawn as shown in fig.7.

Oxidation at the
crack tip
Stress triaxiality
Oxidized zone Large forward plastic zone
-compressive mean stress.

IP cycle
oxidation at the
crack tip, depletion of Tensile mean stress
yphase. Oxide at the tensile loading
smaller plastic zone
large reverse plastic zone.
temp.

OP cycle.

Fig.7. A mechanistic model of TMF

damage accumulation.

The basic to a TMF, IP cycle involves tensile loading at the maximum cyclic temperature.
Beyond a threshold temperature the material is susceptible to oxidation attack and damage is not
determined by creep but by oxidation. Cyclic action causes crack tip sharpening and blunting
because of oxide brittle debris. At high temperature, at the crack tip stress triaxiality enhances
the oxidation rate. The crack advances by oxidizing and depleting y as shown in fig.8(a-d).
The OP cycle is at lower temperature regime and is dominated by fatigue and creep or their
interactions. The studied IF behaviour of Mar M 002, does not show the oxides and ydepletion
at 750 °c as they occur at 1000 °c. The described phenomenon as shown in fig.7, states that the
OP cycle has a compressive stress acting in lower temperature, this gives rise to a positive mean
stress, that reduces the life. However, the temperature being at a lower side the action of creep-
fatigue is limited. The IP cycles are more damaging because at high temperature and higher
straining conditions, the damage accumulation is by creep-fatigue and oxidation and their
interactions. The IF lives based on inelastic strain range criterion, were found higher at 1000
than at 750°C, this may have been by the coarsening effect of the y phase, which is more creep
resistant. This should occur at the temperature more than the solutioning temperature for this
material.

(a) [ 750°C Δεί η = 0.00076]

(b) [1000O C, A e i n = 0.00411]
90

(c) [1000° C, Δ ε ί η = 0.00465, W) I 1 0 0 0 ° C Δ ε ί η = 0.00541,

5 min
5 min. tensile hold] · compressive hold]
The damage mechanism of IF behaviour of Mar M 002, was compared from the TMF behaviour
of Mar M 200 polycrystal material (Bill et al, 1984), and a similar trend of oxidation dominated
damage growth, was found exists for Mar m 200. Fig.8(a-d), demonstrates crack path,
oxides and Y depletion in the case of the studied material at different temperature and inelastic
strain conditions. However, this particular mechanism is found to dominate the damage kinetics
for Mar M 200 under TMF conditions as shown in fig. 8 (e,f) (Bill, et al, 1984). Based on the
above, oxidation mechanism needs to be included in formulating a life prediction model for TMF
from IF.

(e) IP oxidation mechanism.

(f) OP oxidation mechanism.

Fig.8. Photomicrographs of IF and TMF (a) Oxidation free crack growth at
750 °C. (b,c,d) oxide formation and γ' depletion at 1000°c. (e,f) IP
and OP for a Mar M 200 Oxidation assissted growth (Bill et al, 1984).

CONCLUSION
TMF life prediction was attempted from the isothermal data within the perspective of
phenomenological models. A time dependent Ostergren's, hysteretic energy failure criterion,
strain range partitioning together with inelastic strain-life criterion, were found to overpredict the
TMF life. A reverse trend, with IP cycles grater than the OP cycles, was observed with the
above approaches.
Oxidation in the damage mechanism has been ignored in modelling isothermal life prediction.
The models studied above did not include oxidation in the parametric relationships. A
development of life prediction approach to TMF from IF, should incorporate oxidation damage
mechanism.
 91
ACKNOWLEDGMENT

One of the authors (T.G.) acknowledges Mr. A. Prasad (Emeritus Scientist), Mr. R.
Padmanabhan (Project Director), Dr. K. Ramchandra (Head, Materials and Structures group) of
Gas Turbine Research Establishment Bangalore India.

REFERENCES
Antunes, V.T.A, and Hancock, P. (1978)'Strain range partitioning of Mar M 002,
over the temperature range of 750 -1040 C . AGARD CP No. 243.
Bill,R.C,Verrilli,MJ,McGaw,M.A and Halford,G,R. (1984) 'Preliminary study of
thermomechanical fatigue of polycrystalline Mar M 200* NASA TP 2280, 84.
Ellison,E.G, Plumbridge, WJ,and Dean,M.S. (1984)' Turbine blade material behaviour and life
prediction' research project no. 327, Dept. of Mechanical engineering, University of Bristol.
Goswami,T. (1988) 'Thermal fatigue analysis of gas turbine blade materials' Unpublished work
at the Gas Turbine Research Establishment Bangalore.
Haiford, G.R, (1987) ' Low cycle thermal fatigue' Chapter 6, Thermal Stresses II Ed.
Hetrarski,R.B. 87.
Mughrabi. H. (1985)' Dislocation in fatigue' Dislocation and properties of real materials. The
Institute of Metals.
Ostergren,WJ. (1976)' A damage function and associated failure equations for predicting hold
times and frequency effects in elevated temperature low cycle fatigue' Jr. Of Testing and
Evaluation . 4, No.5. sept.76.
Plumbridge WJ,and Ellison. E.G. (1987) Low cycle fatigue behaviour of superalloy blade
materials at elevated temperature' Mat. Sc. and Tech., 3.
Plumbridge,WJ. (1987) 'Metallography of high temperature fatigue1 High temperature fatigue
properties and prediction Ed. R.P. Skelton Elsevier Applied Sc. 1987.
Taira,S.(1973) ' Relationship between thermal fatigue and low cycle fatigue at elevated
temperature' Fatigue at elevated temperature ASTM STP 520, Ed. Carden, A.E, McEvily
A.J, and Wells,C.H. 1973.
Taira, S. andFujino,M. (1979) Trans. ISIJ 19, 1979.

APPENDIX 1

CONSTITUTIVE EQUATIONS

IF data was represented in terms of Manson-Coffin equation form. The total strain concept was
evaluated as a failure criterion.

Aet = A ( N f ) « + B ( N f ) ß (1)

where, A and B are intercepts of elastic and plastic strain range versus cyclic lives plots, a and ß
are slopes of the same. These parameters are temperature dependent and are tabulated in Table 1.
IF Cyclic stress-strain behaviour was given in terms of

Δσ= a ( A e t ) b (2)

The Cyclic Stress-Strain (Δσ-Δε) was related in the time dependent form. This was achieved by
incorporating the strain rate parameter.

Δσ = ( έ · )m a(Ae- )b (3)
92
where, ε· η , is the inelastic strain rate, a, is the strength coefficient and is temperature dependent.
Δε· η , is inelastic strain range.

The energy term was obtained from the following

AW = A e i n a t / ( l + b ) (4)

Failure Criterion: Ostergren's failure criterion was evaluated for the TMF life prediction in the
time dependent form. The peak tensile stress together with inelastic strain range was considered
in a product form. A hysteretic term AW was also evaluated separately.

Ae in ct = F ( N f ) Y ( έ ^ ) ™ (5)

where, F is the intercept and γ the slope of the product form and is equals to (a + ß). F was
obtained (Halford, 1987) from this equation.
1+n
F = a/2 ( B ) (6)
Inversion of temperature -cyclic lives in terms of strain range life relationship was made
following the spanning function method (Taira. 1973). This determines the TMF life cycling
between two temperatures limits.

N f (T lf T 2 ) = 2 [(N f (Tp / NfT2) ] ! - δ / [1+ N f ( T ^ / N ^ ) ] N f (T 2 )

where, δ = 2 B(T 2 )/3 (7)

B can be obtained from the equation 1, and table 1 at the temperature of the interest.

The constitutive equation for the SRP has the form,

ey - A y C N y ) * (8)

where, ij represent the cycle such as PC or CP, and at 850C ranges from (A= 0.70 to 0.89 and
x= -1.21to -1.26) and for CP cycle (A= .024 to 0.019 and x = -0.78 to -0.38) ( Antunes et al
1978).
Empirical model proposed by (Taira et al 1979) has the following form

ΔΦ = (ΔΦ + ΔΦ ■ V2 + η (ΔΦ + ΔΦ ■ )/2 (9)

v
max mm } 'v max mm' yy)

where, Φ is the damage per cycle in TMF and Φ max and min are the damage per cycle of
isothermal fatigue at maximum and minimum temperature of TMF cycle, η ranges, 8 and 4 for
IP and OP cycle respectively.
WS6a7

CREEP CRACK GROWTH AND TAIL PART BEHAVIOR

OF LOW ALLOY STEELS AND Ni BASED SUPER ALLOY

A. FUJI and M. KITAGAWA

Structural Materials Department, Research Institute,
Ishikawajima-Harima Heavy Industries Co.,Ltd.
1-15, Toyosu 3-chome Koto-ku, Tokyo 135 Japan

ABSTRACT
The creep crack growth behavior for low alloy steels and Ni based
super alloy is characterized by the relation between crack growth
rate and displacement rate. The crack growth life will be
represented by Monkman-Grant type formula in the relation with
minimum displacement rate.

KEYWORDS
Creep; Crack growth; Low alloy steels; Ni based super alloy

INTRODUCTION
The characterization of creep crack growth is important to
estimate the life of high-temperature service machines and
structures that have allowed their component parts to contain any
number of cracks. And a work to standardize the testing method and
its evaluation have been done(Yokobori et aJ.,1990a). Recent
results (Yokobori et aJ.,1987,1988) indicate that creep crack
initiation life and the residual life can be characterized by the
relative notch opening displacement criterion and the creep
deformation curve.
In this study, we intend to discuss the relation between creep
crack growth rate and load line displacement for low alloy steels
and Ni based super alloy under various conditions and the fracture
life(creep crack growth life) prediction in the relation with
minimum displacement rate.

EXPERIMENTAL
The materials used are ASTM A336F22 (2.25Cr-lMo, forged), A217WC9
(2.25Cr-lMo, casting), lCrMoV (for turbine rotor) steels and
93
94
IN-100 (Ni based super alloy, casting). The A217WC9 steels include
service degraded materials and the coupons subjected to recovery
treatment. The chemical compositions are shown in Table 1. These
materials have the various room temperature tensile properties as
given in Table 2 and the creep properties as shown in Fig. 1 (the
results for lCrMoV steel and IN-100 alloy were obtained by
NRIM(Tabuchi et aJ. 1990a,b)) . The test piece design was the
so-called compact type(CT)with fatigue precrack, shown in Fig.2.
The dimensions were 50.8mm in width(W) and 6.35, 12.7, or 25.4mm
in thickness(B), without or with a 75% side groove. For the
lCrMoV steel, moreover, auxiliary tests were conducted with
smaller 20mmW and 5mmB specimens. Data of creep crack growth were
acquired through the standard procedure (Yokobori et aJ., 1990a).
Here, the load line displacement was determined with a LVDT meter
which was inserted through the heating furnace, while the crack
length was continuously measured with the electrical potential
technique.

RESULTS
Relation between δ and creep da/dt
Figure 3 shows the schematic drawing in the relation of elapsed
time vs the creep crack length and load line displacement. Namely,
there is a universal decrease in all of the load line displacement
rate(§ ) and the crack growth rate (da/dt), then δ attain their
repective minima after the da/dt has reached #its minimum, and
finally all steadily increase thereafter. The δ are plotted in
Fig.4 and Fig.5 against da/dt. Their mutual correlations are
substantially one-to-one as in the case of low alloy steels,
meaning that the da/dt corresponds well to changes in 5 . The small
deviation of A336F22 steel seen in Fig.4 is due to the specimen
type with or without side grooves(Fuji et aJ.,1987). The data in
A217WC9 steels fall on practically a single trend line mean that
the relations between the da/dt and δ are not subjected to the
state of degradation or to differnce in loading(Fuji et aJ.,1990).
From the results in lCrMoV steel shown in Fig.5, effects of the
specimen thickness rather than testing temperature or loading
conditions are observed(Yokobori et aJ. , 1989b) Although the
relation on IN-100 super alloy falls on a single trend line, the
deviation with about 1/7 decrease in δ were observed.
Yokobori(1990b) suggested that da/dt will be determined by the
rate of some atomistic rearrangement required for occouring of
time dependent plastic flow, thus, h . In that case, the δ as in
usual thermal activation process, and da/dt with an assumption
that the crack extension will results when same atomistic
rearrangement will occurs at the crack tip that is
rate-contorolling, were defined.
The agreement of results shown in Fig.4 and Fig.5 with the
above-mentioned suggestion can be seen.

Tail part and fracture life

As may be seen in the log(S) or log(C*) vs log(da/dt) relations
shown in Fig.6, certain transient crack growth behavior is evident
in the early stage of testing. The tail part behavior has been
attempted to explain in terms of the curve of the creep behavior
 95

and of the crack length against time(Yokobori et al., 1988). The

initial decrease in da/dt has been empirically confirmed as due to
increase in the electrical potential arising from the deformation
that had occurred on application of load(Fuji et al.,1989). On the
other hand, creep crack initiation life and the residual life can
be evaluated by RNOD criterion and the creep deformation
curve(Yokobori et al.,1989a,b)
In this study, from the relation between the critical point in the
tail part, meaning the minimum displacement rate (§min. in Fig.3)
and fracture life(Tf in Fig.3), the life of creep crack growth was
estimated. Figure 7 shows the relation between §min. and Tf of
materials used. The linear relation seen here is represented by:
log(Tf) + m.log(5min.) = c (1)
The values of m, c in each material are given in Table 3 . And
eq.(1) is noted that the relation is represented by
Monkman-Grant(1956) type formula(Yokobori, 1990c). Of these
features, we expect that prediction of the ultimate creep crack
growth life will become possible in due time by the chronological
changes( dmin. in the early stage, or in the tail part).
Furthermore, in Fig.7, it is seen that the behavior of creep crack
growth for IN-100 super alloy which is a low-ductility material,
will be different from those for low alloy steels.

A part of this study is sponsored by the Science and Technology

Agency, Japanese Government.

REFERENCES
Yokobori A . T . , J r and Yokobori T. (1987). Engineering Fracture
Mechanics, 2£, 805-816
Yokobori A . T . , J r and Yokobori T. (1988). Engineering Fracture
Mechanics, 3 1 , 931-945
Yokobori A.T.,Yamaoku T . , N i s h i h a r a T. and Yokobori T . ( 1 9 8 9 a ) . Proc.
of the 67tn JSME Conf. No.890-50, 90-91
Yokobori A . T . , N i s h i h a r a T.,Yamaoku T. and Yokobori T . ( 1 9 8 9 b ) . Proc.
of tne 67tn JSME Conf. No.890-50, 92-93
Yokobori T . , T a n a k a C , Yagi K.,Kitagawa M., F u j i A., Tabuchi M.and
Yokobori A . T . ( 1 9 9 0 a ) . Tetsu-to-ffagane, 76, 503-514
Yokobori A . T . , J r and Yokobori T . ( 1 9 9 0 b ) . I UTAM SYMPOSIUM ON CEEEP
IN STFUCTVFES, POLAND
Yokobori T. (1990c) VAMAS CREEP CPACK GBOWTHMEETING,!ILIA LA MONTA,
ITALY
Tabuchi M. , Yagi K. and Tanaka C. ( 1 9 9 0 a ) . Proc. of tne 4tn Int.
Conf. on Creep and Fracture of Engi. Materials and Structures 4
729-738
Tabuchi M., Yagi K . , F u j i A.,Kitagawa M. and Yokobori A . T . ( 1 9 9 0 b ) .
VAMAS CEEEP CBACK GPOf/TH MEETING, VILIA LA MONTA, ITALY
F u j i A., Yamaya I . , K i t a g a w a M.and Ohtomo A. (1987) . Tetsu-to-ffagane,
73, 1754-1761
F u j i A. and Kitagawa M. (1989) . Proc. of tne 67tn JSME Conf. No.890-
50, 96-97
F u j i A. and Kitagawa M. (1990) . Proc. of JSFM Symposium, 2 7 - 30
Monkman F . C . and Grant N . J . (1956) . Tne 59tn Annual Meeting of tne
Society ASTM, 593-605
96

Table 1 Chemical compositions of materials used (mass%)

C Si Mn P S Ni Cr Co Mo Ti AI B V Zr Others
A336F22 .14 .10 .53 .004 .003 .16 2..45 1 .03 -
A217 WC9[1] .10 .38 .39 .023 .024
-
2,.25 .87 - -
A217 WC9[2] .15 .71 .54 .012 .015
-
2..48 .94 -
-
A217 WC9[3]
lCrMoV
.11
.27
.59
.07
.64
.69
.015
.003
.006
-
2..11
.002 .38 1..19
.90 -
1 .13 -
-
.005 .24 -
IN-100 cast .15 .01 .01 .003 .001 Rem 8,.51 13.47 2 .98 4.77 5.68 .013 .79 .038 .04(Fe)
N o t e : t U C a s t i n g . A s u s e d [ 2 ] C a s t i n g , A s used[3]New
1000 Ί 1 I I I I ll| 1 1 I I I lll| 1 1 I I I lll| 1 1 I I I II
732°C
έ = Α(σ)η ?
850°C_-

" 100

Used 2.25Q1 Mo Cast n = 10.2

Used 2.25Cr1 Mo Cast n = 8.38
Re-heated 2.25Cr1Mo(Cast) n = 7.51
KrMoV n = 7.06 (byNRIM)
KrMoV n = 13.43 (byNRIM)
IN-100 Cast n = 7.6 (byNRIM)
IN-100 Cast n = 19.1 (by NRIM)
10 I I I I Mil I I I I I Mil I I I I I Mil
10 10" 10 - 3 10- 10"
Minimum creep rate, έ (%/h)
Fig. 1 R e l a t i o n between minimum c r e e p r a t e and a p p l i e d
s t r e s s for materials used
Table 2 Tensile properties of
materials used at room
temperature

0.2%PS T.S. El. R.A.

(MPa) (MPa) (%) (%)
A336F22 424 556 28.8 79.
A217 WC9[1] 278 485 24.3 62.
Renew(by NT) 412 559 28.0 69.
A217 WC9[2] 224 528 22.3 50.
A217 WC9[3] 330 493 26.2 66.
lCrMoV 660 807 21.9
IN-100 cast 784 959 7.0

EP Input current lead

output lead
\xh25.4*i

Time

Fig. 3 Schematic drawing of the

curves of time vs load line
displacement, crack length
Fig 2 CT specimen size
 97

Fig. 4 Relation between δ and da/dt of A336F22 and

A217WC9 steels

Fig. 5 Relation between & and da/dt of ICrMoV steel

and IN-100 alloy
98

ω
Η
CD
O

Cmin.—·*
(tfmin.)

da/dtmin.

log(C')
Fig. 6 Schematic, drawing of tail part in relation
of C*(or δ) vs da/dt
10 rnTTj- "I 1 I I I lll| 1 1 llll
Line
u 1 A336F22(540C)
2 A217WC9(570C)
3 lCrMoV(538C) -\
4 lCrMoV(594C)
10 5 IN-100(732C) "3

0)
u
i i02
U
tu

10

log(Tf)+m·log(δ min.)= c

10 0l —^4 i . ..ml i i nil i ■ i t i m l

10" 10" 10-2 10- u

Minimum Displacement Rate,δ min.(mm/h)

Fig. 7 Relation between minimum load line displacement

and fracture life in CT specimens of materials used
Table 3 Coefficient m, c

Material Temp. Coefficient

•C m c

A336F22 540 -1.013 0.366

A217WC9 570 -0.829 0.645
lCrMoV 538 -0.829 0.538
lCrMoV 594 -0.915 0.585
IN-100 732 -0.762 -0.359
WS6a8

Time D e p e n d e n t F a t i g u e L i f e P r e d i c t i o n Methods
and T h e i r A p p l i c a t i o n s

Dong Zhaoqin He Jinrui and Duan Zuoxiang

Institute of Aeronautical Materials, Beijing, China

ABSTRACT

A modified energy approach, Strain Energy-Frequency Separation(SEFS) method, has been

developed in the present paper. Compared to this method, Strainrange Partitioning(SRP),
Frequency Separation(FS), Frequency-Modified Damage FunctionCOstergren M) and Strain
Energy Partitioning(SEP) method were applied to predict the time-dependent fatigue
lives for GH33A disc and raw material at 7ÜTC, lCrl8Ni9Ti stainless steel at 600*C
The results showed that SEP has the best predictability and SEFS has better one. The
fracture mode of GH33A superalloy at 700*C are found to be as follows, PP type is
transgranular fracture mode, PC and CC types are mixed(transgranular and intergranular)
fracture mode and CP type is intergranular fracture mode.

KEY WORDS
time dependent fatigue; life prediction method; energy approach;nickel-base superalloy;
intergranular fracture; transgranular fracture.

INTRODUCTION

Low cycle fatigue at high temperature is a main failure mode in pressure-vessel

design for nuclear reactors and in hot-section components for jet engines, as well as
for other applications. In order to achieve the objective of predicting component life
under service condition many life prediction approaches like 1) linear life fraction
rule[l], 2) Strainrange Partitioning (SRP) method[2, 3], 3) Frequency Modified (FM) [4]
and Frequency Separation (FS) [5] method, 4) Frequency-Modified Damage Function
(Ostergren M) method[6, 7], 5) Damage Rate method(DRM) [8], 6) Strain Energy Partitioning
(SEP) method[9], 7) Strain Energy-Frequency Separation (SEFS) method [10,11] etc. have
been developed to analyse the high temperature synergistic effects of fatigue creep
and/or environment attack and have been applied with varying degrees of success to the
experimental data on different alloys.

In this paper, SRP, SEP, FS, Ostergren M and SEFS were assesed their predictability
to the time dependent fatigue lives of nickel-base superalloy GH33A and a lCrl8Ni9Ti
stainless steel.

METHODS FOR LIFE PREDICTION AND PARAMETERS USED FOR EVALUATION OF THEM

99
100
The methods for time dependent fatigue life prediction and the parameters used for
evaluation of them are summaried in Table 1 and Table 2, respectively.
Table 1. Five life prediction methods

Name the Form of Equations the Number of Constant

SRP Njk =C jk (Ä€jk ?J* ; (LDR) Nf = Σ Njk j , k=p, c 8

SEP Njk =Cjk (Δ^·κ CTT )BJ* ; Nf = Σ NJk 8

FS Nf =C ( Δ 8 ί η f V? ( V c / ΐ Λ ) K 4

Ostergren M Np =C (A£ in σ τ f y M 11

SEFS Nf =c (Δε,π σ τ ) Β y t M c V c / ιΛ ) K 4

where Bjicand Cj|c(j,k= indices p, c)—constant; ^ 6 j k ~ t h e strain component; Njic—the life

component; N.p — t h e number of cycles to falure; C,B,M,K—material constants; 0 " T — t h e
maximum stress; Δ2ίπ— the inelastic strain range; i^, Vi—tension-going and compression-
going frequency, respectively; y —frequency and reflects wave shape effects and the
properties of time dependent. Its value depends on materials sensitive to wave shapes.
Table 2. Parameters used for evaluation of the methods

Name Expression Physical Meaning

Scatter Max { Nobi/NpK , Npri /NobV > how far away from the mean value the
band data points fall

Standard how well the data points group about

deviation / j/n-i £ [ ig<Nobi/flpri )]2 the mean value

Precent how many data points within the

quantity n0/n x 100* desired scatter band of two

where N 0 ^ , Ν Ρ κ — t h e observed life and the predicted life of the ith specimen,
respectively(l — i — n ) ; n — t h e number of data points; η σ — t h e number of data points
which fit the unequation

l^Max { N o b i / / N p r ; , N p r i / N o b ; > < 2

MATERIALS AND EXPRIMENTAL PROCEDURE

The chemical compositions, the heat treatment and the mechanical properties at room
temperature of the materials used in this paper are shown in Table 3. The specimen
layout and dimensions are given in the Ref. 9.

All tests were conducted in a 50KN MTS closed-loop, strain-controlled electro-hydraulic

testing machine using strain control. Strainrange was measured axially by an
extensometer. The test condition was in the air. For GH33A disc and raw material, a
was
temperature of 700'C selected to accelerate the time dependent process and a
temperature of 400'C was selected to simulate the disc center working condition. The
strain wave shapes are a triangular one with constant frequency(20 cpm for lCrl8Ni9Ti,
 101
30 cpm for the other superalloys). The tensile and the compressive strain hold times
are all 60 seconds.

Table 3.

C h e n i c a l C o m p o e i t i on by Weight %
Material Al Si C Tl Cr Pe Cu Mn »b HI
OH33* .β9 .12 .041 2.85 20.9 20.5 .07 .10 Bal
OH33A A r c - F u m a * e .93 .043 2.88 21.3 — 1 . 42 B al
OH33A Duo-Vacuo .97 .35 .005 2.84 20.9 .80 .01 1 . 45 B al

—
1Cr18Hl9Tl 1.5 .120 18.0 B al 9 . 20

T a b l e Heat Treati■ e nt
Material T e e p e r a t u r e 'c Heat T r e a e n t
OH33A 10Θ0 8 Hours A i r C o ol 7 50 C 16 Hours A i r C o ol
GH33A A r c - F u r n a ce 10Θ0 8 Hours A i r C o o l Ϊ 5 0 C 16 Hours A i r C o ol
GH33A Duo-Vacuo 10ΘΟ 8 Hours A i r C o o l 7 50 C 16 Hours A i r C o o l
1Cr18Hl9Tl Quench 1100 C Water C o ol

Table M e c h a n i c al P r o p e r t i e s a t Room Temperature

Material 0.2% y i e :Id U l t i m a te ■ RA

kg/—2 kg/m«2
GH33A 7B.6 121.5 26.3
GH33A A r c - P u r n a ce 91.3 1 2 4 .1 33.5
GH33A Duo-Vacuo 79.0 122.0 21.0
1Cr18Hi9Tl 28.0 62.00 63.0

OC3 A «WC
SRP «JOEL
! ' -V
' ^ PP «R
· C f l » *E«

CYCLE
S TO FHILURE.
N

F i g . I SRP l i f e r e l a t i o n s h i p s for Fig.2 PP l i f e r e l a t i o n s h i p s for arc fn>

GH35A mat. a t 700 C and duo-vacuo disc mat. a t 700 C

L ET
C Y CS O FAILURE.N<P
>P,PC,CP

Fig-,3 SRP l i f e r e l a t i o n s h i p s for

OH33A disc mat. a t 700C
102

Table 4 Predictability of SRP SEP F S Ost. M. and SEFS

for duo-vacuo at 700C
Model scat. band sta. devi. %
SRP 2.16 • 15 83
SEP 1.79 .13 100
FS 2*4 .21 75
Ost. M. 2.25 .18 92
SEFS 2-13 .18 92

ANALYSIS AND DISCUSSION

From Figures 1,2, 3 we can see that there is no significant difference of the fatigue
lives between the two different processes for GH33A turbine discs at both 400'C and
700*C. The predictability of these methods in terms of scatter band, standard deviation
and is summarized in Table 4.
(1) SRP was better than FS and Ostergren M and has many advantages such as in
establishing bounds of cyclic life, simplifying the temperature effects [12], and
dealing with creep-fatigue problems at multiaxial tests [13]. Specialists' Meeting on
Characterization of Low Cycle High Temperature Fatigue by SRP was called in 1978[14].
General census of the investigators appeared to be positive in agreement that the SRP
method is a significant step forward in time dependent fatigue life prediction[15]. But
for high-strength, low-ductility, high temperature alloys, however, the predictability
of SRP is very poor [11], that is because SRP fails to handle mean stress effects. When
the inelastic strainrange is very small (less than 10 ) it is rather difficult for SRP
to partition and measure the inelastic strainrange exactly. Moreover, SRP method
divided the tests into four subsets and determined the two best-fit constants for each
subset. Recently, Radhakrishnan[17] has analysed the method and shown that SRP will not
explain the tension going time or tensile frequency effect on the fatigue life of the
material and that it will not make a difference between a stress hold and strain hold.

(2) According to Table 4, the predictive ability of SEP, developed by He Jinrui et al,
is the best one. The method surmounts some shortcomings both SRP and Ostergren M and
considers the mean stress effects as compared with SRP. However, the form of SEP is as
complicated as SRP.
(3) From Table 4, the predictability of FS is the worst. But FS method only needs four
constants to fit and the independent variables necessary to find out them are known
during the test. It is simple in calculation. Examples of systems with successful
application of FS method are AISI 304 at 593*C, AISI 316 at both566*C and 704*C[16].
But FS fails to successfully explain the mean stress effects.

(4) From Table 4, the predictability of Ostergren M is a little better than that of FS.
Ostergren M has much more meaning for the life prediction of high-strength and low-
ductility nickel-base superalloys like IN738 and Rene'80 at 871'C (time-independent),
Cr-Mo-V at 538*C (time-dependent, wave shape independent) and AISI 304 at 538'C ( time-
 103

dependent, wave shape dependent)[16]. However, the method uses the different frequency
terms to determine the materials sensitive to wave shapes. Since it is impossible to
determine beforehand which frequency term would be appropriate for the material,
different terms were total to fit. In one word, this method is rather tedious and
complicated in calculation.

(5) According to Table 4, the predictability of SEFS appears to be a little better than
that of FS and Ostergren M. SEFS method, presented in this paper, is based on FS
simplicity and Ostergren M energy approach. The independent variables in SEFS are the
inelastic strain energy which considers the effects of the mean stresses. As early as
in 1910, Bairstow[18] recognized the relevance of hysteresis losses within one cycle.
Inglish[19] related the total hysteresis losses to fatigue life and found that the
total losses increase with decreasing stress amplitude. Lefebvre and Eltyin[20] have
studied the hysteresis energy absorption and its relation to fatigue failure life.
Since the fatigue damage is generally caused by plastic cyclic strain, the dissipated
plastic strain energy is an important parameter [21-23]. The irrecoverable plastic
strain energy per cycle is the area of the hysteresis loop. Felther and Morrow[24]
proposed that it is the plastic part of the hysteresis energy which is a constant at
fatigue failure. Miner's hypothesis [25] of the linear summation of fategue damage is
based in the assumption that the total hysteresis losses are independent of stress
amplitude. Gatts [26] analysed cumulative damage in fatigue from the standpoint of
strain energy. Gatts cumulative damage theory was proposed. Izumi, et al [27], attempted
to derive a fatigue crack propagation on the basis of the energy required to damage the
material. Halford[28] summarised the relationship between fatigue failure and plastic
strain energy. Radhakrishnan[29] believed that it is appropriate to take the energy
which combines the stress with the strain as the variable necessary for life prediction
and proposed an interaction diagram for predicting the time dependent fatigue
life. Shahani and Popp [30] believed that there is much more potential as energy
approach for time dependent fatigue life prediction. In summary, life prediction

Fig.4 Transgranular frac. Fig.5 Intergranular frac. and dimplex

Fig. 6 Intergranular frac. Fig.7 Intergra. frac. and secondary cracks

104
In order to analyse the fracture mode, four specimen, PP type (Spec. No. 29), PC
(Spec. No. 23), CP (Spec. No. 17) and CC (Spec. No. 63) of GH33A raw material at 7u(TC
were chosen. Metallographic examination and analysis were conducted on selected
specimens and included the interpretation of the time dependent fatigue results.

Specimen tested with the PP type deformation exhibited primarily a transgranular

fracture mode. As shown in Fig.4. This is a common fracture mode for materials tested
at high frequencies where creep deformation is negligible. This fracture mode reflected
in the highest fatigue lives.

Specimen tested with the PC type deformation exhibited a mixed (transgranular and
intergranular) fracture mode. The intergranular fracture mode is a typical of the creep
fracture. Fig.5 are intergaranular crack + dimlples. This fracture mode reflects the
fact that PC deformation resulted in the lower fatigue lives than those of PP.

Specimen tested with the CP type deformation exhibited a predominantly intergranular

fracture mode. As shown in Fig. 6, this is a typical of the creep fracture. In general,
intergranular crack initiation and propagation occur at a faster rate than
transgranular cracking in a nickel-base superalloys and the presence of this fracture
cycling resulted in the lowest fatigue lives.

Specimen tested with the CC type deformation also exhibited a mixed fracture mode.
Intergranular cracks and secondary cracks are shown in Fig.7. This fracture mode
reflects the fact that CC deformation resulted in the fatigue lives between those lives
between those of PP and CP.

CONCLUSIONS

1. The test results of time dependent fatigue of nickelbase superalloy GH33A turbine
discs with two kinds of melting process shown that there is little difference between
the two different processes at both 400*C and 700*C·

2. The predictabilities of SRP,SEP, Ostergren M and FS were carefully compared and

analysed for GH33A disc and raw material at 7GTC, lCrl8Ni9Ti at 600*C Only was the
SEP able to predict the materials within the scatter band of two. The predictability of
the other three methods is SRP, Ostergren M and FS, in turn.

3. SEFS, presented in this paper, is the syntheses of FS and Ostergren M and has better
predictability.

4. The fracture modes of GH33A raw material at 700'C are PP type is transgranular
fracture mode, PC and CC types mixed (transgranular and intergranular) and CP type
intergranular. At high strainrange, CP type is most damaging.
WS6a9

THE PREDICTION OF THE LCF LIFE AT ELEVATED TEMPERATURE

OF A CT SPECIMEN AT 650 C

JIYUE LI and QINGXIONG YANG

Department of Aircraft Engineering, Northwestern Polytechnical University,
Xian, Shaanxi 710072, PRC

ABSTRACT

In this paper, the authors calculate the cyclic elastic-plastic-creep deformation of a CT specimen
made of superalloy GH36 tested at 650 °C by developing a finite element program CYCEPC. Then,
the low cycle fatigue life at elevated temperature of the specimen is predicted by using the Strain
Range Partitioning method. Both the deformation analysis and the life prediction are in good agree-
ment with the experimental results.

KEYWORDS

Elastic-plastic-creep; FEM analysis; LCF life prediction; SRP method; CT specimen.

INTRODUCTION

The low cycle fatigue life at elevated temperature of the component suffering from both fatigue dam-
age and creep damage (or say, their interaction) is severely limited. The Strain Range Partitioning
(SRP) method has been widely verified for its validity in predicting the low cycle fatigue life at ele-
vated temperature for many types of materials. Based on the SRP method, the LCF life at elevated
temperature of a simple component— a compact tensile specimen is predicted. Usually there are three
main steps to accomplish such a work, they are (1) to determine the hysteresis loops of the critical
points for the specimen under cyclic loading; (2) to divide the inelastic strain range into the plastic
strain range and the creep strain range; (3) to predict the low cycle fatigue life of the specimen under
the test conditions according to the four different life curves of the same material.

THE CALCULATION FOR THE HYSTERESIS LOOPS OF THE CRITICAL

POINTS OF THE CT SPECIMEN

When tested at elevated temperature, there are both elastic / plastic deformation and creep / relaxa-
tion deformation for each point of the CT specimen. So the stress and strain fields vary with time. In
this paper, the authors calculate the elastic-plastic-creep deformation of the specimen for the first
few cycles in accordance with the loading history to obtain the hysteresis loops of the critical points

105
106

for the specimen.

The CT specimen is shown in Fig. 1 and the loading history in Fig. 2. The specimen is made of GH36
superalloy, its chemical composition is shown in Table 1 and the mechanical properties in Table 2.
The loading cycle is composed of the following reversal: oa, ab, ca', ... . For reversal oa, ab, ca' (each
has a time increment Δ ΐ and / or a load increment Δ Ρ ) , we can divide them into several time steps
and load steps. For each step, the elastic—plastic deformation is calculated first and then the creep
deformation. In order to calculate the cyclic elastic-plastic-creep deformation field, the authors
develope a finite element program CYCEPC and its validity is checked by the calculation of a ro-
tating disk as shown in Fig. 3. From Fig. 3, we know that the calculated result is in good agreement
with the analytical solution.

For the CT specimen, due to its symmetry to the X axis, we just consider the upper half of the speci-
men. The FEM grid is shown in Fig. 4. The 8-node isoparametric element is used, the total number
of the elements for the specimen is 40. In the program CYCEPC, the calculation of the elastic—plastic
deformation and that of creep deformation are the two key parts.

THE CALCULATION OF THE ELASTIC-PLASTIC DEFORMATION

In the paper, we assume the material behavior to be tensile / compression symmetrical and isotropic.
When the specimen is tested at constant high temperature, it is better to use the initial stress method.
The equilibrium equation for each load increment Δ{Ρ} is
[K] Α{δ} = A{P} + {R-} (1)
where the second term {R } in the right hand side is the 'initial stress ' equivalent nodal load and it
has the form
{Λ'}=Σί,[*] Τ [ΰ,Ρ]Δ{<5}<ίΚ (2)
2

where £ means that the superposition is carried out only in the plastic zone and [Dp] is expressed as

3{σ}3{σ}
[/>,]- — (3)

where H' can be determined from the stress-strain diagram. For the iteration criterion, the displace-
ment increment between the two succesive iteration is used in the formular
Ι|Δ<*,}-Δ{«.}||
< /ο (4)
||Δ{ί α }||
where Δ{<5 1 }— displacement in the current iteration;
Δ{(5 0 }— displacement in the last iteration.

After finding the nodal displacement increment Δ{<5}, the strain increment Δ{ε} can be obtained
from Δ{ε} = [Β] Δ{<5} and [B] is the geometric matrix. In the plastic zone, we have Δ{ε} = Δ { ε ' }
+ Λ{ε"} , Δ{σ} = [D ] Δ{ε},ίη6η the elastic and plastic strain increments will be
Δ { ε ' } = [D] Δ{σ} and Δ{ε*} = Δ{ε} — Δ { ε ' } .Note that in the above Δ{ε} no creep strain
is included. If we add Δ{ε Ρ } of each reversal, the accumulated plastic strain Δ ε is obtained and
it can be used to predict PP—type life with the SRP method.
 107

THE COMPUTATION OF THE CREEP STRAIN

In Fig. 2, the load increment Δ { P } is zero during each A t i for reversal ab. Owing to the creep / re-
laxation effect, the stress and strain of the specimen will redistribute. Under constant high tempera-
ture, if we neglect the thermal strain, the total strain is expressed as
Δ{ε} = Δ { ε ' } + Δ { ε ' } + Δ { ε ' } (5)
The stress increment is
Δ(«) = [ ί ΐ ( Ρ ] Δ ( 5 ) - Δ ( ( ' } ) (6)
If [2?]Δ{£} < Δ { ε } the stress relaxation occurs in the specimen.

Experiencing Δ ί , the equilibrium equation becomes

[ Κ ] Δ { ί > - { * ' } + iiriB)T[Dp](lS]MS}-A{ec})dV (7)
1+2

where {R°} is the creep equivalent load, it is {Rc} = £ j [B] [De]A{ec}dV and the second term
1+2 2

is the plastic—creep equivalent load. £ stands for elastic zone plus plastic zone and £ for plastic
zone.

The computation of the Α{ε°}

In this paper, the Bailey—Norton law is adopted to describe the creep behavior. It has the form of
e=Aamtn (8)
where A, m and n are constants that depend on temperature. The value of m is greater than one; n is
usually a fraction.

For the multiaxial stress condition, the creep strain rate is

KrXSu ( U = 1,2,3) (9)
η η
where λ = -Αησ t for time—hardening and λ = -Α ησ (ε ) " ,here σ is the Mises equi-

valent stress; Jc is the equivalent creep strain; S.. the stress deviation.

Iteration criterion

In the equilibrium equation, there are two items to be determined: Δε.. and Δ{5}. The iteration pro-
cess is similar to that of the plastic computation. So the norm controlling the converge of the
iteration is similar to eq.(4).

The stress reversal

In the cyclic computation, we cannot avoid the negative loading which yields the phenomenon of
stress reversal. Here, we assume (1) the creep curve of the negative stress is symmetrical to that of the
positive stress; (2) The creep behavior of the negative stress is not affected by the accumulated posi-
tive creep strain as if the material is a virgin one.
108

For the complex stress reversal, the creep curves are shown in Fig. 5. From eq. (9), we know
AsC = i C (εΗ,σ,Τ)Αί
where the creep strain rate is the function of ε ,σ and T and ε is determined by the origin of the
creep curve as shown in Fig. 5. So it is important to know (1) when the stress reversal occurs in the
specimen; (2) the corresponding origin of the creep curve for the cyclic creep computation.

The determination of the stress reversal. Let the creep strain be sJ at an arbitary time /. and the ori-
gin be e . If
( £ / C - 8 + )Afi C <0, or (£/C-e")AeC<0
the stress reversal occurs as shown in Fig. 6. As shown in Fig. 5, whether ε or ε , if it exceeds the
former level, it is necessary to build the new origin ε + or ε ~ from which the creep response will be
calculated; if not, the creep response after the stress reversal will be based on either ε for strain-
hardening or / f o r time—hardening as shown in Fig. 7.

The separation and accumulation for plastic and creep strains

The plastic strain will accumulate only at the plastic zone or when the local stress increases due to the
redistribution of the stress and strain upon unloading. Similar to the computation for the plastic
strain, the creep strain will accumulate at each time increment and at each reversal. Adding up the
accumulated plastic and creep strain increments, we can depict the hysteresis loop of the critical point
of the CT specimen. By partitioning this loop, we can get the three different strain ranges, Δ ε ,
A e c c ,Aspc or Ä 8 c p a n d then the low cycle fatigue life at elevated temperature of the specimen
can now be predicted by using the SRP method.

THE PREDICTION OF THE LCF LIFE OF THE CT SPECIMEN

AT ELEVATED TEMPERATURE

By utilising the procedures stated above, one can calculate the elastic-plastic-creep stress and strain
fields of the two—dimensional component under various loading waves . From the calculation
results, one can also determine the critical point and its separated accumulated plastic and creep
strain ranges on which the LCF life at elevated temperature of the specimen is predicted.

In this paper, the author calculated the elastic-plastic-creep deformation of the CT specimen shown
in Fig. 1 under the loading history of the tensile-holding (the load P = +1000—1000 kg, the holding
time t = 3 minutes). From the calculated results, we know that the point B is the critical point which
is the nearest Gauss point to the notch root and we will use the data of the point B to calculate the
LCF life of the CT specimen. The calculated results of the point B is demonstated in Table 3.

Duan Z.X. (1985) determined the four different SRP life equations of the superalloy GH36 material
at 650 °C and they are
N„ = 2.133Δ*,, - » , Ncc = 0.922Aecc - 0.947

Ncp = 0.274Δε„ - ' " " , Npc = 03362Δε,,

So, substitute the calculated values of the above strain ranges intothese life equations and employ the
 109

interaction rule, the crack initiation life of the specimen will be

F
_L=^PP_ ^cc_ CP _ 0.25984 0.33283 0.40732
4 4 2
N
i N
PP + N
cc +N
CP ·30 + 98
'39 + 50
·03

thus Nf = 82 (cycles)
This predicted life value is in good agreement with the tested value which is 69 cycles in our work
(Jiyue Li, 1986). The deviation is within a factor of two.

CONCLUSIONS

From our work stated above, we have the following conclusions:

(1) It would be impossible to predict the LCF life at elevated temperature of a real component if we
could not predict that of a specimen in the laboratory conditions. The experiment and the theoretical
analysis verified the validity of the procedures we used to predict the LCF life at elevated tempera-
ture of the CT specimen.
(2) From comparison between the calculated displacement and the measured displacement values of
the loading point and the comparison between the predicted life and the tested life, the finite element
code CYCEPC and the calculation method in this paper proved to be reasonable and applicable.
Though some of the assumptions still need to be checked, i.e., the symmetry of the tensile / com-
pression creep curves and the treatment of the stress reversal, etc..
(3) By use of the FEM code CYCEPC presented in this paper, we can calculate the stress and strain
fields cycle by cycle and then determine the critical point and its hysteresis loop upon which the LCF
life at elevated temperature of a real component is predicted.

REFERENCES

Duan Z.X. et al.(1985). The Research on the Creep / Fatigue Interaction Characteristics of the
Superalloy GH36, Internal Report, Beijing Aeronautical Materials Institute.
Li Jiyue (1986). The Experimental Research on the Creep / Fatigue Life Prediction of A CT
Specimen, Internal Report. NorthwesternPolytechnical University.
Kraus H. (1980). Creep Analysis. John Wiley & Sons, Inc., U.S.A.
Mendelson A. et al. (1959). A General Approach to the Practical Solution of Creep
Problems, Trans. ASME J. Basic Engng, v81, Series D, n4,585-598.

Φ 12.5
2 hoi« p

^ ^ a b a' b'
1 ("^*. ~
Φ 10 / y~ £

P
^
**
c
:o
1 30.5
42.5
Fig.2 The loading history
Fig.l The CT specimen
110

stress (Teg/mm")

42
ΓΤ77Ί
35 <rr at inner radius
kJV-V-
28 jsNVT
21

14

10
0.001 0.01 0.1 1 ™ ° 1000
time(hrs.)

Fig.3 The stress relaxation curve for the disk Fig.4 The finite element grid

1 »7
*» ug

■ ri
o i II *4
J
i 1
1
*io
1 t
\~Ä£tNf r
o

.1 t, t *, t

t Fig. 6 Criterion for stress reversal

Fig.5 Stress reversal for different levels of stresses

Table 1 The chemical composition for GH36 alloy (%) o-

ΠΖΓ
:
C | Si i En Cr ! Ni i Mo i Nb Ti j V j S I P : N

0.39 j 0.55 j 8.50 j 12.5 j 8.0 1.25 | 0.375;<0.121 1.335!<0.03'<0.03! <0.1

Fig.7 The origin for stress reversal

Table 2 The mechanical properties for GH36 alloy (kg / mm )

Temp. C E a„ ff
02
20 20700 99 69
300 18340 86 68
400 17400 78 61
500 16490 75 59
600 15600 67 56
650 15185 63 53
700 14745 56 50

Table 3 The three different equivalent strain ranges of point B

^"^"""-^-^^strain ranges
Δί' AiC Αε"
cycle "^~-^_^^

cycle ob 0.00563 0.01702 0.02265

cycle bC 0.01446 0.00721 0.02167

WS6a10

NEW CORROSION-RESISTANT NICKEL-BASE SUPER-

ALLOYS AND TECHNOLOGICAL PROCESSES OF
CASTING GAS TURBINES PARTS WITH DIRECTIONAL
SINGLE CRYSTAL AND REGULABLE EQUIAXIAL
MINIMIZED MIQROPOROSITY STRUCTURE

Y.I.ZVBZDIN, E.L.KATS, Y.V.KOTOV, V.P.LUBENETS,

E.V.SPIRIDONOV, M.L.KONTER
RPO CNIITMASH, Moscow, USSR

ABSTRACT
In recent years with the help of computer technology we have
developed new creep and corrosion resistant alloys and advan-
ced techniques of precision casting of parts of stationary gas
turbins and diesels·
KEYWORDS
Superalloys; creep properties; corrosion resistance; blades;
turbine; cast; vanes; thermal fatique; processes of SC, DS;
structures.
Owing to increase of gas temperature at the inlet of the tur-
bine, use of cheaper sorts of fuel and increase of performan-
ce - life of stationary turbine parte up to 30.000-50.000 ho-
urs a new series of superalloys was to be developed for pro-
ducing high temperature turbine components.
The main features such alloys designed for production of wor-
king blades of the first stage of turbine were high creep re-
sistance characteristics, resistance to thermal and mechanical
fatigue, sufficient level of plasticity, as well as resistance
to sulphur corrosion, which provides for continuous operation
of a blade with a damagen protective loating during a year,
i.e. the whole period between the cheek insections of the tur-
bine.
Alloys from cast leading vanes and segments of combustion cha-
mbers operating without coating had to possess a much higher
standart of corrosion resistance, besides a high sufficient
high resistance to thermfatigue and creep, adiquate weldibi-
lity.

Ill
112
To create the new series of materials a system of sutomated
computer aided design to research new Nickel superalloys has
been as developed (flg.1). This system has a number of substa-
ntial differencies from the previous similar computer systems.
The program includes the calculation of volume ratio and che-
mical composition of jf -matrix, f -phase, carbon and boron
that appear after casting, heat treatment and aging. This com-
puter system has a high accuracy. For example, creep resistan-
ce of alloys in the temperature range of 800-850°C is determi-
ned with an error up to 3-4%.

I ALLOY COMPOSITIONS (mas ) ~)

| ALLOY COMPOSITIONS ( a t ) " |

ΙΐΛΝΟ T $ CALCULATION

DENSITY, THERMAL
EITPANSMN COEFF, ELASTIC
MODUL OF ALLOYS
~i~
5ULFIJMTI0N RESISTANCE SENDRITE COMPOSITION OrTBONil
. . ._.
COMPOSITION 'ACES
SENORITE SPACES I
. 1 IN CRUCIBLE TEST
_ J 2 IN BURNER RIG TEST 1— I 7—
" j RS A N0NCATA5TR0FIC | VOL FRACTION OF y ' - PHASE
MECHANISM PARflMf-
TERS I PARTITIONING RATIOS OF ELEMENTS "|

I CALCULATION OF Y AMD /'COMPOSITIONS 1

&?—r-L- i i τ=ί
[H '-IMNGEB BYN/PHACOMPr I
— i i I
[STACKING FAULT ENERGY
i i
OF γ
i —
1

TCP-3HNGE» BYMdPMACOMP | I LATTICE PARAMETERS AND MISMATCH I

I I I
I J.-W- BANGER | THERMAL EXPANSION COEFF.. LATTICE
PARQMETERS AND MISMATCH AT
I Ni.Ti-Tj ANGER I EXPLORTflTION TEMP _ _ _

I A-C« -HANGER 1 CREEP RUPTURE LIVES AT

1025-U23K ( A S CC ALLOYS)

M U L T I C R I T E R I AL
yp-T^OST OF MATERIALS I
OPTIMIZATION

Pig. 1. Procedure of computer-aided

alloys design. (L - limita-
tions, O.P. - optimization
parameters,

Application of this computer model in RPA CNIITMASH helped in

development in cooperation with other Soviet organization of
several new alloys of type CNK with predetermined operational
characteristics within a short period of time and with mini-
mum research expenditures (fig.2).
The composition (main elements) of type CNK alloys are follo-
wing (medium means) (wt %)t
CNK-7: Cr-15; Co-9; Mo + W - 7,5; Ti + Al - 8;
CNK-8: Cr-13; Co-8,5; Mo + W - 7,5; Ti + Al + Nb - 9,5;
CNK-17: Cr-13,5; Mo + W - 5,5; Ti + Al + Nb - 8,5;
CNK-21: Cr-22; Co-11;.Mo + W - 4; Ti + Al + Nb - 7
CNK alloys alloying B, Mn and C.
This first alloy of this type CNK-7 (fig.2) was developed and
found wide application in the early 80-s. Nowadays this uni-
versal alloy of conventional castings, with directional soli-
dification and monocrystal structure is one the major Nickel
 113

Pig· 2. Gas Turbine's and diesei engines

alloys. (Metall los by not corro-
sion 900°C, 20h in Naά9S0,
4
-
-25% NaCl, mm)
superalloys of the Soviet stationary gas turbine building.
It to a certain degree surpasses alloys IN 738LC and GTD111
in performance characteristics and in direct crystal formation
has creep resistance factor close to In 792 with a considerab-
ly higher corrosion resistance. Alloy CNK-7 has good technolo-
gical and operational records, shows a high phase stability
during a long-term cervice life. A typical structure of this
alloys after heat treatment is shown on figure 3. The volume
ratio of -phase is about 48%.
For manufacturing working blades of modern high temperature
turbines alloy C M - 8 possesing high creep resistance characte-
ristics has been developed and put into operation (fig.2).
Alloying process guarantes the most effective resistance to
group creeping of dislocations through the particles of
-phase due to optimum combination of forming -phase and
strengthening the matrix elements. An alloy with monocrystal
or directional structures has a high tendency to dendritic
strengthening and an exellent technological characteristics -
modification CNK-8M. The volume ratio of -phase - 52-55%·
Alloy CNK-8 surpasses in corrosion resistance both alloys
IN792 and MARM246. C M - 8 and IN792 are similar in creep resis-
tance characteristics, while CWK-8M in no"worse in properties
MARM246 by conventional casting.
The new alloy CNK-9 direction solidification (DS) is similar
in creep resistance properties to alloy MARM246 DS and has
114

a b c
Fig. 3· Morphology of ^'-precipitates
(CNK-7DS) (a - after standard
heat treatment,6 b - after aging
- 5000h at 850 C, c - after
6000h RUN in turbine GTN-25;
X15000)
sifficient corrosion resistance. CNK-9 alloy is characterized
by the volume #" -phase of about 60% and rather high strengt-
hening of matrix
For high-pressure leading blades designed for uncoated opera-
tion alloy BC-5 strengthened by 35-38% of -phase in whitch
carbon is subsituted by boron (0,1%) is used. The alloy surpa-
sses Udimet 720 in corrosion resistance and equals it in creep
resistance.
Weldibility alloy CNK-21 better corrosion resistance characte-
ristics alloy BC-5 but in equals to alloys FSX-4H and IN939.
The advantages of alloy CNK-21 in contrast to the alloy FSX-
- 4 H is its better creep resistance and in contrast to the al-
loy IN939 - much lower cast. Alloy CNK-21 is designed for cas-
ting of leading vanes of imported turbines series MS.3000 and
MS.5000 instead of alloy FSX-414.
Combustion chambers of gas-turbine are traditionally manufac-
tured of sheet materials of type Hastelloy X, characterized by
strengthening of ^ -matrix. Creep-resistance characteristics
of Hastelloy X do not meet the standards necessary for materi-
als used in combustion chambers of the latest design. However,
further rising of temperature in turbines led to necessity of
creating of cooled combustion chambers, const ting of cast
segments of complex profile. Creep resistance requirement to
materials used in combustion chambers are several times than
of alloys of this type.
Alloy CNK-24, the new alloy, made by us, is the best by corro-
sion resistance parametres as compared to above indicate allo-
ys. It equal to alloy IN935 in corrosion and creep resistance
characteristics, but.CNK-24 has tho times lower content of Co
and NB, therefore it lower cast. Besides it has high thermofa-
tigue resistance and crack resistance in welding.
For manufacturing of cast wheels for turbocharging systems a
series of economically alloyed materials CNK-1bf CNK-17, CNK-
 115
-18 has been developed with creep resistance properties equal
to alloys B19H, IN713LC, GMR235D but suprasses the above in
resistance to corrosion · The alloys have good performance
characteristics for manufacture wheels with equally-axed and
radual-directed structures·
However wheels of turbocharging system working under maximum
strain, for instance in racing cars, are manufactured from al-
loy CNK-8M having monocrystal structure.
On the basis of computer models we have developed several tech-
nological processes of casting of parts from superalloys. In
particular we have developed a tho-dimensional model of direc-
tional solidification process of the method of finite elements
which alloys to simulate any combination of cooling conditions
of a given mould providing different results depending on di-
mentions of the casting and shaping of the foundry block, con-
struction of the not zone of furnace and cold zone, specific
features of heat isolation baffle between two.
In consequence of analytic and abequate experimental researches
recommendations have been worked out aimed at optimization of
parametres for technology and manufacture of equipment for di-
rectional solidification of monocrystal castings with liquid-
metal cooling of moulds. The application of this allowed to
obtain castings with fine dendrite monocrystal structure with
high and stable mechanical characteristics.
This process takes plase with changeable programmable velocity
W of mould movement witchin the range of 10-30 mm/min. For
comparison we shall note that when side surface moulds are co-
oled by radiation, as this taken in known process of direction
solidification, velocity W is 3-5 mm/min.
Like that directional solidification with liquid-metal cooling
of moulds secures great increase the productivity of process;
it is compatable with convential casting in cost. That allows
extand use of direction solidification in casting of blades
and vanes.
On the basic of computer analyses we have also developed tech-
nological methods of casting of differents large-scale details
with minimized microposity and controlled equally-axed struc-
ture; technologybof special metallurgical procedure superallo-
ys to increase and stabalize their heat-proof qualities; pro-
grammes for designing and manufacturing of die-moulds for pro-
ducing castings with high dimensional accuracy; optimised re-
gimes of heat treatment for improving of a sat of qualities of
the above said alloys elaborated a CNIITMASH association.
So, the above research programme of developing new high corro-
sion resistance Nickel-based superalloys and progressive tech-
nological processes of casting provided improvement in effi-
ciency of working characteristics and lowered cost of large-
116

Pig» 4. High temperature components manu-

facture according to the developed
technology and from the superalloys
offered
scale production of a wide assortment of cast working and lea-
ding blades, elements of combustion chambers and other parts
of high temperature components of gas turbines as well as tur-
bine wheels for turbocharger of diesels (fig.4).
WS6b1

CREEP LIFE ASSESSMENT TECHNIQUES FOR PIPING

R. Viswanathan and S. Gehl

Generation and Storage Division, Electric Power Research Institute,

3412 Hillview Avenue, Palo Alto, CA 94303, U.S.A.

ABSTRACT

Significant advances have been made during the last five years in predicting
crack initiation and in assessing crack growth in high temperature components
operating in fossil power plants. These advances are reviewed.

KEYWORDS

Creep, hardness, microstructure, rupture tests, crack growth.

LIFE FRACTION RULE FOR CREEP

In a multiclient sponsored project recently completed at the ERA Technology

Ltd.; an extensive body of long time data has been generated, with the specific
intent of verifying the LFR for varying temperature conditions^). Two heats of a
0.5 Cr-0.5 Mo-0.25 V steel were evaluated: A pipe grade steel with a
predominantly ferritic microstructure and relatively high ductility (15%
elongation) under long term service conditions designated MG and a cast turbine
casing steel with a bainitic microstructure and low ductility (3.5% elongation),
designated as FW. Specimens from heat MG were initially subjected to creep
damage fractions of 0.25, 0.45, 0.63 and 0.82 at 575°C at a stress of 69.5 MPa;
specimens from heat FW were also subjected to similar levels of initial creep
damage of testing at 550°C and 84.9 MPa. The predamaged samples were then
subjected to accelerated rupture testing at higher temperatures, holding the stress
at the same level as in the initial creep damage tests.

The correlation between the expected life based on the LFR and the actually
observed life for the two heats (see Figure 1) shows that the LFR predictions are
accurate within a factor of about 2. The correlation between prior expended life
fraction and the remaining life fraction measured in the accelerated tests shown
117
118

in Figure 2 may be used as a modified basis for LFRusing Σ ~ = 1 and <1 as

conservative basis of life prediction of ductile and brittle materials, respectively.

OXIDATION AND SPECIMEN SIZE CORRECTION

Another refinement to calculational procedures being developed by ERA

Technology Ltd., is a correction factor for oxidation and specimen size effects/ 2 )
Preliminary results from one heat of 2 V 4 Cr - 1 Mo steel (Heat BSH) have shown
that the rupture life in air is increased by increasing the specimen size from 2.5 to
9 mm, with a further increase of life in argon. The effect becomes increasingly
pronounced at combinations of time-temperature resulting in large values of
Larson-Miller parameter. The different curves converge at low values of LMP.
Limited data available suggest that rupture curves for the 2.5 m m specimen
argon tests and for the 25 mm specimens tested in air may superimpose; in other
words the argon test results may be treated as being typical of component
behavior in air at thickness levels in excess of 25 mm.

The rupture data for various specimen sizes can be plotted as a ratio of the
rupture lives using data from the 2.5 mm specimen tested in air as the reference
condition. This ratio referred to as the oxidation correction factor (OCF) for
different stress levels is shown in Figure 3. In remaining life calculation
procedures, the stress rupture curves used are generally based on test results
from small specimens tested in air. Application of the OCF can yield more
realistic and less conservative predictions of heavy section component life.

HARDNESS BASED TECHNIQUES FOR CREEP DAMAGE ASSESSMENT

Currently used procedures for calculating creep life consumption, use standard
Larson-Miller plots applicable to virgin material and do not take cognizance of
the fact that the Larson-Miller parameter for rupture decreases with in-service
aging. A model that explicitly takes into account, the decreased rupture life due
to softening has recently been developed for 2 V 4 Cr - 1 Mo steels by Grunloh and
Ryder(3). The effect of aging on creep rupture endurance is modeled by the
incorporation of the UTS (ultimate tensile strength at room temperature) into
the 2nd -degree polynomial shown in Eq. 1.

LMP(rupture) = 40975 + 57 (UTS) - 5225 (log σ) - 2450 (log σ) 2 (1)

In this equation, time, temperature and stress are in units of hours, °F and ksi,
respectively.

The effect of aging is taken into account by applying an aging correction factor to
the original UTS, based on known kinetics of aging for the steel. Using
temperature, applied stress and starting UTS as input, a computer code calculates
the LMP for rupture in the aged condition and hence t r at 1000 hour intervals.
The incremental damage for each time step and hence the cumulative damage
t / t r can be calculated. Kimura, Fujiyama and Muramatsu have developed a
similar approach to calculate creep life consumption of CrMoV rotors^).
 119

CREEP CAVITATION MODEL

Neubauer and Wedel, characterized cavity evolution in steels at four stages—i.e.,

isolated cavities, oriented cavities, linked cavities (microcracks), and macrocracks
and formulated recommendations corresponding to the four stages of
c a v i t a t i o n . ^ To provide a theoretical and quantitative basis for cavity
evolution, Cane et al used a constrained-cavity-growth model and proposed a
relation between the number fraction of cavitated boundaries ("A" parameter)
and the life fraction consumed using heat specific experimental constraints.
Based on interrupted creep tests on simulated heat affected zone lCr-0.5Mo
steels, Shammas et al concluded that the data had too much scatter to verify the
life-prediction model of Cane. The data could nevertheless be used empirically,
by plotting all the data together in the form of a scatterband whose lower limits
are defined by the e q u a t i o n ^ :

A = 0.517 ( r ) - 0 . 1 8 6 (2)

A method of assessment that is an alternative to the A parameter has also been

proposed by Shammas. The damage classifications have been correlated with life
fractions , and thus a life-fraction range has been established for each class. The
Wedel-Neubauer classifications of material condition (undamaged, class A, class
B, class C, and class D) correspond roughly to expended-life-fraction (i.e., t / t r )
values of 0.27, 0.46, 0.65, 0.84, and 1, respectively. Since the expended life fraction
t / t r corresponding to various damage classifications is known, the remaining life
can be calculated using the relationship

trem = t ( j - l ) (3)

where t is the service life expended. The remaining life corresponding to

various damage classifications can be calculated to be 2.7t, 1.17t, 0.54t and 0.19t for
undamaged material, isolated cavitation, oriented cavitation and microcracking,
respectively. By applying a safety factor of 3 to the above values, the safe
reinspection intervals can be established to be 0.9t, 0.4t, 0.18t and 0.061,
respectively. This approach has been developed and applied by Patterson as
shown in Figure A^7\ The figure clearly shows that the reinspection interval is
not only a function of the current damage level, but also the service life elapsed,
unlike in the Wedel and Neubauer approach, where the reinspection interval
prescribed is independent of service life elapsed. For all combinations of damage
classification and service life in regime B in the figure, the new approach results
in increased inspection intervals. Adopting the new approach by several utilities
has resulted in significant savings in inspection costs ®\ An illustration of the
inspection intervals according to the old and the new procedures, for a plant
which has been in service for 30 years is shown in Table 1.
120

ISO-STRESS RUPTURE TESTS

The isostress rupture test procedure consists of conducting accelerated rupture

tests at temperature above the service temperature. The stress is kept as close as
possible to the service stress value. The results are plotted as log t r vs T and
extrapolated linearly to the service temperature to estimate the remaining life.
Results from recent research have identified the limitations and possible
refinements to the technique.

Results described earlier suggest that linear extrapolation of results from

temperature accelerated test may yield optimistic prediction of remaining life
under service conditions in the case of ductile materials; the reverse would be
true for brittle materials. In either case, the predicted values are expected to be in
agreement with the actual value within a factor of ±2. This conclusion is in
agreement with that of M e l t o n ^ . Unfortunately it is generally difficult to define
"brittle" and "ductile" class of materials since ductility can vary from heat to heat
and with the test conditions. For our purpose we can define a "brittle" steel as
one prone to creep damage by cavitation and a ductile material as one in which
creep damage occurs primarily by softening. This is consistent with the
observation by the ERA researchers that the ductile cast MG showed no evidence
of cavitation even at a life fraction consumption of 0.82 while the brittle cast FW
cavitated profusely. Using this definition, castings, coarse grained heat affected
zones in welds and fusion line in welds may fit under the 'brittle' category, while
the base metal in forgings and piping and tubes may fit in the "ductile" category.

Since isostress tests are normally conducted in air, oxidation correction factor
described earlier is also important. The extrapolated remaining life values
obtained from the accelerated tests should be corrected for oxidation effects. If
tests are conducted in inert environments, no correction factor would be needed.
A further refinement to the technique consists of the use of miniature
specimens, to minimize sample requirements. It has been demonstrated that
miniature specimens (10 mm long, 3 mm dia.) tested in argon, yield results
representative of large specimens tested in air<10).

CREEP CRACK GROWTH

Extensive creep crack growth data pertaining to CrMo piping steels have been
collected, analyzed and consolidated ^11' 1 2 \ It has been observed that a crack tip
driving force parameter termed Q , that takes time-dependent creep deformation
into account correlates much better with crack growth rates, d a / d t than the
traditionally used elastic stress intensity factor K. The relation between d a / d t and
Q can be expressed as

da m
bc
dt = t W)
 121
To perform a remaining-life assessment of a component under creep-crack-
growth conditions, two principal ingredients are needed: (1) an appropriate
expression for relating the driving force Q to the nominal stress, crack size,
material constants, and geometry of the component being analyzed; and (2) a
correlation between this driving force and the crack-growth rate in the material,
which has been established on the basis of prior data or by laboratory testing of
samples from the component. Once these two ingredients are available, they can
be combined to derive the crack size as a function of time. The general
methodology for setting inspection intervals using this approach has been
described elsewhere^13' 14>.

A number of variables have been identified as affecting the crack growth rate by
modifying b, Q or m. The effect of these variables is summarized below.

• In service degradation increases da/dt by increasing Q in the case of ductile

materials and by increasing m and/or b for brittle material.

• Crack growth rates at welds, fusion lines and heat affected zone materials
are at least a factor of 5 higher compared to base metal.

• Presence of localized chains of inclusion, further assisted by segregation of

impurities to interfaces such as grain boundaries and fusion lines cause
significant increases in creep crack growth rates

• Presence of large amounts of impurities in the steel acclerates crack growth

by increasing m

• All material and experimental variables that reduce creep ductility result
in higher crack growth rates

• Temperature can have mixed effects on crack growth. In cases where the
effect of temperature is merely to increase creep rate, the da/dt increases
with increase in temperature due to increase in Q. On the other hand, if a
transition from a brittle to ductile condition is involved, increase in
temperature may actually decrease the crack growth rates.

• Crack tip constraint has a pronounced effect on crack growth.

Assumptions regarding plane stress or plane strain conditions can have a
pronounced effect on da/dt

• Inclusion of primary creep, in addition to the secondary creep in

calculating Q results in larger value of da/dt and reduced remaining life

REMARKS

The authors regret that extensive advancements in this field could not be
properly reviewed due to space constraints.
122
REFERENCES

1. Brear, J.M. and McCarthy, P. ERA Report 89-0230, EPRI project RP2253-2.

2. Brear, J.M. (Dec. 1989). The Effect of Oxidation Upon Long-Term Stress
Rupture Data of ICrMo and 2 V4 CrlMo Steels, ERA Report 89-0662, EPRI
project RP2253-4.

3. Grunloh, H. and Ryder, R.H. (1989). Results from EPRI project RP2253-10,
Private Communication, General Atomics, San Diego.

4. Kimura, K., Fujiyama, K.F., and , Muramatsu, M. (1988). Creep and Fatigue
Life Prediction, in High-Temperature Creep-Fat, Ohtani, R., Ohnami M.,
Inow, T., Ed., Elsevier Applied Science Publishers Ltd. and The Society of
Materials Science, Japan.

5. Neubauer, B. and Wedel, V. (1983). Restlife Estimation of Creeping

Components by Means of Replicas, in Advances in Life Prediction Methods,
Woodford, I.A. and Whitehead, J.R., Ed., ASME, New York, pp307-314.

6. Ellis, F.V., Shammas, M. and et al (Nov. 1989). Remaining Life Estimation

of Boiler Pressure Parts, Vol. 4: Metallogrpahic Models For Weld Heat
Affected Zones, EPRI Report CS-5588, Vol. 4.

7. Paterson, R.S. (1989). Private Communication, APTECH Engineering,

Mountain View, CA.

8. Field Metallography Research Leads to Improved Re-Examination Interval

For Creep Damaged Steampipes, (Dec. 1990). EPRI First Use Report B197.

9. Melton, K.N. (1983). The Isostress Extrapolation of Creep Rupture Data,

Materials Science and Engg., 59, pi43-149.

10. Askins, M.C. and Marchant, K.D. (Jan. 1988). Remaining Life Estimation of
Boiler Pressure Parts, Vol. 2: Miniature Specimen Testing, EPRI Report CS-
5588, Vol. 2.

11. Saxena, A., Han, J. and Banergi, K. (Jan. 1988). Creep Crack Growth in Boiler
and Steam Pipe Steels, EPRI Report CS-5583.

12. Saxena, A. Creep Crack Growth in CrMov Rotor Steels, EPRI RP2481-5
report, in press.

13. Liaw, P.K. and Saxena, A., (July 1986). Remaining Life Estimation of Boiler
Pressure Parts - Crack Growth Studies, EPRI Report CS-4688.

14. Viswanathan, R. (1989). Damage Mechanisms and Life Assessment of High

Temperature Components, ASM International, Metals Park, Ohio.
 123
Table 1. Suggested Re-Inspection Intervals For A Plant With
30 Year Prior Service

1 Damage Classification Wedel-Neubauer EPRI-APTECH 1

Method, years Method, years |

Undamaged 5 27
A. Isolated cavities 3 12
B. Oriented cavities 1.5 5.4
C Linked cavities 0.5 1.8
(Microcrack)
D. Macrocracks Immediate repair Based on fracture
mechanics

O MG
• FW

1000 10,000 100,000 0.4 0.6 0.8

Expected Life Based on LFR Expended Life Fraction
Figure 1 Correlation between actual life in accelerated tests and Figure 2 Expended life fraction versus remaining life fraction in
expected life for two heats of Cr-Mo steel. accelerated test for two heats of Cr-Mo steel.

10 15 20 25 30 35
Service Life Expended (yr)
0.5 1.0
Specimen Thickness (in.)
Figure 4 Service life versus reinspection interval for
Figure 3 Oxidation convection factors with reference to APTECH/EPRI remaining useful life method and the
0.1 inch (2.5 mm) thick specimen. Neubauer-Wedel method.
WS6b3

Correlation Between Magnetic Properties and Microstructural

Changes of Low Alloy Steels Used for Hish Temperature
Components in Thermal Power Plants

Kyung Tae Hong, Jung Man Do and Sung-Kang Hur

Division of Metals, Korea Institute of Science and Technology

P. O. Box 131, Cheongryang, Seoul, Korea

ABSTRACT

2.25CrlMo steels used for boiler tube were creep-tested at 873, 923 K with 100, 50 MPa respectively.
At the various creep damage levels, the carbides were analyzed with EDS and the magnetic
properties were measured with VSM The frequency of occurrence in M 2 C, M 7 C 3 , M^C type
carbides show the relationships with the creep damage. The average Fe, Mo contents in the carbides
can be used to denote the creep damage levels. The coercivity (He) among the magnetic properties
have a similar trends with the frequency of occurrence in M 7 C 3 type carbide. But the absolute
values of He is so small to be used as a main criteria for the creep damage levels.

KEYWORDS

Creep damage, thermal degradation, carbide, coercivity (He)

INTRODUCTION

Low alloy ferritic and bainitic steels were extensively used for the high temperature components
in thermal power plants. The component materials, however, undergo severely the thermal
degradation by long-term service at high temperature. As the microstructure of those steels in
the components was markedly changed with the thermal degradation, it can be used as an parameter
for evaluating the degree of thermal degradation. Long term operation in high temperature changes
the initial carbide into the more stable state (in the thermodynamic view-point). Since these changes
depend on the operating time, temperature and applied stress, the monitoring of carbide
transformation during operation can make it predictable the damage in the high temperature,
pressure components. On the other hand, it was known that the carbides had the tendency to
impede the motion of magnetic domain wall (Cullity, 1972). Since magnetization depends on the
motion of magnetic domain wall, the microstructural changes of carbides might be represented
as those of magnetic properties. This principle can make use of developing new techniques.

In this research, the relationship between magnetic properties and thermal degradation was
investigated. The results showed that the coercivity (He) decreased with the increase of creep
damage.

125
126

EXPERIMENTAL PROCEDURE

Creep tests were performed at 823, 873 K with 100, 50 MPa, respectively. Creep tests were
terminated at various creep damage levels (including rupture) during creep. Carbon extraction
replica was prepared by conventional techniques from creep tested specimen and replicas were
examined in JEOL 200CX equipped with X-ray energy dispersive analysis system (Model LINK,
Software RTS2). Magnetic properties were measured with the Vibrating Sample Magnetometer
(Model Toei VSM-5) and the size of specimen is φ2πιπι χ 5mm

RESULTS AND DISCUSSION

At each creep damage level, the compositions of Fe, Cr, Mo in carbide are measured with micro
EDS analysis system. With these EDXS spectrum patterns, the carbides are identified as M3C,
M
23^6' ^V-, M2C and M 7 C 3 types. From the literature survey and data (Lee, 1989), the criteria
can be formulated as in Table L

Table I. Criteria for carbide classification in this research

Carbide Type Criteria for classification

M3C Fe>Cr, Cr>Mo and 0.2Fe>Cr

M
23 C 6 Fe>Mo, Cr>Mo and 0.2(Cr+Fe)>Mo>0.1(Cr+Fe)

M6C Mo>Cr, 0.4Fe>Cr>0.1Fe

M2C Mo>Cr>Fe

M7C3 Cr>Fe>Mo

For each carbide type, Fe, Cr, Mo contents are said to be changed as the creep damage increased
(Afrouz, 1983). However, since the carbide types are classified according to the composition profiles,
the change in composition may have a limitation. For example, if Fe contents in M2C type carbide
is increased over Cr, the carbide types are changed to M$C type. For such a case, there are actually
a large increase of Fe content in M2C type carbide but it is just obtained a large decrease of Fe
in M2C and M^C type carbides because of no account for the change of carbide types. Among
our results on the composition profiles in M^C^ M ^ , M2C, M 7 C 3 type carbides, M^Cg type
carbide shows the smallest standard deviation of data. Figure 1 shows Fe, Cr, Mo compositional
changes as the creep damage fractioa Fe seems to have a increasing trends but Cr a decreasing
one as the creep damage. In spite of such trends, there are some problems to be used for the
creep damage assessment because of the data deviations.

For another approach, the carbide-type frequency can be used as a creep damage parameters.
In Fig. 2, M2C type carbide seems to be disappeared as creep damage increased. M 7 C 3 type shows
a gradual increase near the 60% creep life consumption. N^C type carbide takes a small portion
but ever increasing (up to 10%) with the creep damage. In case of M^Cg type carbide, the deviation
of data are too large to predict the creep damage. For M7C3, M^Cg type carbide, there is small
difference in compositional profiles or carbide-type frequency with respect to the creep testing
condition (temperature and stress). For Mo rich carbide (M 2 C carbide, M6C type carbide), the
temperature and stress have some effects on the compositional profiles and frequency. In Fig.
3, it can be said that the frequency of M2C type carbide has a relationship with the creep testing
conditions. When the stress effects play a more dominant role, M2C type carbide becomes to
 127

disappear more rapidly. Figure 3 shows that in the frequency of occurrence, the data deviation
is so small and the amount of change is so large to be used for the creep damage parameters.

Since the components of the carbide were changed to a more stable state by the creep damage,
the average compositions of carbide will be continuously decreased or increased. Figure 4 shows
the relationship between the average contents of Fe, Cr, Mo and creep testing time at 600 °C,
100 MPa. The average contents of Fe in carbides were linearly increased as creep damage. Mo
is linearly decreased and Cr has no tendency. In other researches (Yu, 1989; Biss and Wada,
1985), Mo in matrix is said to be precipitated to the carbide. From such a concept, Mo content
in carbide must be increased as creep damage. But, even though Mo is absorbed into the carbides,
the average content of Mo can be decreased if Fe is much more precipitated.

To investigate the above trends in Fe and Mo at other conditions, it was analyzed the field used
materials (ruptured tube by over heating (A), the opposite side of A (B), 1.7 x 105 hours used
but about 20% damaged (C)). These data were plotted with the creep testing results using new
materials. If they were located at the appropriate creep damage level, the same trends can be
obtained in spite of the different temperature and stress histories, as in Fig. 5. The average Fe,
Mo compositions in carbides seem to be used as the well-defined creep damage parameters as
shown in Fig. 5.

The mobility of magnetic domain wall can be altered as the carbides are changed in the morphology
and type (Cullity, 1972). To enhance the creep ductility, the fine carbide (M 2 C type carbide)
was made to be precipitated in the matrix by the appropriate heat treatment and alloying. These
carbides can also hinder the motion of magnetic domain wall. As the creep deformation, these
carbides were dissolved and coarsened to reduce the creep ductility. Due to such a carbide
coarsening, the magnetic domain can also be more easily moved. As the coercivity denote the
ability of magnetic domain wall motion, the carbide coarsening can reduce the coercivity
(He). Figure 6 shows the coercivity decreasing after the about 60% creep life consumption. This
trend can be found in the occurrence frequency of M 7 C 3 type carbide. But the amount of change
in He is so small to predict the creep damage quantitatively and it must be explained the reason
why He increased at the initial creep stage.

REFERENCE

Afrouz, A , M J . Collins and R. Pilkington (1983). Microstructural examination of lCr-0.5Mo

Steel during creep. Metals Technology, 10, 461-463
Biss, V . A and T. Wada (1985). Microstructural changes in lCr-0.5Mo steel after 20 years of
service. Metall. Trans. A, 16A, 109-114
Cullity, B.D. (1972). Introduction to magnetic materials. Addison-Wesley Pub.
Lee Yeung Jo (1989). Assessment of creep damage in weldment oflCr0.5Mo steels. Ph.D. Thesis,
Monash University, Clayton, Victoria, Australia
Yu Jin (1989). Carbide stability diagrams in 2.25CrlMo steel. Metall. Trans. A, 20A, 1561-1564
128

.Λ ι ι ι i i i i i i I I I I I
0 40 80 120
Creep Life Fraction(%)
Fig. 1. Percentage of alloying elements in M^C^ type carbide as
creep life fraction, creep tested at 873 K, 100 MPa and 923 K,
50 MPa

20 40 60 80 100 120
Creep Life Fraction(*)
Fig. 2. Carbide type frequency with creep life fraction during creep
testing at 873 K, 100 MPa and 923 K, 50 MPa
 129

Fraction of li«C type carbide

Creep Test Condition
" 73 K. 100 tfPa
Δ : 923 K. 50 MPa

0 r i l l l i . i i l l l n u i i i i i l i n n n i i t p i i n t n ^ i i i i i i i | l n Mi i m |

0 20 40 60 80 100 120
Creep Life Fraction(*)
Fig. 3. Variationin M2C type carbide frequency with creep life
fraction at different creep testing condition (873 K, 100 MPa and
923 K, 50 MPa)

200 400 600 800 1000

Creep Test Time(hrs)
Fig. 4. Variation in average composition of all carbides on creep
testing time (creep testing condition is 873 K, 100 MPa)
130

t
L Components In carbide (wbl]
»60 a : Fe
: Cr
; Mo
A
a |
£40 ■

^il. 5Γ*·*
A □ Λ - -f&'
~A
Δ
$= A j
Ώ
h

I ι i i. 1 t t 1i i 1 Λ-Λ—X. l i t■j--t-
l 1 t i i i1—4-1 ,i i i.l

0 40 80 120
Creep Life F r a c t i o n ^ )

Fig. 5. Variation in averaging composition of all carbide on creep

life fraction (creep tested at 873 K, 100 MPa and 923 K, 50 MPa)
(ruptureed tube by overheating(data lable A), the opposite side
of ruptured area(data lable B), 1.7 x 105 hours used but about
20% damaged (data lable C)

20 40 60 SO 100 120
Creep Life Fraction ( Ä )
Fig. 6. Relation between the coercivity (He) and creep life fraction
(Creep tested at 873 K, 100 MPa and 923 K, 100 MPa)
WS6b5

STUDY OF RESIDUAL LIFE ASSESSMENT OF CREEP DAMAGE

AT ACTUAL STRESS FOR 2.25Cr-lMo STEEL
BY MICROSTRUCTURE EXAMINATION

Masashi Nakashiro, Kouichi Murakami and Shigemitsu Kihara

Research I n s t i t u t e
Ishikawajima-Harima Heavy Industries Co. Ltd.,
3-1-15, Toyosu, Koto-ku, Tokyo, 135 Japan

ABSTRACT

Microstructual examination by TEM t o assess the creep damage has been

performed on 2.25Cr-lMo s t e e l . Subboundaries were formed in p a r t i c u l a r
grains a t t h e e a r l y secondary creep stage. The r a t i o of t h e grains with
subboundaries (named Nsb) has good c o r r e l a t i o n with t h e creep life friction.
Microstructures. of a c t u a l b o i l e r tube a f t e r long term s e r v i c e were similar
t o t h o s e of c r e p t specimens in l a b o r a t o r y . Nsb will be able t o be applied t o
assess t h e creep damage.

KEYWORD

Creep; 2.25CrlMo steel; Microstructure; TEM(Transmission electron

microscope); Subboundary; SAD(Selected area diffraction) technique;

INTRODUCTION

The purpose of t h i s study is to assess the creep damage for 2.25CrlMo s t e e l

by m i c r o s t r u c t u a l observation. As a technique using d i r e c t m i c r o s t r u c t u a l
observation, a dependence of changes of carbide on creep life consumption
is known. However t h i s technique can estimate service time o r / a n d
temperature, i t can not assess s t r e s s effect. Changes of carbide occur by
simple aging without s t r e s s . Effect of s t r e s s on carbide change is not
clarified well, especially in case of low s t r e s s as a c t u a l b o i l e r . The effect
of s t r e s s , even low s t r e s s , on creep damage will appear on matrix (
a - f e r r i t e ) change, dislocation s t r u c t u r e , r a t h e r than carbide change.
Dislocation s t r u c t u r e would be expected to change during low s t r e s s creep.
Nevertheless, only a few studies of dislocation s t r u c t u r e s on t h e s e kinds of
a c t u a l s t e e l s during low s t r e s s creep or t h e materials used in a c t u a l
b o i l e r s have been performed. In our previous study, polygonized dislocation
wall (subboundary) were found in creep r u p t u r e d tubes of a c t u a l b o i l e r s and
also l a b o r a t o r y creep r u p t u r e d specimens c n . Therefore i t is considered t h a t
t h e formation and development of subboundaries has good r e l a t i o n s h i p s with
131
132
creep deformation.

EXPERIMENTAL PROCEDURE

The specimens for creep t e s t were cut from 2.25CrlMo (ASTM T22) t u b e s and
taken p a r a l l e l to the axial direction of tube. These t u b e s were full
annealed. Specimens were loaded uniaxial. Creep t e s t conditions a r e shown
in Table 1. These t e s t conditions were conducted under t h e a c c e l e r a t e d
temperature and s t r e s s was chosen close t o the p r a c t i c a l use. Creep t e s t of
both s e r i e s were i n t e r r u p t e d at c e r t a i n creep stages and i n v e s t i g a t e d . In
o r d e r t o compare the samples in l a b o r a t o r y with t h e samples used
p r a c t i c a l l y , s e v e r a l specimens were cut from a c t u a l b o i l e r and were
investigated. Thin foil for TEM observation were cut from p e r p e n d i c u l a r t o
t h e s t r e s s axis of creep t e s t specimens and prepared by e l e c t r o p o l i s h i n g .
Table 1 Creep Test Conditions

Temp Stress Interruption Time Rupture

°C kgf/mm2 h h

Series 1 670 2.7 500.1 764.0 1556.4 2257.8 3017.7

(16%) (25%) (75%) (75%)

Series 2 650 3.0 95.0 197.0 500.0 4000.0

(2%) (5%) (12%) (expected)
In o r d e r t o q u a n t i t a t i v e l y evaluate the changes of s u b s t r u c t u r e , t h e
r e l a t i o n of numbers of grains with subboundary to t o t a l grains observed,
and misorientation among the subgrains were used. The misorientation among
t h e subgrains were measured by SAD technique < S D .

RESULTS AND DISCUSSION

Fig.l shows TEM s t r u c t u r e s of virgin material (before t e s t ) . This

m i c r o s t r u c t u r e is typical f e r r i t e p e a r l i t e s t r u c t u r e . Large carbides
p r e c i p i t a t e d on grain boundaries. Clear lamellar carbide s t r u c t u r e can be
found in t h e p e a r l i t e field. Small carbides less than 1 μ a r e in t h e f e r r i t e
field. Dislocations networks, c e l l s t r u c t u r e s or c l e a r subboundaries a r e
r a r e l y observed in t h i s s t r u c t u r e .

Fig. 2 shows TEM s t r u c t u r e of the creep damaged sample. The c l e a r

subboundaries is observed in only a few grains,(a). Subboundaries were not
found in t h e creep stage e a r l i e r than t / t r is 0.13. These subgrains a r e
mostly observed near t r i p l e points of grain boundary. Numbers of subgrains
per one grain a r e 1-3 and subgrain sizes a r e s c a t t e r e d widely. Numbers of
grain having subboundary increases with the increases of t / t r , (b),(c). But
also a l o t of grains have no subboundaries. At t h e t / t r is of 0.25 and 0.5,
subboundaries a r e observed not only around the t r i p l e points of grain
boundary but in t h e c e n t e r of the grain. Almost a l l grains have
subboundaries a t t h e t / t r of over 0.75. Almost a l l grains have subboundaries
and a l o t of tangled dislocations in the subgrains a r e observed on t h e
r u p t u r e d specimen (d). Above observations revealed following significant
 133

phenomena occurred during creep of t h i s p r a c t i c a l s t e e l under t h e service

(low) s t r e s s level.
(1)Creep p r o g r e s s by dislocation c e l l formation mechanism which is the
t y p i c a l creep mechanism for the materials used in l a b o r a t o r y base study,
like p u r e metal.
(2)The subboundary (cell) is initiated near t h e t r i p l e point of grain
boundary and propagated toward the c e n t e r of grain.
(3)The subboundary formation does not p r o g r e s s simultaneously in a l l
grains, but in some specific grains.
(4)The number of grain with the subboundary increases with processing
creep.
(5)Change of subgrain size throughout the creep life is not significant. The
subgrain size seems to depend on the space of fine carbide in the grain.
The schematic diagram for the sequence of substructural change is shown in
Fig. 3.

In o r d e r t o quantify s u b s t r u c t u r a l change, numbers of grains with

subboundaries were measured. Fig.4 shows r e l a t i o n between Nsb (the r a t i o of
grains with subboundaries to a l l grains observed) and t / t r . Total numbers of
observed grains for each specimen were about 50. This figure suggests t h a t
Nsb has good c o r r e l a t i o n with t / t r .

Fig. 5 shows TEM s t r u c t u r e of a f t e r 30,000h service a t a r e l a t i v e l y high

temperature which was ruptured. All grains have subboundaries and t a n g l e d
d i s l o c a t i o n s . Fig.6 shows TEM s t r u c t u r e of another b o i l e r tube a f t e r long
time s e r v i c e in a c t u a l boiler. Some grains with subboundary n e a r t h e t r i p l e
point of grain boundary a r e observed. The b o i l e r tube was used for 167,000h
a t 573 °C, 2.7kgf/mm2. Since t h i s s t e e l is expected t o be r u p t u r e d a t about
1,800,000h under t h i s condition by using modified NRIM creep d a t a C 3 \ t h e
c a l c u l a t e d t / t r is 0.09. These observations suggest t h a t t h e s u b s t r u c t u r e s
formed under a c t u a l service conditions a r e very similar t o those under t h e
l a b o r a t o r y creep t e s t conditions used in t h i s study. Therefore, i t can be
concluded t h a t t h e creep mechanism in t h e a c t u a l s e r v i c e conditions is
identified with t h a t in l a b o r a t o r y creep t e s t a t same s t r e s s l e v e l and high
temperatures. Consequently, the p l o t s of Nsb vs. t / t r for t h o s e samples
used in a c t u a l b o i l e r s a r e on t h e curve obtained by l a b o r a t o r y data, as
shown in Fig. 4. These r e s u l t s suggest t h e measurement of Nsb can be a
promising method for creep life evaluation of a c t u a l b o i l e r t u b e .

Nakagawa has r e p o r t e d t h a t SAD analysis was useful t o e v a l u a t e fatigue life

of a low a l l o y s t e e l for p r e s s u r e vessel* 2 5 . Since t h e SAD technique is a
method for assess t h e deformation of grain by measuring t h e misorientation
of d i s l o c a t i o n c e l l , i t may be applicable for e v a l u a t i n g t h e creep
deformation by t h e dislocation c e l l formation mechanism. Fig. 7 shows r e s u l t s
of SAD analysis performed on c r e p t specimens of s e r i e s 1. Although θ Μ
value s l i g h t l y increases by creep, i t does not change in most p a r t of creep
life and t h e difference is only about 1.5' even between virgin and r u p t u r e d
samples. C r y s t a l l o g r a p h i c a l evaluation for small deformation of grain with
subboundary should be based on the measurement of misorientation done
around a r o t a t i o n axis between two neighbor subgrains, not around a fix
134
axis, like <111> used in this study.

CONCLUSION

Creep t e s t s were performed on 2.25CrlMo s t e e l at higher temperature than

service one under the same s t r e s s level. These c r e p t specimens and
specimens cut from s u p e r h e a t e r tubes were observed by TEM. Following
conclusion have been obtained;

l.Subboundary formation was observed in both samples c r e p t in l a b o r a t o r y

and in a c t u a l boiler. The TEM observations indicated t h a t p r a c t i c a l creep
damage in a c t u a l boiler can be modeled with a temperature a c c e l e r a t e d
l a b o r a t o r y creep t e s t .

2.Nsb has a good c o r r e l a t i o n with creep life fraction, t / t r , even in low life
fraction range.

REFERENCE

DM.Nakashiro, K.Murakami and S.Kihara:

Rep. ISIJ Meeting,3(1990),p.l876
2)Y.Nakagawa, H.Yoshizawa and M.E.Lapides:
Met. Trans.A,Vol.21A(1990),pl989
3)M.Nakashiro, S.Kihara, F.Kishimoto and
T.Fujimori: ISIJ Int.,30(1990) 10, p.823

a
Fig. 1 TEM s t r u c t u r e of virgin material.
( before creep t e s t )

Fig. 2 TEM s t r u c t u r e s for the sample c r e p t in l a b o r a t o r y .

(a)series 2:t/tr=0.13, (b)series l:t/tr=0.25
(c)series l:t/tr=0.75, (d)series l:t/tr=1.00
 135

Subbouiidaries (dislocation cell wall)

S t r u c t u r a l change as damage accumulation
a c
I N^< J-
inboundary

Formed at
some grains Formed at
a lot of grains
b

Developed at Formed at
some grains a l l grains
Tangled Dislocations

Fig. 3 The schematic diagram for the

sequence of substructural change.

O Series 1 tr=3,000h
Δ Series 2 tr=4,000h
_■ In actual boiler
serviced

6 h
(A

.4 h

2 h

0 .2 .4 .6 .8 1
t/tr
Fig.4 Relationship between Nsb and t / t r .
136

Fig. 6 TEM structures of the actual

boiler tube. (Temp. =573 °C,
σ =2.7kgf/mm2, time=167,000h)

Fig. 5 TEM structures of the actual boiler

tube creep ruptured by over heated.
Mean orientation difference

O s e r i e s 1 tr=3000hr
4h Π an actual boiler

<D
3h
Ό
3?
O
Π
o o

0.2 0.4 0.6 0.8

Creep damage ratio ( t / t r )

Fig. 7 Relationship between θ Μ and t / t r .

WS6b6

An Approach for N o n d e s t r u c t i v e Remaining Life Estimation

of High Temperature Materials for C r e e p - F a t i g u e Failure.

M. Hashimoto, M. Okazaki and T. Yada

Department of Mechanical E n g i n e e r i n g , Nagaoka U n i v e r s i t y

of Technology, Nagaoka 9 4 0 - 2 1 , Japan.

ABSTRACT

C r e e p - f a t i g u e s t r e n g t h of p o s t s e r v i c e 2 · 1/4 C r - l ' M o s t e e l utilized for s e c o n d

s u p e r h e a t e r boiler t u b e in a f o s s i l fuel power plant for about one
h u n d r e d - t h o u s a n d s h o u r s was s t u d i e d . The c r e e p - f a t i g u e s t r e n g t h of t h e
p o s t s e r v i c e material was lower t h a n t h a t of t h e v i r g i n material, w h e r e a s it was
comparable to t h a t of thermally a g e d material. The n o n d e s t r u c t i v e d e t e c t i o n of
t h e long term degradation damage, due to c r e e p - f a t i g u e , a s well a s due t o long
term thermal a g i n g , was also i n v e s t i g a t e d b y a p p l y i n g an ultrasonic t e c h n i q u e .
The e n e r g y a t t e n u a t i o n coefficient, a, p r o p o s e d b y t h e a u t h o r s , w a s a s u c c e s s f u l
parameter to d e t e c t c r e e p - f a t i g u e damage. Based on t h e r e s u l t s t h u s o b t a i n e d , a
new remaining life estimation method for c r e e p - f a t i g u e failure of h i g h
temperature s t r u c t u r a l materials was p r o p o s e d . The application of t h e method t o
the p o s t s e r v i c e material g a v e good p r e d i c t e d r e s u l t s .

KEYWORDS

Remaining life estimation; long term d e g r a d a t i o n damage; c r e e p - f a t i g u e damage;

ultrasonic t e c h n i q u e ; e n e r g y attenuation of ultrasonic w a v e .

INTRODUCTION

According t o a r e c e n t i n c r e a s e of n u c l e a r electric power p l a n t s and a g r e a t

v a r i e t y of e l e c t r i c demand, fossil fuel e l e c t r i c power p l a n t s of small c a p a c i t y in
s e r v i c e h a v e b e e n compelled t o f r e q u e n t s t a r t - u p , s h u t - d o w n and load c h a n g e ,
which s u b j e c t t h e h i g h - t e m p e r a t u r e s t r u c t u r a l materials to more s e v e r thermal
s t r e s s c y c l i n g t h a n u n d e r p r e v i o u s loading (Gotoh,1983; Ohnami e t al.,1987;
Okazaki e t al. t 1989; Yoneyama e t al.,1987; Viswanathan, 1985). In addition, most of
t h e fossil fuel power p l a n t s u n d e r s u c h a situation h a v e b e e n working for t h e
p a s t 10 to 20 y e a r s , or are w o r n - o u t . From t h e a b o v e b a c k g r o u n d , thermal f a t i g u e
failure of t h e s t r u c t u r a l materials in old f o s s i l fuel power p l a n t s becomes a matter
of g r a v e c o n c e r n , and h e n c e an e s t a b l i s h m e n t of t h e remaining life estimation
method for c r e e p - f a t i g u e failure i s e a r n e s t l y n e e d e d . For t h e establishment of
remaining life estimation methods, following t e c h n i q u e s are n e e d e d ; One i s t h e

137
138
development of a t e c h n i q u e to d e t e c t t h e long term d e g r a d a t i o n damage of h i g h
temperature components n o n d e s t r u c t i v e l y . The o t h e r i s an accumulation of c r e e p
and c r e e p - f a t i g u e s t r e n g t h s of t h e materials in s e r v i c e for a long time at h i g h
t e m p e r a t u r e s , and t h e i r d a t a - b a s e . Although many s t u d i e s on c r e e p r u p t u r e of
r e t i r e d materials h a v e b e e n carried out, u s e f u l methods to p r e d i c t t h e remaining
life have not been e s t a b l i s h e d y e t .

In t h i s work, t h e c r e e p - f a t i g u e s t r e n g t h of 2 · 1/4 C r - l ' M o s t e e l , e x t r a c t e d from

t h e p o s t s e r v i c e 2nd s u p e r h e a t e r boiler t u b e u s e d for about 102000 h o u r s in a
f o s s i l fuel power plant, i s e v a l u a t e d . The n o n d e s t r u c t i v e detection of long term
degradation damage i s also i n v e s t i g a t e d b y a p p l y i n g an ultrasonic method, and a
new estimation method of remaining life for c r e e p - f a t i g u e failure i s p r o p o s e d .

EXPERIMENTAL PROCEDURES

In general, t h e materials in s e r v i c e at h i g h t e m p e r a t u r e s for a long term are

s u b j e c t e d to at l e a s t t h e following two typical t y p e s of damages; One i s a
"metallurgical damage", which i s p r o d u c e d b y thermal a g i n g at h i g h temperature
e v e n without load. The o t h e r i s a mechanical damage i n d u c e d b y c r e e p , corrosion,
fatigue and t h e i r interaction, which i s more or l e s s related t o external load. In
o r d e r to s t u d y t h e metallurgical and mechanical damages s e p a r a t e l y , t h e
following materials were specified in t h i s work; v i r g i n 2 · 1/4 Cr-l*Mo s t e e l , t h e
thermally a g e d 2 * 1 / 4 C r - l ' M o s t e e l , and t h e p o s t s e r v i c e 2 · 1/4 C r - l ' M o s t e e l ,
which had b e e n u s e d for 2nd s u p e r h e a t e r boiler t u b e at 823 K approximately for
about one h u n d r e d - t h o u s a n d h o u r s in a f o s s i l fuel power plant. The thermally
a g e d material were p r e p a r e d b y holding t h e v i r g i n material in a n e l e c t r i c f u r n a c e
at a temperature of 923 K for one t h o u s a n d h o u r s , s o t h a t t h e a g i n g l e a d s to an
e q u i v a l e n t Larson-Miller parameter, LM (=T(C + log t ) , w h e r e C=20, T:heating
temperature in Kelvin, and t:heating time in h o u r s ) , t o t h e p o s t s e r v i c e material,
a l t h o u g h t h e a g e d material d o e s not e x p e r i e n c e mechanical damage. The
microstructure of t h e v i r g i n material had a mixed s t r u c t u r e of ferrite and
pearlite. In t h e p o s t s e r v i c e and a g e d materials, on t h e o t h e r hand, t h e pearlite
was s p h e r i o d i z e d , and t h e carbide precipitation was remarkable at t h e grain
boundaries.

F u l l y - r e v e r s e d s t r a i n - c o n t r o l l e d l o w - c y c l e c r e e p - f a t i g u e t e s t s were carried out

b y means of c l o s e d - l o o p hydraulic f a t i g u e machine at a temperature of 873 K in
air by u s i n g solid cylindrical smooth specimens with a g a g e s e c t i o n diameter of 5
mm, which were t a k e n from boiler t u b e . The strain wave s h a p e s applied were a
symmetrical triangular one of f a s t - f a s t t y p e , and an asymmetrical t r i a n g u l a r one
of s l o w - f a s t t y p e . The upward and downward s t r a i n r a t e s in f a s t - f a s t t y p e are
2 x l O ~ s / s e c T h e s e strain r a t e s in s l o w - f a s t t y p e are 1 0 ~ V s e c . and 2 x l 0 ~ 3 / s e c ,
r e s p e c t i v e l y . The variation b e h a v i o r of an e n e r g y attenuation coefficient of a
longitudinal ultrasonic w a v e , or, with t h e c r e e p - f a t i g u e damage was also
i n v e s t i g a t e d , w h e r e a i s defined b y t h e ratio of i n p u t e n e r g y to o u t p u t e n e r g y
of an ultrasonic wave (Okazaki e t al.,1989). The measurement s y s t e m of a i s
illustrated in Fig. 1, w h e r e a t r a n s d u c e r of a central f r e q u e n c y of 20 MHz was
employed (Panametrix Co., Ml 16).

EXPERIMENTAL RESULTS AND DISCUSSION

Creep-Fatigue S t r e n g t h

Creep-fatigue strengths in all materials are summarized in Fig. 2. The

 139

2-1/4 Cr-1-Mo, 873 K

O: Virgin
A:Aged
Transducer D: Postservice

Open; fast-fast
Solid;slow-fast
Specimen i i i nil
Synchroscope L
iL·

Fig. 1 Measurement system for energy

attenuation coefficient of ultra-
sonic wave. Fig. 2 Creep-fatigue l i v e s .

creep-fatigue strength in the postservice material is lower than that of the

virgin material, especially at low strain range, whereas it is comparable to the
aged material. All materials exhibited cyclic softening behavior, and the
deformation resistance of the postservice material, which was comparable to the
aged material, was lower than that of the virgin. The fracture surface of the
postservice material, as well as in the aged material, under slow-fast cycling via
SEM indicated that intergranular fracture was dominant, while in the virgin
material it was the mixed mode of intergranular and transgranular fracture
surface. These characteristics suggest that the metallurgical damage due to
thermal-aging is dominant in the postservice material. This will be discussed
later.

Variation of Energy Attenuation in Ultrasonic Wave with Creep-Fatigue Damage.

An energy attenuation coefficient of ultrasonic waves, a, is one of the hopeful

parameters to nondestructively detect the long term degradation damage of high
temperature components (Okazaki et al.,1989). The energy attenuation coefficient,
a, is defined by the ratio of input energy to output one of an ultrasonic wave,
and it is evaluated by a following equation:

N/2 N/2
a = ( 2 0 / L ) l o g ( Σ I X κ. i I 2 / Σ I X, I2) (1)
k=0 k=0

where | X κ. i | and | X K .s I are the frequency spectrums of the input and

output ultrasonic waves, which are calculated by the Fourier transformation of
the ultrasonic reflection echo. L in Eq.(l) is the propagation distance of an
ultrasonic wave.
Variation behaviors of a with creep-fatigue damage in respective materials are
shown in Figs. 3 and 4, where the marks of I and the plots indicate the scatter
bands and their average values, respectively. In these figures the creep-fatigue
damage, D, is represented by the ratio of number of strain cycle to the
corresponding creep-fatigue life, N-r. These figures show that a in all materials
increases with creep-fatigue damage. Such an increase of a can be notably seen
after a half life. A significant dependence on strain range can not be found.
Focussing on the variation behavior of a in the respective materials in Figs. 3
and 4, the following features can be seen; First of all, the a -D curves in the
virgin and the aged materials are similar, although the difference of absolute
value of a between the both materials can be seen. In fact, as shown in Fig. 5,
140

1.5 2-1/4 Cr-1-Mo, 873 Κ, slow-fast

Virgin

Open; Δ£=0.5 %
Γ Half-solid;A6=0.7 %
*ΊΙ Solid; Δ£=1.0 %

?—=—5—-f 1.5
2*1/4 Cr-1-Mo, 873 K, slow-fast
ω ω
c ο OiVirgin
1 DiPostservice
A'.Aged

?
0.5 -J I L_ J_ _J_ L Open; Δ£=0.5 %
O/
0.5 1.0
Γ Half-sol id;A£=0.7 % 7
Creep-fatigue damage,
"f,v Solid; Δ 8 =1.0 %
Fig 3 Variation of a with creep-
;ue damage in virgin material.
fat ig·
u 0/
2-1/4 Cr-1-Mo slow-fast
ΏΔ o
1.0 rPQ O —n*^A

° O

1.01 0.8 1 i J L i l l . L__ l

0 0.5 1.0
o
c4 in
in virgin Creep-fatigue damage,
s - «4- N
ω ω f,v^A,Nf,s
c o
Open; Δ£=0.5 % Fig. 5 Variation of the normalized
Γ* Solid;A£=1.0 % a with creep-fatigue damage.
0.5 J l l l I I I I L
0.5 1.0
N
Creep-fatigue damage, ττ— N
N
"f,A f,s
Fig. k Variation of a with creep-
fatigue damage in the aged and post-
service m a t e r i a l s .

when a is normalized by an initial value of a, a o, in respective specimens, the

a / a o-D curves in the both materials can be represented by a single curve.
This indicates that, when a significant change of microstructure during the
creep-fatigue fracture process is negligible (i.e., the metallurgical damage does
not progress), the degree of mechanical damage can be nondestructively
detected by pursuing the change of a / a o. The a -D curves in the postservice
and the aged materials are comparable each other, not only qualitatively but also
quantitatively (Figs. 3, 4 and 5), indication that the postservice material was
subjected mainly to metallurgical damage due to thermal aging, and to a
negligible mechanical damage. In fact, a significant difference of creep-fatigue
lives between the postservice and the aged materials was not found (See Fig. 2).
 141
Measurement of J, in the virgin material

I
Evaluation of d^/eiy-LM curve Evaluation of LM in Measurement of
with aging. the service material. in the service
(ct.: «i in aged material (LM:Larson-Miller material.
eCß,: o< in the aged material which parameter) ids*)
has a comparable LM value to
the service ir.aterial.)

^A)Estimation of possible Evaluation of

degree of metallurgical
damage in the service
material by ot^o^-LM

LM=T(C+log t)

Calculation of
Evaluation of the changing curve of
οί/οί., with creep-fatigue damage, D,
in the aged material.
(D=N/N.
'f A' ^f /\» ;Creep-fatigue l i f e
(ß) Evaluation of creep-fatigue
damage, D, in the service
material objected.

Fig. 5

Estimation of remaining l i f e
for creep-fatigue f a i l u r e
in the service material.
Remaining life
"f,A ,0-D c )
Fig. 6 Remaining l i f e estimation method proposed by
applying ultrasonic technique.
Remaining Life Estimation by Ultrasonic Technique.

As shown by the authors (Okazaki et al.,1989), the decrease of hardness, a typical

type of metallurgical damage due to thermal aging, is successfully detected by
the medium of a. By applying these results and foregoing results, remaining life
for creep-fatigue failure of high temperature materials is estimated by following
procedures (Fig. 6):
Step 1: Previously evaluate the energy attenuation coefficient in the virgin
material, a v . In addition, obtain beforehand the variation curve of a with
thermal aging (The a in the aged material is denoted by a A).
Step 2: Calculate the value of Larson-Miller parameter, LM, in the service
components from the history of its service condition, and then account how much
is the degree of possible metallurgical damage only due to long term aging, i.e.,
a A / a v. This corresponds to the process of @ in Fig. 6.
Step 3: By using the aged material under an equivalent LM value to the service
components, evaluate experimentally the creep-fatigue life, N-r. A, as well as the
variation behavior of the normalized energy attenuation coefficient, a / a A, with
creep-fatigue damage, D (e.g., Fig. 5).
Step 4: Measure the energy attenuation coefficient in the service material, a s ,
and then calculate a */ a v .
Step 5: Estimate how much is the creep-fatigue damage in the service components
142
(i.e., D e ) , by i n t r o d u c i n g t h e value of a */ a A =( a */ a v ) / ( a A / a v), into t h e a /
a A - D c u r v e . This p r o c e d u r e c o r r e s p o n d s to t h e p r o c e s s of ® in Fig.6.
Step 6: From t h e r e s u l t s obtained in S t e p 5 and t h e N-r. A a l r e a d y e v a l u a t e d in
Step 3, p r e d i c t t h e remaining c r e e p - f a t i g u e life of t h e s e r v i c e material b y an
equation of Ντ. A * ( 1 - D e ) .
The application of t h e a b o v e method to t h e p o s t s e r v i c e material in t h e p r e s e n t
work r e s u l t s in t h e following estimation; From t h e experimental r e s u l t s shown in
Fig. 5, t h e value of a « / a A in t h e s t e p 5 i s u n i t y , and h e n c e t h e c r e e p - f a t i g u e
damage in t h e p o s t s e r v i c e material i s small e n o u g h to be n e g l e c t e d . This p r e d i c t s
that the c r e e p - f a t i g u e life of t h e p o s t s e r v i c e material i s comparable to t h a t of t h e
a g e d material, which a g r e e s well with t h e experimental r e s u l t s shown in Fig. 2.
The method p r o p o s e d p o s s e s s e s some a d v a n t a g e s . One i s t h e h i g h p o s s i b i l i t y to
n o n d e s t r u c t i v e remaining life estimation of h i g h temperature components in situ.
The other i s that, b e c a u s e t h e p r o p e r t i e s of t h e v i r g i n and a c c e l e r a t i n g l y a g e d
materials which can be supplied for a s h o r t time are utilized e f f e c t i v e l y , t h e
method e n a b l e s u s to estimate t h e remaining c r e e p - f a t i g u e life of s e r v i c e
materials for a s h o r t time, by t a k i n g t h e l e a s t p r o p e r t i e s of t h e s e r v i c e materials
t h e m s e l v e s . The applicability of t h e p r o p o s e d method to a u s t e n i t i c s t a i n l e s s s t e e l ,
which show a cyclic h a r d e n i n g behavior, i s now on a way of i n v e s t i g a t i o n , and
the r e s u l t will be r e p o r t e d in a couple of y e a r s .

CONCLUSION

The main c o n c l u s i o n s reached in t h i s work are a s follows:

(1) The c r e e p - f a t i g u e s t r e n g t h of t h e p o s t s e r v i c e material was d e g r a d a t e d ,
compared with t h a t of t h e v i r g i n material, w h e r e a s it was comparable t o t h a t of
t h e a g e d material.
(2) The e n e r g y attenuation coefficient of ultrasonic w a v e s , oc, correlated well
with the development of c r e e p - f a t i g u e damage in all materials.
(3) A new remaining life estimation method for c r e e p - f a t i g u e failure was p r o p o s e d
b y a p p l y i n g an ultrasonic t e c h n i q u e . The application of t h i s method to t h e
p o s t s e r v i c e material g a v e good p r e d i c t e d r e s u l t s .

REFERENCES

Gotoh, T., (1983), "Non-Destructive Detection of Creep Damage for Cr-Mo-V S t e e l s

Forgings", Trans. Jap. Soc. Mat. Sci. f vol.32, pp.563-569.
Japan I n s t i t u t e of Iron and Steel, (1988), "Feasibility S t u d y on Detection
Technique for Remaining Life Evaluation of S t r u c t u r a l Materials", Japan
I n s t i t u t e of Iron and Steel, Tokyo.
Ohnami, M., Endoh, Y., Kitagawa, M. and Nitta, A., (1987), "Remaining Life
A s s e s s m e n t of Fossil Fuel Power Plants - C u r r e n t Situation and A c t i v i t i e s - " , J.
Jap. Soc. Mech. E n g r s . , vol.90, pp.556-561.
Okazaki, M. Yada, T. and Hashimoto, M., (1989), "Approach for N o n d e s t r u c t i v e
Detection of Long Term Degradation Damage in High Temperature Components
b y Ultrasonic Technique", Proc. ASME PVP-89 Conf., ASME, Honolulu, NDE vol.5,
pp.253-258.
Okazaki, M., Yada, T. and Hashimoto, M., (1989), "An Approach for Non d e s t r u c t i v e
Detection of Creep Cavities in High-Temperature Components b y Ultrasonic
Technique", Trans. Jap. Soc. Mech. E n g r s , vol.55, p p . 1900-1907.
Viswanathan, R.D., (1985), "Dissimilar Metal Weld and Boiler Creep Damage
Evaluation of Plant Life Extension", Trans. ASME, J . P r e s s . Vess. Tech., vol.107,
PP218-224.
Yoneyama, H., Nakashiro, M., and Ohtomo, A., (1987), "Assessment for Creep
Damage b y Ultrasonic Techniques", Proc. Annual Meeting of Jap. Soc. of NDI,
pp.670-672.
WS6b7

Expert System for Life Assessment and Maintenance

of Steam Turbine Components

I. Murakami, K. Fujiyama and K. Kimura

Heavy Apparatus Engineering Laboratory

Toshiba Corporation
1-9 Suehiro-cho, Tsurumi-ku, Yokohama, 230, Japan

ABSTRACT

An expert system has been developed for life assessment and maintenance of
steam turbine components which can deal qualitative information in addition
to quantitative data through certainty factor combination method and
production system. For practical inspection data, we have proved this system
to be effective for practical life assessment of steam turbine components.

KEYWORDS

Steam turbine; life assessment; maintenance; expert system.

INTRODUCTION

Recently, fossil-fuel power plants operating beyond their original design

lives are increasing in number in Japan. The turbine components in these
plants may have suffered from damage and degradation during long term
service at high temperature.

Quantitative life assessment procedure of the turbine components have been

developed in the combination of non-destructive measurement and damage
analysis (Kimura et a l . , 1 9 8 6 ) . But there still remain a lot of factors
affecting practical component life, such as difficulty of repair, degree of
integrity and individual history (Viswanathan,1989). These qualitative
factors have not been fully reflected on the above quantitative life
assessment in spite of intensive requirements from utilities and vendors.

This paper describes the life assessment expert system which can deal
qualitative information and the process of inference by human expert in
addition to quantitative data used in the conventional system.

INTEGRATED LIFE ASSESSMENT APPROACH

Life assessment of steam turbine components has been done through a method
143
144
shown in Fig. 1 (Fujiyama et al. . 1988), in which the creep and fatigue
damage are analyzed using stress and temperature FEM analysis results, the
operation history and the nondestructive measurement of material degradation
(softening and embrittlement). The run-retire decision of specific steam
turbine component has been done by experts of design and maintenance
engineering based on the several other information such as crack initiation
history, repair history, design parameters as well as the life assessment
result obtained by procedure shown in Fig. 1 above.

In order to make run-retire decision more easily and automatically, the life
assessment expert system was designed and built with an engineering work
station and originally developed expert tool. Figure 2 shows the expert
system for life assessment and maintenance of steam turbine components.

Fig.1 Life assessment and maintenance of turbine component.

Fig. 2 Expert system for life assessment and maintenance

of turbine components
 145
This system has three functional sections as shown in Fig. 3. In the input
section, man-machine interface gets operating conditions, inspection
records, design information and expertise of design and maintenance.
Information and data are stored in database section. We divide the input
data into following types.

1. Data which indicate the present condition of component (inspection

record, operating time, start/stop number, etc. )
2. History of component (crack initiation history, repair history, trend
of operating conditions, etc. )
3. Common data for many units (material properties, temperature, stress,
strain ,etc.)
4. Expertise

Data of the first type are entered on the occasion of assessment, and stored
in temporary database. The second type data are stored in unit database by
operator. The third type data have been stored in common database by design
engineer. And the forth type data have been stored in knowledge base by
human expert for design, maintenance and life prediction.

In the expert system section, this system at first predicts component life
from four kinds of data, and next, makes guideline for repair or replace.

INPUT DATA DATABASE EXPERT SYSTEM

Operating > Temporary

Conditions Database
*
LIFE
ASSESSMENT
Inspection Historical
Record " Database
*
Repairment
Record

Common
{}
Design Database
Information GUIDE FOR
& MAINTENANCE
Expertise of
Maintenance > Knowledge-
base

Fig. 3 Data flow of life assessment and maintenance expert system

EXPERT SYSTEM

LIFE PREDICTION SYSTEM

As steam turbine components can't be used in the crack existing state, crack
initiation is the most important issue in the life assessment. For assuring
the reliability of steam turbine, crack propagation life prediction is also
necessary including repairabi1ity assessment. The component life scatters
mainly caused by the scatter of material properties as shown in Fig. 4 for
the fatigue property for example (Itoh et al., 1990). In the expert system,
the scatter of material properties is analyzed.

Life prediction system is carried out through following four items.

146
1.Prediction of crack initiation life
2. Judgment of repairabi1ity
3.Prediction of crack propagation life
4.Integrated judgment of component life

The life prediction system makes assumptions on the crack initiation life,
crack propagation life and repairabi1ity. For example 'crack initiation life
is in 4 years' and 'Repair is difficult' and so on. From qualitative
information and quantitative data, certainty of assumption is estimated.
This certainty is expressed by a certainty factor (CF) value between -1 to
1. The positive sign means assumption is true and the negative sign means
false. Absolute CF-value indicates degree of belief or disbelief. This
system adopts CF~values shown in Table 1.

99.9 y ^ ^
99.0
g 90.0
& 50.0
h
10.0 E:

: yf
/
5.0
Veibull
distribution
1.0 parameters -
0.5 L / 2 parameter m—3·7 β~Π-ΛΠ
3 parameter m=1.70 β = 0 . 4 9 j
Γ=0.29
0.1 1 1 1 1 1 1 1 t, 1 1 1 1 J i I i il m i
0.2 0.4 0.6 0.8 1.0 2.0 3.0 4.0 5.0
Experimental value/Estimated value β
Fig. 4 Weibull distribution of low cycle fatigue life

Table 1 Certainty factors

MEANING VALUE
TRUE 1
POSITIVE+++ 0.8
POSITIVE++ 0.3
POSITIVE+ 0.1
UNCERTAIN 0
NEGATIVE+ -0.1
NEGATIVE++ -0.3
FALSE -1

Certainty factors estimated from any information are combined by following

formulae. (Rich,1983)

CF comb = CF! CF 9 - CFi CF 2 (when C F p CF 2 > 0) (1)

CF comb CF
1 CF 2 CF! CF 9 (when CFj,CF 2 < 0) (2)
CF comb = CF, CF 9 (when CF 1 «CF 2 < 0) (3)

Measure of belief or disbelief is calculated by formula (1) or by formula

(2) respectively. If finally a positive value and a negative value are left,
combined certainty is calculated using formula (3).
 147
This system adopts the assumption with maximum CF-value among the
calculated C F c o m D values as diagnosis result. In the case that lack of
information leads unrealistic maximum value or a pair of inconsistent data
exist in the same data set, the system breaks diagnosis and requires more
reliable information.

MAINTENANCE ADVISOR SYSTEM

The maintenance expertise is greatly differs from component to component.

Maintenance expertise by human experts are translated into IF-THEN rules and
are stored in knowledge base. In the initial state, the diagnosis results
mentioned above, inspection data and another input data are gathered in a
temporary database. If a data-set matches IF-pattern of a rule, THEN-
procedure will be driven and THEN-procedure will add new facts to temporary
database. In the course of pattern matching, the system asks operator some
questions on demands. The answers to the questions by the operator are also
added into the temporary database. These all event may trigger another
rules, and finally this system derives practical advice for maintenance.

EXAMPLE

An example of l i f e prediction rule i s shown in Fig. 5. And an example of

maintenance expertise is shown in Fig. 6.

(rule creep_void_1
(void oriented)
=>
(assert (crackjnitiation A -0.1))
(assert (crackjnitiation C 0.1))
(assert (crackjnitiation D 0.3))
)

Fig. 5 An example of life prediction rule

(If aligned creep voids were shown, then provide
-0. 1 CF for band A, 0. 1 for C and 0. 3 for D. )

(rule roter_bore_1
(component RTR)
(location bore)
(defect NO)
(diagonosis_result crackjnitiation D ?x)
=>
(write t "RESULT : The roter should be"
"replaced in two years." #\newline)
)

Fig. 6 An example of maintenance expertise

In Fig. 7, an example of diagnosis result for the bore of a high pressure

148
rotor. Right window is data input window which can deal both numeric and
qualitative data. After input section was completed, diagnosis section
starts. Left window is diagnosis man-machine window which asks whether
location is bore or surface at first, because failure mechanism and way of
repair depend on location. In this example, status of component is not
severe. This window indicates no repair is required and recommends repeated
diagnosis after 4-6 years. This advice agree with judgment by human experts.
Similar agreements are also observed for another turbine components.

This system has about 200 rules, and about 30 rules are used in one
diagnosis. We have verified this system with real inspection records and
historical data of steam turbine rotors, casings and valves.

DIAGNOSIS WINDOW
START DATA INPUT WINDOW
Input location of diagnosis. ftflCT.CTSSill I File access 1 ΓΕηΠ
l.Borc
2. Surface Steam temperature ('C) [566]
INPUT: 1 Steam pressure (atm) [169]
Frequency (Hz) [60]
The component docs not suffer severe damage. Power rating (MW) [375]
RESULT -.Class A (CF-value0.91) Number of Start/Shutdown [655]
Operating time (h) [127800]
Is any defect detected in bore of the roter? Component VAMAM ICäsTnpl | Valve 1 I Blade I ΓΒΟΪΪΗ
l.Ycs Initial hardness (HV) [276]
2. No Hardness at siagnostic location [240]
INPUT:2 Hardness at low stress location [254]
Degree of carbide coarsening [Nönel ■TCfflf | Mcdiu
No repair is required. Please diagnose the roterl Calculated fatigue damage [0.001]
again 4 to 6 years later. Calculated creep damage [0.46]
Remaining life (analysis) [11]
END of DIAGNOSIS Creep void formation
Macro-crack initiation
Embrittlemcnt
Defect frequency

Fig. 7 An example of diagnosis display

CONCLUSIONS

An expert system was developed for integrated life diagnosis of steam

turbine plants. This system supports certainty factor combination method and
production system. We have tested the system using some sample data. In all
test cases, the result obtained by expert system agrees with the judgment by
human expert. It was proved that the diagnosis method in the system is
effective for practical life assessment of steam turbines. Through the tests
on practical data, upgrading of the system is in progress now.

REFERENCES

Kimura. K. . K. Fujiyama, K. Sai to, M. Muramatsu and M. Akiba (1986). Life Assessment
and Diagnosis system for steam turbine components. EPRI Conf. on Life
Extension and Assessment of Fossil Plants.
Viswanathan, R. (1989). Damage Mechanisms and Life Assessment ol High-
Temperature Components. ASM international.
Fuj iyama, K. , K. Kimura, M. Muramatsu, H. Kashiwaya, E. Tsunoda, S. Ayano and H. Aoki
(1988). Life Diagnosis Experience and System Technology for Steam Turbine
Components. Proc. o± Int. Conf. "LIFE ASSESSMENT AND EXTENSION", vol. 2. 20-30.
Rich, E. (1983). Artificial Intelligence. MacGraw-Hi11 Book Company.
Itoh, H. . T. Inukai, N. Okabe and K. Kimura(1990). Proc. p_f 4th Int. Conf. on.
Fatigue and Fatigue Thresholds, vol. 4. 2265-2276
 WS6b8
Failure Assessment of Weldments at Elevated Temperatures

G.R. Stevick and I. Finnie

Department of Mechanical Engineering

University of California, Berkeley, CA 94720 USA

ABSTRACT

This paper treats the initiation and propagation of cracks along a weld metal/base metal
interface at elevated temperature. For the case in which the creep properties of the weld and
base metals differ, it has previously been shown that significant stress concentrations may
develop at the interface in a double-V weld which may lead to localized cracking early in life.
For crack propagation calculations, the C* integral for typical applied stresses is evaluated as
a function of crack size and different ratios of weld/base metal creep properties. Life
predictions are presented using two procedures. One is based on data in the literature for
creep crack growth rate as a function of C*. The other procedure takes a more fundamental
approach based on the growth of voids from second phase particles on grain boundaries. The
predictions are similar and suggest that a more detailed study of metallurgical variables in
creep-crack propagation experiments could enhance our understanding of this topic. From a
practical point of view, this study suggests that the weld efficiency factors permitted by the
ASME/ANSI B31.1 Piping Code may need to be reevaluated for longitudinal pipe welds at
elevated temperatures.

KEYWORDS

Creep; Crack Growth; Welds; Voids

INTRODUCTION

Two major failures of longitudinally welded hot reheat lines in 1985 and 1986 in the USA
prompted a greatly increased concern about the long term reliability at elevated temperature
of this type of construction. A valuable summary of this problem is given by Jaske (1988),
while Viswanathan et al. (1988) have given a detailed description of flaws detected during
inspection of longitudinally welded pipe in steam power plants.

The service failures referred to earlier initiated near the weld fusion line in the mid-wall region
and were not surface connected (Jaske 1988). Examination of longitudinally welded power
plant piping following these failures detected 25 flaws of which 15 were located at the mid-
wall region either at the fusion line or in the weld metal (Viswanathan et al., 1988).

As a starting point in discussing the initiation of this type of crack and its subsequent
propagation, we note that the Code used in the USA for power plant piping (ASME/ANSI,
B31.1) allows longitudinally welded pipe which has been heat treated in accordance with Code
specifications and 100% radiographed to be used at the same stress levels as seamless pipe.
149
150

MID-WALL CRACK INITIATION

A distinctive feature of both the service failures and many of the cracks found in subsequent
examinations of longitudinally welded pipe is initiation in the mid-wall region at or near the
fusion line as shown in Fig. 1. Recent work by the authors (Stevick, Finnie 1990) has shown
that the double-V configuration results in a large stress concentration if the creep properties
of the base and weld metals differ significantly. Stress concentrations at the root of this type
of weld were determined for a variety of weld angles and creep coefficient ratios using the
finite element method and assuming power law creep deformation rates of the form:

= Bo, w
n
= B.o" (1)

In these equations, strain rates, e, and stress, σ, are related through the constants, B and n,
with subscripts, w and b, referring to weld and base metal. It was assumed that η„ = nb. The
idealized model used in this and the previous study by the authors is shown in Fig 2.

Fusion Line Finite Element

Crack Model Boundary

6.4 mm Alb, 30 deg.

Fig. 1 Idealized longitudinal pipe weld model. Pipe

curvature is neglected and plane strain conditions
assumed. A typical fusion line crack is also
shown.

Development of the stress concentration as a function of time is shown in Fig. 2 for a 30

degree l-l/4Cr-l/2Mo double-V weld and a BJBb ratio of 5 (Stevick, Finnie, 1990). The
applied stress and temperature were 45.5 MPa and 538 °C, respectively. An almost identical
result is obtained for 2-l/4Cr-lMo at the same stress and 566 °C. Creep test curves of service
exposed pipe and weldments given by Henry et al. (1990) indicate that BJBb ratios may be
as high as 10 in some cases.

With this magnitude of stress concentration, it would not be surprising to find early crack
initiation at the mid-wall based on tensile creep rupture data. This is in accord with field
observations that cracks, while not detected initially, were observed after a period of operation.

The question of "crack initiation" is in general by far the more difficult aspect to treat in any
fracture calculation. For this reason, now that we have pointed out that crack initiation early
in life may be inherent to longitudinally welded pipe, we put this aspect aside at this time and
will concentrate on crack propagation.
 151

1.6
ö
o

£ 1.4
Ö
ω 30 Deg. D o u b l e - V Weld
o
ö l-l/4Cr -l/2Mo
o
u R=5
w
w 1.2

1.0
Π 10 90 ^0 40 R0
Time (Thousand Hours)

Fig. 2 Stress concentration vs. time (uncracked weld).

CRACK PROPAGATION

There is a large and growing literature on the conditions determining creep crack propagation.
One of the earliest which attempted to correlate creep crack propagation with the crack tip
singularity was presented by Sakata and Finnie (1975). Subsequently, with the development
of non-linear fracture mechanics, extensions of the J integral have been used to relate creep
crack propagation, da/dt, and the time dependent version of J, C* or the more general
formulation Ct. These approaches have great value, but they are empirical and provide no
insight into the metallurgical parameters involved. For this reason, in the present work, we
begin our study of creep crack propagation by evaluating C* for a weld line crack with
different creep properties on opposite sides of the crack. Using tabulated values for da/dt vs.
C", we predict life as a function of initial crack size for a nominal stress typical of reheat
piping. A more important step is to attempt to develop a simplified physical model in which
da/dt is predicted for given values of C\ grain size, particle size, and particle spacing. This
approach while admittedly simplified, is shown to agree well with the conventional approach.
To start we compute the C* integral.

C* as a function of crack length and creep constant xzno,BJBbi was determined for the typical
double-V weld configuration shown in Fig. 1. To ensure accuracy, element sizes were
decreased by factors of 2 until the C* results varied less than 1 percent from one size to the
next. For small crack to thickness ratios, elements sizes were as small as 30 by 30 microns
(0.0015 inches). As a check, an analysis of a center cracked plate (plane strain) was compared
with the fully plastic J integral solutions published by EPRI (Kumar et al., 1981). The results
were within 1 % of the EPRI solution.

The power law coefficients used in the finite element analysis for the base metal are n = 5 and
B = .94xl016. These constants are an average of those for l-l/4Cr-l/2Mo at 538 °C and 2-
l/4Cr-lMo piping at 566 °C given in EPRI's Users Guide for their high temperature crack
152
growth program, SLIC 2 (Dooley 1989). The exponents n in the EPRI reference are the same
for both materials and the constants B differ by 12% for the temperatures given above.

The stress level away from the weld for all of the work described in this paper was assumed
to be 45.5 MPa. This stress level is the present code allowable for l-l/4Cr-l/2Mo at 538 °C
and is typical of operating stress levels for 2-l/4Cr-lMo piping operating at 566 °C.

C* results for various crack sizes and creep constant ratios are shown in Fig. 3 with the EPRI
solutions for a center cracked plate (ccp) of the same dimension. In the center cracked plate
model, the crack is oriented perpendicular to the sides of the specimen and all material
properties are assumed to be constant. The half crack length, a, is measured along the fusion
line of half length b; t is the specimen thickness. For the weld specimens, the crack is
assumed to be symmetric, growing along the fusion line in both directions.

0.0 0.2 0.4 0.6 0.8 1.0

Crack Length ( a / b )

Fig. 3 C* as a function of crack length and creep constant

ratio for a fusion line crack.

The crack growth assessment presented here for low-chrome weldments is based on the growth
and coalescence of cavities ahead of the crack tip and is similar to that performed by Wong
et al. (1988) in their analysis of two-phase solders. The primary difference is the addition of
an adjustment to the expressions for cavity growth to account for triaxiality in the stress field
surrounding the growing cavities. Calculation of C* allows us to characterize the stress and
strain field near the tip of the crack for steady state power law creep (Hutchinson 1983):

(2)
°&<T±f**,
where x is distance along the weld fusion line from the crack tip and I„ and atj are
dimensionless functions (Shih 1988). The crack is assumed to proceed by the growth and
 153
coalescence of cavities along grain boundaries adjacent to the crack tip. The cavities nucleate
from particles along the weld fusion line. Nucleation time is assumed short due to high local
stresses (Raj 1978). The growth rate of individual cavities via creep flow is derived from the
work of Rice and Tracey (1969) and Beere and Speight (1978):

— = (-)0.283exp(-^X = (-) 0.283 exp(-^)£o/ (3)

dt 2 oe 2 ae
where R is the void radius, om is the mean stress, oe is the effective stress and ee is the
effective strain. Assuming the nucleation and growth of cavities is confined to the HRR
region, the growth rate of the cavities can be obtained by substituting (2) into (3). For
simplicity only cavities on the facet adjacent to the crack tip are assumed to grow. It is also
assumed that when the first cavity grows to a size equal to half the interparticle spacing, λ/2,
the cavities interlink and the crack grows a distance equal to the length of one grain boundary
facet, Δ. Thus, the rate of crack advance for steady state creep conditions can be expressed
in terms of the decreasing distance, x, between the crack tip and the first cavity:

£ = -2(7>(f) <4>
dt λ dt
Combining (2), (3) and (4):

f^ = _o.283exp(-^)—*_(-^1)<«+1> ö, f Ϊ^<Ε (*)

PK
>mR öe\daldt)KInB <J_m

where d is the particle diameter. Integrating and solving for the crack growth rate, da/dt:
1
^da « 0 . 2 8 3 e x p ( ^ ) ( n + l X ^ ^ ) ^ ( ^ ) ^ + 1 ) - ^ ^ - d £ (6)
dt öe 2 In \n(X/d)

Failure time of an individual facet can be calculated as a function of crack length by dividing
the average facet length by the corresponding da/dt from (6). From Wong et al. (1988) the
average facet length is approximately 36 percent of the average grain diameter. Assuming an
initial flaw size, remaining life is the summation of the failure times for all of the facet lengths
in the remaining ligament.

For low-chrome weldments, typical microstructural data along the weld fusion line was
obtained from a recent study (Henry et al, 1990). Average grain diameter was taken as 50
microns. The data on particle size and spacing were not extensive, however, they indicate an
average spacing of 10 microns and an average particle size between 0.25 and 1.0 microns.
Using (6), remaining life was calculated for the typical low-chrome weld configuration shown
in Fig. 1 as a function of initial crack size, weld/base metal creep constant ratio, and particle
size. The results are shown in Fig. 4, for weld/base metal creep constant ratios of 1 and 10.
The results for a ratio of 5 are similar, but not shown because of space.

The solid line in each graph represent life calculations based on da/dt=A(C*)m data for 2-
l/4Cr-lMo from Dooley (1989).
154

Crack Length ( a / b )

Fig. 4 Remaining life vs. initial crack size.

DISCUSSION AND CONCLUSIONS

The crack growth model described above shows good agreement with the traditional C* vs.
da/dt method. This indicates that it may be possible to reduce the scatter in some C* vs. da/dt
data by considering microstructural variables. The dependence on particle spacing explains
why cracks often grow along the weld fusion line where there is a relatively higher number
of particles in low-chrome welds. However, the new model also raises many questions. The
weld angle and difference in weld and base metal creep properties almost certainly result in
mixed mode loading for a crack along the fusion line. This is not accounted for in the current
model. Physical relations between microstructural variables, grain size, particle size, and
particle spacing are also not considered. These variables are probably not independent and
additional work will be necessary to characterize their dependence on each other and the
welding process. We hope to address these issues in future work.

REFERENCES

Beere, W., M.V. Speight (1978). Met. Sei., 12, 172-176.

Dooley, R.B (1989). Users Guide for SLIC2, EPRI Project no. 2595-7.
Henry, J.F., F.E. Ellis, C D . Lundlin (1990). Welding Research Council Bulletin 354.
Jaske, C.E. (1988). Proc, Ses. II, Int. Conf. on Life Ext. and Assess., The Hague.
Kumar, V., M.D. German, C.F. Shih (1981). EPRI Research Project no. 1237-1.
Raj, R. (1978). Acta. Metall, 26, no. 6, 995-1006.
Rice, J.R., D.M. Tracey (1969). J. Mech. Phys. Solids 17, 201-217.
Stevick, G.R., I. Finnie (1990). Proc. 4th IUTAM Sym., Creep in Structures, Crackow.
Sakata, M., I. Finnie (1975). Trans. Japan Soc. Mech. Engrs., 41, 1089-1094.
Viswanathan, R., Dooley, R.B., Saxena, A. (1988). ASME J. PVT, U 0 , 283-290.
WS6b9

EVALUATION OF CREEP RUPTURE PROPERTIES WITH MINIATURE TEST PIECE

Keiji Sonoya, Yoshihiko Sakai, and Masaki Kitagawa

Research Institute
Ishikawajima-Harima Heavy Industries Co., Ltd.
3-1-15, Toyosu, Koto-ku, Tokyo 135, Japan

ABSTRACT

As much as about 60 % of Japanese thermal power plants have been in service

for over 100,000 hours, so that many of them are time-worn. To maintain a
high level of safety for these plants, a highly refined maintenance system
is called for. For these plants, development of methods of evaluating the
remaining service lifetime for the aged equipment is indubitebly an
importantr task, for which various diagnostic methods, including the one
shown in Fig. 1 that comprises three steps1*, have been proposed. Now, it
has been shown that the lifetime of a part or member of an equipment can be
predicted with satisfactory accuracy if the degradation in the mechanical
properties, that in the creep chracteristics, in particular, of that part
is known2'. Although several non-destructive methods of evaluating such
degradation on the basis of changes in the physical properties are
available, correlations between physical properties and mechanical
properties remain unclarified. All in all, therefore, higher accuracy in
lifetime prediction can only attained by performing destuctive mechanical
tests on speciments that have been sampled directly from the part in
question. In reality, however, taking large specimens from an operating
equipment is a highly difficult proposition, even if such an undertaking is
allowed. It is for these reasons that we have been examining a number of
testing methods that may be donducted with a small quantity of sample. In
the present communication, we intend to discuss an experimental creep
machine we have devised so as to make use of miniature-size test pieces and
the results obtained with it.

KEYWORDS

Evaluation of remaining life; thermal power plant; 2jCr-1Mo steel;

miniature specimen creep tester; oxidation; Ar atmosphere.

SAMPLE STEEL AND METHODS OF EXPERIMENT

Sample Steel and Miniature Test Piece

155
156
For the sample, the 2.25Cr-1Mo steel, which is widely used for the major
components of various kinds of equipment of thermal power and chemical
plants today, was elected. To simulate those parts that are expected to
call for serious evaluation of remaining service life-time soon, moreover,
the sample steel was made so as to accord the practice of some twenty years
ago by raising the Si, P, and S contents than the current practice. Its
chemical composition and the heat treatment conditions are presented in
Table 1.
The specimen, called here the miniature test piece, on the other hand, was
designed so as to be as small as possible, yet to fracture in the gauge
length on creep rupture testing. The final configuration arrived at, which
is illustrated in Fig. 2, was of a parallel portion with a diameter 2mm and
a length 27mm. Specimens of conventional configuration, i.e., those with a
parallel portion of 8mm in diameter, were also tested for comparison.

Testing Method

Since the miniature specimens were thought to require a protective

atmosphere to guard them from inordinately excessive oxidation arising from
their smallness, hence from giving false estimates of the applied stress, a
special creep machine, called the miniature specimen creep tester, was
devise so as to maintain an Ar atmosphere during test (to be described in
3.1).
The creep tests were conducted using this miniature specimen creep tester
at three temperature levels in a range of 570° to 680°C, the range that may
be considered as most appropriate for assessing the performances of the
materials for boilers and like equipment, either in an Ar atmosphere or in
air (i.e., by allowing the ambient air to enter freely via the relief
valve) up to 1,000 h. The effects of oxidation were examined by comparing
the results obtained in Ar with those obtained in air, while the specimen
size effect was appraised against the results obtained with the
conventional 8mm specimens.

RESULTS AND DISCUSSION

Design of the Miniature Specimen Creep Tester

The miniature specimen creep tester is presented in Fig. 3 by a schematic

drawing. It is a direct loading (up to 200 kgf) type machine of 2m high,
0.5m wide, and 0.5m deep. The most conspicuous feature of this machine is
found in its atmosphere controlled testing chamber: while it holds specimen
at a chosen temperature to ±1°C, it maintains an Ar atmosphere by means of
an atmosphere control unit, comprising an evacuation unit and an Ar feeding
unit, so as to prevent excessive loss of effective cross section due to
oxidation.
Since the internal pressure of the testing chamber is upheld with a pair of
0-rings, the combined effect of the 0-rings and the internal pressure as an
additional load on the specimen was examined by reading the total load with
a strain gauge attached to the specimen for varied Ar pressures, and by
noting the difference to when it was released. The results are shown in
Fig. 4: although the load on the specimen does increase somewhat with
increasing Ar pressure, the increment, being about 0.5 kgf at the most,
remains insignificant even for a pressure difference of 19.5 kPa.
The standard procedure of making the Ar atmosphere thus decided upon was as
follows: first evacuate the chamber to 10-3 Torr, then fill it with Ar to
 157
14.7 kPa, the effect of which may safely be ignored.

Creep Rupture Tests

The results are presented in Fig. 5, both for the miniature test pieces and
the conventional test pieces. In the case of the miniature specimens, the
effect of oxidation is such that, while the rupture time in air is about
the same as that in Ar at 570°C, the former becomes noticeably shorter at
630°C and beyond. This is revealed more clearly in Fig. 6, where the creep
rupture data are plotted in terms of the Larson-Miller parameter, P: the
air data run lower to the Ar data for P's larger than 1.8X104, the
difference being the larger, the larger the P.
On the other hand, no effect of specimen size was seen in the Ar atmosphere
tests: at least up to 680°C, i.e., within the scope of this study, the
rupture times obtained with the miniature specimens agreed satisfactorily
well with those obtained with the 8mm specimens.
It was observed, moreover, that the reduction in area was much the same in
all cases. This has been taken as indicating that neither the testing
atmosphere, i.e., whether it is Ar or air, nor the specimen size affects
the ductility of the steel.

Effects of Oxidation on Creep Rupture Time

It is known that the 2.25Cr-1Mo steel exhibits inordinately large

degradation in the creep rupture time on higher temperature, longer time
side. Since the surface oxidation is considered to play an important role
in this phenomenon, the effects of oxidation were quantitatively assessed.
Figure 7 presents the thickness of the surface oxide layer, as determined
postmortem at specimen shoulder, i.e., the part where the oxide film should
have been subjected to the creep elongation the least, as a function of P.
Here, the inscribed regression curve, which is due to the National Research
Institute for Metals (NRIM), is given by3):

T(l4.68+log t r ) = 1.703X104+1.698x103· (log d)+2.673x 102· (log d )2, ...(1)

where T is the testing temperature in K: t r , the rupture time in h; and d,

the thickness of oxide film in mm.
The figure shows that, while the oxide film hardly forms in Ar even at
680°C, as shown in Fig. 8 by a cross sectional metallography, it gros
rapidly at and above 600°C, so fast that it is as thick as about 1mm at
680°C (Fig. 9 ) , even though it is only about 5um thick at 570°C.
These observations, when considered in view of the results pertaining to
the creep rupture behaviors described earlier on, may be taken as proving
that the experimental methodology adopted in this study is quite adequate
to revealing the true creep characteristics of the steel with specimens of
grossly reduced size.
Now, it has been argued that the inordinately large degradation in the
creep strength often observed in high temperature creep test is actually
due to increase in the true stress arising from the decrease in the
effective cross section due to surface oxidation*). The validity of this
theory has been examined by deducing the effect of oxidation in comparing
the air data and the Ar data obtained with the miniture test pieces, as
followsS).
If the initial stress is σ0, the true stress after a time t, or the stress
corrected for the change in the cross section, at, should be:
158
ot=o0-(D0/Dt)2 .(2)

where D 0 is the initial diameter of the specimen, and Dt, the effective
diameter at time t.
Now, assuming the linear damage accumulation law holds true for the creep
rupture times based on ot, we write:

tr(t)=tr/trM(o0)-trM(ot), .(3)
where trM(o0) · trM(o), denotes the creep rupture time to be read off the
master curve for a stress o, which can be given for the 2.25Cr-1Mo steel
as:

(T+273.15)-08.77+log trM(o)) =
21598-334.9-(log o)-23l8-(log σ)2 (4)

The creep damage factor, D e , can then be calculated from (3) as:

(5)

whereby the first round calculation gives a corrected time trG1 as:

trd = Dc* ^r
Subsequent calculations are a reiteration: first, correct the master curve
with the data corresponding to the t r c l, then re-enter (2) with the newly
corrected figures, and carry the computation through to (6).
For the case at hand, we have obtained the finally corrected master curve
as:

(T+273.15)-08.77+log trM(o)) =
22600-1779* (log d)-l808-(log d)2. ...(7)

where d=D 0 -Dt, i.e., the amount of diametric loss in the time t at T°C.

Figure 10 presents a comparison of the Ar data obtained with the miniature

test pieces with calculations on (7), which are really the air data
obtained with the same specimens but corrected for the effects of
oxidation. Since the two agree quite well, we conclude that the major
factor that goes rise to degraded creep rupture time in air at temperatures
600°C and above is the increased true stress arising from the loss of the
material due to oxidation.

SUMMARY AND CONCLUSIONS

The miniature specimen creeptester, with its testing chamber maintained

airtight with a pair of 0-rings, performed quite well, in that, for
example, the combined effect of internal Ar pressure and 0-rings could be
safely ignored.
With Ar for the testing atmosphere to forestall oxidation, the rupture time
obtained with the 2mm diameter miniature test pieces agreed quite well with
that obtained with the 8mm diameter conventional test pieces.
The effect of oxidation to degrade the rupture time became manifest from
about 600°C and above.
 159
The major cause of this degradation is increase in the true stress arising
from the loss of material due to oxidation.

REFERENCES

Kitagawa, etal., Ishikawajima-Harima Engineering Review, No. 5 ( 1 9 8 8 ) , 9.

Umaki,e*ai., ibid, No. 3 ( 1 9 8 9 ) , 5 .
Kaneko, etal., Tetsu-to-Hagane, CAMP-ISIJ, 1, ( 1 9 8 8 ) , 900.
NRIM Creep Data S h e e t , No. 3B ( 1 9 8 6 ) .
Nakashiro, et at., Preprints to 27th High Tempeerature Strength Symposium, ( 1 9 8 9 ) , 1.

Table.1 Chemical composition of 2 !4Cr-1Mo (mass %)

C Si Mn P S Cr Mo Ni Cu Nb Al N

STPA24 0.125 0.34 0.53 0.014 0.011 2.38 1.12 0.15 0.17 0.01 0.002 0. 0073

JIS 0.30 1.90 0.87

<0. 15 <0.50 \ <0. 030 <0. 030 S S - - - - -
Spec. 0.60 2.60 1.13

Normalized for 2h at 970°C and Tempered for 9h at 720°C and PWHT for 7. 5h at 720°C

Fift 2 Specimen for miniature creep rupture test

Fig. 1 Remaining lifetime evaluation system

Fig. 4 Relation between dead weight and load under various gas pressure

Fie. 3 Sketch of miniature creep testing machine

160

Fift 5 Creep rupture test results of 2 ViCr-IHo Fig. 6 Creep rupture life of 2 '/iCr-llto

p— Regression line of
Regression curve of
: 2/<Cr-Mo in NKIM ' i specimen in Ar gas
O : 57CTC
Δ : 630°C
D:680°C
$--· /
; : Open : in Ar gas
Solid: in Air
Atomosper
e

I A
AJ
Sp2iim«
(.Φ2)
n
O

•
Ar

Amen
3 Air
(*8>

— A- 1 Qi 1 .
15 16 Π 18
10 , I
P = (273.15+T) x (14.68+logtr) x 103 1700
0 18000 19000 20000 21000 2
Parameter(T+273.15)x(log(Tr)+18.8)
Fia 7 Oxide scale growth kinetics for 2%Cr-1Mo steel
Fia 10 Stress vs L.M.parameter for 21/4Cr-1Mo steel corrected for oxidation effect

100 M. 100 uf

Fig. 8 Microstructure of creep rupture specim Fig. 9 Microstructure of creep rupture specim
 WS6b11

Strain Bursts in Cyclic Creep of an Al-Mg alloy at

an intermediate temperature

S.J. Zhu Z.A. Yang Z.G. Wang

Laboratory for Fatigue and Fracture of Materials,

Institute of Metal Research, Academia Sinica,
Shenyang, 110015, P.R. China

ABSTRACT

Strain burst behavior in Al-0.87%Mg alloy has been investigated at 100'C. With an in-
crease in frequency, the magnitude of strain bursts increases. There is no strain burst in
static creep. The strain bursts become evident as grain size decreases. The observation of
dislocation structures seems supporting the explanation that strain bursts are caused by
cyclic latent softening. However, the presence of solute atoms seems important and their
effects on strain bursts must be taken into account. Dynamic strain aging strengthening
is affected by loading conditions and grain size. From this view, strain bursts are ex-
plained.

KEYWORDS

Strain bursts; cyclic creep; Al-Mg alloy; dynamic strain aging.

INTRODUCTION

Plastic deformation is usually not a smooth and continuous process. The yield drop and
stress serrations are well-known phenomena as discontinuous plastic deformation. The
strain burst which is some kind of discontinous plastic deformation was frequently re-
ported in creep, cyclic creep, cyclic ramp loading and fatigue in the past years(Silveira
and Monteiro, 1979; Kirk eUil., 1977; Neumann, 1969; Hong and Laird, 1990).

Unlike the strain bursts observed in pure metal(such as copper), the strain bursts in
Al-Mg alloys occur more periodically. The strain bursts can only be observed beyond a
161
162

critical stress and in a certain intermediate temperature range . The strain burst behavior
in Al-Mg alloy was explained in terms of dynamic strain aging (Hu et al., 1990), al-
though in pure copper it was suggested to be caused by a pure dislocation mechanism
without alloying effects. However, little work has been done on dislocation structures
with or without strain bursts in Al-Mg alloys. In this paper, not only do we report the
mechanical behavior of strain bursts, frequency and grain size effects, but we also pro-
vide a detailed description of the dislocation structures and explore the micromechanism
of strain bursts.

EXPERIMENTAL PROCEDURES

The alloy for the present study was smelted and cast in a vacuum furnace and posseses
the following chemical composition(in wt.%): 0.87Mg, 0.003Si, 0.0022Fe, 0.00006Ti,
0.000085Ca and the balance Al. After homogenizing at 500 <C for 1 h, the cast ingot was
hot-forged into rods of around 25mm in diameter and then cold-rolled into cylindrical
rods with a diameter of 18mm. These rods were finally cut and machined into the re-
quired round section specimens with thread heads and a diameter of 7.5mm. Prior to me-
chanical testing, the specimens were annealed in the temperature range of 300-5 50 "C in
order to obtain different grain sizes from 0.11 to 2.08mm.

The static and cyclic creep tests were performed on a floor mode MAYES ESM 100 test-
ing machine under the condition of complete unloading. A saw-tooth waveform was se-
lected and load was used as the control parameter. All the tests were conducted at 100 ±
VC . The test frequencies were 0.1, 0.5 and 1.0 Hz. The creep strain was measured by
means of a linear variable differential transducer.

Slices were cut from the statically and cyclically crept samples both parallel and perpen-
dicular to the tensile axis for TEM studies. Slices were thinned for electron microscopy
using standard techniques and they were observed in a Philips EM 420 operated at 100
or 120kV.

RESULTS

Static and cyclic creep curves for Al-0.87%Mg alloy are presented in Fig.l. Strain bursts
occur in cyclic creep tests, but no strain bursts exist in static creep curves. These results
agree with previous results for A l - l % M g alloy (Shin et al., 1988). Unlike pure copper
where strain bursts occur only during stage Π cyclic creep (Lorenzo and Laird, 1982),
strain bursts in Al-0.87%Mg alloy occur right after loading. The strain burst incubation
period increases with time in stage I creep and tends to be constant in stage Π creep. It
should be noted that cyclic creep strain rates in one incubation period are lower than
static ones although the total strain rates of cyclic creep are higher than those of static
creep. At room temperature and 80% ultimate tensile stress, cyclic creep strain for
 163

Al-0.87%Mg alloy does not change with time while cyclic creep strain for Al-0.09%Mg
increases with time, as shown in Fig.2. These demonstrate that there are great strength-
ening effects of dynamic strain aging in cyclic creep for Al—0.87%Mg alloy.

Since cyclic creep rates are defined as strain / time, it is important to ask whether or not
the cyclic creep rate is frequency-dependent. No significant frequency effect on cyclic
creep was reported in copper in the range of 0.1—2.0 Hz at room temperature (Lorenzo
and Laird, 1984b). However, strain burst behavior was not observed during cyclic creep
of copper at a frequency of 0.01Hz (Chandler and Bee, 1985). The variation of strain
bursts with frequency for the Al-0.87%Mg specimens cyclically crept at the maximum
stress of 80MPa and 100"C is shown in Fig.3. With an increase in frequency, strain burst
magnitude increases and creep strain rates increase. This agrees with the results shown in
Fig.l.

2 o
(r> o AI-0 09V.Mq

240s
Timt

AI-0-877.M9

Fig.l. Static and cyclic creep Fig.2. Cyclic creep curves for
curves for Al-0.87%Mg alloy at Al-0.09%Mg and Al-0.87%Mg
the maximum stress of 80MPa and alloys at room temperature and 80%
100 °C. ultimate tensile stress.

There are great effects of grain size on discontinuous deformation in Al-Mg alloys in
tensile tests. The magnitude of serration increases with a decrease in grain size (Fujita
and Tabata, 1977). The effects of grain size on strain bursts and cyclic creep deformation
in Al-0.87%Mg alloy are shown in Fig.4. With a decrease in grain size, the strain bursts
become more evident and strain burst incubation period increases and cyclic creep strain
rates decrease.

In order to study the dislocation structures, the specimens crept statically and cyclically
at different frequencies were interrupted at 80MPa. This stress gives the more enhanced
strain burst behavior.

Figure 5 shows the dislocation structures crept statically at a strain of 0.04. It can be seen
that there is a tendency for the cell walls in Fig.5(a) to lie along the trace of the [111]. In
some grains, the dislocation walls along the trace of the [111] are formed as shown in
164

Fig.5(b).

Fig.3 Variation of strain burst Fig.4. Effect of grain size on

with frequency for the specimens cyclic creep strain for the
with a grain size of 0.28 mm specimens cyclically crept at the
cyclically crept at the maximum maximum stress of 80MPa and 100'C
stress of 80 MPa and 100'C.

^ V
v
\ 1i 111 1 v\ 111
\ \

Fig.5. Dislocation structures crept statically at 80MPa and a strain

of 0:04. foil zone axis [011], (a) g[200], (b) g[l 11].

Figure 6 shows the dislocatuon structures crept cyclically at 0.1 Hz and a strain of 0.05
Similar to the dislocation fectures obtained in copper(Lorenzo and Laird, 1984a), Fig.6
shows some straight cell walls with preferential orientations. Figure 7 shows the disloca-
tion structures crept cyclically at 0.5 Hz and a strain of 0.05. Unilike dislocation struc-
tures induced by static creep, dislocation walls are along two intersecting traces.
 165

Λ
χ
I .
ι
• ^
/ *^*/
***'

Fig.6 Dislocation structures crept Fig.7. Dislocation structures

cyclically at 80MPa and 0.1Hz and crept cyclically at 80MPa and
a strain of 0.05. foil zone axis 0.5Hz and a strain of 0.05. foil
[112], ß[220]. zoneaxis[Il2],ß[lTl]

DISCUSSION

The dislocation structures of specimens crept statically and cyclically are charaterized by
dislocation cells and dislocation walls along main slip system. Dislocation walls induced
by cyclic creep are oriented along the traces of the secondary slip system. This structure
was suggested to be resulted from repeated micro-slip on secondary systems and the
subsequent rearrangement of the dislocations, and be associated with burst
behavior(Lorenzo and Laird, 1984 a). Examination of the dislocation of cell structures
provided evidence that such structures change continuously during cycling and
deformation proceeds by breakdown of cell walls, producing localized areas of high uni-
form dislocation density from which new cells can form and grow during subsequent cy-
cling before their eventual breakdown (Chandler and Bee, 1985).

Figures 5 and 6 are very similar to the dislocation structures before and after a strain
burst for pure copper(Lorenzo and Laird, 1984a). This seems to support the suggestion
that the strain bursts can be interpreted by cyclic latent softening and dislocation
avanlanches originating from secondary-rich dislocation clusters. However, the impor-
tance of solute stoms for strain bursts behavior can not be neglected. Dynamic strain ag-
ing decreases creep strain owing to solute atoms pinning dislocations. In static creep,
steady creep stage occurs after establishing a balance between dynamic strain aging and
thermal activation processes in cyclic creep, cyclic loading and unloading produce more
dislocation tangles which are quite necessary for the onset of a sudden burst of disloca-
166

tion motion (Tabata, et al., 1980) and more vacancies which enhance the diffusion of
magnesium atoms to the dislocations. On the other hand, cross-slip of dislocations dur-
ing cyclic unloading permits those cross—slipped dislocations to escape the obstacles.
This decreases dynamic strain aging hardening and becomes more effective as frequency
increases. This is why strain bursts magnitude increases with increasing frequency. The
fact that grain size affects both serration and strain burst in a similar way also indicates
that dynamic strain aging is very important for strain bursts. With decreasing grain size,
the amount of grain boundaries as obtactales against dislocations motion increases in a
certain volume and therefore the effects of dynamic strain aging are more evident. As a
result, the magnitudes of serration in tensile test and strain bursts in cyclic creep test in-
crease with decreasing grain size.

ACKNOWLEDGEMENTS

This work was supported partly by the Chinese Academy of Science under special Grant
No.87-52 and partly by the National Nature Science Foundation of China under con-
tract No. 59071020.

REFERENCES

Chandler, H.D. and J.V. Bee(1985). Acta Metall., 33,1121-1127.

Fujita, H. and T. Tabata(1977). Acta Metall., 25, 793-800.
Hong, S.I. and C. Laird(1990). Mater. Sei. Eng., A124,183-201.
Hu, X.B. Z.A. Yang and Z.G. Wang(1990). Scripte Metall., 24,1535-1539.
Kirk, J.H., D.K. Matlock, G.R. Edwards and W.L. Bradley(1977). Metall.
Trans. 8A, 2030-2032.
Lorenzo, F. and C. Laird(1982), Mater. Sei. Eng., 52, 187-194.
Lorenzo, F. and C. Laird(1984a), Acta Metall., 32, 671-680.
Lorenzo, F. and C. Laird(1984b), Acta Metall., 32, 681-692.
Neumann, P. (1969), Acta Metall., 17,1219-1225
Shin, D.H., K.T. Hong and S.W. Nam(1988), Scripta Metall, 22, 1607-1609.
Silveira, T.L. da and S.N. Montiro(1979), Metall. Trans., 10A, 1795-1796
Tabata, T., H. Fujita and Y. Nakajima(1980), Acta Metall., 28, 795-805.
 WS6b12

THE APPLICATION OF SSR METHODIN FRACTURE

TOUGHNESS ASSESSMENT OF WELDED JOINT

A. L. Lu and H. Z. Fang
Tsinghua University, Beijing, 100084, China
A. W.Pense
Lehigh University, Bethlehem, Pal8015, USA

ABSTRACT

In the present work the fracture toughness parameter JIC of the repair—welded joints in a
Ni—Cr—Mo turbine rotor was successfully determined by using the single specimen resistance curve
method (SSR method). The results indicate that the weakest region in toughness of the repair—weld-
ed joints locates at the coarse—grained zone of the HAZ where JIC value is between a range of 115~
186 in-lb / in2 (20.1 ~ 32.6KPa · m). The results also indicate that the JIC value of an entire joint is
basically governed by the weakest region of the joint and therefore adopting SSR method to assess
JIC value of an entire joint is an effective approach to assess the fracture toughness of repair-welded
workpieces.

KEYWORDS

SSR method, elastic-plastic fracture assessing, J—integral, single specimen, entire joint.

INTRODUCTION

For many years the fracture toughness assessment of welded joints has been a subject to which a lot
of attention is paid (Satoh et al., 1982;Prasannakumar et al., 1983; Fang et al., 1985). Meanwhile,
how to determine the fracture toughness parameter JIC of bond zone and coarse—grained zone in
welded joints and what is the exact implication of the JIC value for an entire welded joint are two
particularly attractive topics. If adopting the conventional multiple-specimen risistance curve tech-
nique to determine the JIC values, obviously, it is difficult to obtain the satisfactory answers to
above—mentioned questions. This is because the heterogeneity of welded joint makes the problem
more complicated. The serious heterogeneity of welded joints, both in structure and in properties,
makes it difficult to control the front zone of the precrack in a predicted zone (for example, in
coarse-grained zone) during fatigue precracking. This naturally makes the JIC value obtained from
the resistance curve with these specimens lose its clear physical conception. Therefore, the
conventional multiple—specimen method deos not satisfy the requirements of fracture toughness as-
sessment in repair—welded joints, especially when only a small amount of material which is cut from
an in-service workpiece to be repaired is available, but as reliable as possible result is needed.

167
168

Fortunately, in recent years, a new SSR method (i.e. single specimen resistance curve method)for de-
termining JIC value (Clarke, 1981) is being developed which has some advantages to solving the dif-
ficult as stated above.
The emphasis of the present paper is not only to apply the SSR method to determine the JIC value of
the lowest toughness zone of repair-welded joints in an in-service Ni-Cr-Mo turbine rotor, but al-
so concerned with investigating the real physical meaning of the JIC value of an entire joint and
thereby creating further basis for more effectively assessing the fracture toughness of a welding—re-
paired in-service workpiece.
All the SSR tests described in the present paper were performed with computer controling technique
which makes the fracture toughness assessment of an in—service workpiece quicker and more accu-
rate.

MATERIALS AND EXPERIMENTAL DETAILS

The in-service workpiece investigated in the present work is a turbine rotor made of Ni-Cr-Mo
steel which was produced in America (the commercial name of the steel is BSC-3 A) while the code
of the wire used for the repair—welding is E91T1—K2. The chemical composition and mechanical
properties of the rotor steel and deposited metal are listed in Tab.l. The welding parameters are list-
ed in Tab.2.

Tab.l Chemical Compositions and Mechanical Properties of the Materials

Chemical Compositions (wt%) Properties

Material ays UTS Elong

C Mn P S Si Ni Cr Mo V Sn Al
MPa MPa (%)
BSC-3A 0.27 0.28 0.005 0.008 0.05 2.81 1.73 0.37 0.08 trace - 647.1 784.3 23

E91T1 0.5- 1.00-

-K2
0.15 0.03 0.03 0.8
2.00
0.15 0.35 0.05 - 1.8 539.2 618-755 17
1.75

Tab.2 Welding Conditions for the Welded Joint (25.4mm thickness plate)

Heat Input Voltage Current Speed

Specimen Pass
(KJ/cm) (v) (A) (cm / min)

BSC-3A
-20 29-30 300 -28 7
Weld Joint

In the present work, the JIC specimens used in SSR test were a standard 1 / 2 T CT type (thickness
B= 12.7mm), some with a 20% side groove. Two kinds of precracking positions at welded joints of
the Ni-Cr—Mo rotor steel are designed, for one of them the notch is made along bond, for another
the notch is made across bond. Before fatigue precracking is made the two sides of the precracking
zone were pre—pressed. After fatigue precracking 20% side groove at the two sides of the specimens
are made. All these will be helpful to reduce so-called tunnel-effect (Devries, 1983) occurring at the
fractured surface during tests.
The procedures of the single specimen JIC test in this work are conducted the in accordance with
ASTM specification E813-81. All fracture toughness tests are performed on a computer controlled
 169
Instron machine. The partial unloading amount at each turn is 10~20 percent of the calculated limit
load and the magnification of the partial unloading plot is about ten times of its original
loading-displacement diagram. SEM technique was used to analyse the fracture appearance of some
specimens.

RESULTS AND DISCUSSIONS

The Region with Lowest Toughnes in Welded Joints

The results of SEM fracture appearance analysis for welded joint of Ni-Cr-Mo turbine rotor re-
paired with E91T1-K2 wire illustrate that the base metal zone shows coarse dimple pattern and
presents ductile rupture, the fine-grained zone in HAZ shows fine dimple pattern and presents
ductile rupture, the coarse-grained zone in HAZ shows rock candy pattern and presents brittle frac-
ture, the weld metal zone shows fine dimple pattern and presents ductile rupture. It is obvious that
the coarse-grained zone in HAZ is the lowest toughness region of the joint. The SEM fractographs
for the three parts of the joint (the base metal, the coarse-grained zone and the weld metal) are
shown in Figure 1 (a), (b) and (c) respectively.

SSR Tests for The Base Metal and HAZ

Figure 2 is the load-displacement curve of SSR test for specimen B S C - 3 A - 4 # . The qualifying
regression line data for R-curve is carried out in accordance with ASTM specification E813-81. The
R-curve and the regression results for the specimen BSC-3A-4 tested with SSR method are illus-
trated in Figure 3. From Figure 3 a JIC value of 878 in-lb / in2(154KPa · m) can be obtained.
SSR tests for HAZ of the joint were done with specimen A t and A2. The load—displacement curve
for specimens Ax and A 2 tested with SSR method are shown in Figure 4 and 5 respectively. It is ob-
vious that the two patterns shown in Figure 4 and 5 are completely different in fracture behavior and
there is a great difference between the two JIC values corresponding with the two patterns (A^JSJ
KPa · m, A2: 20.1 KPa · m). Although the fatigue pre-crack of the two specimens (A t and A2) are
all located along the coarse-grained zone of HAZ in design, in fact, it is known on the basis of the
fracture analysis results that the pre-crack is at the right position for specimen A2 and at a wrong
position (at fine—grained zone in HAZ) for specimen A t , and there is a great difference originally
both in structure and property between the coarse—grained zone and the fine-grained zone in HAZ,
this certainly results in the serious scatter of SSR results tested in the two kinds of HAZ specimens
mentioned above.
The above—mentioned results of SSR test in the HAZ specimens clearly illustrate that the single spec-
imen resistance curve method can make the JIC value of the narrow and low toughness zone in joint
have definite physical meaning, but the SSR method can not ensure that the fatigue pre-cracking ex-
actly locates along the predicted narrow zone. Consequently, in order to meet the special require-
ments of assessing the fracture toughness for in—service workpiece (i.e. using as small as possible
amount of test material to obtain reliable data), it is necessary to find another more effective ap-
proach based on adopting SSR technique to overcome the unnegligible dispersity problem in data of
the weakest toughness region for the welded joints.

The Jic Value of Entire Joint

Figure 6 is the load-displacement curve of the SSR test for specimen A5 at which the pre-crack is
made across all the three regions of the welded joint. Because the fatigue pre-crack of specimen
170

A5 is made across the bond, the load—displacement curve shown in Figure 6 is implicated in the syn-
thetic result from the fracture toughness of each heterogenious part afFecting each other. Obviously,
"Pop—in'' in Figure 6 is related to the phenomenon of the brittle unstable fracture which appears in
the coarse-grained zone of specimen A5. The above-mentioned points are easy to be confirmed by
the fracture appearance of specimen A5. Figure 7 shows the JIC value of the entire
joint(JIC= 186in-lb/in 2 , i.e. 32.6 KPa · m) which is obtained from the R-curve of SSR test and
regression of the result.
By comparing with the experimental JIC value for the three kinds of specimen, i.e. JIC =154 KPa ·
m for the base metal, JIC = 20.1 KPa · m for the coarse—grained zone of HAZ and JIC = 32.6 KPa · m
for the entire joint, it is not difficult to find that the JIC value of the entire joint specimen is quite
close to that of the coarse-grained zone specimen. This result is absolutely not a mere coincidence
while it reveals again following physical essence under the new JIC test method. This essence is that
the brittle region in the joint is the main controlling factor which governs the fracture initiation
toughness JIC for the entire joint. An important inspiration can be drawn from the above experimen-
tal result, that is, determining the JIC value of an entire joint with SSR test may be an effective ap-
proach to obtain the basically correct JIC value for the lowest toughness region of the joint.

CONCLUSIONS

The result of fracture analysis with SEM shows that the lowest toughness region for the repair—weld-
ed joint of BSC—3A turbine rotor steel is at the coarse—grained zone in HAZ. The result of SSR test
indicates that the JIC value for the coarse—grained zone is 115—186 in—lb/ in (i.e. 20.1 ~ 32.6 KPa ·
m).
When the pre-crack of the specimen is located along HAZ, the JIC value of HAZ can be determined
by the SSR test method, but it is not sure that if the JIC value determined is exactly the JIC value of
the coarse-grained zone in HAZ. The main reason for above-mentioned points is that the width of
HAZ is narrow and the gradient in its constitution and property is great. This makes it diffcult to
pre—crack the HAZ specimen exactly along the coarse-grained zone in HAZ. Therefore, when the
specimens with pre-crack along HAZ are adopted the data of JIC value will seriously be scattered
and this will directly affect the reliability in the fracture toughness assessment of in-service
structures.
The results of SSR test for the entire joint indicate that the brittle region in the joint is the main con-
trolling factor which governs the fracture initiation toughness of the entire joint and determining the
JIC value of an entire joint with SSR test method may be an effective approach to reliably assess the
fracture toughness for repair—welded workpiece of in—service structures.

REFERENCES

1. Kunihiko SATOH, Masao TOYODA and Fumiyoshi MIN AMI: 4JWS-ÜI-7 Osaka 1982.
2. S. Prasannakumar, E.G.Ramachandran and J Ruge:Metal Construstion 1983 (3) 142-146.
3. Fang Huizhen, Su Yi and Lu Anli: WELDING RESEARCH: The State of the Art ppl32~ 141,
(Conference Proceedings, ASM) Toronto, 1985.
4. G.A.Clarke: ASTM STP 743 1981, pp553~575.
5. M.I.DE VRIES:" Ductile Fracture Test Methods'" ppl59-168 PARIS 1983.
 171

(a) Base Plate: Coarse Dimple Rupture

(b) Coarse—grained Zone in HAZ: Intergranular Fracture
(c) Weld Metal: Dimples and Dendrites

Figure 1. Fracture Appearances in the SEM of Various Regions

in Cross Weld Specimens of BSC—3 A

172

2500

2000H

1500U

1000h

500

0.000 ü. 020 0.040 0.060 0.080 0. 100 0.000 0.020 0.040 0.060 0.080 0.10
Figure 2. Loading-Displacement Diagram Figure 3. R-Curve of SSR Test
for Specimen HSC-3A-4*
for Specimen B S C - 3 A - 4 *

2500 2500 h

2000

1500L5

1000

500

0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07
Figure 4. Loading-Displacement Diagram Figure 5. Loading-Displacement Diugram
for Specimen A, for Specimen A2

2500 h
2500 i-

2000

1500L

1000

0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.000 0.020 0.040 0.060 0-080 0.100
Figure 7. R-Curve of SSR Test for specimen A s
Figure 6. Loading-Displacement Diagram
for Specimen A5 (the entire joint specimen) (the entire joint specimen)
WS6C1
FATIGUE DESIGN, QUALITY CONTROL
AND MAINTENANCE OF THE SETO OHASHI BRIDGE

CHITOSHI MIKI and ATSUSHI OKUKAWA

Department of Civil Engineering, Tokyo Institute of Technology,

0-okayama, Meguro, Tokyo, 152, JAPAN

Design Section, Honshu-Shikoku Bridge Authority

4.5-Mori Building, Toranomon, Minato, Tokyo, 105, JAPAN

ABSTRACT
In order to examine the influences of weld defects, residual
stresses, secondary stresses due to structural details on
fatigue strengths, various fatigue tests were carried out under
Honshu-Shikoku Bridge project which includes 45mm and 75mm
thick welded joint specimens, full scale and large scale
structural models of high strength steels. Based on these
tests, the fatigue design code was established and quality
control procedures were in corporated into the fabrication
code .

KEYWORDS

bridge; fatigue; design; fabrication; defect.

INTRODUCTION

On April 10, 1988, the Seto Ohashi Bridge of the Honshu-Shikoku

Bridge Project was opened which cross the Seto Inland Sea in
Japan. The Seto Ohashi Bridge is about 10 km long which
consists of three suspension bridges, two cable-stayed bridges
and one truss bridge. All of these bridges are the world's
longest in each bridge type as combined highway and railway
bridges. Main members of these bridges are made of 600, 700
and 800 MPa class high-tensile strengths steels of which
thicknesses are up to 75mm.

The fatigue design code for the Honshu-Shikoku bridges was set
in 1974- based on the 1970 design specification for steel
railway bridges. However, the application of high strength
steels to bridge structures was not common and the fatigue test
results of welded joints of these steels were not sufficient.
Therefore, Honshu-Shikoku Bridge authority has conducted
173
174
fatigue tests on large scale structural models and various
kinds of welded joints made of 4.5mm and 75mm thick 600 MPa and
800 MPa class steels since 1975, by using the fatigue testing
machine which has a capacity of 4.00 tons dynamic loading.
Based on these studies, the fatigue design code was revised in
1983 for the Seto Ohashi Bridge.

LARGE SCALE FATIGUE TESTS

The fatigue strengths of structural members are governed by the
local stress range which depends on structural systems, joint
details and in particular weld details. Therefore, all of
specimens under this program were fabricated by the same
welding methods and conditions as these for actual members.

Corner Joints

Usually, partial-penetration groove welds or fillet welds are

used to build up box section truss chords. Therefore, these
longitudinal welds are the most fundamental joints among
various joints in stiffened truss structures and the fatigue
strengths of these joints often decide the section size of
member.

Fig.1 shows the results of various tests on the partially

penetrated longitudinal welded, plate type specimens, lower
chords of truss specimens and box section specimens (Miki e_t
al., 1979, 1982, Tajima et al. . 1984-, Shimokawa et al. . 1987).
Fatigue strengths varied with specimen type. In particular, the
fatigue tests on truss point structures made clear the
significant decreasing of fatigue strength of truss chord due
to blowholes in corner joints[Fig.2]. Based on these test
results and fracture mechanics analysis, the concept of
permissible sizes of blowholes were introduced in the
fabrication code of the Seto Ohashi Bridge [see Fig.10].

^400 U

900
• ·• o·
• s •o · ·
2200 _§oo i—r
ho T FL oq
V FL(SM58) t = 40 Ή
T FT(SM50)
□ Box 1040
10θ|_Δ Truss ■ 11 l l i i ml
m i l1 0 5 106 10?
NUMBER OF STRESS CYCLES N

F i g . 1. L o n g i t u d i n a l l y welded j o i n t s and c o r n e r joints

 175

Truss
Box 114MPa
215MPa 2158000cycles
1005000cycles
Fig. 2. Fatigue failure surfaces with blowhole
I^iä£hragmj3

A diaphragm attached detail is usually considered as a non-load

carrying type cruciform fillet welded joint. Fig.3 shows the
fatigue test results on cruciform joints, box section and H-
section specimens with diaphragms [Shimokawa et al. , 1986]. In
box section specimens, BA type, scallops were made at the two
corners of the diaphragm and the other corners were welded
continuously. The main crack initiated from the weld toe of
the fillet weld at the corner of the diaphragm [ Fi g . 4. ( a )] .
These results suggest that scallops do not decrease the fatigue
strength and may be more advantageous than continuous welding
at corners. HC and HD type specimens simulate a box section
truss chord with a diaphragm which have scallops slightly
greater than those of the BA type specimens.

In order to keep the inside of a box section truss chord water-

tight, both ends of the chord are sealed by diaphragms, which
are welded from the outside only. In this detail, the root of
fillet welds may become critical locations for fatigue
cracking. Fatigue cracks initiated from the fillet weld root
in all HA and HB specimens[Fig.^(b)]. However the fatigue

o
RA«=
400 % 2400
300 •
• RB, c£_
2800
< 200
ZUUL c* ΗΑ,ΗΒ,
• RA
MM
3n
RB
"o BA
D BA 300
100 - φ ΗΑΗΒ
t=15| HC,
A HQHD
1 1 ..-_i —1 13d =20 Ekj[
B
F
105 10 6 10?
NUMBER OF STRESS CYCLES N

Fig. 3. Non-load carrying cruciform j o i n t s and diaphragm d e t a i l s

176

BA-2 HB-2
133MPa 103MPa
1304000cycles 2517000cycles
Fig. 4. Fatigue f a i l u r e surfaces
strengths of HA and HB specimens are almost equal to the those
of HC and HD specimens.

Gusset-Plates
The transition radius of fillets, the length of gusset plate,
the width, thickness of base plate and many other factors are
known to affect the fatigue strength of gusset joints. Fig.5
shows fatigue test results of specimens with various gusset
plate detai1s[Shimokawa et a 1. . 1985]· Three types of
specimens were used to study two different design : in one
group, in-plane gusset, two gusset plates were groove welded to
a main plate on the same plane (GC, GD, GF), and in the other
group, out-of-plane gusset, two gusset plates were fillet
welded perpendicular to the main plate (GA, GB, GE). In the
three types of in-plane and the three types of out-of-plane
gusset joints, the fatigue strength decreases as the stress
concentration increases. In in-plane and out-of-plane gusset
joints with similar stress concentration factors, the fatigue
strength of in-plane gusset joints is much lower than that of
out-of-plane gusset joints. Based on these results, the
allowable stresses for gusset joints are determined based on
the gusset types, the transition radius of fillets, the width
of plate and the presence or absence of toe finish.

300

-200E

O GA
Αθ ΔΡ 200
a GB o-
100C Δ GC 8
■ GD
• GE
A GF
C/3

mil »I » ■■■ ι ιιΐ

10 J 10υ
NUMBER OF STRESS CYCLES N

Fig. 5. Gusset plate attached details

 177

T£H££_Pänel_Point£

In order to obtain compact and strong nodal joint, various

types of panel point structures were designed and fatigue tests
of the structural models on the scale about one quarter were
carried out (Tajima et al, 1984-) · Fig.6 gives details of the
vicinities of panel points of test specimens. The major points
of difference between the each types lie in the methods of
connecting the diagonal members, the numbers of diaphragms and
fillet radii of gusset plates. Fig.7 shows the general view of
fatigue test for this specimen. Fatigue cracks were initiated
in gusset plates of type B and C specimens. All of these
fatigue cracks initiated from the toes of fillet welds at the
end of inserted flange plate. At that point, there are stress
concentration due to the stop of weld bead and out-of-plane
bending.

When the axial loads of diagonal and vertical members of truss

are heavy, the connection detail of which fatigue strength was
conformed by using type E specimen were adopted in the Seto
Ohashi Bridge. The connection detail with only gusset plates
such as type D specimens were adopted when the gusset plate
standard size could be obtained.

Fig. 7. Fatigue testing

Fig. 6. Truss panel point details

178
welded details(600-800MPa steels)
welded details(400-500MPa steels)
non welded details

NUMBER OF STRESS CYCLES N

Fig. 8. Fatigue design curves

Fig. 9. Classification of joints

FATIGUE DESIGN (600-800 MPa class steels)

Fig.8 shows the fatigue design curves in each category. The

slope of design curve will be assumed -1/m. Judging from the
large scale fatigue test data, the value of m was fixed at 4-
for the welded details of mild steels U00-500 MPa class), 3
for the welded details of high tensile steels (600-800 MPa) and
5 for the non welded details of all types of steel. Fig.9
shows the classification of the joints. The joint details have
been classified into four grades.

FABRICATION
The codes for fabrication of the bridge members were determined
based on the large scale fatigue test results and fracture
mechanics analysis. With respect of corner joints of box
section truss chord, the permissible size of blowhole were
established as shown in Fig.10. The permissible sizes of
blowhole were classified with respect to the ratio of design
stress range and allowable stress range. In order to minimize
the occurrence of weld defects in corner joints, special
treatments were applied on the start and stop positions of tac
welding beads, the grooves were kept clean, and stabilized
electric source was utilized in addition to the improvements of
welding process.
 179

W: Projection blowhole

H · Longitudinal projected
length of blowhole
AA : OJ^R

A : 0.5^/?<0.7

B : R<0.5
-._ design stress range
permissible stress range

W(mm)

Fig. 10. Permissible size of blowhole

C o r n e r j o i n t s of l o n g i t u d i n a l g r o o v e w e l d i n g were i n s p e c t e d
using a u t o m a t i c u l t r a - s o n i c t e s t i n g s y s t e m s . These a u t o m a t i c
u l t r a s o n i c i n s p e c t i o n s y s t e m s were d e v e l o p e d t o d e t e c t s m a l l
b l o w h o l e s a t t h e r o o t of p a r t i a l l y p e n e t r a t e d g r o o v e w e l d s and
f i l l e t w e l d s , which were l a r g e r t h a n 1.5 m i l l i m e t e r s d i a m e t e r ,
and t h e r e b y s a v e d i n s p e c t i o n t i m e . An e x a m p l e of the
i n s p e c t i o n r e s u l t s i s shown i n F i g . 1 1 . D e f e c t s of w e l d i n g were
r e c o r d e d w i t h r e g a r d t o s i z e and l o c a t i o n s i m u l t a n e o u s l y and
t h e s e r e c o r d s w i l l be u s e d p r a c t i c a l l y f o r maintenance
inspection.

Record of U.T. Longitudinally

r e v e a l e d weldment
Fig. 11. Example of automatic u l t r a s o n i c inspection r e s u l t
180

TEST ON FULL SCALE TRUSS MEMBERS

In order to prove the appropriateness of the fabrication
procedure, one box-section member and one transverse chords
whose dimensions were almost equal to the truss chord of the
Seto Ohashi bridge, were trially fabricated. These member were
then used in a fatigue test after the fabrication investigation
(Sakamoto et al. , 1984, Shimokawa et al., 1984). Fatigue
design allowable stress and joint classification were conformed
and some structural details were charged.

CLOSING REMARKS
Since the Seto Ohashi Bridge has no alternative highway,
maintaining the safe, stable and convenient transportation is
an essential purpose in the operation. On the major points of
b r i d g e s of the Seto O h a s h i B r i d g e , a c c e l e r o g r a p h s ,
seismographs, anemometers and displacement gauges are installed
to collect and retain data on bridge behavior caused by the
wind, earthquake and traffic loads. In order to maintain these
long span bridges in good condition for a long period of time,
it is necessary to inspect and repair then carefully and
regularly. To be able to perform these operations for truss
bridges, well equipped maintenance vehicles for both inspection
and repair were provided.

REFERENCES

Miki, C. et al., (1979). Fatigue strength of longitudinal

single-level-groove welded members. Proc. of JSCE, 291 ι 27-
40 (in Japanese).
Miki, C. et al., (1982). Fatigue of large sized longitudinal
butt welds with partial penetration. Proc. of JSCE, 322,
U3-156.
Sakamoto, K. et al., (1984). An investigation on fatigue
strength for transverse chord of stiffening truss. Structural
Eng./Earthquake Eng., 1-2, 2715-2815.
Shimokawa, ΪΓ. et al.,(1984)· A fatigue test on the full size
truss chord. Structural Eng./Earthquake Eng., 1-1, 57s- 64s.
Shimokawa, H. et al., (1985).Fatigue strengths of" large-size
g u s s e t j o i n t s of 800 MPa class s t e e l s . S t r u c t u r a l
Eng./Earthquake Eng., 2-1, 255s-263s.
Shimokawa, ΪΓ. e~t al. , (1986) . Fatigue strength of diaphragm
joint in box-section truss chords of high strength steels.
Structural Eng./Earthquake Eng., 3-2, 277s-286s.
Shimokawa, W, et al. , (1987). Fatigue strength of box section
truss chord with corner joints. Structural Eng./Earthquake
Eng., 4-1» 41s-49s.
Tajima, J. et al., (1987). Fatigue strengths of truss made of
high strength steels, Proc. of JSCE, 341 t 1-10.
WS6c3

DURABILITY DESIGN OF GROUND VEHICLE STRUCTURES

RONALD W. LANDGRAF

Department of Engineering Science & Mechanics

Virginia Polytechnic Institute & State University
Blacksburg, Virginia, 24061 USA

ABSTRACT

Modern approaches to durability assurance in ground vehicle design are reviewed in the context of
recent developments in computer-based analytical and experimental tools for use by designers and
development engineers. Examples are presented to illustrate the application of this new
technology in product development. Major challenges associated with the linking of various design
tools into integrated networks appropriately configured for industrial problem solving are then
presented along with an assessment of the potential benefits to be gained from such integration.

KEYWORDS

Mechanical durability; structural analysis; service loads; fatigue; life prediction; computer
integrated engineering (CIE).

INTRODUCTION

Ground vehicle engineers have traditionally relied upon extensive proving ground testing of proto-
type and production vehicles to assure adequate structural durability. In the current competitive
climate, such an approach is ineffective in achieving optimized designs since problems are
identified too late in the design cycle - after tooling commitments have been made. Full scale
testing is also costly and time-consuming. In response to the continuing market pressures to
develop safer, more efficient and durable structures, in less time, and at reduced cost, designers
are relying increasingly on a variety of recently developed experimental and analytical tools
relevant to structural durability assurance. These tools offer immense potential for streamlining
the product development cycle by allowing the establishment of more realistic design objectives, by
anticipating possible problems through early design studies, and by the systematic consideration of
a wider range of design alternatives.

Substantial progress has been made in incorporating this new methodology in ground vehicle
design (Soc. of Auto. Engrs., 1987, 1988); some examples are presented in the next section.
Problems and opportunities associated with the linking of the individual design tools into truly
integrated networks appropriate for industrial problem solving are identified with emphasis on
software development and information management.

181
182

DURABILITY DESIGN TECHNOLOGIES

Analytical and Experimental Tools

In simplified form, the steps of a durability analysis procedure are shown in Fig. 1. Activity
progresses from the development of system loads information, to component stress determination,
to damage analysis and life prediction. The experimental side includes: service loads measurement
to document the vehicle environment and establish and validate performance objectives, strain
gage measurements to determine local response at critical regions of a component, and materials
testing to determine deformation and fracture parameters for inclusion into structural and damage
analysis routines. Analytical tools include: computer simulations of vehicle kinematics and
dynamics to develop operating loads, finite element modeling for component stress analysis, and
material deformation modeling for use in damage analysis routines.

Fig. 1. Analytical and experimental approaches to durability assurance.

The computer serves as an important enabling device for the effective utilization of these design
tools in practice. In addition to its use as a computational tool for detailed simulation studies, it
also provides data acquisition and storage capability, as well as programming and control functions
for sophisticated materials and systems tests. It is this commonality of computer dependency
across technical specialties that provides an implementation vehicle for integrating the separate
tools into more cohesive product development procedures.

Of particular value is the incorporation of computer simulations early in the design cycle, prior to
prototype builds and tooling commitments. Here a range of design alternatives can be studied and
optimized. At later stages, computer analysis can guide the design of laboratory tests to quickly
 183
evaluate prototypes under simulated service conditions and can aid in identifying and correcting
problem areas. In this scenario, field testing is employed as final validation procedure with the
expectation that few, if any, surprises will be encountered.

Durability Design Examples

Suspension componentry provide a particularly challenging exercise for designers because of the
complexity of service loading inputs during various vehicle maneuvers. Until recently, this
information had to be collected experimentally using instrumented test vehicles. System dynamics
models are now available that allow service loads to be developed analytically by "driving"
computer models over digitized road surfaces. In Fig. 2 is shown the results of a computer
simulation of the loads through the lower ball joint of a front suspension as in encounters a
chuckhole (Thomas, 1987). This "worst-case" information is useful early in the design cycle to size
suspension components such as control arms. Note that it is important to maintain the time-base
for these loading events since the peak load vectors encounter maxima at different times.

CHUCKHOLE IMPACT

2
2.

Fig. 2. Computer simulation of lower ball joint forces during a chuck-

hole event.

An increase in system complexity can lead to substantial difficulties in determining damage at

potential failure locations. A rear suspension, lower control arm, shown in Fig. 3, provides such an
example. Here the designer must consider the combined effects of six independent load input
vectors. The intuitive selection of a few worst-case fatigue load sets for such a situation becomes
virtually impossible. One solution (Conle, 1987) is to use the principle of elastic superposition in
conjunction with the loads determined from proving ground runs or computer simulations. Finite
element modeling is employed to develop unit load-local stress calibrations, that is, stress
solutions for each of the individual load vectors. This information, when combined with the actual
load-time histories, allows the individual element stress-time histories to be derived. An example
is shown in the lower right of Fig. 3.
184

Fig. 3. Multiaxis load-time histories for suspension arm and resulting

local stress-time histories.

Armed with this, information, the analyst can proceed with a local stress-strain determination
using deformation modeling routines available with modern fatigue analysis software (Conle and
Landgraf, 1983; Landgraf and Conle, 1990). An example of such a local stress-strain simulation is
shown in Fig. 4. In addition, the service history is represented in the form of strain
range-mean-occurrence plot to the right of the figure. Shown at the top of the figure is related
plot indicating the percent of total damage associated with each strain level. This information is of
use in setting up accelerated laboratory simulation tests for product evaluation and quality control.
In this particular example, because the bulk of the damage is caused by the few largest strain
levels, a great deal of cycle compression is possible while still maintaining the overall character of
the service history.

A LOOK TO THE FUTURE

Clearly, the individual computer tools illustrated above: system dynamics modeling, finite element
modeling, and durability analysis, are already having an impact on automotive design. Of greater
value, and hence a major challenge for the next decade, is the integration of these separate tools
into powerful workstation environments in which a designer, or design team, will have ready
access to the complete spectrum of analysis capabilities. The benefits to be gained from this inte-
gration have the potential to far surpass those realized to date. In effecting this transfer of
technology from individual "experts" to the design community at large, it will be necessary to make
significant improvements in the on-line "intelligence" of the software. Just as enhanced graphics
capability has had a marked influence on the user interface of current software, the major
 185

Fig. 4. Example of local stress-strain simulation with associated strain

histogram and damage distribution.

advances in the analysis environment of the future will be in the software intelligence that assists
the engineer in seeking and maintaining a consistent analysis path, and in sensibly interpreting
and utilizing the results of various analyses.

An associated challenge entails the development of computer networks to assure that all design
activities have ready access to complete and up-to-date information. In Fig. 5 is shown a
generalized scheme of information flow in the design process. Structural analysis programs, for
vehicle dynamics or stress analysis, as well as durability analysis routines, are intensely "data
hungry," requiring timely access to data bases relating to component geometry, service loads and
material properties.

Geometry data bases are necessary to expedite the time-consuming building of models. Current
work in solid modeling leading to libraries of generic parts can greatly benefit the finite element
analyst. This would allow quick access to standard component shapes which could be sized and
input into automatic meshing routines in preparation for analysis. Likewise, subsystem libraries
for use in building vehicle models are under development. Generic suspension systems, for
example, can be accessed, sized, and used in modular fashion to quickly develop a full vehicle
model (Thomas, 1987).

Service loads information presents problems because of the large size of the data files involved.
Even if sufficient computer memory is available, it is still difficult to transfer such large data sets
between, say, testing and analysis facilities. Techniques are needed to summarize this information
for more efficient storage and retrieval while still retaining data integrity and cross-channel
relationships.

Finally, materials property information is utilized in a variety of structural and durability analysis
calculations. While large amounts of such data exist, there are few easily accessible, central
repositories of this information outside of individual companies. Major efforts are underway to
confront this problem but, in the short term, it remains an obstacle to the effective utilization of
durability design tools.
186

Geometry Service Material

Loads Properties

Fig. 5. Information flow for structural and durability analyses.

REFERENCES

Conle, F. A. and R. W. Landgraf (1983). A fatigue analysis program for ground vehicle components.
In: Proceedings, SEECO '83, Int'l. Conf. on Digital Techniques in Fatigue, pp. 1-28. Soc.
Environ. Engrs., London.

Conle, F. A. (1987). Durability analysis under multiaxial loading. In: Durability by Design:
Integrated Approaches to Mechanical Durability Assurance, SP 730. pp. 141-147. Soc. Auto.
Engrs., Warrendale, PA.

Landgraf, R. W. and F. A. Conle (1990). Vehicle durability analysis. In: Proceedings, First Annual
Symp. on Mechanical System Design in a Concurrent Engineering Environment (E. J. Haug,
ed.), pp. 239-259, Univ. of Iowa, Iowa City, IA.

Society of Automotive Engineers (1987). Durability by Design: Integrated Approaches to

Mechanical Durability Assurance, SP 730. Warrendale, PA.

Society of Automotive Engineers (1988). Fatigue Design Handbook, AE-10. Warrendale, PA.

Thomas, D (1987). Vehicle modeling and service loads analysis. In: Durability by Design:
Integrated Approaches to Mechanical Durability Assurance, SP 730. pp. 49-72. Soc. Auto.
Engrs., Warrendale, PA.
WS6C4

FATIGUE S T R E N G T H OF FABLICATED T R U C K FRAME

Takeshi HORIKAWA, Hiroshi NAKAMURA

Faculty of Science and Engineering, Ryukoku University
Shigeki KOE,Kenichi FUJISHITA
Technical Research Inst., Kawasaki Heavy Industries, Ltd.
Akira IWAMURA
Rolling Stock Division,Kawasaki Heavy Industries,Ltd.

ABSTRACT
Fatigue design standard for fabricated truck frame (JIS E4207) is compared with
U. S. standard AASHTO and Japanese standard JSSC, and the difference between
the standards are discussed. Then new criterion for fatigue endurance of SMA50B
material is proposed, and fatigue endurance tests of fabricated truck frame are
conducted under load condition simulating service load. Fatigue test results
prove that the proposed criterion may affords an ample margin of safety.

KEYWORDS
Fatigue;Fabricated truck frame;Design standard;JIS E4207;AASHTO;JSSC

PREFACE

Fabricated construction of welding and casting are both used in producing

truck frames for rolling stock. In fabricated construction, some concern is
posed over the strengths of materials at welded joints. Cast steel, on the
other hand, cannot be made into a thin plate, which sometimes gives rise to
weight problem.
The welding method and the finite element method for stress analysis have been
improved, and strength evaluation methods have also been enhanced by means of
static load tests on actual truck frames and stress measurements of rolling
stock in service operation, and many truck frames are fabricated truck frames
in Japan. By contrast in the U. S., use of the fabricated truck frame has only
recently been introduced in rolling stock truck frames. So discussion is
frequently over the problems regarding rules of strength evaluation. The main
point on the discussion lies in differences between the allowable stress
187
188
values in Japan Industrial standard(JIS) E4207 and American standards AASHTO
for highway steel bridge. JIS E 4207 has a wealth of information including
stress measurements by JNR (Japan National Railway) performed on rolling stock
in service.
This paper focus on the standards for the fatigue strength assessment of truck
frame, and new criterion on fatigue strength evaluation is proposed for the
fabricated truck frame.

ALLOWABLE STRESS OF FABRICATED TRUCK FRAME

The fabricated truck frame is basically composed of box-shaped side frames and
transoms welded together,with end beams added to the front and rear as
necessary. So one-sided fillet welded sections are inevitably created, give
notches which decrease fatigue strength. These sections naturally have less
allowable stress compared with the full penetration sections.
JIS E4207
JIS E4207,"General Design Rules for Rolling Stock Truck Frames", was
instituted in 1984 in place of JIS E4047, providing an endurance limit diagram
which described the amount of allowable stress at welded joints made of the
materials SS41 and SM41, and SMA50. Fig. 1, the endurance limit diagram,
29
Fatigue Test Results Criteria f or l·yiaximum Allowable Stress
on Fabric ate<i Truck (Welded Joint)
O Truck - A (SS41B) · Side Beam (SS41)

D i ruck - ö ^5>4i B; ■ [ ruck - u (.5541 BJ ■ JIS

r Annealed
sA W e d ed JIS E4207 (for SMA50)
O Truck -CCSMA50B) '
. AASHTO (Category C) Not Ground
Δ Bolster - C (SMA50B) 21 JJA s Welded
JSSC (Class E)
* Open symbol shows "Not cracked". r-20- 20 <
Solid Symbol shows "Crack observed".
Proposed Criteria

A
R-0
R=0

Grou id <ε
^"*>
s/ί ]
•
Mot (iroun i j ^"5
?4>* * · - (
'-««. ^> ί ^
R=n A
jr ^ /Δ
7 ^ ^ , ^1 ^_S,
\-
3.5 ^r - P^
21 j

-20 -10
A^ ^ W21
26

Mean Stress Kgf/mm2

Fig. 1. Allowable stress for fabricated truck frame and fatigue

endurance test rsults of actual truck frames.
 189
shows the standards for the welding joints. In the figure, allowable stress
of SS41 and SM41 is represented by the area defined by two lines. The first is
between point 7 Kgf/mm2 and point 41 Kgf/mm2 (the reversible fatigue limit and
the tensile strength of the base material, respectively), and the second is
the line on which the maximum stress (the sum of the mean stress and stress
amplitude) is equal to 21 kgf/mm2, the yield stress. As for welded joints of
SMA50 material, although the reversible fatigue limit remains constant,a
tensile strength of 50 Kgf/mm2 and a yield stress of 31 Kgf/mm2 are possible.
Note that the reversible fatigue limit when the welded toe is ground, can be
raised to 11 Kgf/mm2, much higher than in the case of as welded condition.
Also significant is the fact that the establishment of the standard is based
upon static load tests on a actual objects, and strain measurements on actual
rolling stocks in service conditions. The standard is applicable principally
to bending stress and torsional stress, and works well when stress
distribution is such that the maximum stress comes at the welded toe section.

AASHTO STANDARD
AASHTO(American Association for State Highway and Transportation Officials)
standard classifies various welded joints into categories and provides
allowable stresses for each category. Category C of the AASHTO Standard is
applied to the rolling stock truck frame joints. As shown by the long broken
line in Fig. 1, allowable stress amplitude at 2 x 106 is 3.5 Kgf/mm2. Even if
the mean stress decreases, an increase in allowable stress is not permitted by
the standards, since it is based on characteristics only to bridges: first,
annealing is not performed after welding; secondly, there is high tensile mean
stress at work, which is greater than the reoeated stress; and thirdly, welded
toe sections are not ground. Consequently, it is not reasonable to apply the
same standard to a truck frame, yet the standard is often used when truck
frames, exported to the U.S. This means that U.S. trains operate with heavy
truck frames which have an excessive safety factor.

FATIGUE DESIGN RECQMENDATION OF JSSC

JSSC (Japan Steel Structure Committee) has proposed a recomendation for
fatigue design in order to check the safety of the steel constructions and its
structure members under fatigue condition. The strength category E
isapplicable to the welded joints of rolling stock truck frames. By the
standard, shown by the two-dot chain line in Fig. 1, allowable stress can be
slightly higher compared with AASHTO Category C. The major difference between
the JSSC standard and the AASHTO standard lies in the fact that when the mean
190
stress is compressive, the allowable stress can be set higher under the JSCC
standard by allowing for its effect. Also under the recomendation, the effect
of annealing is not taken into account.

PROPOSED CRITERION FOR SMA5QB MATERIAL

As shown in Fig. 1, the difference of allowable stress between AASHTO Category
C and JIS E4207 is greatly observed. The stresses of truck frames are
frequently characterized by a stress ratio R[=(a m -a a )/(cr m + σ 3 )] of 0.5 or
less. Within this range, the use of allowable stress as prescribed by AASHTO
Category C would place serious restrictions on truck frame design. In
addition, it is unreasonable to equate the allowable stress of a truck frame to
that of a bridge, because, unlike bridge structures, l)the welded toe portion
of a truck frame is ground, 2)annealing is performed, and 3)the stress on each
section of a truck frame is mainly caused by bending and torsion. However,
considering that the larger stress ratio R is, the higher crack propagation
rate is, a criterion for SMA50B material as shown by the short broken line in
Fig.1 is proposed here. To provide support for such a proposal,fatigue
endurance tests at the stress values displayed along the line(proposed) are
conducted. If fatigue cracks do not appear or develop, and static load
resistance capacity does not decrease, it is concluded that the standard can
reasonably be adopted.

RESULTS OF FATIGUE ENDURANCE TEST OF TRUCK FRAMES

The endurance of a truck frame is assessed by static load and fatigue

endurance tests. The fatigue endurance test were conducted under the loading
condition which simulated vertical loading as well as right and left, and
front and rear. Braking force and motor load were also reproduced as if on a
running truck frame. Loads for 2 ^ 3 xlO6 were cycled by an electro hydraulic
serbo-type fatigue testing machine.
After the test, magnetic particle inspections or dye checks were conducted to
determine if cracks were present. In some cases, the rigidity of a truck frame
is checked by stopping the fatigue test and applying static load. The results
of a fatigue endurance test on truck frames, bolsters, and side frames are
shown in Fig. 1. Stress value is obtained by multiplying the Young's modules
with the strain measured in the fatigue test. For the SS41 and SS41B truck
frames, a strain gauges were put on the grinder-finished welded toe sections.
For the SMA50B truck frame, the strain gauge was located away from the stress
concentration. As a result of the tests. Truck-A showed no fatigue cracks even
 191

at s t r e s s l e v e l s slightly 12
/
DT38A TRUCK
h i g h e r than the standard /
O Truck frame /
/
p r e s c r i b e d by JIS E4207. h- · Bolster
liol· /
Truck-B and Truck-D were * Welded part /
/
subjected to experiments
/
designed to check the effect /
/
of annealing after welding. /'
In contrast to Truck-B, on 0''

which annealing was performed Ao

/ •
and fatigue cracks did not #_ / n
appear, Truck-D, where P
.a 2
annealing was not performed, E / \
CD

suffered from fatigue cracks

c /
/
a.
which appeared under the same 0 2 4 6 8 10
load condition. These results Calculated stress at static load test Kgf/W

demonstrate that the JIS E4207 Fig. 2. Comparison between measured maxi
s t a n d a r d has an adequate m u m stress and calculated stress.
margin of safety, and that annealing, which is standard procedure, has a
reinforcing effect. In a test on Truck-C and Bolster-C, which are made of
SMA50B, no fatigue cracks appeared at the stress level, either above or below
the proposed criterion shown by the short broken line. Thus, the endurance of
the truck frame was proven even at stress levels higher than those prescribed
by ASSHTO and JSSC.

DISCUSSION ON ALLOWABLE STRESS

JIS E4207 STANDARD

When the endurance of a truck frame is evaluated with JIS E4207 Standard, a
strain gauges are put on the high stress locations which are known either
through stress analysis or experience. Subsequently, a static load test is
conducted by applying maximum loads from various directions to the truck
frame. The stress created by each load will be measured. From the measured
stress, mean stress and stress amplitude can be found based on the composing
method of stress prescribed in JIS E 4207. If the stress is within the limits
defined by the endurance limit diagram(Fig. 1), the endurance of truck frame is
assured. In this case, what matters is the relation between the composed
stress and the maximum stress which appears when a truck frame actually moves
on rails. Fig. 2 shows the results of comparison between actual maximum stress
measured on a truck frame by JNR and maximum stress calculated from a static
192
load test. The results show that the calculated values are near the upper
limit of the measured stress, In addition, maximum stress does not usually
emerge on a truck frame and the frequency of such emergence is very low.
Therefor, it can be concluded that the endurance requirement of a truck frame
is satisfied if the maximum stress gained by a design load is set to within
the endurance limit diagram specifications.

PROPOSED STANDARD OF SMA5QB MATERIAL

Welded joints for each part of a truck frame were constructed with SMA50B
steel plate 9 mm in thickness, so the plane bending fatigue tests were
conducted with the joints. The test results showed that the fillet welded
joints with a bevel cut on one side showed the lowest fatigue strength at
approximately 13 Kgf/mm2 after a load application 2xl06. In order to realize
sufficient safety, the S-N diagram is extrapolated to below the fatigue limit.
When the fatigue strength at 107 is reduced to 80%, the value comes to 7. 6 Kgf/
mm2 which is the close value designated by JIS E4207. This means that the JIS
value has a safety factor of approximately 1.8 compared with the fatigue
strength at 2xl06 in plane bending. In addition, the fatigue endurance test of
a truck frame is designed to check the validity of the proposed standard for
the SMA50B. This is why the test is conducted with a repeated load
approximately 1. 7 times higher than the specified load of the truck frame.
Further taking into account the fact that specified design loads have a built-
in margin of safety, it is concluded that although fatigue strength of welded
joints vary to some extent, the proposed standard for allowable stress of a
truck frame affords an ample margin of safety.

CONCLUSIONS

With a focus on the endurance limit diagram for the fatigue strength
assessment of rolling stock truck frames, the difference between JIS E4207
and AASHTO/JSSC standards for welded joints used in bridges, is considered
based on the results of fatigue endurance tests performed on actual truck
frames. The findings show that AASHTO and JSSC standards are excessively
safe. The new criterion is proposed for SMA50B material, and it is known that
the criterion affords an ample margin of safety.
With regard to Japanese standards, fine-tuning of standards for effects of
annealing and grinder-finishing as well as upgrading of evaluation standards
for route cracks will be a necessary task for the future.
WS6C7
RESIDUAL TOUGHNESS DUE TO CRACK EXTENSION

T. BUI-QUOC and M. BERNARD

Professors

Department of Mechanical Engineering

Ecole Polytechnique de Montreal,
Montreal, Quebec, H3C 3A7, CANADA

ABSTRACT

The toughness related to the plane stress fracture of a material subjected to

cyclic loading decreases with an increase in the number of applied cycles;
ultimately it reaches a critical value at the onset of failure. The
deterioration of this material property is usually attributed to the damage
accumulation during the cyclic loading. In this paper, the basic crack
propagation behaviour at room temperature of a stainless steel is studied and
the effect of the cyclic loading on the variation of the toughness as
determined from a tensile test is presented. An analytical model is proposed
to describe this behaviour.

KEYWORDS

Crack extension; constant ΔΚ loading; residual toughness; fatigue life.

INTRODUCTION

Since the fatigue phenomenon has widely been recognized as being governed
mainly by the crack initiation and extension mechanisms, the deterioration
of material strength is the resulting effect of the damage process. For
example, the loss of the yield and the tensile strengths due to cyclic loading
has been recently investigated (BUI-QUOC et_al., 1987).

In the crack propagation study, the compact tensile specimen (CT) is, in
general, used in conformity with the ASTM Standard E-647. In particular, the
crack propagation properties are usually characterized by expressing the crack
growth rate da/dn in terms of the stress intensity factor. Failure is the
ultimate phase of the material life.

The plane strain fracture toughness KIC is obtained by static loading on a CT

specimen, after it has been fatigue-precracked, according to ASTM Standard E-
399. Under plane stress conditions, the affected zone ahead of the crack tip
is closely related to the crack length and the experimental value of this
toughness depends upon the damage state due to the presence of the crack. The

193
194
value associated with a given fatigue crack length is thus denoted as the
residual toughness, Ks.

In this paper, the variation of the toughness obtained in a tensile test on

the CT specimens previously subjected to cyclic loading with a specified crack
length is presented. On the basis of this residual property, damage state
incurred can be defined using the concept outlined in (DUBUC et al.. 1971).

EXPERIMENTAL PROCEDURE

Compact tension specimens of 50 mm in width and 10 mm in thickness were

machined from a 304 stainless steel bar, according to the ASTM
recommendations. The specimens were tested at room temperature using a
closed-loop servo-hydraulic fatigue testing system. The basic crack
propagation behaviour was obtained from a first series of tests, in which the
specimens were cycled at 10 Hz under a constant value of ΔΚ (with R^K^n/K,^-
0.1) until failure. During these tests, the crack length was monitored with
a video camera and the corresponding number of cycles was registered. To
determine the residual toughness a second series of tests was conducted. For
a specified value of ΔΚ, the CT specimen was cycled until a predetermined
crack length was reached. After the precracking, this specimen was then
statically loaded until failure; during that part of the test, the load vs
piston displacement was registered. The residual toughness is then calculated
with the maximum load using the CT calibration. Two values of ΔΚ combined
with several crack lengths were considered in this work.

EXPERIMENTAL RESULTS AND ANALYSIS

Crack Length Extension

The evolution of the crack length (from a0 to a critical value a*) in terms of
the number of applied cycles, n, is shown in Fig. 1. For each value of ΔΚ,
the crack length is essentially linear with the applied cycles; this means
that the crack growth rate is practically unchanged for a given value of ΔΚ.
The slope of the straight line associated with a high value of ΔΚ is larger
than that associated with a lower value; thus, the crack growth rate depends
upon ΔΚ, as expected.

The critical crack length corresponding to the onset of failure was determined
by the instability condition of the crack extension behaviour. This behaviour
is characterized by a rapid increase of the crack opening displacement and by
the deviation of the linear behaviour of the crack length in terms of the
number of applied cycles (Fig. 1). The critical crack length may be defined
in terms of the crack tip opening displacement (CTOD). The CTOD corresponding
to the applied stress intensity factor ΔΚ is given by (BROEK, 1986):

CTOD - αΔΚ2Φ/(Εσγ) (1)

where a: geometric factor; Φ: plastic zone correction factor;

E: elastic modulus; oy : yield stress.

At the critical situation corresponding to Kc (the fracture toughness), the

CTOD* is obtained as follows:

CTOD* = aKc2/(Eay) (2)

 195

Οθ+O 1e+5 2e+5 3e+5

Number of Applied Cycles, n

Fig. 1. Evolution of crack length during fatigue loading with

constant ΔΚ (ΔΚ in MPa7m).

During the propagation period with constant ΔΚ, the crack extension is limited
by CTOD*; then, the critical crack extension length, Aac may be written:

Aac = a [1 - Φ (ΔΚ/Κ.)2] / (Εσ„) (3)

For small plastic zone at the crack tip (small value of ΔΚ), the factor Φ «
1. In this case, eq. (3) may be put in the following form:

Aac/Aac* - 1 - (AK/KC)2 (4)

2
where Aac* = (Kc/Jnay)

The first limiting condition of eq. (4) is related to ΔΚ = AKth (threshold

value); in this case, the critical crack length is relatively large. For the
second limiting condition, i.e., ΔΚ - Kc, this length becomes very small.
With the material properties and the specimen configuration used in this
experimental work, the critical value of the crack, given by eq. (4) is also
shown in Fig. 1. The dotted line defines the critical condition for Aac, as
specified by eq. (4). For simplicity, Φ = 1 has been considered in the
present study; however, in the case were the plastic zone around the crack tip
is important, Φ may deviate significantly from unity.

Residual Toughness

The residual toughness Ks associated with a number of applied cycles n, for

a given value of ΔΚ, has been obtained from a tensile test performed on a
cracked specimen. This toughness is expressed in terms of the life fraction
ß which is defined as the ratio between n and the cycles at failure N (for a
given testing condition). The results are shown in Fig. 2 with two values
of ΔΚ, i.e. ΔΚ = 30 and 60 MPa Jm. It is seen that, for a given value of ΔΚ,
196
the toughness decreases with an increase of ß; furthermore, the rate of this
decrease depends also upon ß. In addition, the residual toughness depends
upon the imposed value of ΔΚ. For a given life fraction, this toughness is
smaller with a lower value of ΔΚ. These observations are similar to the
characteristics concerning the residual ultimate tensile strength of a
material subjected to cyclic loading and an analysis of this strength loss has
already been made (BUI-QUOC et al.. 1971, 1987).

IfU -
Mat: 304 SS
120- ^ ^ D T = 20° C
f = 10 Hz
*^*£L R = 0.1
100- »vCL^

80-
Φ
e
ΔΚ Eq.(8) Exp. \ XJ
60-
XS
30
O
\
40 - 60 n
\
ft)

■o
20-

U i
0.0
" 0.2
1

0.4
1 1
0.6 0.8
1 1
1.0
Applied Life Fraction, ß

FIG. 2. Variation of the toughness in terms of the used life

fraction (ΔΚ in MPa7m).

On the basis of a phenomenological approach outlined in (GOMUC, 1990), the

loss rate of the toughness may be expressed in terms of the following
parameters:

a) its instantaneous value (<ps = Ks/AKth)

b) the imposed stress intensity factor (φ - AK/AK t h )
c) the difference between its instantaneous value and the imposed stress
intensity factor.

Thus, the loss rate of the dimensionless toughness d<ps/dn is suggested by the
following expression:

&PS <ff* <Ps

l Ψ - (" -)k ] (5)
dn C φ/ _ 1 cpu

where C, m, k are material constants and <pu - K c /AK th .

Solution of eq. ( 5 ) , with the initial condition <ps — φχ1 for n — 0, leads to a
relation between the toughness φ& and the applied cycles n:

[■ (6)
(ft* φ-1 Ψ ~ (<PS/Vu)k

At f a i l u r e , n - N, <ps φ, then (6) becomes:

 197

[ (7)
(fP φ-1 φ - (φ/φη)Υ

Equation (7) is the basic expression describing the life in terms of the
applied (dimensionless) stress intensity factor φ. The application of this
equation to the present data will be discussed later.

Dividing eq. (6) by eq. (7) and rearranging, with notation ß = n/N, one
obtains:

Ί l/k

(8)
1 -β

φ (φ/φ*ν
Equation (8) describes the theoretical variation of the toughness in terra of
the life fraction ß. It is seen that for a given value of ΔΚ, when ß = 0, Ks
- Kc and when ß = 1, Ks = ΔΚ; furthermore, the degree of concavity of the
curve depends upon the numerical value of constant k. The theoretical curves
for eq. (8) have been shown in Fig. 2 with a typical value of k = 2.0. In
this work, the value of Kc is obtained from a specimen with a very short
precrack; Kc may thus be considered as the limiting value of Ks.

It is also noted that the theoretical loss of the toughness due to the crack
extension is dependent upon the stress intensity factor especially in the
region of large crack length (large values of ß). These theoretical results
are in agreement with the experimental data.

Fatigue Propagation Curve

10'

9 Mat: 304 SS
U
0 T = 20° C
H 10 6 -d
TI f = 10 Hz
« R = 0.1

10 =

H
0 10«-J
>i Eq. (7)
υ D Exp.Data
t Ref. Point
0 10*
u
9
10<
0 20 40 60 80 100 120
Stress Intensity Factor, ΔΚ (MPa ym")

FIG.3. Life under crack propagation stage in terms of stress

intensity factor.
198
During the fatigue loading with constant value of ΔΚ, the crack extends from
an original value a0 (at n - 0) to a critical value a* corresponding to failure
characterized by the fatigue life N. The characteristic of the material under
this condition is described by a diagram in which N is expressed in terms of
ΔΚ, as shown in Fig. 3. When ΔΚ tends towards AKth, the fatigue life tends to
be infinite, as expected. On the other hand, for a high value of ΔΚ, the life
becomes very small; at the limiting condition ΔΚ - Kc, the fatigue life would
be 1/2 or 1 cycle.

The behaviour of such a diagram N vs ΔΚ may be represented by eq. (7). With

constant k — 2, already obtained in the previous section, the evaluation of
two constants C and m has been made using two reference points; the
representative curve is given in Fig. 3. It is seen that the theoretical
curve describes correctly the limiting condition related to the extreme values
of ΔΚ.

The crack propagation behaviour (e.g. diagram da/dn vs ΔΚ) may be investigated
from the foregoing development; the crack growth characteristics in the entire
diagram, from Kth to Kc, may be described by a unique expression. This subject
will be presented in a forthcoming paper.

CONCLUSION

Tests have been carried out on CT specimens of 304 SS under constant value
of ΔΚ to investigate the residual toughness due to the crack extension. The
main conclusions are as follows:

a) the toughness decreases continuously from the beginning to the end of

the material life.
b) the residual toughness is not only governed by the crack length (closely
related to the applied cycles) but also by the applied stress intensity
factor, especially in the region of large crack length.
c) a formulation has been suggested for describing the loss of the
toughness due to the crack extension and for predicting the crack
propagation life; the theoretical results correlate well with the
experimental data obtained in the present program.

ACKNOWLEDGMENT

This work was supported by NSERC (Grant OGP0038203) and by FCAR (Formation
des chercheurs et de l'aide ä la recherche), Gouv. du Quebec (Grant EQ 00276).

REFERENCES

BROEK, D. (1986), Elementary Engineering Fracture Mechanics, Martinus Nijhoff

Publishers, Dordrecht.
BUI-QUOC, T., DUBUC, J., BAZERGUI, A., BIRON, A. (1971), Cumulative Fatigue
Damage Under Stress-Controlled Conditions, ASME. Jl of Bas. Eng. 93. 691-98.
BUI-QUOC, T., ELGHORBA, M. and BIRON, A. (1987), Effect of Previous Cyclic
Loading on Yield and Tensile Strengths of a Mild Steel, ICM5. Perg.. 777-84.
DUBUC, J., BUI-QUOC, T., BAZERGUI, A. and BIRON, A. (1971), Unified Theory of
Cumulative Damage in Metal Fatigue, WRC Bulletin. 162. 1-20
GOMUC, R., BUI-QUOC, T., BIRON, A. and BERNARD, M. (1990), Analysis of Type
316 Stainless Steel Behaviour Under Fatigue Creep and Combined Fatigue-Creep
Loading, ASME Jl Pressure Vessel Techn.. 112. 240-250.
WS6C10

PREDICTION OF FATIGUE LIFE FOR WELDED GUSSET

PLATES UNDER VARIABLE AMPLITUDE LOADING

Y. KITSUNAI, E. YOSHIHISA and Y. MAEDA

National Research Institute of Industrial Safety

1-4--6 Umezono, Kiyose, 204- Japan

ABSTRACT

Service stresses acting on an actual component of a crane were monitored and

stress distribution was determined by rain-flow method. The fatigue
initiation and propagation tests of gusset plate specimens were carried out
under the program loading determined from the service stress monitoring.
The fatigue life was governed by crack initiation rather than propagation.
The crack growth rate was correlated with the effective stress intensity
factor range which takes into account the residual stress and applied stress
distribution. The predicted fatigue crack propagation life was roughly the
same as experimental test result.

KEYWORDS

Fatigue; service stress; life prediction; residual stress; welded joint.

INTRODUCTION

Overhead travelling cranes have been used over long period of fifty years or
more. The operation rate of the cranes has remarkably increased as compared
with 10-15 years ago. Many fatigue cracks have been observed at points of
high stress concentration in bridge or runway girders of overhead travelling
cranes. The locations of cracks in the bridge girders are concentrated near
the welded joints between a bottom flange and attached members, such as
gusset plates and cover plates, auxiliary lattice members and their joints,
and the underneath of the rib plate welded in the web. In particular, the
cracks at the gusset plates welded to bottom chord members are more serious,
because these cracks often cause collapse of the cranes. Hence, periodical
inspection and repair are necessary to assure the safety of cranes. The
present study focused on the following issues to assure the safety of the
bridge girders in overhead travelling cranes, (1) monitoring the stresses
acting on the bridge girders under service conditions, (2) examining the
fatigue strength of gusset plates which tend to be origin of cracking, and
(3) predicting the life of fatigue crack growth for the gusset plates.

199
200
MPa
£ 20
-p 10 ^{M^$$
CO

30 60 90 120 SEC
Time
Fig. 1 Typical stress wave pattern acting on girder.

MONITORING OF STRESS CYCLE

An overhead travelling crane was used to examine the peak stresses and
stress range distributions acting on the bridge girders which were made up
of conventional pipe structure. The principal specifications of the crane
were: the maximum hoisting load was 5 tons, the span was 16.3 m and the crab
trolley wheel base was 3· 25 m. Monitoring of the stresses were carried out
using strain gages pasted on the selected components of the bridge girders.
The data obtained were recorded into a histogram recorder and a data
recorder. Rain-flow method was applied to count the stress range acting on
the girders. The stresses acting on the girders are a function of the
hoisting load and trolley position. A 5 tons weight which corresponds to the
maximum hoisting load of the crane was used during the stress measurement.
Typical example of stress-wave pattern obtained from a component near the
mid-span of the girders are shown in Fig. 1. The stress-wave pattern
shown in Fig. 1 is obtained under the following condition: the test weight
was lifted at an end of the girder's span, then the trolley was traversed
from the end to the opposite side in the span, further the bridge girders
with the crab trolley was traveled approximately 20 m on the runway girder,
at that location the test weight was lowered on the floor. The peak stress
appeared around 4.0 sec on the abscissa in the stress-wave pattern is due to
crossing of the trolley near the component with strain gages. A series of
crane operation mentioned above was cycled 20 times during each stress
measurement, to make histogram of stress range using rain-flow method.
Figure 2 shows the histogram of stress range acting on the selected
component in the girders. As can be seen in the figures, relatively low
stress ranges below 20 MPa occupy the majority of the histogram . These
low stress ranges may have little influence on the fatigue damage of the
girder. Hence, for the determining service stresses of the girders, the
stress ranges above 20 MPa were approximated by the Weibull distribution.

SPECIMENS AND FATIGUE TEST PROCEDURES

To determine the fatigue strength of the fillet welds between the bottom
chord and the gusset plate under the as-welded condition, two types of the

0 10 20 30 MPa
Fig. 2 Histogram of stress range acting on girder.
 201

1o 1 =1.1 o 11
1 vo I 1o -
11 60° ·'1I 300 s ° I
*AI_L

^ =4= Type B
Type A

Fig. 3 Gusset plate specimens

specimens shown in Fig. 3 were fabricated. A gusset plate in the specimen is

attached to one side of the main plate by partial penetration fillet welds
with coated electrodes of 4 mm dia. The material used to fabricate the
specimens is JIS SM50 steel plate with 8 mm thick. The yield stress and the
tensile strength of the plate are 422 MPa and 549 MPa, respectively. Prior
to fatigue testing, weld profiles near the weld toes of the specimens were
examined using either a dental mold or cross sectioning method. Strain gages
with gage length of 1 mm were used to measure the local strain at high
stress regions. Welding residual stresses in the specimens were measured
by using a X-ray diffraction method. Fatigue crack initiation and
propagation tests under the constant loading and the program block loading
which is determined from the stress distribution acting on the component of
bridge girders were carried out using two servo-controlled hydraulic
testing machines attached with computers. The program block loading used
is composed of 5 steps in a block, and normalized stress, AÖi/AOmax, and
number of elapsed cycles, ni, at each step are given in Table 1. From
averaged operation rate of the crane in factories per day, the total elapsed
stress cycles in a block were determined as 100 cycles. Stress ratio, R,
was ranged between 0.05 and 0.2, and the frequency was in the range of 0.5-
10 Hz in a sinusoidal wave form.

FATIGUE CRACK INITIATION TEST RESULT

Figure 4 shows the program loading test results which are plotted in the
form of ACfe - Nc orACfe - Nf, whereAOfe is the equivalent stress range which
is given by Eq(l).

H 1/q
Acre = ( Σ Δσι Η ) (1)
i=1 Ση,
where Nc is the number of elapsed stress cycles until the crack grows up to
2 mm in length, Nf is the number of elapsed stress cycle to failure,JXfls the
stress range, i.e., (Xinax - Gfmin, i is step number, and q is constant.

Table 1 Program block loading used in fatigue test

Step No ΔΟι^Cfmax n
i
1 0.846 34
2 0.884 41
3 0.923 19
4 0.961 5
5 1.000 1
202

Fig. 4 S - N curve for program loading.

Based on the fatigue design recommendation proposed by JSSC, the constant q

was adopted 3.0. The best fit curves for the relations between Nc andAOTe,
or Nf andAtfe are given by Eqs. (2) and (3), respectively.

Nc = 1.87 x 10^(AcTe)-|·^ (2)

Nf= 3.16 x lO'nAcTe)- 3 · 1 0 (3)

Judging from the value of Nc/Nf, the majority of fatigue life of the
gusset plate specimens under the program loading is found to spend the crack
initiation process. The fatigue strength of the gusset plate specimens under
the program loading remarkably reduced as compared with that of the smoothed
base metal specimen under constant loading. The majority of the stress
ranges in the program loading used in this tests exceeded 100 MPa of fatigue
limit obtained under constant loading test, except for some stress ranges.
In case of the program loading with stress ranges below 100 MPa, however,
the fatigue life evaluation by using the Miner rule gives an unconservative
estimation of Nc and Nf, as shown by the data with a slash mark in Fig. 4.

FATIGUE CRACK GROWTH BEHAVIOR AND LIFE PREDICTION

To determine the fatigue crack propagation life of gusset plates attached

with bottom chord in a crane, growth behavior of fatigue crack initiated
from weld toe in the gusset plate specimens was examined under the constant
stress range and the programmed block loading. The average crack growth
rate in a block, da/dN, as a function of the stress intensity factor range,
ΔΚπι, under the program loading is shown in Fig. 5. The ΔΚπι is given by

, 5 m n i V) m
AKm = ( Σ Δ Κ ί (4)
1=1 Ση±

where Δ Κ ί is the stress intensity factor range at each step, m is

experimental constant. From the crack growth properties of the base metal
under constant loading, m was adopted 2.7. The ΔΚί for the gusset plate
specimens was computed using formula for a single edge cracked-tension
specimen and is given by

ΔΚί = MkAdi/"TUT F(a/W) (5)

where Mk is correction factor for stress concentration, a is crack length,

and W is specimen width. As shown in Fig. 5, the da/dN for the gusset plate
specimens under program loading is approximately equal or slightly lower
than that of the base metal under constant loading. The reduction of the
 203
I
I °
I Type A TypeA | /

is -j
Δ

■tf —
I V
TypeB α
Γ Type B * j f .
Iff z 5* J
a I >Fι=αο5
R=0.05 _*«►

I -
f.*
107 - - *<
a
ft
■r
a?
/·
»tal
/- n
/ * \ " Base metal
L ... . J 1 . I
20 50 100 20 50 100
AKm MPa/m AKRtm MRa/rS

Fig. $ da/dN versus AKm. Fig. 6 da/dN versus AKRem.

da/dN may be cause the interaction effects between the welding residual
stress and loading history. The crack closure model (Elber, 1971) can be
used to examine the interaction effects on the da/dN. It has been shown
that the crack opening stress intensity factor, Kop, in a program loading is
approximately equal in each block and governed by the maximum stress
intensity factor in the block, (Jono et al, 1987). Assuming that the same
phenomenon exists in the program loading used in this study, the effective
stress intensity factor range which takes into account residual stress at
each step, AKireff7can be expressed as

AKireff = Kbrmax - Kop (6)

where AKbrmax is the maximum stress intensity factor which takes into
account residual stress at each block. The Kop is given by

Kop = Kimax + Kres - (A + BRires)AKi (7)

where A and B are constants and given as 0.82 and 0.3, respectively, and
Rires is stress ratio which takes into account residual stress and given by

Rires = (Kimin + Kres)/(Kmax + Kres) (8)

where Kres is the stress intensity factor due to residual stress. The Kres
can be evaluated by using the weight function or the stress intensity
formula for a point force acting on crack face(Tada et al., 1985)· The later
method was used in this study. Substituting AKireff in Eq. (6) into AKi in
Eq. (Λ), the effective stress intensity factor range estimated based on
linear accumulation of the stress intensity factor range considering
residual stress, AKRem, can be expressed by

1/m
AKRem = ( Σ AKireff (9)
Σηι
i=1
The da/dN shown in F i g . Λ was r e p l o t t e d a g a i n s t AKRem r e p r e s e n t e d by
Eq.(9)· As can be seen in Fig. 6, the da/dN in the gusset plate specimens
204

D Type A 1 '
* Type B
/ 4*
Prediction / .*

•W
/ / / '
•
. ■
.'
../'
/

> ^ \
i^-- ^ Prediction
\^^^--
0 5 10
N x 10* cycle

Fig. 7 Comparison between predicted life and test result.

under the program loading is roughly the same as that of the base metal
under constant loading, except for some data. To predict the fatigue life of
the gusset plate specimens under program loading, fatigue crack growth life
was calculated by using the da/dN - AKRem relation.

da
(10)
· ■ /
aQ C(AKRem)11

The initial crack length, a Q , was taken as 2 mm, and the final crack length,
a c , was determined as the maximum crack length which is satisfied
criterion on the small scale yielding. Slight deviation is found between
the prediction and experimental result, as shown in Fig. 7. However, the
prediction is within 20 percent of the total crack growth life. Hence, it
seems that the prediction of crack growth life of the gusset plate by using
the method mentioned above does not matter in practical application.

CONCLUSIONS

(1) The fatigue strength of the gusset plate specimens under program loading
which is determined from stress measurement acting on the actual component in
bridge girders was remarkably reduced as compared with that of the smoothed
base metal specimens under constant loading.
(2) The fatigue life of the gusset plate specimens under the program loading
was governed by crack initiation rather than propagation.
(3) The da/dN of the gusset plate specimens under the program loading is
correlated with the effective stress intensity factor range, AKRem,
estimated based on the linear accumulation of the stress intensity factor
range considering residual stress at each step in a block.
(4)The predicted fatigue crack growth life under the program loading agreed
with the crack growth test result in the range of error within 20 percent.

REFERENCES

Elber, W. (1971). The significance of fatigue crack closure. ASTM STP486,

230-2Λ2.
Jono, M and A. Sugeta (1987). Effect of residual stress on fatigue crack
growth rate and crack closure under varying loadings. J. Soc. Mater.
Science. 36, 1071-1077.
Tada, H., P. C. Paris and G. Irwin (1985). In: The stress Analysis of
Cracks Handbook ( Del Research Corp.), 2.33
WS6d1

M E T H O D O L O G Y OF R E M A I N I N G L I F E A S S E S S M E N T
IN H I G H T E M P E R A T U R E A P P L I C A T I O N S
B A S E D ON A M O N T E C A R L O S I M U L A T I O N OF
GRAIN BOUNDARY CRACKING

R. OHTANI, T. KITAMURA AND N. TADA

Department of Engineering Science, Kyoto University

Kyo to 6 0 6 , Japan

ABSTRACT

Microstrueturally small cracks along grain boundaries are focused as a substance of

creep and creep dominated fatigue damage in steels and alloys. A method of computer
aided simulation is proposed for remaining life assessment of high temperature
components, based on the results of detailed observation of small cracks and a
stochastic model on random behavior of crack initiation and growth.

KEYWORDS

Remaining l i f e assessment; Monte Carlo simulation; s t o c h a s t i c model; small cracks;

grain boundary cracking; creep; c r e e p - f a t i g u e .

INTRODUCTION

A number of techniques of nondestructive inspection (NDI) for determining the damage

of materials have been provided, and the application of the methods to specific
product types and the reliability as quantitative evaluation were discussed (Metals
Handbook, 1989). Concerning fossil power plants in Japan, some of the methods, for
example, Vickers' hardness, replication microscopy for determining microstructure,
deformation of grains, voids (A-parameter) and microcracks, ultrasonic inspection,
electric potential drop, X-ray diffraction and so on, are tried to adopt at the
periodical inspection (Jaske and Kitagawa, 1989). The authors have no mind to refer
to the present state of such nondestructive inspection or evaluation. In this paper,
from the standpoint of the idea that small scale fracture is acceptable in the
materials of high temperature components, grain boundary small cracks of less than
lmm in length and/or cavities under a few um in diameter are focused as a substance
of creep and creep dominated fatigue damage in steels and alloys. As was already
reported (Qhtani et.al., 1984, 1986, 1988), quantitative evaluation of creep and
fatigue life of smooth specimens is not always satisfactory when determined on the
basis of the fracture mechanics equations on large crack propagation rates. Thus, a
stochastic approach must be considered in place of the deterministic fracture
mechanics approach. In this paper, a methodology of remaining life assessment in
high temperature applications (Kitamura et.al., 1990d) is discussed. The method
proposed is based on a stochastic model of the initiation and growth of

205
206
microstructurally small cracks and a Monte Carlo method on their numerical
simulation.

BACKGROUND

Precise observation of the behavior of small crack initiation and growth in the
process of monotonic creep and creep-fatigue was conducted in the laboratory tests
over the past decade (Ohtani et.al., 1982, 1984, 1987a, b, 1989a, b, 1990a, b, d;
Kitamura et.al., 1990b). The results indicate that the failure of smooth specimens
under creep dominated fatigue is governed by the grain boundary facet cracking on
the surface even in a vacuum, which initiates at random from less than 10% of the
failure life and grows discretely with the coalescence of adjacent cracks, although
most of the cracks are arrested at grain boundary triple points just after
initiation. The number of surface cracks as well as their increasing rate per
fatigue cycle are larger in high strain ranges, slow-fast type (c-p type) strain
waveforms, and ductile steels than in low strain ranges, slow-slow or slow-very slow
(c-c type) cycling, and low ductility materials. The test results also indicate that
fracture mode changes from the surface cracking to the inner cavitation and cracking
when materials are subjected to the fatigue at higher temperatures and/or lower
strain rates in slow-fast type strain waveforms (Ohtani et.al., 1990d). This is
quite similar to a diffusion controlled fracture being characterized by the grain
boundary cavitation throughout the material in monotonic creep. The growth and
coalescence of these cavities lead to void-like cracks, which may sometimes bring
about the rapid and unstable fracture without the process of slow crack growth. A
fracture map showing the morphology of cavitation and cracking as functions of
loading conditions will enable us to give the qualitative estimation of damage
accumulation and remaining life. However, a method of quantitative estimation is
more helpful to the systematic assessment of mechanical components.

Thus, the authors (Ohtani and Kinami, 1986) have been proposed a simple equation for
estimating the creep crack growth rate, supposing that the growth rates of
individual small cracks are the same at equal crack length, that is, there is a
distribution of crack initiation but no distribution of growth rates. This equation
is expressed as a function of a cumulative probability of crack length at an
arbitrary time, which seems to be useful for giving a rough estimate of the longest
crack growth rate. The equation is applicable not only for small cracks but also for
cavities or voids, if only the distribution of their length or size can be
determined by means of some inspection methods. It is, however, a question that the
assumption of no distribution of crack growth rates involves uncertain behavior of
cracking; for example, the dependence of the rates on the crack length and their
remarkable fluctuation of the discrete growth in the regime of microstructurally
small cracks, can not be accurately predicted by this method.

A stochastic model and a method of numerical simulation of microstructurally small

crack growth were then developed (Ohtani and Kitamura, 1987c; Kitamura and Ohtani,
1989a) based on a detailed observation of the creep fracture process of 316 and 304
stainless steels ( Ohtani et.al., 1982, 1984, 1989b). In this model, a random
variable technique is used to deal with the scatter of small crack growth rate data
caused by microstructural inhomogeneity. Taking into account multiple cracks with
continuous initiation during creep, the probability of the length of randomly
distributed cracks can be obtained numerically using a Monte Carlo method. It might
be, therefore, more reasonable to apply this method to the estimation of the future
cracking state of damaged parts in a component. However, there still remains a hard
problem to solve. Random variables adopted in the model and calculation, which
represent the scatter of grain boundary lengths and crack growth rates between two
adjacent grain boundary triple points, are rather difficult to be determined in
comparison with the cumulative probability of actual crack length through trial and
error. Moreover, as this method aims to predict a stochastic process of small crack
 207
growth, detailed information on crack initiation can not be obtained.

In this paper, methodology based on another Monte Carlo simulation is proposed for a
remaining life assessment of high temperature components (Kitamura et.al., 1990d).
Ihis method is based on a model of random fracture resistance of grain boundaries
(Ohtani et.al., 1989c, 1990c), and it can offer a computer aided visual image of
cracking materials of two or three dimensions as well as quantitative information
about the initiation and growth of small cracks.

PROPOSED METHOD

Description of the proposed method is made with reference to the flow chart in
Fig.l. The method consists of three steps; preparation for the simulation (Step 0 ) ,
prediction of small crack initiation life (Step 1), and prediction of small crack
growth life (Step 2 ) . Moreover, the operations in each step are classified into
three categories; field operation, laboratory operation, and computer operation.

Step 0

It is impractical and uneconomical to analyze the whole parts of a large component,

as the simulation proposed requires enormous computer memories and calculation time.
The critical region, which needs the precise damage evaluation, is usually specified
by case study of troubles and the current stress analysis. Even a personal computer
is available for the calculation using the concept of extreme statistics, only if
the region is properly chosen. Higher class computer such as an engineering work
station is recommended for the quick response and the graphic representation as well
as the linkage with other computer resources; e.g., data base about materials
properties, stress analyses, and nondestructive evaluation.

The replication of microstructure is taken from the selected region, and the grain
shape and size are measured by means of an optical microscope using a system of
computer aided image analysis. Although the actual grain structure thus obtained can
be directly used for the simulation, it is more practical to reproduce a
statistically similar pattern of grains and grain boundaries by means of a computer.
The detailed scheme of numerical reproduction is seen in the previous paper
(Kitamura, et.al., 1990c; Ohtani et.al., 1990c). The simulation area should contain
at least one thousand grain boundaries in order to evaluate about one hundred pieces
of cracks.

Next, the fracture resistance, R, is given to each grain boundary as shown in

Fig.2(a). As pysically meaningful values of R are difficult to determine, a suitable
set of random numbers must be adopted for the fictitious values. Based on the
laboratory tests on some kinds of steels and alloys, the number of small cracks
increases in nearly proportion to the creep time or the fatigue cycle, which brings
the conclusion that uniform random numbers from more than zero to unity are
appropriate for the first approximation (Ohtani et.al., 1989c, 1990c). The future
requirement is to get additional data on the distribution of the values of R for
service condition.

Step 1

This step deals with the small crack initiation, which is supposed to take place at
every grain boundary. The initiating cracking is revealed as a segment of grain
boundary facet at the surface or the inner section of a critical region.

The fracture driving force, D, is imposed on each grain boundary in Fig.2(a) in

every unit creep time or fatigue cycle, as shown in Fig.2(b). Although D is
essentially stochastic variable, it is handled as a deterministic variable by
208

Field Operation Laboratory Operation Computer Operation

STEP 0: PRELIMINARY ANALYSES

Selection of component Determination of variables

for evaluation of in grain generation model
remaining life
1 Generation of 2- (quasi 3-)
Sampling, ηImage analysis dimensional grains
Replication
Statistical data of Statistical data of
grain size and shape simulated grain size
and shape

Investigation of Generation of grains for

damaged area simulation of crack
initiation and growth

Observation of crack Determination of fracture

density in resistance, R, at grain
laboratory tests boundaries

STEP 1: PREDICTION OF CRACK INITIATION

Operation condition Stress and strain Determination of fracture

analyses driving force for crack
Temperature, initiation, F
pressure, etc.

Sampling, ■>| Image analyses Simulation of crack

Replication initiation
Statistical data
of crack density Data of simulated cracks
and crack length

YES / Is the longest crack

I ( over one grain
\ boundary? Revision of
driving
force, F
I Determination of F f-
j in imaginary (severe)j
• operation condition ! Prediction of crack
initiation

I Predicted data

Judgement of crack
initiation life
based on
Crack Density

—ι
to STEP 2
 209
STEP 2: PREDICTION OF CRACK GROWTH

Stress and strain Determination of fracture

obtained from STEP 1 driving force for crack
growth, K
Sampling, ->| Image analysis"
Replication | Simulation of crack growth^
Statistical data
of crack density Data of simulated crack
and crack length length

NO
^Comparison*

YE3 Revision of
driving
force, K
Determination of K 5j
I in imaginary (severe) I
'operation condition Prediction of crack
growth

a
(Predicted data
| Extreme statistics |-

Judgment of crack
growth life based on
Crack Density,
Longest Crack
Length,
Maximum Crack
Growth Rate

Fig.1 Flow chart showing the operation in the process

of predicting small crack initiation and growth
for remaining life assessment.

Fig.2 A part of simulation grain structure and description

of computational procedure of giving (a)fracture
resistance,/?, and (b)driving force, F, to every grain
boundaries and f+K,to cracking grain boundaries.
210
imposing the random effect only on the fracture resistance, R in present study,
because it has been clarified that this treatment virtually gives the identical
result with that of the simulation in which both R and D are stochastic (Kitamura
and Ohtani, 1990a). Then, D is given as
D=F+K, (1)
where F is the driving force for crack initiation, which is a function of the ratio
of normal stress acting on the grain boundary facet, σ η , to the applied stress, O ,
and the loading condition, F ;
F=F0(a /0) m =F o /(l+tanV+tan^e ' ) m , (2)
where Θ p an& Θ Q' a r e t n e surface ana the inward inclinations of a crack to the plane
perpendicular to the applied stress, and m is the material constant which is nearly
equal to the stress exponent of power law creep. K in eq.(l) is the^ driving force
for crack growth, which is in proportion to the creep J-integral, J , or the creep
J-integral range, Ä J C , of nonlinear fracture mechanics parameter (Ohtani et.al.,
1988). It is formulated as a functions of the crack length, a, and the loading
condition, K , as follows:
K=K 0 a. (3)
The values of F, or F and m, in eq.(2) is determined beforehand as a laboratory
operation, by extrapolation of the results of accelerated tests such as isostress
tests. The numerical calculation in Step 1 is opened with this value. The fracture
resistance, R, decreases by a magnitude corresponding to the driving force, F, at
every loading time interval. Grain boundary fracture takes place when the residual
resistance reaches zero. Small cracks thus initiate here and there in order of the
values of R.

On the other hand, the density of small cracks and the distribution of crack length
are examined as a field operation by replication at every regular inspection of
component. A computer-aided image-analyzing system is again of great help to avoid
personal error of the measurement as well as to save the observation time (Kitamura
et.al., 1990c). The value of F for the numerical simulation is revised by comparing
the actual information from replication. Such a revision at every regular inspection
is recommended to attain accurate prediction of remaining life. To repeat the
revision is not always possible in the practical applications, but even only one
adjustment brings the improvement of the reliability.

The remaining life is defined as the crack initiation life when the crack density,
n, reaches a critical value, n c . In general, the value of n depends on materials,
operating temperatures, loading conditions, environmental effects, cracking modes,
component dimension and size, and safety margins. For example, in the case of a
large component made of a ductile steel with multiple surface cracks under creep-
fatigue interaction condition, a considerably high density per unit surface area
must be allowable as the criterion. For a small and thin part subjected to overall
creep cavities through a wall thickness, the criterion should be settled by a lower
density per unit volume(Kitamura and Ohtani, 1989b; Ohtani et.al., 1990d).

Step 2

It was found from the experimental observations that the process of small crack
growth governs the greater part of the failure life in strain controlled fatigue
even in creep dominated condition. The fact requires the prediction of crack growth
behavior. In the present simulation, the crack growth takes place in such a discrete
manner that the adjoining grain boundary(ies) to an existing crack dissipates its
resistance, R, and fractures. Similar operation to those in Step 1 are conducted for
remaining life prediction; field inspections of service condition and crack
replication, laboratory tests and analyses for determining the driving force, K, in
eq.(3), and numerical calculation.

It might be rational to assume two different driving forces, F and K in eq.(l), in

 211
the present simulation, as the experimental results show that, once a crack
initiates, it tend to grow easily due to the stress intensity of the initiating
crack. Therefore, cracking behavior can be classified as a crack initiation type and
a crack growth type corresponding to a large and a small magnitude of the ratio,
F /K , respectively (Kltamura et.al., 1990e). It is also found in the experimental
observation that few cracks initiate and grow within a circular zone containing a
pre-existing crack due to its stress relief (Tada et.al., 1990). Then, the fracture
driving force is not given to the grain boundaries within this stress relief zone
(Ohtani et.al., 1990c; Tada et.al., 1990). Another additional procedure in the
present numerical simulation is that when two adjacent cracks happen to coalesce,
the crack is assumed to become immediately a large crack of semi-circular shape at
the surface or of penny shape at the inside.

The remaining life evaluation is made on the basis of the criteria that one of three
quantities; the crack density, the longest crack length, and maximum crack growth
rate, reaches the critical value. In the case of a crack growth type, which is
characterized by a few main cracks growing from the surface accompanied with few
small cracks or cavities, a critical length of the longest crack is most available
for the criterion. On the other hand, when the material is subjected to the damage
of crack initiation type and governed by a number of small void-like cracks or
overall cavities, a critical value of the crack density will be more practical
similarly to the criterion in Step 1.

REFERENCES

Jaske,C.E. and M.Kitagawa(1989). Evaluation of Material Degradation and Prediction

of Service Life, presented at FVP Tutorial, ASME 1989 PVP Conf., Honolulu, Hawaii.
Kitamura,T. and R.0htani(1989a). Creep Life Prediction Based on Stochastic Model of
Mlcrostructurally Short Crack Growth, J.Engineering Materials and Technology,
Trans. ASME, 111, 169-175.
Kitamura,T. and R.Ohtani(1989b). Stochastic Damage Variables Based on Randomly
Distributed Microcavities During Creep, In: Advances in Plasticity 1989 (A.S.Khan
and M.Tokuda, eds.), pp.687-690. Pergamon, Oxford.
Kitamura,T. and R.Ohtani(1990a). Stochastic Analysis of Small Crack Initiation in
Creep and Creep-Fatigue by Convolution Integral Method, Trans.JSME,Ser.A, 56, 196-
202.
Kitamura,T., N.Tada, M.Abe, M.Yumita and R.Ohtani(1990b). Effect of Compression-
going Strain Rate on Initiation and Growth of Small Cracks under Creep-Fatigue
Condition, Trans.JSME,Ser.A, 56, 575-581.
Kitamura,T., N.Tada, Y.Kuriyama and R.Ohtani(1990c). Distribution* of Grain-Boundary
Length and Inclination of Type 304 Stainless Steel and Its Effects on Small Crack
Initiation and Growth under Creep-Fatigue Conditions, Trans.JSME,Ser.A,56,702-707.
Kitamura,T., N.Tada and R.0htani(1990d). Method for Evaluation of Remaining Life in
High Temperature Components Based on Numerical Simulation of Small crack
Initiation and Growth in Creep-fatigue, presented at the 68th JSME Fall Maeting,
No.900-59, Vol.A, pp.368-370; to be submitted to Trans. JSME, Ser.A.
Kitamura,T., N.Tada and R.Ohtani(1990e). Characterization of Creep-Fatigue Failure
Process Based on Stochastic Behavior of Small Crack Initiation and Growth,
presented at Fourth IUTAM Symposium on Creep in Structures, Cracow, Poland.
Metals Handbook,Ninth Edition(1989). Vol.17, Nondestructive Evaluation and Quality
Control, ASM International.
Ohtani,R., M.Okuno and R.Simizu(1982). Microcrack Growth in Grain Boundaries at the
Surface of Smooth Specimen of 316 Stainless Steel in High Temperature Creep,
J.Soc. Materials Science,Japan, 31, 505-509.
Ohtani,R., S.Nakayama and T.Taira(1984). Application of Creep J-integral to
Microcrack Propagation of Creep in 304 Stainless Steel, ibid., 33, 590-595.
212
Ohtani,R. and T.Kinami(1986). Nucleation, Propagation and Distribution of Creep
Microcracks in 304 Stainless Steel, In: Proc.Int.Conf.on Creep, pp.167-172. Japan
Society of Mschanical Engineers, Tokyo.
0htani,R., T.Kinami, H.Murayama and T.Watabe(1987a). Observation of Initiation and
Early Growth of Small Cracks during High-Temperature Low-Cycle Fatigue in 304
Stainless Steel, J.Soc. Materials Science,Japan, 36, 974-979.
0htani,R., T.Kinami and H.Sakamoto(1987b). Small Crack Propagation in High
Temperature Creep-Fatigue of 304 Stainless Steel, In: Role of Fracture Mechanics
in Modern Technology (G.C.Sih, H.Nishitani and T.Ishihara, eds.), pp.381-392.
North-Holland, Amsterdam.
0htani,R. and T.Kitamura(1987c) Numerical Simulation of Microstructurally-Short-
Crack Propagation in Creep, JSME International Journal, 30, 1741-1749.
0htani,R.,T.Kitamura,A.Nitta and K.Kuwabara(1988). High-Temperature Low Cycle
Fatigue Crack Propagation and Life Laws of Smooth Specimens Derived from the Crack
Propagation Laws, In: Low Cycle Fatigue, ASIM STP 942 (H.D.Solomon, G.R.Halford,
L.R.Kaisand and B.N.Leis, eds.), pp.1163-1180. American Society for Testing and
Materials, Philadelphia.
0htani,R., N.Tada and T.Hashimoto(1989a). Difference Between Monotonie Tension and
Creep-Fatigue in the Behavior of Small Crack Initiation and Early Growth of 304
Stainless Steel at Elevated Temperature, J. Soc. Materials Science, 38, 89-94.
0htani,R. and T.Kitamura(1989b). Behavior of Initiation and Growth of Creep and
Creep-Fatigue Small Cracks in Austenitic Stainless Steels, In: Advances in
Fracture Research, Proc.ICF7 (K.Salama,K.Ravi-Chandar,D.M.R.Taplin and P.Rama Rao,
eds.), Vol.1, pp.213-221. Pergamon, New York.
Qhtani,R., T.Kitamura and N.Tada(1989c). Numerical Simulation of Initiation and
Early Propagation of Creep-Fatigue Small Cracks Based on a Model of Random
Fracture Resistance of Grain Boundaries, In: Structural Design for Elevated
Temperature Environments— Creep, Ratchet, Fatigue, and Fracture (C.Becht IV,
R . O h t a n i , L.K.Severud, and S.Y.Zamrik, e d s . ) , ASME P V P - V o l . 1 6 3 , Book
No.H00478,pp.123-127. American Society of Mechanical Engineers, New York.
0htani,R. and T.Kitamura(1990a). Initiation and Propagation of Microstructurally
Small Cracks under Creep-Fatigue Condition, In: Proc. 4th Int. Conf. on Creep and
Fracture of Engineering Materials and Structures (B.Wilshire and R.W.Evans, eds.),
pp.791-802. The Institute of Metals, London.
0htani,R., T.Kitamura, M.Abe, Y.Kuriyama and H.Miki(1990b). Surface Small Crack
Initiation and Growth of Heat Resisting Alloys in Creep-Fatigue, J. Soc. of
Materials Science, Japan, 39, 529-535.
0htani,R., T.Kitamura and N.Tada(1990c). Stochastic Simulation of Initiation and
Growth of Small Surface Cracks in Creep-Fatigue Condition, In: Fatigue 90, Proc.
4th Int. Conf. (H.Kitagawa and T.Tanaka, eds.), Vol.IV, pp.2143-2148. Materials
and Component Engineering Publications, Birmingham.
0htani,R., T.Kitamura and N.Tada(1990d). Cracking Behavior of Heat Resisting Steels,
Alloys and a Carbon Fiber Reinforced Polymer at Elevated Temperatures, presented
at the US-Japan Seminar on Advanced Materials for Severe Service Applications,
Honolulu, Hawaii; to be published as a Special Issue in Materials Science and
Engineering A.
Tada,N, T,Kitamura and R.Ohtani(1990). Monte Carlo Simulation of Creep-Fatigue Small
Cracks Based on a Three-Dimensional Model of Random Fracture Resistance of Grain
Boundaries, Trans. JSME, Ser.A, 56, 708-714.
WS6d2

CYCLIC DAMAGE EVOLUTION AND PREDICTION

A. PLUMTREE AND G. SHEN

Department of Mechanical Engineering

University of Waterloo, Waterloo, Ontario, N2L 3G1 Canada

ABSTRACT

Cyclic damage evolution throughout the life of a specimen or component may be expressed
by the application of a model developed from earlier continuum mechanics concepts. By
monitoring the development of cracks during the life of the material, damage accumulation
may be represented accurately for either stress or strain controlled fatigue. Using this
approach the life of single and multiple level tests may be predicted successfully for
aluminum alloys and steels.

KEYWORDS

Fatigue, damage accumulation, life prediction, damage mechanics.

INTRODUCTION

Lemaitre and Plumtree (1979) have shown that damage mechanics may be applied to
predict the mechanical deterioration of structural materials under cyclic conditions. These
studies incorporated constitutive equations for damage derived from thermodynamic
principles by Kachanov (1958) for creep and extended for fatigue by Chaboche (1978).
Damage may be presented as a continuous variable, represented by the density of defects
produced in the material on loading. For fatigue, damage is the initiation as well as the
growth of microcracks and ultimately the complete rupture of the material.

This work will show how continuum damage mechanics can present a more realistic unified
concept of fatigue which may be applied to express fatigue damage evolution under either
stress or strain control and give accurate life predictions.

213
214

FATIGUE DAMAGE UNDER STRAIN CONTROL

The damage, D, resulting from cyclic deformation may be expressed as an internal variable
which describes an irreversible microscopic rupture process involving the formation and
growth of short fatigue cracks and their development into long fatigue cracks. To account
for strain controlled fatigue, Lemaitre and Plumtree (1979) developed Chaboche's (1978)
model, which allowed damage evolution to be expressed as follows:

(δΖ)/(δΛΓ) = [1 / (p+l)] [1-D]P W

where p is the damage exponent and N = N/Nf, is the normalized number of cycles since
N is any given number of cycles and Nf is the number of cycles to failure. However,
Plumtree and Shen (1990) have shown that p is dependent upon the cyclic strain amplitude
Δ£ρ/2 and the number of cycles; hence p = ρ(Δ£ρ/2, Ν). Consequently the equation for the
evolution of damage may be written:

dD/dN = 6DI&N \p + bD/Öp \χ dp/dN 0)

Integrating equation (2) gives

— —=— IJI
D = 1 - (1 - N)m+1

Fatigue damage in aluminum alloy 6066-T6 at total strain amplitudes ranging from 0.20%
to 1.00% (O'Connor and Plumtree, 1988) may now be considered for identification of the
model expressed by equation (3). The cyclic strain controlled damage was defined as the
ratio of the cracked area (A^) to the original cross sectional area (A0) of round, unnotched
specimens (i.e. D = Ac/A0)._The increase in cracked area was dependent upon strain level
and the variation of p with N was found to obey a In-linear relationship according to

In p = a N + b or p = exp (a N + b) '4'

where a is a strain independent material constant (=-9.1) and b is strain dependent given
by
b = 7.89 - 1.60 log teJ2 (5)

At the higher strains and hence shorter lives, b will take lower values. The relationship
between B and Nf may be written
b = 6.01 + 1.43 log Nf (6)

Using these exponents, the work carried out on aluminum alloy 2024-T4 at two strain
levels by Topper and Sandor (1968) was analyzed. It was found that the predicted number
of blocks to failure corresponded very closely with that observed experimentally. Also by
using the same approach, it was possible to predict the lives corresponding to different
sequences imposed on steels using two (Miller and Zachariah, 1977) and multiple (Golos
and Ellyin, 1988) strain levels. The agreement between predicted and experimental data
was very good, particularly when it is realized that no allowance was made for the
difference in material under consideration. Table 1 gives the data for the multiple level
 215

Table 1.Multiple level strain controlled fatigue test results of A-516

Gr 70 Steel (Golos and Ellyin, 1988)

Sequence Level 1 Level 2 Level 3 Level 4 Predicted

of Cycle Cycle Cycle Cycle Cycle
Levels Ratio Ratio Ratio Ratio Ratio
Δε/2(%) N3/Nf Na/N, N3/Nf N3/Nf Last Level
.8A6/.2 .50 .30 .07 .02
.8/.2Λ6 .50 .18 .30 .29
.2/.6A8 .18 .50 .62 .47
.2/.8A6 .18 .62 .54 .29
.8/.6A4/.2 .30 .19 .21 .10 .10
.2/.8A4A6 .09 .10 .54 .59 .31
.8/.2A6/.4 .10 .50 .10 .39 .26
.2/.4/.6A8 .27 .27 .37 .44 .28

strain tests.
FATIGUE DAMAGE UNDER STRESS CONTROL

Chaboche (1978) developed a differential equation for fatigue damage evolution under
stress control:

(7)
6D
6N B(o) (1 -D)
Viz»

where om is the maximum stress during the cycle and σ is the mean stress. Also
f(D) = [1 - (1 - ί))λ+1]α(σ"*δ) (8)

where a is a stress dependent material constant and B, β, λ are temperature dependent

material constants. Lemaitre and Plumtree (1979) used the term / (D) = [1 - D]~p to
replace equation (8) allowing the damage to be expressed in a simplified form:
(9)
D = 1 - [1-iVJP^ 1

However, on re-evaluating the results of stress controlled tests conducted by Otegui (1988)
on automatically and manually welded steel sections, the damage evolution exponents, β
and p, were found to be dependent upon the number of cycles and the imposed stress level,
as shown in Fig.l. Fatigue cracks developed at the weld toe. Continual measurement of the
cracked area throughout the life of these weldments allowed the damage evolution to be
monitored for different stresses and from the experimental data, it was found that the
216

ooooo 400MPA
D a a a a 250MPA
DESCRIBED

I Γ-
0.0 0.2 0.4
0.4 0.6 0.8 1.0
NORMALIZED CYCLES (N)

Fig. 1 Variation of (ß + p) with cycles for manually welded

steel joints, after Otegui (1988)

exponents could be expressed as follows:

p = exp (AN + B) (10)

where A is a stress independent material constant (A« - 18) and B is a stress dependent
constant (B = 2.18 x 10~*N* + 9.69 for the manual welds and for the automatically
welded samples B = 1.94 x 10*Nf + 4.99). Also

ß = ß0 exp C (1 -N) dl)

where ß0 is a stress independent material constant (ß0~7) and C is a stress dependent

constant which decreases as the stress increases (C = 2.13 x 10^Nf + 2.32 for manual
welds and C = 0.78 x lO - 6 ^, + 2.38 for automatic welds). It is important to note that
the variation of p with cycles (equation 10) took the same form as that for strain controlled
fatigue (equation 4). In the microcracking stage p » ß and hence ß may be omitted in
simplified calculations indicating that in the early stages of crack evolution there is little
difference between_ stress and strain control. The shift from micro to macrocracking
occurred at about N = 0.4 for the manual welds, as seen in Fig. 1 where an abrupt change
in slope occurred. However, the change from micro to macrocracking took place at about
N = 0.25 for the automatic welds. In the macrocracking stage ß » p and p may be
omitted for simplicity which leads to the Lemaitre-Plumtree equation for stress control.

The experimental and predicted damage accumulation for both types of welded sections are
shown in Fig. 2. The model gave very good predictions for the different stress levels. If
the behaviour at a stress of 250MPa is considered then it is seen that the damage
 217

30-
κ •* AUTO
οα MANUAL
DESCRIBED
< 20 Η
Ü

Lü
Ο ιοΗ
<
<
0.0 0.2 0.4 0.6 0.8
NORMALIZED CYCLES (N)

Fig. 2 Stress controlled fatigue damage evolution in welded

sections, after Otegui (1988)

accumulated more slowly in the manually welded components. A slight waviness in the
weld toe caused the small fatigue cracks to be out-of-plane, which resulted in bridging by
the ligaments and delayed coalescence.

CONCLUSIONS

1. Good agreement between measured and predicted fatigue damage was achieved by
modifying the Lemaitre-Plumtree equation for either cyclic stress or strain control. In
this case, the damage exponents were dependent upon the stress or strain imposed and
the number of cycles.

2. The modification gave accurate life predictions when applied to different metals and to
multiple level strain controlled tests. Damage evolution in manually and automatically
welded joints was predicted accurately using the model modified for stress control.

ACKNOWLEDGEMENTS

The authors would like to thank Mr. B.P.D. O'Connor for conducting the experiments on
6066-T6 aluminum alloy and Dr. J. L. Otegui for the use of his fatigue results on welded
steel joints. The work was supported by the Natural Sciences and Engineering Research
Council of Canada through Grant A2770. The authors express their thanks to Mrs. Anita
Fonn for typing the manuscript.

REFERENCES

Chaboche J.L. (1978). Description thermodynamique et phenomdnologique de la

viscoplasticite cyclique avec endommagement. These Universit6 P et M. Curie, Paris
VI.
218

Golos, K. and F. Ellyin (1988). A total strain energy density theory for cumulative fatigue
damage. J. Press. Vessel. Tech. 110, 36-41.
Kachanov L.M. (1958). Time of the rupture process under creep conditions. Izvest. Akad.
Nauk. SSSR PTN, 8, 26-31.
Lemaitre, J. and A. Plumtree (1979). Application of damage concepts to predict creep-
fatigue failures. J. Eng. Mats. Techn. Trans ASME, HU, 284-292.
Miller, K.J. and K.P. Zachariah (1977). Cumulative damage laws for fatigue crack initiation
and stage I propagation. J. Strain Analv. 12, 262-27.
O'Connor, B.P.D. and A. Plumtree (1988). In: Fracture Mechanics: Nineteenth Symposium,
(T.A. Cruse Ed.). STP 969, ASTM, Philadelphia, 787-79.
Otegui, J.L. (1988). Initiation and coalescence of fatigue cracks in welded joints in steel,
Ph.D. Thesis, University of Waterloo.
Plumtree, A. and G. Shen (1990). Cyclic deformation and life prediction using damage
mechanics. In: Constitutive Laws of Plastic Deformation and Fracture, (A.S. Krausz et
al, Eds), Kluwer Acad. Pub., Netherlands, 77-85.
Topper T.H. and B.I. Sandor (1968). Effects of mean stress and prestrain on fatigue
damage accumulation. T and AM. Report No. 318, Theor. and App. Mech., Univ. of
Illinois.
WS6d3

LOW CYCLE FATIGUE AND LIFE PREDICTION

OF NOTCHED COMPONENTS

M. GIGLIO and L. VERGANI

Dipartimento di Meccanica, Politecnico di Milano, Italy

ABSTRACT

Experimental tests have been conducted on smooth and on notched specimens

with different values of the theoretical stress concentration factor, Kt·
The local stresses and strains at the notch root have been measured, using
electrical strain gauges, and have been compared with the values calculated
by means of Neuber's rule. A strain gradient exceeding the yield limit has
been defined and measured; the influence of the gradient has been studied.
It is shown that Neuber's rule overstimates the strains, particularly if the
strain gradient is large. The fatigue life of the notched specimens have
been predicted by calculating the inelastic strains using Neuber's rule and
the fatigue data from smooth specimens. These previsions are always
conservative and the disagreement varies with the gradient, increasing when
the gradient increases.

KEYWORDS

Fatigue, notches, strain, strain gradient, plastic strain, Neuber's rule,

life prediction.

INTRODUCTION

Several approaches can be used to predict the fatigue life of notched

mechanical components. The most frequently used is derived from Neuber
(Seeger and Heuler, 1980) and determines the local stress-strain values at
the notch root. Once these local values have been determined, the life is
estimated by comparison with the smooth bar fatigue data. Accurate
calculations of the inelastic stresses and strains near notches can be
conducted by using finite element programs, which are however very lengthy
especially for cyclically loaded structures. The application of Neuber's
rule represents a simple approximate method, which, however, generally
overestimates the values of the inelastic stresses and strains (Mblski and
Glinka, 1981).

It is shown that this method does not consider the influence of the stress
219
220
gradient, which is, on the contrary, very important in order to first
calculate the local stress-strain history of the material component at the
notch and then to predict the fatigue life.

EXPERIMENTAL TESTS

Test specimens

Experimental tests were carried out on a series of cylindrical, smooth

specimens and on several sets of keyhole specimens with different notch
radiuses and hence different theoretical stress concentration factors, K^·
In table 1 the principal dimensions and the K^ values of the specimens are
shown. Electrical strain gauges were applied at the notch tip and on the
specimens faces to measure the strain patterns.

Table 1. Dimensions and K^ values of keyhole

specimens (see fig.l).

Dimension (mm) R (mm) Kt theor. Kt exp. Kt num.

B = 24, b = 26.5, W = 48 2 2.89 2.86 3.00

4 2.16 2.30 2.20
12 1.48
B = 17, b = 20.0, W = 36 2 2.58 2.56
B = 22, b = 27.0, W = 73 12 1.44 1.52

Material

All the specimens were cut from a sheet of A 533 B steel 50 ram thick. The
strength and cyclic characteristics of this material were determined on
other specimens from the same sheet, see tables 2 and 3.

Table 2. Monotonie properties of A 533 B.

Oy(MPa) ar(MPa) E(MPa) V A(%) Z(%)

566 682 210700 0.28 21 79.8

Table 3. Cyclic properties of A 533 B.

K'(MPa) n' a'f(MPa) e'f b c

725 0.100 728 0.157 -0.060 -0.491

Fatigue tests

The different groups of specimens, with equal notch radiuses, were

subjected to pulsating loads, from P=0 to P=Pmax, the values of which are
such as to produce the same values of K^S, where S is the nominal stress at
the notch tip. In particular the following values have been considered:
 221
KtS=1050 MPa, KtS=1120 MPa, KtS=1200 MPa and KtS=1260 MPa. The tests were
interrupted when a crack was revealed by means of penetrating liquids. The
pulsed loads were applied with a 250 kN Schenck hydropulse. The strains were
measured, by means of electrical strain gauges, during the first load cycle
and at constant intervals of cycles during the nucleation tests.

EXPERIMENTAL RESULTS

Local strains

The severity of a notch is characterized by the elastic stress concentration

factor, Kt, which depends only on the geometry. If S is the nominal stress,
proportional to the applied load by a geometry dependent constant, the
product KfcS is the maximum principal stress value at the notch if the
material behaviour is elastic. Over this yield stress value, characteristic
of the material, the real stresses are lower than those calculated on the
hypothesis of linear-elastic behaviour and the strains are larger than the
elastic solution. The values of these is necessarily influenced by the
plastic yielding extension around the notch and by the surrounding material,
which still behaves linearly.

Fig.l shows the strain pattern along the y direction on a blunt notched
compact specimen. The specimen is loaded with tension and bending and the
nominal stress is also shown.
P,1
LOCAL STRAIN
(Γ
1
....NOMINAL STRAIN
,Sy
B-THICKNESS

L·*
P 4.6P(Wb/2)
S=-!-±
^***^ b-B b'B
1

b
""""

P
L * J
Fig. 1. Local and nominal strains in y direction.

Fig.2 shows the plot of the load, KtS, versus the notch y strains,
experimentally measured by means of electrical strain gauges and calculated
according to Neuber's rule, during the first load cycle, on specimens
which although similar have different notch radiuses meaning that
they are characterized by different K f
Until the material yield limit the strain values of the three specimens
(with Kt=1.4, 2.4, 2.8 respectively) are equal, whereas the notch strain
values are different after the yielding point if the values of K^ are
different. For example by considering KtS=1000 MPa the notch strain y
measured on the specimen with Κ^=2.8 is €y=0.54 % ; on the other hand the
value measured on the specimen with Κ^=1.4 is €y=0.65 % with an increment of
about 20 %. Even if the nominal stress is the same, the strain and stress
pattern are very different: if the K^ value is larger, and the notch radius
is smaller, the strain gradient is higher meaning that, consequently, the
plastic yielding is more localized. If the Kt value is lower a more
extensive plastic zone is caused by a lower strain gradient.
222
Threedimensional finite element model of the specimens has been set up.
An elasto-plastic analysis has been conducted to simulate the first load
cycle, considering the real σ-e curve of the material.

1 Neuber
KtS[MPa] 2 Kt-1.40
3 Kt-2.39
4 Kt-2.84

0.1 0.2 0.3 0.4 0.5 0.1 0.7

Fig. 2. Experimental and calculated strains for keyhole

specimens with different K^ values.

Fig.3 shows the y strain measured experimentally for two specimens, one with
Kt=1.4 and one with Κ^=2.8. The K^S value is the same for both specimens.
The same figure shows the calculation of the plastic zone size, r p ,
considering the y strain equal to the yield strain. It should be noted that
the plastic zone size, rp, calculated is not exact because the multiaxiality
of the stress state is not considered. However the numerical analysis
described below enables us to verify that this error is not significant,
since the y stresses are much larger than the stresses along the other
direction. Fatigue life behaviour of notched members is strongly influenced
by the strain pattern; in fact, the notch cyclic strain values also largely
differ owing to the K^·

The residual, medium, elastic and inelastic notch strains y are defined in
fig.4. This figure also shows that after the first loading cycle the medium
stress fully relaxes, thus creating test conditions similar to a strain-
controlled test with an imposed main strain.

• LOAD
■ UNLOAD

s
0.6-

0.4H
βγίΕΐο

J t rp ^ J
Γ-0.4-

Fig. 3. Experimental y strain at 1° load cycle

(KtS=1050 MPa) for specimens with Kt=1.4 and 2.8.
 223

800-
i
σ ^
400 Ht=em+8a,t
e

200-
/ /
/
/ %.l
/ /
«4 / / 0 . I 1.8 m

200- ft 1 6V[%]

400-

800-
su£M 4\ ^Ι^Α,Ρ
Α,Τ

Fig. 4. Strain values of hysteresis cycle.

This behaviour depends on the highly strained region in a zone being

constrained by the elastic matrix surrounding it. In this way it is possible
to compare the behaviour of the keyhole specimen subjected to a pulsating
load with that of the strain control specimen. In the smooth specimen K-t
is equal to 1 and there is no strain gradient since all the specimen
sections are subjected to the same strain and stress field. The plastic zone
is more extensive than in the notched specimens and the stabilized cycles
are very different. A comparison between the stabilized cycles is shown in
fig.5. The value of K^S is equal in all the specimens while the resulting
value of the inelastic strain varies with K^ value.

800 °^ iri.i M.4

400

200H

-200H

-400

-600

(a) (b)
Fig. 5. Stabilized hysteresis cycles for smooth (a) and keyhole
specimens with Kt=2.8 and 1.4 (b), with KtS=1050 MPa.

Strain gradient

The stress concentration factor, Kt is not a complete characteristic of the

stress distribution around the notch. A further, equally important,
parameter is the stress gradient, defined as the slope of the stress versus
the distance from the tip notch. The relative stress gradient is defined as
(Schijve, 1980):
X= l—.(*£) (i)
onotch ldx/x=0
224
If the stress distribution around the notch is linear elastic, it is
possible to calculate a strain gradient equivalent to the stress gradient,
using the strain experimental measurements . If the strains are considered
linearly variable between the measuring points the experimental relative
strain gradients of the notched specimens are defined as:

% = 1 A£ considering Ax=lmm. (2)

enotch Δx

In table 4 the linear relative strain gradients are shown. If the yield
limit is exceeded^it is necessary to distinguish between the stress and
strain distributions, meaning that the respective gradients are no longer
equivalent. Above the yield limit in order to also consider the cyclic
behaviourit seems more significant to define a strain gradient .
The total strain trend, e^, is calculated as the sum of the residual, e r ,
and the cyclic, ea^,strains, which is the real strain distribution, measured
Table 4. Strain gradients of keyhole specimens

Specimen KtS [MPa] R notch [mm] Kt •^eelastic Xe r p [mm]

2R-1 1050 2 2.84 0.66 0.76 0.7

2R1-1 1050 2 2.68 0.64 0.75 0.3
2R1-2 1120 2 2.57 0.64 0.73 0.3
2R1-3 1200 2 2.50 0.63 0.86 0.7
4R-2 1120 4 2.40 0.38 0.44 1.3
4R-4 1260 4 2.20 0.40 0.56 1.3
12R-1 1050 12 1.40 0.27 0.39 3.7
12R-2 1120 12 1.46 0.26 0.50 3.7
12R-3 1200 12 1.39 0.26 0.52 5.2

on two specimens shown in fig. 3. The relative strain gradients

calculated by means of the total strains, e-^ = e m + e a -£, measured on the
specimens at the third load cycle are also shown in table 4. Above the yield
limit the strain gradients vary owing to the value of K^S. If, for example,
the specimen with the notch radius equals r=2 and Κ^Α2.6 is considered, the
linear strain gradient is about 0.64 and the strain gradient above the yield
limit gradually increases, from 0.75, with K-tS=1050 MPa, to 0.86, with
KtS=1200 MPa.

LIFE PREDICTION

Monotonie loading

The stress and strain values at the first load cycle are normally determined
by Neuber's rule (Neuber,1961), which relates the theoretical stress
concentration factor K^ to the plastic stress and strain concentration
factors K Q and Kg:

Kt 2 = KoK e (3)
where
KQ = σ/S (4)
and
K e = e/e (5)

σ and e are local stresses and strains, while S and e are nominal stresses
and strains:
 225

e = S/E + (S/K) ± / n ; e = σ/Ε + (σ/Κ) ± / η (6)

where n is the monotonic strain hardening exponent and K is the strength

coefficient. Although Neuber's rule is often used for convenience it does
not, however, consider the strain gradient influence; in fact the e value
calculated only depends on the KtS value and not on the K^ value.
The strains measured experimentally at the first load cycle, the
corresponding strains calculated by means of the numerical analysis and
those calculated according to Neuber's rule calculated are shown in fig.2
and in table 5. The finite element analysis values of strains give a good
appoximation of the experimental strains, while the strains calculated by
means of Neuber's rule are generally higher.

Table 5. ^sx. (P^1^) a

"t th e first loading cycle

KtS(MPa) Neuber Kt-1.4 Kt=2.3 Kt=2.6 Kt=2.8

Exp. Num. Exp. Num. Exp. Num. Exp. Num.

1050 9245 7670 8000 6382 5554 5708 6600

1120 10519 8990 8200 6965 7800 6461 6617 7500
1200 12075 11165 11200 7888 7561 - 8200
1260 13313 9613

Cyclic loading

These calculations were based on the stabilized cyclic stress-strain curve in

the form (Glinka, 1985):
1 /n'
% = (tfa/E) + ( a a / K ' ) ± / n (7)
The fatigue life is then determined by means of the Coffin-Manson strain
life relations :

ea = (a'f/E) (2N f ) b + e' f (2N f ) c (8)

Table 6 shows both the theoretical and experimental rsults.

Nf is the value of the cycle number measured experimentally and corresponds
to the crack nucleation in the specimens; Nf (1) is the value of the cycle
number determined by using the experimenal e a t values in the Manson-Cof f in
law, eq. (8), with the fatigue data from the smooth specimens. It is
apparent that these life values are very conservative, especially if the Kt
values are large. It is probably necessary to correct the fatigue data
by considering the different strain gradients. Nf (2) is the value of the
cycle number calculated by using the experimental e a t in the modified
Manson-Cof fin law modified, considering the effect of tne medium strain:

ea - (σ'£/Ε) (2Nf ) b + (e'f-em) (2Nf ) c (9)

This disagreement is even larger, because the influence of the strain and
stress gradient has not yet been considered and the fatigue data obtained
from smooth specimens where the strain and stress field is the same in the
specimen section are too conservative if applied to notched specimens with
a non uniform strain and stress trend in the section.
226
Table 6. Cycles of failure: experimental and
predicted values

Specimen K t KtS[MPa] ^ t t J u r o / 1 1 1 ] emed^111] Nf exp. N f (l) N f (2)

2R-1 2.84 1050 2553 3216 70000 26120 25390

2R-2 2.83 1120 2811 4028 50250 16050 15380
2R1-1 2.68 1050 2550 3144 85000 26370 25390
2R1-2 2.57 1120 2721 3709 53000 18800 18070
2R1-3 2.50 1200 3061 4605 24500 10800 10250
4R-1 2.39 1050 2629 3590 61000 22460 21610
4R-2 2.40 1120 2861 4135 27000 14770 14160
4R-3 2.23 1200 3166 4363 13000 9340 8910
4R-4 2.20 1260 3496 6141 14600 6170 5750
12R-1 1.40 1050 2837 4968 22000 15380 14530
12R-2 1.46 1120 3079 6094 20000 10560 9830
12R-3 1.39 1200 3438 8140 10000 6590 6010

CONCLUSIONS

Neuber's rule does not consider the influence of the strain gradient, which
on the contrary seems very important in order to calculate the local
stresses and strains at the notch root.

Experimental tests, carried out on notched specimens with different notches,

show different behaviours during the monotonic load and during the fatigue
tests if the K^ values are different.
A strain gradient exceeding the yield limit has been defined.

The Manson-Coffin law using the fatigue data from smooth specimens and the
experimental strains e a t does not give good results; this is probably due
to the influence of the strain gradient.

ACKNOWLEDGEME3SIT

This work is supported by the CNR grant CT 88.02797.07.

REFERENCES

Molski, K. and Glinka, G. (1981). A method of elastic-plastic stress and

strain calculation at a notch root. Material Science and Eng., 50 f 93-100.
Glinka, G. (1985). Calculation of inelastic notch-tip strain-stress
histories under cyclic loading. Eng. Fracture Mech., Vol.22, N.5, 839-854.
Seeger, T. and Heuler, P. (1980). Generalized application of Neuber's rule.
J. Test. Eval.f N.8, 199-204.
Neuber, H. (1961). Theory of stress concentration for shear strained
prismatical bodies with arbitrary non linear stress-strain law. J. of
Applied Mech., 544-550.
Schijve, S. (1980). Stress gradients around notches. Fat, of Eng. Mat, and
Structures, Vol.3, N.4, 325-338.
WS6d4

CONCURRENT FIELD SERVICE AND LABORATORY

TESTING AS A MEANS OF IMPROVING RELIABILITY IN
CREEP-RUPTURE APPLICATIONS

S.S. MANSON
Professor of Mechanical & Aerospace Engineering Dept.
Case Western Reserve University, 10900 Euclid Ave., Cleveland,
OH 44106, U. S. A.
and
JONGHWA PARK
Graduate Student of Mechanical & Aerospace Engineering Dept.
Case Western Reserve University

ABSTRACT

A method is presented whereby long-time creep rupture data on several heats of one
material are used to extrapolate the long-time behavior for a new heat of the same
material. Use is made of short-time data on the new heat, which can be obtained during
early design or concurrent with the service of the component.

KEYWORDS

Time-temperature parameter; Minimum Commitment Method; long-time extrapolation;

creep-rupture strength; concurrent engine service; standard deviation; NRIM data;
multi-heat; fingerprint constants; Larson-Miller parameter; Manson-Haferd parameter

INTRODUCTION

In the design of gas turbine blading for stationary power-generating turbines it is common
to choose stress levels for the creep-rupture life of 100,000 hours or longer. To insure
such long life the designer must be confident that the stress is lower than that which is
indicated by appropriate prior creep-rupture tests. However, the designer cannot have
information on such long-time tests for the very heat of material from which the blades
are to be fabricated. At best he must rely on data from material of similar composition
but fabricated sufficiently earlier that long-time testing could have preceded the new
application. But, material produced at a different time often displays properties different
from those that might be expected from the current heat because of either composition
or production variables. Therefore, the designer must incorporate large safety factors,
often reducing the efficiency of the turbine.

In this report we explore a procedure whereby effective use can be made of prior data
involving the long-time testing, but also incorporating short-time testing on the new
material in order to obtain improved knowledge of the expected long-time creep-rupture
properties of this heat. Ideally, also, testing concurrent with engine service can provide
longer-time data on the new heat so that the operator can more intelligently estimate
whether stresses or temperatures may be increased (or, reduced) in order to assure the
desired lifetime. Use is made of the Minimum Commitment Method proposed by Manson

227
228
in 1967, but the implementation has been refined recently. To illustrate the approach
we have applied the proposed method to an extensive set of data generated over many
years at the National Research Institute for Metals (NRIM) in Tokyo, Japan. Here a
number of materials, comprising many heats for each material, have been extensively
tested, some to rupture times of approximately 100,000 hours. By separating one of the
heats and operating on the extensively tested remaining heats, it becomes possible to
apply our methodology to estimate the performance of the separated heat (we shall refer
to it as the "new heat"). Use is made of the data for several short-time tests on the "new"
material to extrapolate them effectively. The scatter in the data of the several base heats
allows estimate of the scatterband for the "new" material. The attempt is to demonstrate
that a few tests on the lot of material actually used in a component can provide a good
estimate of its long-time expectations. We also examine the cases where the new heat
is either considerably stronger or weaker than any of the base line heats, and consider
how the designer is aided in choice of design stress compared to the alternative of applying
safety factors to the scatterband of the base line heats.

BACKGROUND
Time-temperature parameters have been used for nearly 40 years to correlate creep-
rupture data. The concept wasfirstintroduced by Larson and Miller (1952), and shortly
afterwards Manson and Haferd (1953), in analyzing the validity of the L-M parameter,
proposed a new one that appeared to be more accurate. This parameter is still used with
considerable success even at the NRIM in correlating their massive data on the many
materials. As time passed many new time-temperature parameters were suggested by
other investigators, to the point that Grounes (1969) cited at least 31 different forms
that were used. The Minimum-Commitment Method proposed by Manson in 1967 was
intended to unify many of the conflicting approaches with one method that had suffi-
ciently generality to include most of them. After considerable modifications, and some
loss of generality, the method that emerged was in the form
\ogt + AP\ogt + P = G (1)
where A = constant, probably dependent on the metallurgical stability of the alloy

/> = /?1T + — ; T=absolute temperature, /? : and R2 are constants

G = B + CIogo + Do + Eo2 ; σ = stress, ksi B,C,D and E are constants
In practice each experimental datum provides an equation among the seven constants.
Thus, in principle, only seven data points are needed to determine the constants. Actually,
many more data points must be generated to allow accurate determination of the con-
stants by a linear least-square procedure. The stability constant A is usually determined
by some forms of iteration since the equations are non-linear when both A and K\ or
R2 are treated as unknowns. We have developed an effective procedure for optimizing
A, but in this report we shall use A=0.
Initially the MCM was quite successful for correlating data for individual heats of many
alloys. Later it was recognized that when dealing with multi-heats (many heats of the
same material) data scatter could be very large, possibly because of composition and
processing differences. However, any single heat showed quite consistent properties,
with much less scatter than the data of the multi-heat taken collectively. We found that
it was better to apply a "fingerprint" for each heat by assigning individual values of B
and C for each heat, but retaimng the constants A, Rj, R2, D and E as common values
for all the heats. In this way each heat could reflect its own particular behavior through
its special value of B and C, but the data from all heats could be useful in determining
the common constants A, R^, R2, D and E. The long-time data in any of the heats would
 229
therefore be useful in determining the common constants, while only a small amount of
data would be needed to establish the fingerprint constants for a new heat. Thus the
method could be applied to the estimation of long-time properties for a new heat using
data established for other heats of the same material over a prolonged prior time. This
concept was successfully applied by Manson and Muralidharan (1983) to the prediction
of the long-time properties of 316 stainless steel, but no consideration was given to
statistical aspects of the problem. With the availability of the wealth of NRIM data, it
seemed appropriate to apply the methodology already developed, and to introduce
advancements, especially considerations of data scatter.
One of the important modification that seemed appropriate was the abandonment of the
"data-centering" procedure used in 1983 to determine the fingerprint constants. In our
early work the attempt was to develop a procedure suitable for an analyst who had
available only a state-of-the-art personal computer. Because of the large number of
constants and corresponding equations involved in the handling of a large multi-heat
(say, 7 heats, resulting in 18 constants) a method was developed whereby most of the
fingerprint constants were eliminated from the solution of the major matrix, and then
determined, (with some sacrifice in accuracy) through the "data-centering" process
(Booker and Booker, 1980). However, with increase in calculating power of PCs cur-
rently available, it is no longer necessary to make the sacrifice in accuracy and some of
the ambiguity by use of the short-cut. The computer program used therefore determines
all the constants involved in the analyses through the solution of a single matrix.
A second modification involving the use of statistical analyses was also possible in the
present investigation because of the extensiveness of the NRIM data base. Since data
scatter in each of the heats could be analyzed, it became possible to estimate the scatter
to be expected in any one heat for which limited short-time data are extrapolated to
longer times.

ANALYSIS
Two multi-heats were chosen for analysis on the basis of the quantity of data generated
at NRIM. Thefirstis a nickel-base superalloy designated IA; the second a steel designated
VA. There were eight individual heats in IA and nine heats for the VA set. The designations
of the individual heats and the rupture times at selected temperatures and stresses are
shown in Table 1 for the IA heat. Data for the VA multiheat are omitted for brevity. For
purposes of demonstration we assumed that heat IAB was not initially available in the
IA set, and the VAR heat was not initially available in the VA set. Thus a complete
analysis was made of the seven remaining IA heats, and eight remaining VA heats. Based
on these analyses the common constants were determined as shown in Table 2.
To apply these results it was next assumed that short time data (less than 300 hours for
the LA heat and 200 hours for the VA heat) were generated for the two heats. Using
Eq.(l) for each of these heats, and recognizing that the constants A, Ri, Ro, D and E
are already known the values of B and C could be determined from the few data points
for the IA and VA heats as listed in Table 3.
The equations for the creep rupture curves for heats IA and VA using the above constants
were then plotted as shown in Fig. 1. These are the curves in the center of each scat-
terband. The scatterbands shown apply one median value of the standard deviations
of the base heats. Other analyses were also based on the scatterbands involving more
than one standard deviation, but are omitted here for brevity. The accuracy of the
long-time creep-rupture predictions is determined from how well the actual long-time
data, shown by the experimental data points in the region designated "extrapolated"
range fall within the predicted scatterbands. It is seen that in both cases using the average
scatter for all the known heats would have produced acceptable scatterband for both
alloys IAB and VAR.
230

Additional analyses were also made for the case where the "new heat" was stronger than
the previously tested heats, and when it was the weakest of the group. For the IA
multiheat, the results are shown respectively in Fig. 2 (IAA heat) and Fig. 3 (IAD heat).
For these cases it was necessary to choose the time cut-off at 1,000 hours since inadequate
data were available in the 300 hour range. The results will be used to discuss the
advantage of the method presented compared to alternative methods whereby the
scatterband of the entire multiheat is used to choose a design stress.

DISCUSSION
The first result seen from Figures 1,2 and 3 is that whichever heat is chosen as the "new
heat", very few relatively short-time data are needed to obtain a good estimate of the
long-time creep-rupture properties to lives approaching 100,000 hours. In most cases
such tests could be conducted while the engine is in the design stage. However, it is
clear that improved long-time predictions could be accomplished if the longer time data
points could be included in the analyses. If these tests cannot be completed before engine
design is finalized, they could be conducted concurrently with engine service. As the
results become available, new analyses could be made, and the improved estimates of
long time properties could be used to gauge the original design assumptions. If necessary,
operating temperatures or stresses (speeds) could then be adjusted either upward or
downward, to maintain the desired confidence that the design is appropriate.
The special advantage of the method is emphasized when the new heat is either stronger
than the other heats of the data set, or weaker, especially the latter. In the absence of
this method, the designer is likely to base his choice of stress level on the scatterband
of the baseline heats. For the two cases shown in Figures 2 and 3 the bottoms of the
scatterbands are shown by the dotted lines. Depending on the degree of conservatism
chosen by the designer, he may prefer to subtract from the median behavior either one
or two standard deviations, as shown by two sets of dotted lines in these figures. If the
new heat is stronger than the baseline heats (e.g. heat IAA, Figure 2) the designer might
choose stresses 20 to 30 % lower than would be needed if based on the lower estimated
scatterband for the described method. When the new heat is weaker than the baseline
heats (e.g. Heat IAD, Figure 3) the chosen design stress may be as much as 20 to 60 %
too high. For the case shown in the figure, a stress chosen to produce 100,000 hours
of service could result in a life of only 20,000 hours if the failure fell on the lower line
of the scatterband determined by the method discussed.

CONCLUDING REMARKS
The fingerprint MCM method provides a relatively inexpensive way to estimate accurately
the expected long-time behavior of a new heat based on available long-time data in other
heats of the same material. The method makes use of short-time tests on the new material
which can be conducted prior to the choice of design stresses for a given application.
Additional tests can be conducted concurrently with the service of the component in
order to establish confidence in the life expectancy, or in suggesting minor changes in
the service temperatures and stresses that will bring life to expected values.
The method is especially useful if the new heat has properties either worse or better
than the scatterband of the available heats. When the new heat has lower properties
an unconservative design could result if the designer chose stresses based on the lower
scatterband of the available data, and premature failure could occur. The method
described would avoid such mishap by alerting the designer and causing him to choose
lower stresses. On the other hand, if the new heat is on average stronger than the heats
for which prior data are available, the method would alert the designer to the fact that
he can use higher stresses or temperatures, thereby increasing the efficiency of his
component.
 231

REFERENCES
Booker, M.K. And Booker, B.L.P. (1980). New Methods of Analysis of Materials Strength
Data for the ASME Boüer and Pressure Vessel Code. In: Use of computers in managing
material property dataT MPC-14, ed. by Graham, J.A., American Society of Mechanical
Engineers, New York, 31-64
Grounes, M. (1969). A Reaction-Rate treatment of the Extrapolation Methods in Creep
Testing. ASME Journal of Basic Engineering
Larson, F.R. And Miller, J. (1952). A Time-Temperature Relationship for Rupture and
Creep Stresses. Trans. ASME. Vol. 74. p. 765
Manson, S.S. And Haferd, A.M. (1953). A Linear Time-Temperature Relation for
Extrapolation of Creep and Stress Rupture Data. NACA TN 2890
Manson, S.S. And Muralidharan, U. (1983). Analysis of creep rupture data for five
multiheat alloys by the Minimum Commitment Method using double heat term
centering technique. EPRICS-3171

MEDIAN S.D. (.0829)

932°F

DATA RANGE
- USED IN — I EXTRAPOLATE!)
ANALYSIS - RANGE EXTRAPOLATED
- RANGE CH

100 1000 10000 100000 10 100 1000 10000 100000

RUPTURE TIME (HOUR) RUPTURE TIME (HOUR)

Fig. 1. Creep rupture curves for heats IAB and VAR

100 1000 10000

100 1000 10000 RUPTURE TIME (HOUR)
RUPTURE TIME (HOUR)

Fig. 2. Creep rupture curves Fig. 3. Creep rupture curves

for strongest heat for weakest heat
(IAA) at 1562°F (IAD) at 1832°F
232

Table 1. Creep rupture data for Nickel based 13Cr-4.5Mo-

0.75Ti-6Al-2.3(Nb+Ta)-Zr-b super alloy
HEAT TEST TEMPERATURE: 1562<>F
REF CODE STRESS 51.22 38.45 31.34 22.78 19.88 17.12 15.67 14.21 12.77
IAA 44.0 626.6 1214.5 10822.5 33793.0 . . .
IAB * 92.1 481.1 2039.5 11511.9 8619.8 34860.6 - - -
IAC RUPTURE 88.7 326.9 704.3 3514.7 7122.4 - 52149.0 -
IAD ΉΜΕ - 119.3 287.2 1736.3 16837.7 - 41101.6
IAE 91.6 550.5 2522.3 17485.3 35423.6 - - - -
IAF 89.9 347.2 813.9 4405.9 9587.8 42705.5 - -
IAG 12.5 174.2 734.8 2319.9 12278.0 33178.2 - 89830.0 -
IAH 18.4 314.7 2348.6 16553.4 25541.1 - - -
HEAT TEST TEMPERATURE: 1652°F
REF CODE STRESS 38.35 28.44 22.78 17.12 14.22 12.77 11.32 10.01
IAA 44.6 273.3 945.0 13441.0 20172.3 39549.9 .
IAB * 79.5 427.4 2006.5 11000.8 23942.6 28267.2 -
IAC RUPTURE 62.4 331.2 1237.4 7420.8 14076.8 - 41418.3 -
IAD ΉΜΕ 4.2 195.4 240.3 4866.0 2639.0 - - 14917.2
IAE 66.6 753.4 3119.8 14395.6 25632.8 31774.4 - -
IAF 62.2 396.4 1342.0 7323.4 17178.1 29201.5 -
IAG 18.7 133.8 290.4 4376.0 2341.4 4100.0 - -
IAH 43.5 321.5 767.4 7881.5 15840.6 38769.1 - -
HEAT TEST TEMPERATURE: 1742°F
REF CODE STRESS 28.44 22.78 17.12 14.22 11.32 8.85 7.69 6.82 5.37
IAA . 116.0 572.7 2482.9 5537.6 32809.2 . . .
IAB * 50.3 230.9 995.1 2345.0 7882.8 19854.0 18567.4 - -
IAC RUPTURE 71.6 317.9 1726.2 4302.2 6704.8 - 36305.0 - -
IAD ΉΜΕ . - 75.8 1644.2 787.0 3098.2 . 15278.3 41690.6
IAE 62.3 254.9 1237.8 2903.2 8511.2 31236.3 18247.4 - -
IAF 77.2 242.5 1452.3 3214.7 9409.0 23639.4 - - -
IAG - 52.1 418.4 1588.1 1297.4 17961.8 51154.9 . -
IAH - 107.0 777.3 2259.2 8479.3 34824.3 - - -
HEAT TEST TEMPERATURE: 1832QF
REF CODE STRESS 22.78 14.22 11.32 8.85 6.82 5.95 5.37 4.79 4.50 4.21
IAA 26.8 381.2 714.5 6003.4 28895.2 15460.4 . . .
IAB * 21.5 476.9 1082.9 3029.7 3870.3 - 13001.4 . 15989.0
IAC RUPTURE 26.6 517.2 1587.0 2505.8 13994.8 - 17263.0 - .
IAD ΉΜΕ - 22.4 541.7 511.9 1700.3 - 4260.5 - 12062.8
IAE 24.6 409.5 1161.4 3170.8 7635.8 - 23298.1 . 51511.1
IAF 24.2 336.2 807.6 2880.8 9569.1 - 13415.6 19799.8 .
IAG -8.7 73.8 421.4 1670.8 7892.3 - 5572.4 -
IAH 181.9 357.5 3698.4 12629.9 - 47538.6 - -
(STRESS: KSI, TIME: HOUR)

Table 2. Common constants for each material

Heat Set A R^ R2 D E
IA 0.0 1.34 E-2 17180.55 -6.13 E-2 3.22 E-4
VA 0.0 -1.67 E-3 -40965.42 -9.58 E-3 -1.22 E-3

Table 3. Fingerprint constants for each heat

Heat B B
IAB 13.0961 -2.7469
VAR 7.7726 -1.6256
WS6d5

LIFE PREDICTION OF SURFACE CRACK PROPAGATION IN PLATES

WITH OR WITHOUT RESIDUAL STRESSES UNDER FATIGUE LOADINGS

K. OHJI, S. KUBO and M. TSUJI

Department of Mechanical Engineering, Osaka University,
2-1, Yamadaoka, Suita, Osaka, 565 JAPAN

ABSTRACT

The present authors proposed a method for predicting fatigue lives of a two-dimensional crack
propagating in residual stress fields, by making use of data of the crack propagation and
effective range ratio U, which were characterized by taking the crack closure phenomenon into
account. In this paper an attempt was made to extend this method to problems of a three-
dimensional crack propagating in plates with or without residual stresses. This method was
based on the assumption that both the relation between U and stress ratio R and the relation
between the crack propagation rate da/dN and effective stress intensity range < C f f determined
for two-dimensional cracks could be applied at each point along the tip line of the three-
dimensional crack. To examine the applicability of this extended method, the propagation
behavior of surface cracks was compared between the experiments and the predictions. Good
agreement was observed.

KEYWORDS

Fatigue crack propagation; life prediction; surface crack; residual stress; effective stress
intensity factor range; effective stress range ratio; crack closure.

1. INTRODUCTION
It is widely accepted that residual stress causes a significant effect on the fatigue crack
propagation behavior. In other words, the residual stress is an important factor in predicting
the fatigue lives. Several life prediction methods (Glinka, 1979, Nelson, 1982, Parker, 1982,
Nihei e t a L , 1982, Ohji e t a l . , 1987, Todoroki e t a l . t 1989) have been proposed so far to take
the effect into account.
In a previous paper (Ohji e t a L , 1987) we proposed a self-consistent and comprehensive
approach for predicting the fatigue lives of two-dimensional cracks propagating in residual
stress fields. This approach was based on the assumption of the small scale yielding and the
evaluation of effective mechanical environment in the vicinity of the crack tip, which was done
by superposing the stress intensity factors both for the residual stresses and for the applied
stresses.

Cracks and flaws found in structures or in their components are usually three-dimensional.
233
234
However, a life prediction method of the three-dimensional cracks propagating in the plates
with or without residual stresses has not been established yet. In this paper an attempt is
made to extend our life prediction method for two-dimensional cracks to three-dimensional crack
problems.

2. LIFE PREDICTION METHOD FOR THREE-DIHENSIONAL CRACKS

The life prediction method proposed by the present authors for a two-dimensional crack is based
on the following two findings established for various kinds of materials.
(1) The crack propagation rates are expressed as a single-valued function of the effective
stress intensity factor range AlLt* determined by taking the crack closure phenomenon into
account.
(2) Under the small scale yielding condition a crack closure stress can be uniquely
determined from actual stress intensity factor K, which includes the effect of both the
residual stresses and the applied external loads; this may be done by employing crack closure
properties obtained by using cracked specimens without initial residual stresses.
These assumptions may basically hold also in three-dimensional crack cases.

The following two assumptions are made in extending the prediction method into three-
dimensional crack cases.
(1) Both the da/dN vs. ΔΚ„** relation and the U vs. R relation can be established uniquely,
regardless of whether the cracked body is two-dimensional or three-dimensional.
(2) The crack propagation behavior may be controlled primarily by a local state of mechanical
variables. So the tfvs. £ relation for two-dimensional cracks can be applied to each point on
the three-dimensional crack front, and the effective stress intensity factor at each point on
the three-dimensional crack front determines the crack propagation behavior at that point.

Figure 1 shows a flow chart of the extended life prediction method for three-dimensional
cracks. If initial residual stress distribution is given, then the stress intensity factor for

Crack Shape, [Initial Residual Residual Stress\

Depth a, Length Stress Distribution I \ ίMeasurement /

Calculation of Stress

I
Intensities Kmax, Km in
Due to Applied Load tt Calculation of Stress Intensity
Kr Due to Residual Stress by
[Elastic Analysis tt
Effective Stress Ratio R
[=(K mi n+Kr)/(K m ax+Kr)]
U-R, M *
1(2-D Crack)
Estimation of Effective
Stress range Ratio n U

Estimation of M 9 t t Determined by Fatigue Crack Propagation

(=U x J O Experiment Using Two-Dimensional Through
da/dN-Jieff * Crack Specimens Without Residual Stresses.
](2-D Crack) Estimation i s Made a t Each Point or
da/dN, dc/dN Particular Points on Crack Front of Three-
(Change in Crack Shape) Dimensional Crack.

Fig. 1 A flow chart of the extended l i f e prediction method for three-dimensional cracks.
 235
the residual stress specimen at each point on the crack front, /fr, is calculated by an elastic
analysis. Effective stress ratio R at each point on the crack front is then evaluated by
superposing the stress intensity factor due to the cyclic applied stress on that due to the
residual stress:
R = ( & l n + Κ Γ ) / { Κ ^ + £.) -.(I)
In this equation L·^ and &,i„ are the maximum and the minimum value of the stress intensity
factor due to the applied load, and are allowed to have negative values. The stress intensity
factor range ΔΚ is expressed by the following equation.
e,,
ΔΚ - Km** — Km\n (2)
The V vs. R relation of the material is obtained from two-dimensional crack propagation
experiments with plates having no initial residual stresses. The U v s . £ relation allows us to
estimate the value of U from R values of the specimen with residual stresses. Then the
effective stress intensity factor range άΚ9±± is evaluated as the U value multiplied by the ΔΚ
value. The da/dN vs. M 9 t t relation is also obtained from the crack propagation experiments
with plates having no initial residual stresses, and can be used to estimate da/dN.

In the stage II crack propagation regime it has been reported that U is a function of R (Katoh
e t a h , 1982) and is little affected by M or AL«. If U is a function of M or A L « as well
as R, this function can be employed for evaluating the U value.

In the present paper the cases where the crack is propagated from tensile residual stress
fields are treated, and accordingly, it may be plausible that the elastic contact of crack
surfaces demonstrated by Mukai e t ai.(1987) does not occur.

3. EVALUATION OF STRESS INTENSITY FACTOR

The stress intensity factors for semi-elliptical surface cracks due to applied loads of the
tensile mode and the bending mode were calculated by employing the Newman-Raju formula
(Newman,Jr. e t a l . 1981, Fett, 1987). The stress intensity factors due to residual stresses
were calculated by employing the influence function method proposed by Shiratori e t a l .
(1986).

4. EXPERIMENTAL PROCEDURE

The material used in the present experiments was a rolled steel plate for welded structure,
SM41B, whose chemical composition and mechanical properties are shown in Tables 1 and 2.

Three kinds of specimen configurations shown in Fig. 2 were used in the experiments. The
configuration in Fig. 2 (a) was employed in the experiment for a two-dimensional through crack.
The configurations shown in Fig. 2 (b) and (c) were employed in the experiments of tensile
mode loading without and with residual stresses for three-dimensional surface cracks. The
configuration in Fig. 2 (b) was also employed in the experiment of four-points bending loading.
Residual stress was introduced by electron beam welding melt-run on a plate with thickness of
15mm, and the specimens having the configuration of Fig. 2 (c) were machined out of this plate.
An X-ray or magnetic type instrument was employed for measurements of the initial residual
stresses. Electric polishing was conducted on areas of the specimen surface prior to the
measurement. An example of the residual stress measured is shown in Fig. 3. An initial notch
was introduced in these specimens as a crack starter by means of the electric discharge
machining.
Table 2 Mechanical properties
Table 1 Chemical composition
(wt.%) Yield Tensile Elon-
Material stress stress gation
Material C S i M n P S MPa MPa %
SH41B 0.15 0.23 1.15 0.017 0.008 SM41B 314 471 29
236

(a) Non-residual stress specimen 1 I I I I

r - I I i
with a two-dimensional crack _CTo=200MPa S"
β
-x.
\ H
6 O

ώ^-—Φ^ φ ω
in
to
Ϊ 0
(b) Non-residual stress specimen with tn \ T

a three-dimensional surface crack

— 9-
m
/ \ _J
D
■o
w

or
JL\ /
\ Ih
-jnr£r^iiiiiiiimM&M-/immiii»444w
b = 25mm Ί
- 1 I I I l I I I I _J
-l o
(c) Residual stress specimen with x/b
a three-dimensional surface crack
Fig. 3 An example of measured
Fig. 2 Specimen configurations residual stress
Crack propagation experiments for two-dimensional through cracks and three-dimensional surface
cracks were conducted under load-controlled conditions by using electro-hydraulic servo testing
machines. The crack length of two-dimensional through cracks and the front-surface crack
length of three-dimensional surface cracks were measured by a traveling microscope with a
magnification of X200. The crack depth was measured from beach marks introduced during the
test on the fracture surfaces.

The measurements of the effective stress range ratio U were made by means of the unloading
elastic compliance method. The displacement of a specimen for this purpose was measured by a
strain gauge attached on the specimen surface across the crack mouth for the two-dimensional
through crack. To determine the U values of the surface crack at the deepest point and at the
front specimen surface, strain gauges were attached on the back surface and on the front
surface across the crack, respectively.

5. RESULTS AND DISCUSSION

Crack propagation experiments were conducted for two-dimensional through cracks and three-
dimensional surface cracks. The results for three-dimensional surface cracks were compared
with the results predicted by the proposed life prediction method for three-dimensional cracks.
In this prediction the crack was assumed to keep a semi-elliptical shape, and the method was
applied only to the deepest point and the front surface points on the crack to predict the
behavior of a and c.

Figure 4 shows the experimental relationships of crack propagation rate da/dN expressed in
terms of stress intensity factor ΔΚ and effective stress intensity factor ΔΚ**Χ. Circular
symbols in the figure show the results for the two-dimensional through cracks, while square and
triangular symbols show the results for the three-dimensional surface cracks. In each case
solid symbols show da/dN plotted against ΔΚ, and open symbols show da/dN plotted against Δ Κ Μ .
A single-valued relation is observed in Fig. 4 between da/dN and ΔΚ***, regardless of whether
the cracks are two-dimensional or three-dimensional. The solid line indicates a regression
line, expressed by the following equation, which was calculated by applying the least squares
method to the results of the two-dimensional cracks.
 237

10" Ί I I i i i 1 1—i i i i i y
ΔΚ AKeff

CCP Δσ = 8 0 MPa
R = 0. 0
SFC Δσ = 1 8 8 MPa ■ D (Surface)
10" R = -0. 5
A Δ (Depth)

o
u 10- 7

10"

■o

10"

d a / d N = 2.32X10-" (AKerr) 2· 42

10' -10 I I I I I I I I I J I I I I I I I
10 100
ΔΚ , AKeff MPa\/m

Fig. 4 The relation of da/dN vs. ΔΚ and M«,**

rfa/dV=2.32xlO- (4Äre«)2·42
11
...(3)
Figure 5 shows a relation between U and R for the two-dimensional cracks. The solid curve is a
regression one calculated by the least squares method and is expressed by the following
equation.
U= (1.38-0.839^+0.0828/F)- 1 (for £<0.48) ,..
0=1.0 (for Afc0.48) '" w
Equations (3) and (4) were employed in predicting the crack propagation behavior of the three-
dimensional surface cracks.

5?
·> 0.2

_J I I I I I L_
-1 0 0.6
Stress ratio R

Fig. 5 The relation of ί/vs. R

238

Δ σ = 188 M P a

R = -0.5
20 1 Γ" Γ ™Ί Ί 1
Depth Half length
£ r Experiment a c -
E 1 (with residual stress) Δ O
16hΓ Experiment
D
L (without residual stress)
1 o Prediction /
fO 1 2 0

L o
r c&/ residual stress p-'vX
c
<u

u
m without J
residual stress Ί
O
1 1 1 1 1 1 1

8 12 16
Cycles N x10
Fig. 6 Experimental and Predicted crack propagation behavior

Figure 6 shows the experimental and predicted behaviors of surface cracks in plates with and
without residual stresses under tensile loadings. Symbols " Δ " and " O " in this figure show
experimental results of the crack depth a and the half crack length c on the front surface with
residual stresses, while symbols " V " and " D " illustrate a and c without residual stresses.
It is found that da/dN in the case with residual stresses is accelerated as compared with ones
in the case without residual stresses because of the presence of the tensile residual stresses
in the central portion of the plate. The solid curves show the predicted behavior of a and the
broken curves show the predicted behavior of c. It is found that the predicted behaviors are
in good agreement with the experimental results both with and without residual stresses, in
particular when a is smaller than 6mm.

Figures 7 and 8 show the variations of the experimental and predicted crack shapes in the case
without and with residual stresses, respectively. In Fig. 7 good agreement is seen between the
experimental and predicted results, while in Fig. 8 fair agreement is obtained between the

(a) Experimental (a) Experimental

10 ηΐθ

J
o
-25 25 (mm) -25 25 (mm)
(b) Predicted (b) Predicted
Fig, 7 The crack shapes in specimen Fig. 8 The crack shapes in specimen
without residual stresses with residual stresses under
under tensile loadings. tensile loadings.
 239

25 (mm)
(b) Predicted

Fig. 9 The crack shapes in specimen without residual stresses

under 4-point bending.

experimental and predicted results. Figure 9 shows the experimental and the predicted crack
shapes in the plate without residual stresses under four-point bending loading. It is found
that the predictions are in good agreement with the experimental results.

6. CONCLUSIONS

The life prediction method for two-dimensional cracks was extended to the three-dimensional
cases. The three-dimensional crack propagation experiments showed that the present life
prediction method was valid for three-dimensional surface crack in the cases with and without
residual stresses.

ACKNOWLEDGEMENTS

The authors would like to thank Mr. Y. Iseki and Mr. M. Togami for their help in conducting the
experiments and the simulations.

REFERENCES

Fett, T. (1987). Int. J. Frac, 33, R47-R50.

Glinka G. (1979). In: ASTM STP Ml pp. 198-214.
Katoh, A., M. Kurihara and M. Kawahara (1982). J. Soc. Naval Architects Jpn., 153, 336-343.
Mukai, Y., M. Murata and E. Kim (1987). Quarterly J. Jpn. folding S o c , 5-2, 269-272.
Nihei, K., Ono and T. Tsunenari (1982). J. Soc. Naval Architects Jpn., 152, 390-396.
Nelson D. (1982). In: ASTM STP 776 pp. 172-194
Newman J. Jr. and I. S. Raju (1981). Eng. Frac. Mech., 15-1,2, 185-192.
Ohji, K., Kubo, M. Tsuji, H. Ogawa and K. Sakurada (1987). Trans. Jpn. Soc. Mech. Eng.,
A53-492, 1516-1524.
Parker, A. P. (1982). In: ASTM STP 776 pp. 13-31
Shiratori, M. , T. Miyoshi, and K. Tanikawa (1986). Trans. Jpn. Soc. Mech. Eng., A52-474, 390-
398.
Todoroki A. and H. Kobayashi (1989). In: Proc. of ICRS 2 (G. Beck, S.Denis and A. Simon, ed.),
pp.933-938. Elsevier Applied Science, London.
WS6d6

FATIGUE LIFE PREDICTION OF CIRCUMFERENTIALLY NOTCHED

COMPONENT BASED ON ELASTIC-PLASTIC FRACTURE MECHANICS

K.HATANAKA, T.FUJIMITSU and J.OMORI

Department of Mechanical Engineering, Yamaguchi University,

Ube City, 755 Japan

ABSTRACT

The elastic-plastic fracture mechanics parameters for the three dimensional

surface and circumferential cracks generated in the circumferentially
grooved cylinder component were analyzed from the viewpoint of engineering.
Then, fatigue life spent during crack growth was estimated for the bluntly
and acutely notched cylindrical components. Consequently, it was found that
the crack propagation life of the notched cylinder component was
successfully predicted by analyzing the extension of the semielliptical
surface crack and the circumferential crack based on the proposed method.

KEYWORDS

Fatigue life prediction; circumferentially notched component; elastic-

plastic fracture mechanics; semielliptical crack; circumferential crack.

INTRODUCTION

In general, the great proportion of fatigue life is occupied by the crack

growth process in the notched component. The analysis of the fatigue crack
growth, therefore, are greatly significant from both the academic and
practical viewpoints in the notched components. Nevertheless, the problem
on surface fatigue crack growing in the field where the stress/strain
gradients are developed remains unsolved at present. The present study,
therefore, aims to analyze the growth of the three dimensional surface
crack and circumferential crack in the grooved cylinder components with the
notch root radii of R=3 and 0.3mm.

MATERIAL AND TEST PROCEDURES

JIS S35C medium carbon steel was used in the present study. This material
was heated for 30 minutes at 865 °C, and then air-cooled. The heat-treated
material was machined into the circumferentially notched cylinder specimens
with the notch radii of R=3 and 0.3mm. Their stress concentration factors
241
242

Fig.l. The schema of the semielliptical surface crack

calculated elastically by the finite element method are 1.61 and 4.44,
respectively.

Push-pull fatigue tests were performed under axial load-controlled

condition. In these tests, the stress ratio was maintained at -1.0 during
the test.

Plastic replica films were removed from the specimen surface at proper
intervals during fatigue tests. Then, the life spent before the crack
initiation was measured, which was defined as the number of cycles required
for the surface crack to grow to about 50 Urn in size.

The displacement between the two points prepared on the both sides of the
notch was measured by means of the differential transformer. Then, the
closure point of the circumferential crack was determined from the
displacement and load responses described on a X-Y recorder.

ANALYSIS

F.E.M. analysis

The elastic-plastic F.E.M. analysis was performed for the circumferentially

grooved components, using the Yamada's method which is based on an
incremental strain theory connecting with the Mises yield criterion. The
details were given in the earlier paper (Hatanaka et al., 1989).

The stress-strain response was calculated at the notch root in the

monotonous tensile mode through the F.E.M. analysis, where the cyclic
stress-strain response was introduced as the basic material property. The
cyclic stress-strain hysteresis loop was obtained at the notch root by
scaling this up to double size.

Estimation of cyclic J-integral range

Figure 1 shows the schema of the semielliptical surface crack extending in

the cross section at the notch root of the specimen. The cyclic J-integral
ranges for the surface crack at the points, A and C in Fig.l, which are
denoted as A j ^ and A J Q , are derived as follows,
 243

Δ JA = 2 T T F A 2 c { A W e A + f(n)AW p A } (1)
and
Δ J c = 2 T T F C 2 c { A W e C + f(n)AW p C } (2)

, where c is half the crack length on the specimen surface ; F^ and F Q are
the geometrical correction factors for the stress intensity factor at the
points, A and C; A W ^ and A W p, and AW » and AW n are the elastic and
plastic strain energy densities, which are determined from the stress-
strain hysteresis loops described at the points, A and C during strain
cycling (Hatanaka et al. , 1989, Hatanaka £t_ a]^., 1988). The cyclic stress
and strain responses were calculated at the corresponding points at the
notch root containing no cracks by the F.E.M., and then, the respective
hysteresis loops were determined in the present study. The shape of the
semielliptical surface crack was determined from assuming that the crack
grew so that the requirement of AJ^= AJ^ was fulfilled (Hatanaka _et_ al.,
1989).

We assumed that the circumferential crack was equivalent to the

circumferential crack with 0 = Qf+ a' ' in depth generated in the smooth
cylindrical specimen with diameter, r, where a' is the notch depth and α τ '
is the crack depth at the notch root. The J-integral range for such a
circumferential crack is evaluated by the following equation,

AJ = 2TJF2 a {AW e + f(n) AW p } (3)

, where F is the geometrical correction factor of the stress intensity

factor for the circumferential crack contained in the smooth specimen (Tada
et al. , 1985) ; AW and AW are the elastic and plastic strain energy
densities determined from the cyclic stress-strain response of the smooth
specimen.

By the way, a crack closure occurs in the circumferential crack,

specifically when it extends to fairly large size. At that time, the
elastic and plastic strain energy densities were determined taking account
of the crack closure.

Prediction of Crack Growth Life

The following equation has been obtained for the crack initiation life, N·,
of the smooth specimen of the normalized S35C medium carbon steel
(Hatanaka, 1990),

( Δ ε ρ ) Ν, ° · 5 2 6 = 10 - ° · 3 9 8 (4)

The crack initiation life of the notched specimen is assessed by

substituting the equivalent plastic strain range, Δε e q , for the plastic
strain range, Δε , in eq.(4), where Δε ec* is calculated at the notch root
by the F.E.M. in the way stated before.

The relationships between crack growth rate, da/dN, and cyclic J-integral
range, AJ, are expressed for the semielliptical surface crack in the smooth
specimen and the large through-thickness crack of the center cracked plate
specimen as follows,
244

ιο(
0
| — ι — ι ι ι ιιιιι 1—ι ι ι ιιιιι τ|
10 I—i—i i i IIH| 1—ττττττη
Notch root radius R=3 mm Ε Notch root radius R=0.3 mm 3

10
F
σ
a
>
~3
10
<
ω
10
σ
*-
~σ 10 E Analyses:
σ» Circumferential crack
Analyses: α>
:AJ
-Variation of Aspect ratio-^ c Semielliptical surface crack
I is not considered ~D 10 Δϋι
-:Variation of Aspect ratio Δϋ^
I is considered I O :Maximum pointy
10" 10 i i i i i ml i i i i i nil ι

10' 10' 10* 10' 10' 10°

Crack depth a.m.xlO" 6 Crack depth a.m.xlO" 6

( a ) R=3mm-notched specimen (b) R=0.3mm-notched specimen

Fig.2. The variations of A J w i t h t h e c r a c k e x t e n s i o n

d a / dN = 10 ~ 3 * 5 1 A J 1
· 3 5
(5)
and
2 70 7 6
dQ / dN = 10 ~ - AJ ^ (6)

The life spent during the growth of the semielliptical surface crack is
assessed by introducing AJ calculated for the semielliptical surface crack
generated at the notch root into eqs.(5) and (6), and then by integrating
these equations as follows,

ra r 1
1 3 5
N -- N.
1 = ( ij) · da (7)
c a 10 - 3 51
i
and
fac 1
N -- Nj
1 = ( 4J) 1·76 da (8)
c 10 - 2 70
a-,·
, where N. and N are the number of cycles at which the crack attains to
the size defined as the crack initiation, a.^ and changes its shape from the
semielliptical to the circumferential at a c in depth, at the notch root.

The life spent during the growth of the circumferential crack is assessed
by introducing A J for the circumferential crack into eq.(6), and then, by
integrating this equation as follows,

1
Nf - N c ( A j) ^ 7 6 da (9)
-2.70

, where N^ is the number of the cycles required before the specimen

finally fails at 0^ in the crack depth. Incidentally, the crack closure was
taken into account for the estimation of AJ for the circumferential crack.
 245

Number of strain cycles N

Fig.3. Crack initiation and final failure lives predicted

for the notched specimen with RÄ3mm

RESULTS

Figures 2 (a) and (b) show the variations of the cyclic J-integral range,
A J calculated by eqs.(l), (2) and (3) with the crack extension in the
notched specimens of R=3 and 0.3mm, where ΔJ and Δ J are evaluated from
the equivalent and axial stress-strain responses calculated at the notch.
According to Fig.2 (a), the value of AJ for the semielliptical surface
crack increases monotonously as the crack extends. Meanwhile, the value of
A J for the semielliptical surface crack initially increases and then
decreases through the maximum point with increase in the crack depth in
Fig.2 (b). Such a AJ-CI relationship is induced by the stress and strain
gradients greatly developed around the notch root in the notched specimen
with R=0.3mm.

The cyclic J integral range for the circumferential crack increases

monotonously with the crack extension. It is considered that the value of J
integral range must monotonously increase with the crack extension so that
the crack generated at the notch root propagates without reducing its
growth rate. Then, we assumed that the crack generated in the component
with the acute notch such as R=0.3mm changes its shape from the
semielliptical to the circumferential at the maximum point on the Δ J-a
curve for the semielliptical surface crack in the crack extension process.
After the change in the crack shape, the circumferential crack grows to
final failure of the specimen. Incidentally, the crack depth estimated in
this way agreed quite well with the experimental data.

The calculated fatigue lives of the notched specimens with R=3 and 0.3mm
are compared with the experimental data in Figs. 3 and 4. The small open
and large solid circles show the experimental data on the crack initiation
and final failure lives, respectively.

The calculated life for the crack initiation is in quite good agreement
with the test data in Fig.3. Furthermore, the final failure life calculated
using the dd/dN- Δ J relationship of the long through thickness crack gives
the better prediction than the one based on the crack growth law for the
surface crack of the smooth specimen in this figure. Meanwhile, the
calculation on the crack initiation life predicts the shorter life than the
experiments in the lower stress range in Fig.4. The final failure life is
hardly influenced by this error, since most proportion of the fatigue life
is spent by crack growth process in such an acutely notched component. The
246
α>0_ 500 1 1 ΙΙΙΙΙΙΙ 1 1 1111111 1 1 11 Mill 1 1 ΙΙΙΙΙΙΙ 1 1 ΙΙΙΙΙΙΙ 1 I ΙΙΙΙΙΙ
"5^.400 1 ' Notch root radius R=0.3 mm"
csq a>ce· | | |
ο.\ 300 -[ \ 1N \ l Experiment:
o:Ni
<η < 200
\ l\ \ >
\ \\ 1
1 O :Nc
\ [s \ ·*«

"5 100 _h—'Analyses:

Ni for crack initiation
Ε -He for circumferential crack
_
ο
2 50
- Nf for failure
i i uiiiil i i mini ι ι mini ι ι nun! ι ι min
_
1 1 llllll

10'
10* \οό 10" 10°
Number of strain cycles N
Fig.4. Crack initiation, crack propagation and final
failure lives predicted for the notched specimen
with R=0.3mm

final failure life, therefore, is successfully predicted through the

proposed analysis, as shown in this figure.

CONCLUSIONS

The fatigue life of the circumferentially grooved components with notch

root radii, R=3 and 0.3mm was calculated based on the finite element
stress-strain analysis and the elastic-plastic fracture mechanics.

The fatigue crack propagation life for bluntly notched component was
successfully predicted by analyzing the extension of the semielliptical
surface crack. Meanwhile, the life for the acutely notched specimen was
satisfactorily calculated by adding the number of cycles required for the
semielliptical surface crack to reach the circumferential crack and the
number of cycles required for the circumferential crack to grow to the
final failure.

The crack initiation life is also calculated by combining the Δε - Ν·

relationship of the smooth specimen and the F.E.M. analysis of the notched
components. Then, the final failure lives of the notched components are
satisfactorily assessed by adding the crack initiation life and the crack
propagation life calculated through the proposed analysis.

REFERENCES

Hatanaka, K., T. Fujimitsu and S. Shiraishi (1989). An analysis of surface

crack growth in circumferentially grooved components under low-cycle
fatigue. JSME International Journal, Ser.I, 32, No.2, 245-255.
Hatanaka, K. and T. Fujimitsu (1988). Growth of small cracks and an
evaluation of low cycle fatigue life. ASTM STP, 942, 257-280.
Hatanaka, K., T. Fujimitsu and S. Shiraishi (1989). An analysis of surface
crack growth in a circumferentially notched specimen low-cycle fatigued.
Trans. Jpn. Soc. Mech. Ens., 55, A, 681-688.
Tada, H., P.C. Paris and G.R. Irwin (1985). The stress analysis of cracks
handbook, Second edition. Paris Production Incorporated, 27.1a.
Hatanaka, K. (1990). Cyclic stress-strain response and low-cycle fatigue
life in metallic materials. JSME International Journal, Ser.I, 33,
No.l, 13-25.
WS6d7

A CUMULATIVE FATIGUE DAMAGE CONSTITUTIVE EQUATION AND ITS

APPLICATION TO LIFE PREDICTION

WEI HUA TAI

Department of Mathematics & Mechanics, University of Science and

Technology Beijing, Beijing 100083, People's Republic of China

ABSTRACT

A cumulative damage constitutive relation for low-cycle fatigue is

proposed in this paper based on continuum damage theory. The relative
experiments for low-carbon steel #20 are done with the smooth tensile bar
specimens, where the surface plastic replicas and optical microscope
techniquess are applied to determine the basic microcrack behaviors, and
experimental damage evoluion curves are obtained· The results show that
there has a qualitative agreement existing between the theoretical results
and the experimental ones·

KEYWORDS

Cumulative fatigue damage, low-cycle fatigue, life prediction, short

cracks·

INTRODUCTION

Fatigue failure is due to a crack having grown to a critical size and

remaining ligament not having sufficient strength to sustain the next
cycle of load. It has been shown that in the machine components which do
not contain inherent defects and operate at stress levels close to the
fatigue limit most of their lifetime is spent in the initiation and slow
growth stages of microcracks, and the microcracks and the fatigue damage
play a more important role in fatigue failure of the machine components.
For this reason, great interests have being shown in studying behaviors of
the microcracks, small cracks and cumulative fatigue damage(Miller et a h ,
1981, Lemaitre & Plumtree, 1979, Lemaitre,1984, Hua & Socie, 1984).

In this paper, a cumulative damage constitutive relation for low-cycle

fatigue is proposed based on continuum damage theory and is applied to
life prediction. Some experimental results for the cumulative fatigue
damage evolution are also reported.

247
248

THE CUMULATIVE FATIGUE DAMAGE MODEL

Damage Variables

Lemaitre and Plumtree(1979) applied continuum damage mechanics priciples

to quantitatively describe the evolution of damage in material subjected
to cyclic straining, and expressed the damage D as follows:
i/c i+p;
Y
Dl-l-a-H/NcK (1)
where D is the damage variable which represents the damage occurring after
N cycles, Nc is the number of cycles to produce a critical value of
damage, Dc, which corresponds to the initaition of a dominant macrocrack ,
and p is a damage coefficient· On the other hand, the damage variable D
could be defined by the cracked area(Lemaitre, 1984):

D 2 - I/A (2)

where A is the area of the microcracks and A is the original cross-section

area* Also, the damage D can expressed in terms of variation of elastic
modulus:

D3=l-E/E (3)

where E is the apparent modulus of the damaged material and E is the

modulus of the undamaged material·

Under cyclic loading condition, the damage value D may be determined

experimentally by the variation of stress amplitude <*6 or strain amplitude
46 (Lemaitre e_t al·, 1979):

D^I-ΔΟ/ΔΟ* (4)
or
m
Os-l-i*e/A?) (5)

for constant strain-fatigue or constant stress-fatigue, where m is a

material constant·

Here, the damage variable D is defined as line density of micro-cracks:

Λ
D=Zla{/n (6)
where n is the number of the small cracks per unit surface area and a
denotes the length of ith crack·
The Cumulative Damage Model

Lemaitre(1984) obtained the constitutive equation for fatigue damage by

integrating the corresponding static plastic damage evolution equation
over one cycle· It is reasonable mathematically, but is not physically,
because the fatigue damage is caused principally by microcracks even if in
ductile materials, while the plastic damage is caused mainly by micro-
voids, where the microcracks play a less important role.

In the present paper, the damage constitutive equation is expressed as

follows:

dD/dN~A-f(6»/o) ■2^rm¥X— *» (7)

 249
where
f(om/6) = |(l+^)+3(l-2^)(6m/6)
K'
A~ ZESO * s a m a t e r i a l constant, n' is the cycle hardening exponent ( ^6=
ΚΆε"), vis the Poisson's ratio, *Sp is effective plastic strain amplitude,
and 6m/ό is the stress triaxiality. For one-dimensional cyclic loading we
have

dD/dN=B-^£pn/+l · D (8)

Integrating eqn.(8) under the following condition

N=No«-*· D=Do and N=Nc«*-*-D=Dc

the damage evolution equation may be changed into

dD/dN=C-D/(Nc-N0) (9)

in which C=ln(Dc/Do)

The fatigue damage equation then is

D=Do-exp{C-(N-No)/(Nc-No)} (10)

EXPERIMENTAL RESULTS

Materials and Specimens

The material used in this study was a low-carbon steel #20, The chemical
compositions and the static mechanical properties are listed in Table 1.

Table 1. Chemical compositions and mechanical properties

S Chemical composition Mechanical properties !

! C ! Mn ! Si ! P ! S oy(MPa)! 6b(MPa)! E(GPa)! T.E.(%)!

! 0.201 0.65! 0.24J0.03510.025 279 ! 468 1 205 ! 26 !

The smooth cylindrical fatigue specimens with 140 mm in length and a

nominal diameter of 8 mm were used in experiments.

Experimental Procedure

The tests were finished at room temperature under strain control by using
a 500KN MTS880 material testing machine. Axial strain was controlled by an
extensometer with a gauge length of 25 mm connected with the central
process unit. More than ten total strain amplitudes, ^Εχ /2, ranging from
0.1% to 5% were imposed. The fatigue damage D is measured only from the
specimens under total strain amplitudes of 0.3%, 0.5%, 1.5% and 2.5%
respectively.

After loading to a prescribed cycle N, the specimen was loaded to the

maximum stress, then the extensometer was removed and acetate replicating
papers were pasted over the gauge length. The dried replicas were then
examined under an optical microscope and the tipical microphotographes
250
were taken, from which the density and length of microcrack can be
measured and the damage D can be obtained according to eqn.(6).

On the other hand, the hysteresis loops and relative data corresponding to
every cycle are all recorded, from which the elastic modulus E and the
stress amplitude Δό can be plotted as function of cycle number N, and
the damage D3 and D^. could be determined using eqns.O) and (4).

Experimental Results

Figure 1 shows the measured fatigue damage D using eqn.(6) for four strain
amplitudes at different life fraction N/Nc, togather with the calculated D
r^N/Nc curves from eqn.(10). It is easy to see that the theoretical curves
agree qualitatively with the experimental data.

Examining the measured damage D 3 defined by eqn.O), it is found that the

fatigue damage D3 is approximately zero during the life of each specimen,
because the elastic modulus remains almost unchanged.

It is interesting that "negative damage" D^. is obtained using eqn.(4),

because the stress amplitude Δ6 increases with the cycle number in the
present tests. It is evident that the negative damage results from the
interaction of cyclic hardening and fatigue damage.

PCmmj L \3Wc-hl0)
X
x
=0.50%
1.0 • *i.so£ I 5.0
0 =2.50%
*
0.8
i *°
0.6 M 30

04 71 20

0.2 (.0
tyAZf)
0.0 n »1 «ai'iiit^n*!ÜL-J 1 -1 cto
0.+ 05 Q6 0.7 Q8 *9 »0 0*5 -3.0 -20 -10

Fig. 1. Fatigue damage evolution Fig. 2. Strain-control fatigue

curves for different Δ6ρ life curve

LIFE PREDICTION

Generally speaking, the fatigue life of a specimen consts of three parts,

they are microcrack initiation life Ni, microcrack growth life Nc and
macrocrack propagation life Np:

N=Ni+Nc+Np (11)

where Np can be predicted by the Paris formula, and Nc may be calculated

by the present fatigue damage model.

It is assumed that the microcrack grows to a macrocarck when damage D

 251
reaches its critical value Dc, then from eqn.(7) we have

(Nc-Ni)^t7+T^C· (12)

where C is a constant. This is similar to the Manson-Coffin equation·

Figure 2 shows the calculated strain-fatigue life curve from eqn.(12)

compared with the experimental data for steel #20· It is found that there
is an aggrement between the calculated life and the measured one.

For two-step cyclic loading, the above fatigue damage model can also give
a life prediction equation that is as the same as one discussed by Miller
and Ibrahim(1981).

DISCUSSIONS

Comparison of Fatigue Damage Model with Small Carck Model

Taking that damage D as an equivalent microcarck length a, where a may be

either length of a dominant carck or an average length of microcracks per
unit area, then the damage equation(7) is changed into

da/dN=Ao^eplnVa (13)

which i s as the same as that proposed by Solomon(1972). Also,

eqn.(4) can be written as

da/dN=Co· a ^ ' + , / ( 2 n ' + l ) (14)

which is similar to the Tomkins1 equation(1968).

As have discussed by Miller(1984), eqns.(13) and (14) agree the small

crack growth well.

Comparison of Fatigue Damage Model with Plastic Damage Model

The internal damage generated in materials are caused principally by

microdefects whatever under static loading or under cyclic loading. The
damaging processes are initiation, growth and coalescence of microdefects
and the critical damage state is the microdefect grows to a macrocrack
although the defects are in form of microvoids under ductile fracture
condition(Tai et_a^.t 1986) while the defects are in form of microcracks
under fatigue failure condition. This similarity between fatigue damage
and plastic damage may lead one to analyze the damage behavior
conveniently, as listed in Table 2.

Damage Measurements

The damage variables, defined by the cracked area, and by the crack line
density, and by the variation of elastic modulus, and by the variation of
stress and strain amplitudes, can all describe the damage behavior of
materials under cyclic loading condition, but it is not reasonable to
equate one to another. For example, we can not define the damage by the
cracked area while measure it according to eqn.(4) or eqn.(3). As shown in
the previous section, the damage D3 is almost zero and the damage D^. is
negative during the life of specimens, but the damage defined by the
cracked area and crack density do increase.
252
Table 2. Comparison of fatigue damage model with plastic damage model

fatigue damage plastic damage

microd efects

cycle number No strain (stress)

%>
1
\
Icrack initiation void initiation
Damaging
processes ciycle number N strain (stress)
h
crack growth | void growth

c:ycle number Nc strain (stress) £ c

crack coalescence void coalescence| |

-| macro
*

Damage crack line density void area fraction

Factors Atf, (Δ6), N om/ό, £p

Generation N=No-·—D=Do 6p=?o-*-^D=Do

CDM dD/D=A0*fp'n'"H dN dD/D=A-f(om/6)däp

Growth
D=Do-exp[Co(N-No)] D=Do·exp[C(6p-Üo)]

Critical criterion D=Dc criterion V ^ V j ^

f
state life (lfc-No)*£p =C ductility (ic-^o)f(om/6)=C

Damage microcrack length a microvoid radius R

Nucleation N=No—*-a=ao €p=?o<—^R=Ro

Micro- Growth da/a=Co*fp dN dR/R=C-exp(1.5om/6).d6p

Mechanics
Coalescence a/ao^ac/ao R/Ro=Rc/Ro

Critical
parameters *6p · Nc=C exp(1.5 6m/6)-^c=C

REFERENCES

Hua, C.T. & Socie, D . F . U 9 8 4 ) . Fati. Engng. Mater. Struct., 7, 165-179.

Lemaitre, J. & Plumtree, A.(1979). J. Engng. Mater. Techn., 101, 284-288.
Lemaitre, J.(1984). Nucl. Engng. Design, 80, 233-246.
Miller, K.J. & Ibrahim, M.F.E.(1981). Fati. Eng. Mater. Struct., 4, 263.
Solomon, H.D.(1972). J. Mater., 7, 299-306.
Tomkins, B.(1968). Phil. Magazine, 18, 1041-1066.
Tai, W.H. & Yang, B.X.(1986). Engng. Fract. Mech., 25, 377-384.
WS6e1

High Temperature Structural Design

fur Power Plant

Florian Schubert

Institute for Reactor Materials

- Research Center Julien -
5170 Jülich, FRG

ABSTRACT
Technical rules a n d structural design codes serve as a guide for designers, manufactures,
users and licensing authorities. The main idea of the rules is the limitation of stresses and
strains, strain rates and strain ranges, a s well as the number of operational cycles. By
fulfilling the proposed rules, failures s u c h as ductile or creep rupture, creep-fatigue failure,
excessive ratcheting and buckling strains, environmental attack a n d excessive growth of
flaws can be avoided. The design data for high temperature components are concerned with
the temperature and time dependent properties of the material. Allowable stresses and
deviatoric stresses, safety margin and geometrical factors require a minimal wall thickness to
guarantee to the lifetime. The exhaustion of a component is calculated using linear life-time
fraction rules for creep a n d fatigue.

In nuclear power plants for the different loading cases a detailed stress-strain analysis are
required including simplified inelastic analysis and finite element analysis. For metallic high
temperature components the methods for exclusion creep-rupture, creep-strain, creep-fatigue
exhaustion, creep ratcheting and buckling are discussed with the main emphasis on design
and construction rules for helium cooled high temperature reactor, gained as results of an
extended HTR-materials evaluation programme and the German "HTR-Design Criteria"
project / l , 2 / .

KEYWORDS

6.c High Temperature Reactors, Structural Design Codes

Introduction
High temperature components in fossile fired power plants with working pressures up to
300 bar and temperatures up to 650°C are designed by using quite simple rules s u c h as for
straigth tubes:

s = —^-f +Ci+C2 (1)

L z
2 (K/S) · v + p
s = required wallthickness;
Da = outer diameter;
p= dimensioning pressure, stress value;

253
254
s= safety margin;
v= welding margin;
Cj resp. C2 = wall thickness margin concerning fabrication tolerances resp. high
temperature corrosion

The rule for pipe bends is based on the required thickness "s v " of a straight pipe and takes
into account the lower membrane stress at the bend extrados via the coefficient B a .

sva = sv Ba (2)*

and the higher membrane stress at the bend intrados via the coefficient Bj

Svi = Sv Bj (3)

The coefficients Bj B a are given in the AD rule in dependence on the bend radius / 3 / . Table
1 summerized some dimensioning rules for internal pressurized cylindric components.

Code Dimensioning rule Welding margin Dimensioning Allowable

Da p / s time t stress

AD-Merkblätter 2 · o z ul · v + p v = 0,85- 1,00 > 100 000 h R m, t /1.5

= 0,80

TRD (2 ■ o z ul - p) v + 2p v = 0,80- 1,00 i 100 000 h Rm,t/1.0 |

or 200 000 h R m t/ l , l l nozzles

Rm.t/1.35 '
HTR- Rpi.o.t/i.o
Auslegungs- 2 · «zul + P ' ~ ^Dimensionin
g R t 2 , 3 / t / 1 · 25
kriterien Rm.t,T +15/1.0
R m . t . T + l ö K / 1. 0
BS 5500 2 · ozu\ v + p v « 1,0 i. 100 000 h Appendix k
* 250 000 h

ASME Section I 2 · o z ul v + 2 · p · y v= 1,0 treated 100 000 h

Power Boiler v = 0,0 untreated

ASME Section III

Nuclear Power Plant sRpi.o.t/LO
Components 2 · a z ul + p 100 000 h sRm.t/i.5
ASME Section VIII.2 SRm.t/1.25
ASME Section VIII. 1 v = 1,0 NDT proved 100 000 h
Pressure Vessel 2 · o 2 ul · v + 0,8 p v = 0,7 NDT unproved
2
API-RP 530 · Ozul' v + P v <= ? (not yet £ 20 000 h Rm.t/1.0
defined) έ 250 000 h

Comments plastic stress- ] =zallowable

u - mean value
distribution factor v min. value
y = 1 (1) = 0,4-0,7

Table 1: Survey on some dimensioning rules for internal pressurized cylindric

components
Although these procedures appear quite crude when judged against the present knowledge of
high temperature structural behaviour, they have nevertheless provided acceptable levels of
safety, reliability and cost.
For nuclear power plant for analysis a higher input on data and methods are used to ensure
safety and reliability for the different load cases. Where as it seams impossible to analyse a
complete plant. The practice is to divide the components into a number of component parts
which can be treated seperatly. This has been the practice for the Fast Breeder Reactor
"Superphenix" in France and the "THTR" in Germany. The different tests on procedures are
written down in the RCC-MR / 4 / and the draftl of KTA 3221 / 5 / .
 255
High Temperature Gas Cooled Reactor
In the FRG the regulation of the Nuclear Safety Committee (KTA) are used for the design of
power stations. The ongoing work on rules for design of HTR-components are based on
specifications that are orientated towards non-nuclear design rules, for example,the German
Technical Standards (DIN) [6] or the Pressure Vessel Association Codes of Practice (AD, TRD)
[7], [8]. Foreign codes a s ASME [9] or RCC-MR [10] are in part used as appropriate. Safety-
related requirements were formulated and the HTR integrity concept was established in
conformity with the special properties of a n HTR [11, 12].

The components are classified according to their function and their safety related significance
as follows:
HTR components with barrier and retention functions (fuel elements, reactor pressure vessel,
reactor containment); HTR components whose failure would impair the barrier function;
(reactor internals, s h u t down systems, residual heat removal system); HTR components
whose failure would result in an ingress of foreign matter into primary circuit (steam
generator, steam ducts, Heat exchanging components).

Metallic Components
Safety-related pressurized metallic components are the heat-exchanging units. Their failure
can lead to the penetration of water or process gases into the primary circuit. The mean
materials temperature of the steam generator parts is about 550°C in maximum, temperature
excursion u p to 700°C can occure under emergency conditions. In process heat facilities,
temperatures of u p to 950°C can occur in the hottest regions of the heat exchangers. The
time-dependent behaviour of the materials involved must therefore be taken into
consideration. Stress analysis methods are required which cannot be covered by elastic
approaches. First of all a systematic study of the types of failure and of the related material
behaviour is most important for the selection of design measures (Fig. 1).

reliable operation during lifetime by exclusion o(:

Creep/ Ratcheting, unadmissble rapid time

fatigue creep distortion, dependent
faiura ratcheting creep failure by
distortion defects

Measures:

n
Design of components as the base of component quality by

Selection of materials suitable constructive shaping

quantitative suitable detaäedspecification suitable

stress-strain analysis oftoadingcondHions I construction
evaluation methods
criteria

Li
Measures:
Quality assurance (QA)

Q
i/B ^

Fig. 1: Failure modes at high temperatures, aims and measures

The following three materials have been extensively qualified for HTR-components:
X20 CrMoV 12 1 (ferritic martensitic steel for main steam pipes)
XI0 NiCrAITi 32 20 (Alloy 800, austenitic iron-base alloy for hot-going components)
NiCr 23 Co 12 Mo (Alloy 617, nickel-base alloy for extreme application temperatures)

Data for construction and dimensioning

The required physical properties are given up to 1100°C in the data sheets. Using short term
tensile properties one should be aware, that at temperature higher t h a n 650°C, especially the
0,2 % yield strength becomes sensitively dependant on deformation rate.
256
For dimensioning, the admissible stress parameters has to be derived from creep-strain limits
or creep rupture strength. A scatterband evaluation of all datas help to define the mean and
minimal values in table 1.

time (hrs)
Fig. 2: Inter- and extrapolation of creep rupture strength of Alloy 617 by MCM-
method
In Fig. 2 the creep rupture strength of Alloy 617 is shown for the temperature range between
700°C and 1000°C. The drawn curves are mean isothermal values obtained by calculation
with the MCM-time-temperature parameter methods. The St-values of Alloy 617 for short
term, high stress levels are determined by the 1 % creep-strain limit, the longer term data are
produced by the creep rupture strength.

In order to define the allowable operation duration, both the exhaustion due to creep (DQ.)
and due to fatigue (DfJ must be estimated. For creep, a linear life time fraction rule is
proposed

D - Σ ti (4)
Cr
allow
with t^ = duration of a load level i and IfeUk^ = allowed time for the St-value of the load level
i. The fatigue exhaustion is also estimated with a linear accumulation rule.

= Σ ^ (5)
allow
with Nj = number of cycles at strain level Δ 6j and Nj a jj ow the allowed number of cycles.

These are derived from fatigue design curves, given for Alloy 617 in Fig. 3. The allowable
operation duration is than the sum of both exhaustion terms
D
Cr + D f — D ; which must be less or equal "1".
 257
4.0

10 1 102 103 104 105 106

Number of cycles
Fig. 3: LCF-design curves for Alloy 617

Design by analysis-methods
The integrity of nuclear components must be analysed with orientation on the operational
loadings, on up set and emergency conditions and on the corresponding failure modes. For
the high temperature metallic components inelastic consideration have to be performed. The
inelastic materials behaviour becomes more relevant with increasing temperature.
Temperature-time limit curves, the "creep cross over curves", were derived. These diagrams
are to use as follows. The duration of a load case is predefined on the abscissa; the curves
will then indicate the component temperature beyond which creep must be taken into
consideration (Fig. 4). In a good approximation time-independent characteristics can be
expected below this temperature level.

700
- t mm 2 t: X 10 NiCrAITi32 20 I

1 I: N i C r 23 Co 12 Mo

600 1η 1 || |||
p nffl
illll
ί 3· X 20 CrMnV 12 1

WIT"
^^ΐΓπ Tfflfl ^ mm
I

iffll TjTjjJ
1
ill]]
■2 500
Mill
Π IK 2
11111
111] ;
11ΙΐΙΙ
Q.
E Jill]
If?
Itl JJJJJI
400
Mill
fiK 1111]j|
tllljl
11111 j111|li
iff ^_ 1111|||
JJJJI
300
Illll Illll I 111111
10 υ 10« 10^ 10° 10 q 10 c 10 Ό
Time/h
Fig. 4: Creep cross over curves for the qualified materials

For the time temperature range above this creep cross over cuves, a mathematical description
of stress-strain-time behaviour for the different temperatures are necessary. The stationäre
258
creep strain is well modulated by Norton's creep law. For the inelastic analysis, isochronous
stress-strain curves are provide, which help to define or to fit a constitutive equation.

As a suitable starting point for engineering applications the life time fraction rules were taken
for defining the admissible operation time. Modifications were proposed in connection with
stresses changing in time (e.g. relaxation processes) to better comply with the real behaviour
of materials. The investigations were based on LCF-hold time tests at NiCr 23 Co 12 Mo. The
tests were carried out at 950 C. The typical stress course during a single cycle is shown in
Fig. 5. By using the linear life time fraction rule (damage accumulation rule) in the form (6) it
was observed that the creep damage part was overestimated. Especially the peak stresses at
the beginning of the cycle contribute to the damage integral in an unrealistic manner. The
peak stresses are connected with very high strain rates which are much higher than the
strain rates under stationary creep conditions at the same stress level. So the first part of the
relaxation curve in Fig. 4 is connected mainly with plastic deformation effects. Creep damage
development in a time increment dt is not so strong as the current stress level suggests.

D = N · J + (6)
tf(a) Nf
0
tj_j = hold time of the cycle, N = number of cycles, Nf = number of cycles to failure (same
strain range, no hold time), tf(a) = rupture time for stress σ

The following three proposals try to reduce the influence of the first part of the relaxation
curve:
Replace Jdt/tf(a) bei tpj/tf (cr eq ), where oec. is a mean stress during the cycle. So the
influence of the peak stress can be reduced.
Start the integration at a time value tL (Fig. 5)
Introduce a weight factor c(t) with 0 < c(t) < 1 inside the integral: Jc(t) · dt/tf(a).
Especially at the very beginning of a cycle c(t) can be chosen clearly smaller than one.

Fig. 5: Stress course during a LCF-cycle with hold time tjj

In ASME CC N-47 creep ratcheting is incorporated to treat plastic ratcheting. But if at very
high temperatures the average wall temperatures during the cycle are always in the creep
regime, creep ratcheting must be seen as an independent phenomenon. The yield strength
loses here its meaning, no "elastic" regime exists without ratcheting. Studies for two bar
models with a nonlinear elastic-visco constitutive equation were carried out. Finite element
analysis for tubes was undertaken and compared with experiments on NiCr23Mol2Co tubes
at 950 °C. The estimations of the creep ratcheting were partly very conservative whilst the
FE-calculations were very close to the experimental findings [13], [14]. Nevertheless it is
recommended to use simple two bar models for analysing systematically over the whole
temperature range the ratcheting effect. Constitutive equations should be used which take
into account simultanously elasto-plastic behaviour and creep.
 259
For the treatment of creep buckling of tubes Hoffs procedure [15] was investigated.
Experiments were carried out on relevant tube geometries at 950 °C and pressures in the
range of 40 bars. The experimental buckling times were compared with calculated values t c r
according to the equation [7], in which creep can be characterised by a Norton law [15, 16,
17].

tCr 1 +C*X 1 +D*X

- = ln{1/X0} + 4rC/(C-D)-ln{ ?-} - ±D/ (C-D) Ί η { ?-} (7)
t ° C D
with
x~ = 2-V3-a -R/h (R=tube radius, h=wall thickness, a n =initial out of
° ° roundness=6R/R) °

1 3 ( n + D/2 p-R n
R 2

- = 4-k'rr( ) ·· ( ) · (-) (p=outer pressure,

τ 4 h h k,n=creep law parameter)
(n-1)(n-2) 36(n-3)(n-4) (n-1)(n-2) 36(n-3)(n-4)
c = .{1_ T } D= .{1+ T 1
18 25(n-1) (n-2) 18 25(n-1) (n-2)

By using a load safety factor of 1.5 or a time safety factor of 10 all calculated values had
enough distance from the measured collapse times.

Design on the base of fracture mechanis materials parameters shall not be carried out. But
fracture mechanics is a presupposition for the application of the leak before break criteria. A
survey on the fracture mechanics work is given in [18].

FINAL REMARKS
A five-volume final report was compiled for structural design methodology. At the workshop,
held in early 1989 the results had been presented. The proceedings [1] provide a good survey
of the HTR situation and are the basis for the KTA rules:
metallic components (KTA 3221), safety-related requirements for the design of prestressed,
concrete reactor pressure vessels for HTR systems (KTA 3231), ceramic internals in HTR
pressure vessels (KTA 3232).

REFERENCES
[1] "Structural Design Criteria for HTR", Proceedings of the Workshop Jan. 31 /Febr. 1,
1989, ed. G. Breitbach, F. Schubert, H. Nickel, Jül-Conf-71 (April 1989)
[2] F. Schubert, E. Bodmann, "Grundsätze der Auslegung von metallischen Bauteilen
des Hochtemperatur-Reaktors" in "Werkstoffverhalten und Bauteilbemessung"
DGM-Verlag, ed. E. Macherauch 1986, S. 233
[3] AD-Merkblätter Serie B, Ausgabe Juni 1986
[4] "Design and Construction Rules for Mechanical Components of FBR-Nuclear Istands
RCC-MR", Section I - Class 1 Components, June 1985
[5] Regelvorhaben KTA 3221 "Metallische HTR-Komponenten", KTA-Geschäftsstelle
April 1989
[6] "Normen des Deutschen Instituts für Normung (DIN), published by "Deutsches
Institut für Normung e.V., Berlin"
[7] "AD-Merkblätter der Arbeitsgemeinschaft Druckbehälter (AD)",
published by "Vereinigung der Techn. Überwachungs-Vereine e.V., Essen"
[8] "Technische Regeln für Dampfkessel (TRD)"
published by "Vereinigung der Techn. Überwachungs-Vereine e.V., Essen"
[9] ASME Boiler and Pressure Vessel Code,
published by the American Society of Mechanical Engineers, New York
260
[10] Design and Construction Rules for Mechanical Components of Fast Breeder
Reactors, RCC-MR. Association francaise pour les regies de conception et de
construction des matöriels des chaudieres electro-nucleaires
[11] Nickel H. et al., Erarbeitung von Grundlagen zu einem Regelwerk über die
Auslegung von HTR-Komponenten für Anwendungstemperaturen oberhalb 800 °C,
(BMI-Vorhaben SR 191), Jül.-Spez.-248, März 1984
[13] Zottmaier R., Over H.H., Schubert F., Nickel H., Untersuchungen zum
Kriechratchetingverhalten von Rohrproben, Jül-2019, September 1985
[14] Breitbach G., Over H.H., Schubert F.
Experimentally Verified Creep Ratcheting Analysis, Sixth Int. Seminar on Inelastic
Analysis and Life Prediction in High-Temperature Environment, Paris, 24-25 August
1987
[15] Hoff N. J., Jahsman W. E., Nachbar W.
A Study of Creep Collapse of a Long Circular Cylindrical Shell Under Uniform
External Pressure. J. Aero/Space Science, 1959, 663-669
[16] Ahmed K., Breitbach G., Over H.H., Schubert F., Nickel H.
Theoretische und experimentelle Untersuchungen zum Kriechbeulen von Rohren
aus NiCr 23 Co 12 Mo,
Jül-2224, August 1988
[17] Breitbach G., Ahmed K., Schubert F., Nickel H., Creep collapse of tubes at high
temperatures under external pressure, 10th SMIRT, Anaheim, 1989
[18] Rödig M., Huthmann H., Hartnagel W.
Compilation of fatigue and creep crack growth data for Alloy 800 (X10NiCrAlTi32 20)
and Alloy 617 (NiCr23Col2Mo), obtained in the German HTR materials programme",
5th German Japanese Joint Seminar on reactor safety research, München 11.-
12.10.90
WS6e2

BENCHMARK PROJECT ON THE EVALUATION OF INELASTIC CONSTITUTIVE MODELS

AND FATIGUE-CREEP LIFE PREDICTION METHODS FOR 2.1/4Cr-lMo STEEL
AN APPLICATION OF FINITE ELEMENT IMPLEMENTATION

Subcommittee on Inelastic Analysis and Life Prediction

of High Temperature Materials,
The Society of Materials Science, Japan

Presented by Tatsuo Inoue

Department of Mechanical Engineering, Kowtow University
Sakyo-ku, Kyoto 606, Japan

ABSTRACT

This paper deals with the applicability of inelastic constitutive models to

finite element analysis and the evaluation of fatigue-creep life of notched
bars of 2.1/4Cr-lMo steel as the third phase of the benchmark project by the
Subcommittee on Inelastic Analysis and Life Prediction of High Temperature
Materials, JSMS. Eight types of constitutive models were employed to simu-
late the stress/strain distribution around the notch root, and fatigue-
creep lives for the notched bars were evaluated by eight types of life pre-
diction methods. The both analytical results were compared with the ex-
perimental data of strain concentration, and lives of crack initiation and
failure.

KEYWORDS

Inelastic constitutive equation; life prediction method; plasticity-creep

interaction; fatigue-creep interaction

Members of the Subcommittee are T. Inoue(Kyoto Univ., Chairman), K. Aoto

(Power Reactor and Nucl. Fuel Dev. Co., Secretary), K. Fujiyama(Toshiba
Co.,ibid), Y. Fukuda(Hitachi C o . , i b i d ) , T. I gari(Mitsubishi Heavy
Ind.,ibid), S. Imatani(Kyoto Inst. Tech.,ibid), S. Kishi(Toshiba Co.,ibid),
H. Koto (Mitsubishi Heavy Ind.,ibid), M. Miyahara(Sumitomo Metal Ind.,
ibid), Y. Niitsu(Tokyo Inst. Tech.,ibid), N. Ohno(Nagoya Univ.,ibid), M.
Okazaki (Nagaoka Univ. Tech.,ibid), M. Sakane (Ritsumeikan Univ.,ibid), A.
Suzuki(Ishikawajima Harima Heavy Ind.,ibid), Y. Takahashi(Central Res. Inst.
Elect. Power Ind.,ibid), K. Tamura (Kawasaki Heavy Ind.,ibid), T. Uno
(Toshiba Co.,ibid), F. Yoshida (Hiroshima Univ., ibid); Y. Asada (Tokyo
Univ.), T. Hiroe(Kumamoto Univ.), K. Kanazawa (National Res. Inst. Metals),
M. Kawai(Univ. Tsukuba), S. Kubo(0saka Univ.), K. Motoie (Hiroshima Denki
Inst. Tech.), S. Koue(Kawasaki Heavy Ind.), M. Mizumura (Nippon Steel Co.),
S. Murakami(Nagoya Univ.), K. Nagaki(Okayama U.), K. Nagato(Kawasaki Heavy
Ind.), T. Shimizu(Hitachi Co.), E. Tanaka(Nagoya Univ.), K. Tanaka(Tokyo
Metropolitan Inst, Tech.), K. Tokimasa(Sumitomo Metal Ind.), Y. Wada(Power
Reactor and Nucl. Fuel Dev. Co.), T. Yokobori(Tohoku U.),.
261
262
INTRODUCTION

The Subcommittee on Inelastic Analysis and Life Prediction of High Tempera-

ture Materials (members are listed in footnote) was organized in 1982 under
the sponsorship of the Committee on High Temperature Strength of Materials,
the Society of Material Science, Japan. The subcommittee has been perform-
ing a cooperative project consisting of the following two tasks: (A)
Evaluation of inelastic constitutive models relevant to the material
response under plasticity-creep interaction, and (B) examination of the life
prediction methods in fatigue-creep regime.

As the first step of above two tasks, the benchmark project had been or-
ganized to evaluate ten kinds of constitutive models by simulating inelastic
behavior in uniaxial stress state (Inoue et al.,1985, Inoue et al* , 1988a),
and to examine eight types of fatigue-creep life estimation methods (Inoue
et ai.,1988b) by use of 2.1/4Cr-lMo steel at 600°C . In the second phase of
the project, the models and the methods are applied to multiaxial stress
state of combined tension-torsion (Inoue et ai.,1991a, Inoue et al. 1991b).

The motivation of this third phase of the project arises from engineering
requirement that the schemes are to be used for practical design purposes:
Applicability of the inelastic constitutive models to finite element cal-
culation is examined by comparing the analytical stress/strain response near
notch root of the bar with experimental results, and fatigue-creep lives of
the specimen are evaluated by applying the life prediction methods.

MATERIAL, TEST SPECIMEN AND EXPERIMENTAL PROCEDURE

The material tested is normalized and tempered 2.1/4Cr-lMo steel (SA287,

GR.22), and is the same used in the first and second projects. Two types
of specimens are used as shown in Fig.l; one is round-notched with an elas-
tic stress concentration factor Kt of 1.5 and the other Is V-notched with Kt
of 3.0.

Axial strain at the notch root was measured by means of "Strain-Pecker", a

capacitance type extensometer for high temperature use. The strain-pecker
was spot-welded to the notch root of each specimen. Cyclic straining tests
were carried out by controlling the nominal strain 6 GL along 30mm gauge
length at 600°C, and local strain ε sp at the notch root with 0.5mm gauge
length are also measured.

30 = GL Strain pecker Strain pecker

E
V
# W0_5
&F

50
160

Kt = 1.5 Kt=3.0

Fig.l Shape and dimension of notched bar specimens.

 263
Crack initiation lives under cyclic axial loadings were detected by a direct
current potential drop technique, and failure lives were defined as the
cycles of 25% stress drop from saturation.

Table 1 illustrates the four loading patterns described below:

I . Creep loading under <J nom = 120 MPa, where o" nom indicates nominal
stress in the minimum cross section.
II . Fast-fast cyclic straining under h G L = 0 . 0 2 5 % / S in strain range of
Δ a GL=0.2%.
III .Slow-slow cyclic straining under h G L = 0 . 0 0 1 % / S in the same strain
range.
IV . Fast-fast cyclic straining with a tension hold-time of th=600s.

EXAMINED CONSTITUTIVE MODELS AND LIFE PREDICTION METHODS

The following eight types of inelastic constitutive models were applied to

finite element analysis to simulate the stress/strain distribution near the
notch root. They are (1)superposition model, or classical model, (2)
modified superposition model, (3)Chaboche model, (4)Miller model, (5)Krempl
model, (6)Bodner model, (7)Ohno-Murakami model and (8)endochronic model.
Some finite element codes were developed to utilize the unified constitutive
models (2)-(8), whereas the commercial codes were available for model (1).

Life prediction methods employed can be basically classified into two

categories; One includes the normal methods in which the material parameters
appearing in the equations are to be determined by the experimental data,
and the other way relys on the parameters calculated by the constitutive
modeling which uses fewer experimental data. The methods examined are
(l)linear damage rule, (2)strain range partitioning method, (3)Majumdar
method, (4)0stergren method, (5)Lemaitre-Plumtree-Chaboche method, (6)Bui
Quoc method and (7)Γ -plane method.

Table 1 Illustration of benchmark problems.

Problem Loading Pattern Condition Experiment Analysis

kno.. ; Creep
I ö n o m * 120 MPa - 200 h - 100 h

A
eQ l
i Fast-fast £ Q L = 0. 2 %
Π
Λ ΛA/ CGI = 0 . 0 2 5 %/s to rupture - N=10

[V V V
ε0. . Slow-slow A e G L = o. 2 %
m eGL = 0 . 0 0 1 %/s t o r u p t u r e - N=10

N/
Fast-fast with A e Q L = o. 2 %
IV EG L . tension hold
( έ 0 ι_ = 0 . 0 2 5 %/s to rupture - N=10
th = 600 s

I v V
264
RESULTS OF ANALYSIS AND EXPERIMENTS

Evaluation of Constitutive Models Figure 2 represents the nominal and lo-

cal creep curves at notch root measured by the extensometer (30mm G.L.) and
strain-pecker (0.5mm G.L.) respectively for Kt=1.5 and 3.0 [Problem I ].
Although the nominal creep strain does not differ between Kt=1.5 and 3.0,
local strain accumulation of Kt=3.0 is about 50 percent larger in comparison
with that of Kt=1.5.

Axial stress contours at the beginning and end of hold-time are demonstrated
in Fig.3(a) and (b), being calculated by Ohno-Murakami model at the third
cycle [Problem IV ]. A lOmin. strain hold-time drastically reduces the
stress concentration at the notch root. The maximum axial stress at the
beginning of hold-time is 240MPa, but is relaxed to 160MPa at the end.
The maximum stress is not seen to occur at the very notch root, but just in-
side from the root.

Figure 4 compares the nominal and local hysteresis loops calculated by

Chaboche and Bodner models with the experimental results [Problem II]. The
Chaboche model estimates the local strain range Δ ε sp=0.62%, while the Bod-
ner model as Δ £ Sp=0.58%. Since the experimental strain range is 0.55%,
both models well estimate the actual strain concentration. The Chaboche
model gives slightly large strain concentration with 10% discrepancy.

2.0 K=1.5 K=3.0

CL.s120MPa £SP ^ — £SP
. — εεβ, EoL

50 100
Creep time t ,h
Fig.2 Experimental creep deformation at notch root

No. Value
t 0
2 20
3 40
4 60
5 80
6 100
7 120
β 140
9 160
10 180
11 200
12 220
13 240

(a) At the beginning of hold-time. (b) At the end of hold-time

Fig.3 Axial stress contour at N = 3

calculated by Ohno-Murakami Model.
 Global strain 6 * , % 265
-0.24-Q16 -0.08 0 008 0.16 0.24
400 Γ 300
Chaboch·
Fast-fast

S 2 0 0

j wo h
/ 1 If

L
2 o

■A
In
--100

£-200

-0.3 -0.2 -0.1 0 0.1 0.2 0.3

-300 1
-0.2 0 0.2 0.4
Local strain E%p */· Strain £ e t £ „ , · / .
(a) Experimental (b) Calculated by Chaboche (b) Calculated by Bodner
model model

Fig.4 Stress-strain hysteresis loops at notch root

and between gauge length (Kt=1.5).

Examination of Life Prediction Methods The fatigue-creep life prediction

was made based on some inelastic constitutive models. Here, two kinds of
equivalent strain range were defined by the ASME B. P.V. Code Case N-47 as
2 2 1/2
Δ ε =[(Δ ε ) + 1/3(Δ Ύ ) J , and by path integration as Δ a =1/2 $ cycled^ .
The creep damage was evaluated by the two models; the Mises' equivalent
stress and Huddleston stress base (Huddleston, 1985). The comparison be-
tween the predicted and observed lives and failure lives is shown in Fig.5,
where crack initiation lives and failure lives are plotted as the small and
large symbols, respectively. All the constitutive models give an unconser-
vative estimation for the crack initiation life in the fast-fast (pp) test,
but a reasonable result for the slow-slow (cc) and 10min. hold-time tests.
For the failure life, the four constitutive models gives a reasonable and
conservative estimation. The predicted data moves in conservative direc-
tion when the creep damage is calculated by the Huddleston's stress.

Iff
o : ΟΗΝΟ
p
9/
Δ : SUPERP.
D : MOD. SUPERi
: KREMPL
o * /
£ 10,3L
; U n e /
n A) /
to

10'2L
: Open symbol : PP test
Solid symbol : CC test
Half open symbol : Hold-time test
Large symbol :Nf
Small symbol :Nc
101 1 1 11 1 II I i i t 1 i ml
101 10z 10J
Predicted value Npred Predicted value Npred
(a) ASME-Mises (b) ASME-Huddleston

Fig. 5 (to continue)

266

(c) Path-Mises <d) Path-Huddleston

Fig. 5 Comparison of estimated fatigue-creep life by the Linear

Damage Rule with experimental data.

ACKNOWLEDGMENT

The Subcommittee is grateful to the Ministry of Education to provide the

financial support as Grant-in-Aid for Co-operative Research A (No.
01302026).

REFERENCES

Inoue, T., T. Igari, F. Yoshida, A. Suzuki, and S. Murakami (1985).

Inelastic behaviour of 2*l/4Cr-lMo steel under plasticity-creep inter
action condition. Nucl. Eng. Des. 90, 287-297.

Inoue, T., N. Ohno, A. Suzuki and T. Igari (1989). Evaluation of inelas-

tic onstitutive models under plasticity-creep interaction for 2.1/4
Cr-lMo steel at 600°C . Nucl. Eng. Des. 114» 295-309

Inoue, T., T. Igari, M. Okazaki, M. Sakane and K. Tokimasa (1889).

Fatigue-creep life prediction of 2.1/4Cr-lMo steel by inelastic
analysis. Nucl. Eng. Des. 114, 311-321

Inoue, T., F. Yoshida, N. Ohno, M. Kawai Y. Niitsu (1991). Evaluation of

inelastic constitutive models under plasticity-creep interaction in
multiaxial stress state. Nucl. Eng. Des. (in print)

Inoue, T., M. Okazaki, T. Igari, M Sakane and S. Kishi (1991). Evalua-

tion of fatigue-creep life prediction methods in multiaxial stress
state. Nucl. Eng. Des. (in print)

Huddleston, R.L. (1985). An improved multiaxial creep-rupture strength

criterion, J. Pressure Vessel Tech., 107, 421-429
WS6e3

HIGH TEMPERATURE MULTIAXIAL LOW CYCLE FATIGUE

USING CRUCIFORM SPECIMEN

T. Itoh\ M. Sakane** and M. Ohnami**

* Department of Mechanical Engineering, Graduate

School of Ritsumeikan University, 56-1 Tojiin
Kita-machi Kita-ku Kyoto, 603, Japan.

** Department of Mechanical Engineering, Faculty of

Science and Engineering, Ritsumeikan University,
56-1 Tojiin Kita-machi Kita-ku Kyoto, 603, Japan.

ABSTRACT

This paper describes the high temperature multiaxial low cycle fatigue of type 304 stainless and
lCr-lMo-l/4V cruciform specimens at 823K and 923K in air. Strain controlled multiaxial low
cycle fatigue tests were carried out at the principal strain ratios between - 1 and 1. The principal
strain ratio had a significant effect on low cycle fatigue lives. Fatigue lives drastically decreased
as the principal strain ratio increased. Several multiaxial low cycle fatigue strain parameters were
applied to the experimental data and the applicability of the parameters was discussed.

KEYWORDS

High temperature; multiaxial low cycle fatigue; cruciform specimen; multiaxial fatigue criteria.

EXPERIMENTAL PROCEDURE

This paper used SUS304 stainless and lCr-lMo-l/4V cruciform specimens. Figure 1 shows the
shape and dimensions of the specimen together with the coordinates used in this paper. The former
material received a solution treatment at 1373 K for an hour, while the heat treatment of the latter
material was 15 hours at 1223 K / oil quench and 30 hours at 973 K / furnace cool. The shape
of the cruciform specimen was determined in FEM analyses so that the stress and strain are
distributed uniformly along the gage length (Sakane et al.91988,1989). This study used two types
of specimens. Both the specimens have the same shape but the different thickness in the gage part.
In tests with large principal strain ratios, the thick specimen was used to avoid the buckling.

Total strain controlled tests were carried out for type 304 stainless steel at 923 K and
lCr-lMo-l/4V steel 823 K in air. The amplitude of the principal strain in y-direction (ey) was
fixed and that in x-direction (ej was changed so as to achieve the principal strain ratio (φ) ranged
between - 1 and 1. The principal strain ratio is defined here as zjzr The principal strain rate in
y-direction was 0.1 %/sec. The failure cycle is defined as the cycle at which the tensile stress
amplitude normal to the crack decreases to 95 % of the maximum value for type 304 steel. For
the cyclic softening material of lCr-lMo-l/4V steel, the failure cycle was defined as the cycle
of 5 % rapid stress drop due to the crack initiation and propagation.
267
268
U_ ^ J
A

fcr ,fc-r
o
CM

ρφπζ
y | f A
·β4 -ft.
L JLA
·β>1 *>J

zi .x 5 3
1 ΓοΤ
1 1 ^ψ

« 210^ ,

Fig. 1. Shape and dimensions of the specimen tested (mm).

In tests using the cruciform specimen, the φ=-1 test corresponds to the reversed torsion test using
cylindrical specimen, the φ=-0.5 test the uniaxial tension/compression test, and the φ=1 test
equi-biaxial tension/compression test.

EXPERIMENTAL RESULTS AND DISCUSSION

Multiaxial Low Cycle Fatigue Life

Figures 2 (a) and (b) show the variation of failure cycle with principal strain range in y-direction
for type 304 and 1Q-1MO-1/4V steels, respectively. In some tests using type 304 steel at low
strain ranges, the failure cycle exceeded 105 cycles. In those cases, tests were interrupted at 105
cycle. For both the materials, failure cycle decreases with increasing the principal strain ratio in
Aey controlled tests and the slope of the data does not differ from each other.

Figures 3 (a) and (b) are the replot of Fig. 2 and show the relationship between failure life and
principal strain ratio. It is evident from these figures that the failure life is significantly affected
by the principal strain ratio. For type 304 steel, failure cycle decreases with increasing the
principal strain ratio at each strain range, but the decreasing rate becomes large as the strain range
decreases. This is understood from the result that the slope of the data becomes steeper in the
small Aty test. For lCr-lMo-l/4V steel, on the other hand, the trend of the data is similar to type
304 steel but the effect of the principal strain ratio on failure life is somewhat smaller in the range
of - 1 ^ - 0 . 5 .

Correlation of Fatigue Data with Strain Parameter

There have been proposed many strain parameters for the correlation of biaxial low cycle fatigue
data. This paper discusses the applicability of the parameters by applying those to the experimental
data. The biaxial strain parameters examined are the maximum principal strain, Mises' equivalent
strain(Mises' strain), Γ-plane parameter(BMK strain) (Brown and Miller, 1979, Kandil et al.,
1982), Γ'-plane parameter(LE strain) (Lohr and Ellison, 1980) and the equivalent strain based on
crack opening displacement(COD strain) (Hamada et al., 1984, 1985, 1987, 1989). Since the
 269
SUS304, T*923K in Air ICr-IMo-l/4V, T*823K in Air
I I l|llll| Γ I I |llll| 1 I I |IIM| 1 I I llllll l<J 1 1 1 | 1 III] i i i | i mi ι 1ι M i l l
$S _
I0C : \\\Vb _
ω : \X^ V -

cσ>
o
^S ^^^^^^**»-^
-
Ί
θ φ - Ι .0
c • --0.5
σ D
Δ
- 0.0
- 0.5
"j
w
O - 1 ,0
σ
i i i IIIIII i i i IIIIII i i 111 ml ι ι iliinl £
»- .^-ι ι ι ι 1 mil i i i 1 mil ι ι1 l l l l l l
10" Z 3 4 8 6
I0 I0 I0 I0 I0 I0 2 I0 3 I0 4 I0 5
Number of cycles to failure Nf Number of cycles to failure Nf
(a)type 304 steel (b)lCr-lMo-l/4V steel
Fig. 2. Correlation of biaxial fatigue data with
total strain range in y-direction.

SUS304, T=923K in Air ICr-IMo-l/4V t T=823K in Air

I0 ! 1 "T -
E 1 1 I 1
z
r -
cN

S io4| 'S,
~..x
~-o- \ -d
o F
w
r H
o
υ i- ^•. V Ö Ί
\o
o I0 3
E •\
ω 0 0.3% ^
E L ® 0.4%
- o 0.5% J
z - • 0.7%

I0a - 1 1 _J_ 1 1 1
-1.0 0.0 1.0 -1.0 0.0 1.0
Principal strain ratio φ Principal strain ratio φ
(a)type 304 steel (b)lCr-lMo-l/4V steel
Fig. 3. Relationship between biaxial fatigue life
and principal strain ratio.

detailed description of these parameters has been already made in a previous paper as well as the
physical meaning of the parameters (Sakane et aL, 1987), it is not made here to avoid the
repetition. In the following, we will apply those multiaxial fatigue parameters to the experimental
data and will discuss the applicability of the parameters. However, the graphical representation of
correlation is only made on the Mises' and COD strains because of the space of the paper.

Figures 4 and 5 show the correlation of the biaxial low cycle fatigue data for two materials with
the Mises' and COD strains. A factor of two scatter band is drawn based on the φ=-0.5 data
denoted by the solid circle. In Fig. 4 (a), the Mises' strain estimates the φ=-1 data too
conservatively for type 304 steel. However, in the range of -0.5^φ^1, the Mises' strain estimates
270
SUS304 , Τ=923Κ in Air I C H M o - l / 4 V , T=823K in Air
I I l|llll| 1 I I |llll| 1 I I |IUI| 1 I I 11 HJI

Factor of 2
t»-.io°

10" I I lllllll I I lllllll I I lllllll I I III 10"» i i I mil i i i 1 mil ι ι ι I in

I0 Z I03 I04 10 s I06 I0 2 I0 3 I0 4 I0 5
Number of cycles t o failure Nf Number of cycles to failure Nf

(a)type 304 steel (b)lCr-lMo-l/4V steel

Fig. 4. Correlation of the biaxial fatigue data with
the Mises' equivalent strain range.

Q Q
O O I C H M 0 - I / 4 V , T=823KinAir
O SUS304 , T=923K in Air
O I II | l l |l l 1 1 1 | 1 llll 1 1 Ι7ΤΤΠ
- ' " i " " l ' 1 l | l l l| l 1 1 l | I I |H 1 1 | I MI
x ^ \ Factor of 2 οφ__. 1 .0
0.5
1
10° h s\N
Γ \ ^ Sc / Δ
Factor of 2
—
I0°h \ \ V 7 · - o.o- Γ χ3>* 4 \
0.5 -
:
Γ L 0
1 .0 - ^ ^ :
- θ φ = -| .0 ° ^ j
- l < φ s-0 .5 ^ - σ CJÜ • «-0.5 - Ι < ψ ί - 0 , 5
/S-8.23, m'--2.3 O » 0.0
- " Δ - 0.5 /S-8.23, m' —2.3J
CH> 0 - 1.0 -0.5< φ 5 I
-0.5<
£-1.90, φ £ 1m'—0.7 £-1.90, m'—0.7
10-, 21 1 l l l l l l 3 11 lllllll 4 1 1 lllllll 1 1 11 Ml > 10-, — i i i linil — i _ i 1 1 m i l 1 1 1 1 1111I
I0 I0 I0 10s I0 6 I02 I03 I04 10 s
Number of cycles to failure Nf Number of cycles t o failure Nf

(a)type 304 steel (b)lCr-lMo-l/4V steel

Fig. 5. Correlation of the biaxial fatigue data with
COD strain range.

the fatigue data appropriately. For 1Q-1MO-1/4V steel, the Mises' strain well correlates the
fatigue data excepting the two data points with the positive strain ratio. The data in the φ=-1 test
is estimated conservatively, but these data are still located within a factor of two scatter band.

Figure 5 (a) show the correlation of the fatigue data with the COD strain for type 304 steel. The
COD strain well correlates the fatigue data within a factor of two scatter band, although the data
in the φ=-1 test are located somewhat in the lower side. For lCr-lMo-l/4V steel shown in
Fig. 5 (b), the scatter of data appears to be slightly large in comparison with type 304 steel, but
the COD strain almost correlates the fatigue data within a factor of two scatter band.

As for the correlation with the other strain parameters, the maximum principal strain correlates the
biaxial fatigue data within a factor of two scatter band. The scatter of the data is similar to the
correlation with the Mises' strain. The maximum principal strain has a trend to give a conservative
 271

-1.0 -0.5 0.0 0.5 1.0

Principal strain ratio Φ

Fig. 6. Comparison of several strain parameters.

estimate for the φ=-1 data and conversely an unconservative estimate for the φ=0 data. The LE
strain correlates the fatigue data within a factor of two scatter band for both the materials in all the
range of the principal strain ratio of -Ι^φ^Ι. The BMK strain gives a satisfactory correlation only
for the data in the range of -1^φ^-0.5 but yields a large scatter for the data in the range of Ο^φ^Ι.
The data in the range of Ο^φ^Ι locate far below a factor two scatter band. Such an unconservative
estimate may result from the large gap at φ=-0.5 in the BMK parameter, which is described below.

Figure 6 compares the strain parameters. The ordinate is normalized by the principal strain in y -
direction. The LE and COD strains monotonously increase with increasing φ. The maximum
principal strain (EJ) takes the value of 1.0 in the range of -Ι^φ^Ο, but it increases with increasing
φ in the range of Ο^φ^Ι. The Mises' strain decreases with increasing φ in the range of -1^φ^-0.5,
but conversely increases with increasing φ in the range of -0.5^φ^1. The BMK strain shows a
parabolic shape in the range of -1^φ^-0.5 but monotonously increases with increasing φ in the
range of -0.5<φ^1. The BMK strain has a large gap at φ=-0.5.

As shown in Fig. 3, experimental fatigue lives decrease with increasing φ. Thus, the appropriate
parameter which can correlate fatigue lives with a small scatter in all the range of the principal
strain ratio must increase with increasing φ. The parameter which shows this trend is the LE and
COD strains. The Mises' strain has an opposite trend to experimental data in the range of -Ι^φ
£-0.5, whereas the Mises' strain well expresses the trend of experimental data in the range of
-0.5<;φ<;1. The BMK strain correlates the experimental data in the range of -Ι^φ^-0.5 and those
in the range of -0.5<φ«;1 separately. Since the BMK strain has a large gap at φ=-0.5 and which
results in a large scatter of the data correlation. If the parameter is modified to eliminate a
discontinuity, the correlation will be quite improved.

In conclusion, the maximum principal, LE and COD strains give a satisfactory data correlation for
both the materials. Among them, the LE strain appears to yield a somewhat smaller scatter of the
correlation in comparison with the other two parameters. The Mises' strain gives a sufficient data
correlation in the range of -0.5<;φ<;1 but does not in the range of -Ι^φ^-0.5 for type 304 steel.
For lCr-lMo-l/4V steel, the Mises' strain correlates all the data within a factor of two scatter
band although the Mises' strain estimates the opposite φ-dependence of fatigue data in the range
of -1<:φ^-0.5. This is attributed to fact that the fatigue data in the φ=-1 test are not such in-
272
creased in comparison with the φ=-0.5 data for lCr-lMo-l/4V steel. The BMK strain yields a
poor correlation because of the large gap at φ=-0.5, and it correlates the fatigue data into two
groups depending on the principal strain ratio range.

CONCLUSIONS

(l)In strain controlled tests, biaxial low cycle fatigue lives drastically decrease with increasing the
principal strain ratio for type 304 stainless and lCr-lMo-l/4V steels. The decreasing rate
becomes large as the strain range decreases.

(2)The maximum principal, LE and COD strains nearly correlate all the multiaxial fatigue data
within a factor of two scatter band for type 304 stainless and 1Q-1MO-1/4V steels, tested in the
principal strain ratio ranged between - 1 and 1.

(3)The Mises' equivalent strain also correlates the fatigue data within a factor of two scatter band
as well as the above three parameters excepting the data in the φ=-1 test. The data in the φ=-1
test are conservatively estimated in comparison with the φ=-0.5 data. The BMK strain correlates
the multiaxial fatigue data with a large scatter. This is attributed to the discontinuity of the strain
at φ=-0.5.

REFERENCES
Brown, M. W. and K J. Miller (1979). High temperature low cycle biaxial fatigue of two steels.
Fatigue Eng. Mater. Struct., 1, No.2, 217-229.
Hamada, N., M. Sakane and M. Ohnami (1984). Creep-fatigue studies under a biaxial stress state
at elevated temperature. Fatigue Eng. Mater. Struct., 7, No.2, 85-96.
Hamada, N., M. Sakane and M. Ohnami (1985). A study of high temperature low cycle fatigue
criterion in biaxial stress state. Bull. Japan Soc. Mech. Eng., 28, No.241, 1341-1347.
Hamada, N., M. Sakane and M. Ohnami (1987). Effect of temperature on biaxial low cycle fatigue
crack propagation and failure life of an austenitic stainless steel. Proceedings of the 30th Japan
Congeress on Materials Research, 69-75.
Hamada, N., M. Sakane and M. Ohnami (1989). COD criterion to assess high temperature
biaxial low cycle fatigue. ImThird International Conference on Biaxial/Multiaxial Fatigue, 2,
Paper No.41, 1-15.
Kandil, F. A., M. W. Brown and K J. Miller (1982). Biaxial low-cycle fatigue failure of 316
stainless steel at elevated temperatures. Mech. Behav. Nucl. Appl. Stainless Steel Elevated
Temperature, 203-209.
Lohr, R. D. and E. G. Ellison (1980). A simple theory for low cycle multiaxial fatigue. Fatigue
Eng. Mater. Struct., 3, No.l, 1-17.
Ohnami, M., M. Sakane and N. Hamada (1985). Effect of changing principal stress axes on
low-cycle fatigue life. ASTM STP, No.853, 622-634.
Ohnami, M., M. Sakane and N. Hamada (1986). Biaxial low-cycle fatigue in creep region at
elevated temperature. J. Soc. Mater. Sei. Japan, 35, No.390, 230-240, (in Japanese).
Sakane, M., M. Ohnami and M. Sawada (1987). Fracture modes and low cycle fatigue life in
biaxial stress state at elevated temperature. Trans. ASME, J. Eng. Mater. Technol., 109, No.3,
236-243.
Sakane, M., M. Ohnami, T. Kuno and T. Itsumura (1988). High temperature biaxial low cycle
fatigue using cruciform specimen. J. Soc. Mater. Sei. Japan, 37, No.414,340-346 (in Japanese).
Sakane, M. and M. Ohnami (1989). Creep-fatigue in biaxial stress using cruciform specimens.
IniThird International Conference on Biaxial/Multiaxial Fatigue, 2, Paper No.46, 1-18.
WS6e4

CREEP/FATIGUE CRACK GROWTH IN A 10% Cr

MARTENSITIC STEEL
K.M. NIKBIN+, K. NISHIDA* and G.A. WEBSTER+
+
Dept. of Mechanical Engineering,
Imperial College, London, SW7 2BX, U.K.
* Komatsu Ltd., 5 Yookaichimachi Jigata,
Komatsu-City, Ishikawa-Pref, Japan.

ABSTRACT
Crack growth experiments have been carried out under static and cyclic loading
conditions on a 10% Cr martensitic steel (designated FV 448) at selected temperatures
from 300 to 550°C. The cyclic load tests were performed at a minimum to maximum
load ratio R = 0.1 over the frequency range 0.001 to 1 Hz. The results have been
analysed in terms of linear and non-linear fracture mechanics concepts. Regions of
transgranular fatigue and intergranular creep controlled cracking have been observed.
It has been found that a linear superposition cumulative damage model can be
employed to describe crack propagation when both processes act together.

KEYWORDS
Creep, Fatigue, Fracture mechanics, Crack growth.

INTRODUCTION
Many engineering components are subjected to a mixture of static and cyclic loading
conditions over a range of temperatures which can cause failure by creep, fatigue,
thermal fatigue or some combination of each process. The main purpose of this
investigation was to determine the mechanisms controlling crack growth in the
temperature range 300 to 550°C in a 10% Cr martensitic steel designated FV 448. This
steel is a candidate material for plasma first wall applications in fusion reactors (Ehrlich
1986). During operation it can experience a variety of cyclic loading conditions,
including plasma disruptions, and it is necessary to account for these when making
design lifetime assessments.

Previous work on a nickel base superalloy (Nikbin and Webster 1984; Winstone et
aly 1985) and a selection of low alloy steels (Dimopulos et al, 1986) have identified
regions of fatigue and creep dominated cracking when these materials are subjected to
combined static and cyclic loading conditions. Generally it has been found that
transgranular fatigue processes control at low minimum to maximum load ratios R and
273
274
high frequencies f and intergranular creep processes at high R and low frequencies. It
has also been observed that mixed mode fractures are obtained (which correspond with
the proportion of creep and fatigue damage experienced) when both mechanisms
contribute to failure. Analysis of the data has shown that when fatigue processes
dominate crack growth/cycle da/dN can be described in terms of stress intensity factor
range ΔΚ by the equation,

|j-=CAKm (1)

where m is usually in the range 2 - 5 and C is a proportionality factor which is

sensitive to R and temperature but independent of frequency. When time dependent
effects control it has been found that the non linear creep fracture mechanics parameter
C* is more appropriate for describing crack propagation rate ä, to give

a=DC** (2)

where D and φ are material dependent parameters which can be obtained from a model
of the cracking process that involves ductility exhaustion in a damage zone at the crack
tip (Nikbin et al, 1986). However for most materials it has been demonstrated that eq
(2) can be expressed approximately as

a = %— (3)
fc
f

with ä in mm/h and C* in MJ/m2 h. In this equation £f* is the creep ductility
appropriate to the state of stress at the crack tip. For plane stress conditions it can be
taken as the material uniaxial creep failure strain 8f and for plane strain situations as
£f/50. For most circumstances creep crack growth occurs under conditions
approaching plane stress loading.

In the transition region where creep and fatigue mechanisms both contribute to the
cracking process it has been found (Winstone et al, 1985) that the total crack
growth/cycle can be described by

+ w
dN VdNj f
F

where the first term refers to the fatigue component of cracking given by eq (1) and the
second term to the creep component represented by eq (3).
In this investigation experiments have been carried out to establish the relevance of eqs
(1) to (4) to creep-fatigue crack growth in the 10% Cr martensitic steel.

EXPERIMENTS
The chemical composition and heat-treatments applied to the 10% Cr martensitic steel
are shown in Table 1. This heat-treatment was employed to produce a strength level
representative of neutron irradiated material (NET team, 1985). Compact tension (CT)
 275

and single edge notch tension (SENT) specimens were machined from the heat-treated
material. The CT specimens had a width W of 50 mm, thickness B = 25 mm and were
side grooved 20%. The SENT samples had W = 20 mm and B = 5 mm. All the
specimens were provided with a room temperature fatigue starter crack prior to
elevated temperature testing.

Table 1. Composition and heat treatment of 10% Cr steel

(a) Chemical Compositions (weight in %)

C Si Mn Cr Ni Mo V Nb
0.12 0.3 0.75 10.5 0.8 0.65 0.25 0.3

(b) Heat Treatment

(1) 0.5 hours at 1150°C, (2) Oil quench, (3) 2 hours at 680°C, (4) Air cooled.

Details of the experimental procedure have been reported previously (Nikbin and
Webster ,1984; Winstone et al, 1985; Dimopulos ^ a/, 1986; Nishida 1989). For all
the tests crack extension was measured by a combination of optical and AC electrical
potential methods with an estimated accuracy of 0.1 mm. Some experiments were
conducted under static loading conditions and others under cyclic loading at R = 0.1
and frequencies between 0.001 Hz and 1 Hz at temperatures of 300, 400, 500 and
550°C. The high frequency tests were performed in servo-hydraulic machines and the
low frequency tests in suitably modified creep machines.

DISCUSSION
Examples of the results obtained are indicated in Figs 1 to 5. Figure 1 shows creep
crack growth rate plotted against the stress intensity factor K for a range of
temperatures. It is apparent that crack growth rate increases with increase in
temperature and that there is a tendency for a threshold to be observed which also
decreases as temperature increases. The corresponding cyclic crack growth data are
illustrated in Figs 2 to 4. They show a similar threshold behaviour to the static results.
Little frequency dependence can be detected at 300 and 400°C in Fig 2 and 3
respectively. However, at 550°C there is some indication in Fig 4 that cracking rate
increases with decrease in frequency below about 0.01 Hz. A similar but less
pronounced trend was observed at 500°C. It is apparent that away from the threshold
region all the cyclic data can be described by an expression of the form of eq (1) with
m = 5. However, some geometry dependence is evident. Generally crack growth in
the CT specimens is slower than in the SENT samples.

Characterization of the static and slow frequency crack growth data with C* is shown
in Fig 5. Satisfactory correlation with eq (3) is obtained when the material uniaxial
creep ductility 8f = 0.1 is inserted into the expression implying plane stress behaviour.
The slow frequency data were plotted at the maximum value of C* in the cycle.
Agreement between the slow frequency and static results suggests that crack
propagation in the former is controlled mainly by creep processes. In addition unlike
Figs 1 - 4 no geometry dependence can be detected further reinforcing the view that
276

1 T«300*C Cyclic loadlaf (IU0.1)

4 Static kwdlof
// D
■■/
1
/- a ' / /
S/
j
|
j f 10-2:

V /4 $ 1
' m
/
/
f 1
i V
s
J 10-3 : β 1
if ri
1 - O Jv
11 *
/
] /
V: " f'! v/ /
E
e l 1
5 /
1 *
M

H
ir
\ 4
10- : ί
P
1/
0
| /*
J f (Hz)

10-3-J T-C 10-5- / · o X 0.001 Hz CT FV7A

«s•
•β
5S0«C CT FV2C o 0.001 Hz SENT FV40
H
4 ♦
° 500*C CT FV3A A 0 1 Hz SENT FV38
j X 450-C CT FV56 X •
·♦-
002 Hi
0.02 Hz
SENT
SENT
FV2*
FV37
Ί ·♦- 300»C CT FV6A
X 0 1 Hz SEKT FV38
1 ° 550«C S&<T FV46
A 500»C SEIn FV45
. . .. • • 1 Hz SENT FV28

10-·-

K (MPaVm) ΔΚ (MPaVm)

Fig 1 Crack growth rate under static loading Fig 2 Cyclic crack growth at 300°C

T-400eC Cyclic kMdlag (R*0.1) T«9S0*C Cyclic kwdlnc (R>0.1)

rt
/
10°-
10-2J

io- 1-

I io-aJ
/
./

ß
10-2.

i/r
7
10-*:

f (Hz)
0.001 Hz
0.001Hz
0 1 Hz
CT
SENT
SENT
FV6A
FV44
FV26
4
10- : 1
hi *
f (Hz)
0.001Hz
0.001Hz
0.1 Hz
CT
SENT
SENT
FV1C
FV35
FV34

•:l· t:
0.02 Hz SENT FV27 0.02 Hz SENT FV33
0.02 Hz SENT FV22
1 Hz SENT FV25
1 Hz SENT FV21
10-5-

ΔΚ (MPaVm) AK(MPaVm)

Fig 3 Cyclic crack growth at 400°C Fig 4 Cyclic crack growth at 550°C
 277
s

| Eq.(3)
1 ' y

1 ^ ST

§ 10° J

1 1 Plane strain ^ ^ *i ^
\ (Hz) T *C
e static 550 SENT FV46
static 500 SENT FV45
^^£$jr 0.001Hz 550 SENT FV35

J <!it9&r 0.001Hz 300 SENT FV40

1 **V"r ♦ 0.001Hz 400 SENT FV44

0.001 HZ 500 SENT FV42
J AA A
* Δ 0.001Hz 500 CT FV4A
0.001Hz 550 CT FV1C
1 -< ■ a static 550 CT FV2C
' ^ v * static 500 CT FV3A
static 450 CT FV5B
j ■ ^ Plane stress 2
static 300 CT FV8A
0'6 10'5 10'4 10* 3 1• , D "*
■ , · '
10*1
I
1C
C* (MJ/m2h)

Fig 5 Crack growth rate relation to C* for static and slow frequency tests

Frequency (Hz)

Fig 6 Crack growth/cycle at ΔΚ = 50 MPaVm and R = 0.1 for SENT specimens

a) Fig 7 Fracture surfaces for cyclic tests at a) 0.001 Hz, 550°C,

b) 0.02Hz,550°Cand c) 0.001 Hz at 300°C
278

creep crack growth rate is described better by C* than K or ΔΚ in these circumstances.

The frequency dependence of all the cyclic data at a stress intensity factor range of ΔΚ
= 50 MPa Vm is shown in Fig 6. The experimental points were obtained by
extrapolation from Figs 2 - 4 assuming m = 5 where necessary. Little frequency or
temperature dependence is apparent at 300 and 400°C suggesting that crack
propagation in this region is dominated by cyclic fatigue processes.

Above 400°C there is a progressive increase in crack growth/cycle with increase in

temperature and decrease in frequency. This can be explained by the introduction of
creep effects. When time dependent creep processes control, from eq (4) a slope of -1
would be expected on Fig 6. The predictions of the creep component from Fig 1 at a
maximum K = 55.5 MPa Vm, corresponding to that imposed in a cyclic test at ΔΚ =
50 MPa Vm and R = 0.1, are indicated in Fig 6. Reasonable agreement with the slow
frequency data is apparent. It is clear that a significant creep contribution is only
obtained above about 450°C. The predictions of the cumulative damage law (eq 4) are
also shown in Fig 6. Again a satisfactory correlation is achieved. The main influence
of temperature is to cause the creep component to be extended to higher frequencies
with increase in temperature since the pure fatigue component shows little temperature
sensitivity.

Microstructural confirmation of the cumulative damage creep/fatigue model is

demonstrated in Fig 7. This figure indicates intergranular fracture where creep
processes control (Fig 7a), transgranular fracture where fatigue dominates (Fig 7c) and
an indication of mixed mode behaviour where both mechanisms contribute to the
failure process (Fig 7b).

The results of this investigation have confirmed the trends observed previously on
other materials. They have demonstrated that creep-fatigue failure in the 10%
martensitic steel can be described by a linear superposition cumulative damage law.

REFERENCES
Dimopulos, V., Nikbin, K.M. and Webster, G.A. (1986). Influence of cyclic to
mean load ratio on creep/fatigue crack growth, Met. Trans, 19A, 873-880.
Ehrlich, K. (1986). Formulation of initial design equations to type 1.4914 Martensitic
steel. Internal report Kernforschungszentrum Karlsruhe.
NET team (1985). NEXT European Torus, Status report 51, CEC, Brussels.
Nikbin, K.M. and Webster, G.A. (1984). Creep-fatigue crack growth in a
nickel-base superalloy. In Creep and Fracture of Engineering Materials and
Structures (Eds. B. Wilshire and D.R.J. Owen), Pineridge Press, Swansea,
1091-1104.
Nikbin, K.M., Smith, DJ. and Webster, G.A. (1986). An engineering approach to
the prediction of creep crack growth, J.Eng.Mat.& Tech., ASME, 108, 186-191.
Nishida, K., (1989). Creep-fatigue failure of engineering materials at elevated
temperatures, Thesis submitted for the degree of PhD of the University of London.
Winstone, M.R., Nikbin, K.M. and Webster, G.A. (1985). Modes of failure under
creep/fatigue loading of a nickel-based superalloy, J. Mat. Sei., 20, 2471-2476.
WS6e5

High Temperature Fatigue Properties and Life Prediction of

SUS304 Stainless Steel under Variable Straining

Mitsuo Miyahara and Katsuyuki Tokimasa

Research & Development Division, Sumitomo Metal Industries, Ltd.

1-8, Fuso-cho, Amagasaki, 660, Japan

ABSTRACT

In order to examine the applicability of the proposed fatigue life predic-

tion model under variable straining, PP type High-Low and Low-High tests
were conducted for the as solution-treated SUS304 at 700, 800°C and for the
thermally aged SUS304 at 700°C in air. It was found that the experimental
results for the as solution-treated material at 800°C and for the aged
material at 700°C were well explained by the proposed model. On the other
hand, in the case of the as solution-treated material at 700°C the deviation
from the proposed model was observed in some testing condition. By compar-
ing the cyclic hardening behavior under each testing condition, it was
supposed that the discrepancy from the proposed model prediction was caused
by the influence of the cyclic hardening during the primary straining on the
inelastic strain range of the secondary straining.

KEYWORDS

High temperature, Creep-fatigue, Small crack propagation, Life prediction,

Variable straining

INTRODUCTION

Residual life prediction at high temperature has resently become one of the
most interesting and important problems. Many papers dealing with this
problem have been published recently (for example Jaske, 1985). For the ac-
curate residual life prediction at high temperature, it is indispensable to
clarify the creep-fatigue behaviors of materials under variable straining.

In the previous paper (Miyahara et at. ,1991), the authors conducted some
kinds of two-step variable straining tests for Mod.9Cr-lMo steel under PP
(fast-fast) and CP (slow-fast) straining and the creep-fatigue life predic-
tion model using the strain range partitioned crack growth rate equation
(Tokimasa et αΖ.,1986) was proposed.

In this paper, in order to examine the applicability of the proposed model,

PP type High-Low (HL) and Low-High (LH) tests were conducted for the as
solution-treated SUS304 and the thermally aged SUS304. And by comparing the
experimental results of these materials, the effect of cyclic hardening
behavior on the validity of the proposed model was studied.

279
280
LIFE PREDICTION MODEL UNDER VARIABLE STRAINING

Figure 1 shows the proposed fatigue life prediction model under PP type two-
step variable straining (Miyahara et at. ,1991). In this model small crack
growth curves in the smooth specimen are described as shown in Fig.1(a). In
the high strain range regime, the crack initiation life is negligible and
the crack growth curve is described in the form of the linear relationship
between ln(a/a0 ) p p and n/Npp by H-curve (where a is the half crack length,
( a 0 ) p p the initial half crack length, n the applied cycles and N p p the total
fatigue life) based on the strain range partitioned crack growth rate equa-
tion (Tokimasa et at. ,1986). On the other hand, when Δ ε ρ ρ is smaller than
the critical strain range ( Δ ε ρ ρ ) 0 Γ , the ratio of the crack initiation life
to N p p , α , is not negligible as reported by Skelton (1982) and the crack

Small Crack Growth Curves

vwvw^ t °w^MAM '

V
PP Type Two-step Variable
Straining Pattern
t
o
(c) HL straining pattern (d) LH straining pattern

Life Prediction Model

Considering
Crack Growth Curves

V
Predicted Results of
Fatigue Properties
under
HL and LH Straining

m/Ni 1

Fig. 1 Life prediction model under PP type two-step variable straining

proposed in the previous paper (Miyahara et at. ,1991)
 281
growth curve is supposed to be given by L-curve. And as shown in Fig.1(b)
the lower Ae p p is, the larger the value of a is.

By using these crack growth curves, the fatigue properties under High-Low
(HL) and Low-High (LH) straining can be predicted. When the lower strain
range (Δερρ)|_ is greater than ( Δ ε ρ ρ ) Ο Γ , the crack growth curves for both of
the primary straining and the secondary straining are H-curve. So, the
Linear Damage Rule (LDR) is available, i.e., the sum of life ratios (ni/Ni+
n2/N2 5 where ni/N] and n2/N2 are the life ratio of the primary straining and
the secondary straining respectively) is unity. On the other hand, when the
higher strain range (Δερρ)π is greater than (Δε ρρ ) αι - and (Δερρ)ι_ is smaller
than ( Δ ε ρ ρ ) α Γ , the crack growth curve for (Δε ρρ )Η is H-curve but the crack
growth curve for (Δε ρ ρ )|_ is L-curve. In this case, the η^ /Ν^ -112 /N2 rela-
tionship can be calculated with the model in Fig.1(e),(f). By the change of
the strain range, the sum of life ratios becomes smaller than unity under HL
straining and larger than unity under LH straining. Figure 1(g) shows the
summary of the predicted n1/N1-n2/N2 relationship. As shown in this figure,
the maximum deviation from LDR prediction is given by a.

In the previous paper(Miyahara et at. ,1991), the authors indicated that the
results of HL and LH tests for Mod.9Cr-lMo steel at 600°C were well explain-
ed by this model and that α- Δ ε ρ ρ relationship was evaluated based on the
experimental results. In this case the value of ( Δ ε ρ ρ ) 0 Γ was 0.55% and a-
Δε ρ ρ relationship was given by the following equation.
-0.922 log (Δε ρρ ) - 2.08 (1)

EXPERIMENTAL PROCEDURES

The material studied in this paper is JIS SUS304 steel hot-rolled 50 mm

thick plate which was solution-treated at 1100°C for 70 min followed by
water quenching. In order to investigate the effect of thermal aging, the
as solution-treated material and the thermally aged material were tested.
Aging temperature of 700°C and aging time of 1000 hours were employed. In
the aged material, many precipitates were observed at the grain boundaries
and in the matrix. The fatigue specimen was a round-bar smooth specimen
with diameter of 10 mm and gage length of 25 mm. The specimen surface was
polished with the #400 emery paper to remove circumferential machining
striations. Figure 2 shows the results of the constant strain range tests
for the unaged (as solution-treated) material at 700, 800°C and for the aged
material at 700°C in air. The difference in fatigue life between the unaged
and aged materials is small. For these materials, PP type HL and LH tests
were conducted with the straining pattern shown in Fig.1(c),(d). Loading
and unloading strain rates were 8 x 10_:5/sec. The higher total strain range
( Δεΐ) H was 1% and the lower total strain range (Act)L.was 0.8~0.3%.
1 r
"<>
1.0 °^■%J Aged SUS304
■ : 700°C
<5
Unaged SUS304
O : 700°C %
Δ : 800°C
0.1
1 I
102 103 10* 105
Npp (cycles)
Fig. 2 ΤηβΔερρ-Νρρ properties of the materials studied.
282
EXPERIMENTAL RESULTS

The n^/Ni-n2/N2 relationships obtained in HL and LH tests for the unaged

material are shown in Fig. 3(a),(b). The experimental results are well
explained by the proposed model except for a HL test result ((Aet)|_ =0.4%
and test temperature 700°C). Both at 700°C and at 800°C, LDR is available
when (Aet )L is higher than 0.6%, and not when ( Aet)[_ is lower than 0.6%.
Figure 3(c) shows the η^ /Ν^ -112 /N2 relationships for the aged material. All
experimental results for the aged material are well explained by the propos-
ed model, and LDR is available when (Aet)L is higher than 0.4%.

The deviation from LDR was approximated with the broken lines in Fig. 3 and
the values of a were determined from the results of respective HL and LH
tests based on the proposed model. Figure 4 shows the relationship between
Δ ε ρ ρ and a. For both materials, the value of a is 0 in the high Δε ρρ regime,

0.5 10 0.5 10 0.5

Applied cycle r a t i o ni/Ni
(a) Unaged SUS304, 700°C

1.5; 1
1Unaged 800°C M
I
1 ' 11 ' 1
(A £ t )L = 0.4% (A e t )L = 0.3%
_ (AF*.)\ - n £°z
L_ L i n e a r ! |* Ί J
Γ ν ν ^ ^ Damage 1

0.5 1 ·^
D
L \x°^ J
HL
1· N?
11 °LH 1 >J
0.5 10 0.5 10 0.5
Applied cycle r a t i o n i / N i
(b) Unaged SUS304, 800°C

l.b "T 1

[Aged 700X|

Ue t ) L = 0.8% J
1
• HL 1
0
0 LH |
c\
0.5
is· 1
0 \
■.,.,<N
0.5 10 0.5 10 0.5 10
Applied cycle r a t i o ni/Ni
(c) Aged SUS304, 700°C
Fig. 3 The n l / N 1 - n 2 / N 2 r e l a t i o n s h i p o b t a i n e d i n HL and LH t e s t s . ( ( A e t ) H = 1 % )
 283
and the lower Δ ε ρ ρ i s , the larger the value of a is. For the unaged material
the critical inelastic strain range (Δε ) c r is 0.40% both at 700°C and at
800°C, and for the aged material (Δε ) c r is 0.22%. The value of ( Δ ε ρ ρ ) Ο Γ
for the aged material is smaller than that for the unaged material and the
value of a for the aged material is smaller than that for the unaged
material if compared in the same Δε

1.0h-

0.5h
v (Δερη)ςΓ = 0 · 4 0^
'' \ \ (Unaged)
\
£U*
,(Δερρ)εΓ = 0.22% (Aged)
i i i 11 L L J i ' 1 i i i i l
0.1 0.5 1.0
(%)
SP
Fig.4. The Δε 0ί relationship determined from HL and LH
test results based on the proposed prediction model.

DISCUSSION

Effect of Cyclic Hardening Behavior on Validity of the Proposed Model

The discrepancy from the proposed model prediction was found in HL test when
( Δ ε ί ) Η =1% and ( Δεt ) L =0.4% for the unaged material at 700°C. In this
section the cause of this discrepancy is discussed. Figure 5 shows the
comparison between Δ ε ρ ρ in the constant strain range tests and Δ ε ρ ρ at the
first cycle of the secondary straining in each HL test for the unaged mate-
rial at 700°C. Except for the case of ( A e t ) L =0.4%, Δ ε ρ ρ ί η HL tests are
coincided with Δ ε ρ ρ in the constant strain range tests. In the case of
( Δ ε ΐ )[_=0.4%, Δ ε ρ ρ is lower than that in constant strain range tests, which
indicates that Δ ε ρ ρ at the first cycle of the secondary straining was re-
duced by the influence of the cyclic hardening during the primary straining.
Such a reduction of Δ ε ρ ρ was not found for the unaged material at 800°C and
for the aged material at 700°C, indicating that the effect of the cyclic

Unaged SUS304 700°C

Ast(cons t(ni+l cycle) 1.5
Δ 0.8% 1 +0.8% Unaged 700°C
D 0.6% ■ 1 +0.6% ( A E t ) L = 0.4%
o 0.4% • 1 +0.4%
Predicted-!
1:0.5 ^z by
propodsed
8* 0.5U
model

^ο
W·— °-°-
0.5 0 0.5 1
n/N, Applied cycle ratio m/Ni
PP
Fig. 5. Comparison between Δ ε ρ ρ in Fig. 6. The n 1 /N 1 -n 2 /N 2 relation-
constant strain range tests and ship in HL test modified b y Δ ε p p at
Δ ε ρ ρ at first cycle of secondary first cycle of secondary straining,
straining in HL tests. ( ( A e t ) H = l%)
284
hardening is smaller than in the unaged material at 700°C. Figure 6 shows
the modified ni/Ni~n2/N2 relationship in HL test when (Aet)H = l% and (ket)i=
0.4% for the unaged material at 700°C, where N2 is evaluated based on the
Δερρ-Νρρ property by using Δ ε ρ ρ at the first cycle of the secondary strain-
ing. In the large n] /Ni regime, the modified n] /N^ -112 /N2 relationship is
coincident with the predicted relationship, which is depicted by the
symmetric line of the LH test result in the same condition, whereas the
discrepancy is still observed between the modified n^ /Ni -112 /N2 relationship
and the predicted relationship in the small n ι/Ν·| regime.

Effect of Thermal Aging

As shown in Fig. 4 the values of ( Δ ε ρ ρ ) 0 Γ and a for the aged material are
smaller than those for the unaged material. This indicates that the ratio
of the crack initiation life to the total life for the aged material is
smaller than that for the unaged material. Since the total lives of both
materials are almost the same as shown in Fig.2, this also indicates that
the crack initiation life of the aged material is smaller than that of the
unaged material. Probably the precipitates were responsible for such a
difference in the crack initiation life, i.e., in the aged material the
crack initiates from precipitates more easily than in the unaged material.

CONCLUSIONS

In order to examine the applicability of the proposed fatigue life predic-

tion model under variable straining. PP type HL and LH tests were conducted
for the unaged SUS304 at 700, 800°C and for the thermally aged SUS304 at
700°C in air. And the following results were obtained.
(1) The results of HL and LH tests for the unaged material at 800°C and for
the aged materail at 700°C were well explained by the proposed model.
On the other hand, for the unaged material at 700°C, the deviation from
the proposed model was found in some HL test condition.
(2) It was supposed that the discrepancy from the proposed model prediction
in the case of HL test for the unaged material at 700°C was caused by
the influence of the cyclic hardening during the primary straining on
Δε in the secondary straining.
(3) The critical strain range ( Δε ) c r , above which the crack initiation
life is negligible compared with the total life, was 0.40% for the
unaged material and 0.22% for the aged material. It was supposed that
the precipitates were responsible for such a difference, i.e., in the
aged material the crack initiates from precipitates more easily than in
the unaged material.
(4) The proposed life prediction model under variable straining was applica-
ble for SUS304 stainless steel when cyclic hardening is small.

REFERENCES

Jaske, C. E.(1985). Predicting the Residual Life of Plant Equipment.

Proc. PVP Conf., ASME PVP, 98-1, 3-8.
Miyahara, M. and K. Tokimasa (1991). High Temperature Creep-Fatigue
Properties and Life Prediction of Mod.9Cr-lMo Steel under Two-step Varia-
ble Straining. Proc. 34th Jap. Congr. Mater. Res. ,(in print).
Skelton, R.P.(1982). Growth of short Cracks During High Strain Fatigue and
Thermal Cycling. ASTM STP770 , 337-381.
Tokimasa, K. and K. Tanaka. (1986). Experimental Analysis of High
Temperature Creep-Fatigue Crack Growth Based on Strain Range Partitioned
Concept. Proc. Role Fract. Mech. tn Modern Tech , 393-404.
WS6e6

Proposal of the Simplified Method to Evaluate the Semi-elliptical Crack

Growth Behavior for 304 Steel under Creep-fatigue Condition

by
Isamu Nonaka and Masaki Kitagawa
(Ishikawajima-Harima Heavy Industries Co., Ltd.)
Research Institute
3-1-15 Toyosu, Koto-ku Tokyo 135 JAPAN

ABSTRACT

In order to evaluate the surface crack behavior under creep-fatigue

condition, a nonlinear fracture mechanics seems to be useful. As it is
time-consuming and expensive to calculate the nonlinear fracture mechanics
parameter by the 3-dimensinal numerical analysis, the development of the
simplified method to calculate the nonlinear fracture mechanics parameter
is needed. In this paper, a series of experiments were performed to
develop the simplified method by which the nonlinear fracture mechanics
parameter could be calculated experimentally. As a result of of
experiments, the experimental simplified method could be developed for
four cases: (1) axial fatigue, (2) bending fatigue, (3) axial creep-
fatigue and (4) bending creep-fatigue.

INTRODUCTION

When evaluating the structural integrity of high temperature components,

one runs often enough into the problem of how to evaluate the surface
crack propagating under creep-fatigue conditions. Since this is a
situation that does not admit of the immediate application of the linear
fracture mechanics, few studies have been made on this subject matter:
there exist only two or three simplified J evaluation formulae that have
been proposed on the basis of detailed numerical analysis.

In the present work, a series of experiments has been undertaken in an

attempt to evaluate the propagation of surface crack in creep-fatigue
empirically by utilizing the cyclic J integral range and the creep J
integral range that have proved to be effective to evaluate the
propagation of through cracks.

EXPERIMENTAL

The sample was the stainless steel SÜS304 (in part the Mod. 9Cr-1Mo
steel), from which a number of the axial fatigue specimens and the bending
fatigue specimens were prepared as shown in Fig. 1. At the center of
285
286
these specimens, a notch, either of a semi-circular or a semi-elliptical
in shape, was cut to a length of several mm by the discharge machining
method.

The test comprised the axial fatigue, the bending fatigue, both conducted
at room temperature, the 500°C axial creep-fatigue conducted in the load-
controlled triangular stressing method, and the 650°C bending creep-
fatigue conducted in the load-controlled trapezoidal stressing method. In
the bending creep-fatigue, the stress holding time was 10 min with the
cracked side kept in tension, and the application of the bending load was
as shown in Fig. 2(a), where the axial force was entirely ignorable. The
stress ratio was -1 for all the cases.

The form of the crack front was traced electrically: a dc current of 30 A

was fed from one end of the specimen, and the voltage changes were read
off at y=±1 mm across the crack as shown in Fig. 2(b) at given time
intervals; the progress of crack propagation was chronologically followed
from these data with reference to the beach marks. Also, corresponding
CODs were determined at y=±2.5 mm with an axial extensometer.

RESULTS AND DISCUSSION

Axial Fatigue

On the basis of the results obtained, following formula has been proposed
to define a parameter to represent the crack propagation rate:

AJ=AK2/E+2Sp/(2WB-nac/2), (1)

where ΔΚ is the stress intensity factor amplitude (i.e., the analytical

solution due to Newman and Raju^)); E, the Young's modulus; and Sp, the
energy determined on the load-COD hysteresis curve2) (Fig. 3). It will be
noted that the equation (1) is based on the simplified formula for the
through crack2), where the ΔΚ is that sort which considers the direction of
crack propagation, and the second term on the righthand side means the
energy Sp per unit area of the ligament.

The crack propagation rates of SUS304 at room temperature, da/dN in the z-

direction and dc/dN in the x-direction, are shown in Fig. 4 as reduced by
the AJ. That they agree quite well with their through crack counterparts
gives credence to the AJ defined in the eq. (1). Since the effect of
propagation direction is not considered in the second term on the
righthand side, however, an appropriate correction factor appears to be
called for here it, if da/dN and dc/dN differed too greatly.

Bending Fatigue

The proposed formula for this case is as follows:

AJ=AK2/E+Hj[(n-1)/(n+1)]Aob*A6, (2)

where Hj is the Newman-Raju bending multipliers); n, the work hardening

xponent in the repetitious stress-strain equation; Aob, the maximum
amplitude of the bending stress based on the elastic calculation (i.e.,
=6Mt>/WB2); and Δδ, the increment in COD during a stress cycle (Fig. 3);
other terms being the same as in eq. (1).
 287
The crack propagation rates of SUS304 at room temperature are shown in
Fig. 5 in terms of AJ. Here, although dc/dN is always larger than da/dN,
the ratio being about 10 at the most, the two trend lines fall on
approximately the same straight line when reduced to the dc/dN and da/dN
vs AJ relationships. Since the tangent of this straight line is
different, though slightly, from that the law of propagation of the
through crack gives, however, eq. (2) cannot be said to be very
satisfactory.

Axial Creep-Fatigue

Here, the proposed parameter formula is:

AJC=[(α-1)/(α+1)]·[Sc/(2WB-nac/2)], (3)

where a is the stress exponent in the Newton equation, and S c is the energy
determined in the load-COD hysteresis curve2) (Fig. 3). It is to be noted
that the eq. (3) like the eq. (1), is based on the simplified formula for
the through crack2), and that the second term on the righthand side means
the energy S c per unit area of the ligament.

The crack propagation rates of Mod. 9Cr-1Mo steel at 500°C (load holding
10min) are shown in Fig. 6 in terms of AJ C . Both da/dN and dc/dN agree
with their through crack conterparts well enough, attesting to the efficay
of the AJ C defined in eq. (3). Since the effect of the propagation
direction is not considered here, however, appropriate correction appears
to be needed if da/dN and dc/dN differed too greatly.

Bending Creep-Fatigue

The formula proposed for the bending creep fatigue is:

AJc=[(a-1)/(a+1)]-ob-A8c, (4)

where a is the stress exponent in the Newton equation; ot>, the maximum
bending stress (i.e.,=3Mfc>/WBG2) at the evaluating point; and A8 C , the
increment in COD during the load holding (Fig. 3). Here, the ob has been
defined as follows in consideration of the shift of the figure center with
the progress of crack propagation as shown in Fig. 7:

at the deepest point of the crack,

ob=Mb(n-a)/ß, and (5)

at the plate surface,

öb=Mbii/ß, (6)

where

ß=[2ß3W/3-na3c/8-n2(2BW-nac/2) ],

and η=[(B/2-0.424a)(nac/2)/(2BW-nac/2)]+B/2,

which is the distance between the figure center G and the plate surface.
288
For SUS304 at 650°C (load holding 10 min), the da/dN was calculated on the
AJ C given by eq.(5), and the dc/dN on the AJ C of eq.(6). As shown in Fig.
8, the two trend lines fall on an approximately the same straight line in
agreement with that of the through crack. This proves that the AJ C as
defined by eq.(4) is well suited for the parameter to evaluate the
behavior of the surface crack under creep-fatigue deformation.

CONCLUSIONS

As a result of the experiments, the following conclusions were obtained.

(1) In the case of axial fatigue, the surface crack growth rate was
characterized by the parameter shown as follows:

AJ=AK2/E+2Sp/A

(2) In the case of bending fatigue, the surface crack growth rate was
characterized by the parameter shown as follows:

AJ=AK2/E+H{(n-1)/(n+1)}AoA6

(3) In the case of axial creep-fatigue, the surface crack growth rate was
characterized by the parameter shown as follows:

AJc={(a-1)/(a+1)}Sc/A

(4) In the case of bending creep-fatigue, the surface crack growth rate
was characterized by the parameter shown as follows:

AJc={(a-1)/(a+1)}oA6c

These parameters were the modifications of the parameters which were

useful for the through crack.

REFERENCES

Yagawa, G., et al., ASMEPVP, 103, 43(1986).

Taira, et aL,Zairyo,28-308, 414 (1979).
Nonaka, et al., Preprints, 38th Lecture Meeting ofJSTM. 58(1989).
Nonaka, et al, Preprints, 26th High Temperature Strength Symposium, 80 (1988).
Newman, J.C. and Raju, , NASA TMO-85793( 1984).
 289

f/ «, * tΓ Μ30

!r=gg— J .
:!i\^
j ! S* 1
™ -1 ^ i |
60 t | - \ III t—J
J i r = = e5! ^

-L-φ--^} -Φ I sP.

-Φ- I
+r-^
1 » -1 ' \M 45 J , 30 Γ

(b) Bending fatigue (a) Fatigue (b) Creep-fatigue

Fig.1 Specimen configuration. Fig.3 Definition of energy Sp and Sc.

Specimen

=F

2C

Φ
-2W_

(a) Load conditions

d. c. current

■^ DC

& S 10

Crack
c
N
Electrical 10-' 10° 10' 102
COD^ 1 potential
GL=5mm Cyclic J-integral range, AJ(kgf/mm)
8(
)J
Fig.4 Relation between crack growth rate
(b) Measurement methods of and A J in axial fatigue test.
COD and electrical potential

Fig.2 Bending test apparatus and

measurement method of COD
and electrical potential.
290
10- 304 steel ' "'
RT, Bending fatigue

E
-i 10-

10-

z
O I

10-

+o
7 "2C ^ 3^i
".-*(&)
10-
10-' 10° 101 102
Fig.7 Definition of maximum bending
Cyclic J-integral range, AJ(kgf/mm)
stress.

Fig.5 Relation between crack growth

rate and AJ in bending fatigue
test.

Mod, 9Cr-1Mo steel

Axial creep-fatigue
500°C, tH=10min • 3 0 4 steel

u
O l da/dN . Bending creep-fat gue
A | dc/dlvf - 650°C, t H=10min
O da/dN Δ
Through crack Δ dc/dN
Axial 10Ί -
creep-fatigue

o/
g*
c©
Δ
Through crack
\ Axial creep-fatigue :

Q. 10"

Λ Ι - α _1 σ,Αδ, -

10"' 10°
Creep J-integral range, AJc(kgf/mm) Creep J-integral range, AJ c(kgf/mm)

Fig.6 Relation between crack growth Fig.8 Relation between crack growth
rate and A J c in axial creep- rate and A J c in bending
fatigue test. creep-fatigue test.
WS6e7

CREEP FATIGUE BEHAVIOR OF SUS304 STAINLESS STEEL

TESTED IN CARBURIZED SODIUM AT 550°C

T. ASAYAMA, H. KAGAWA, R. KCMINE and Y. WADA

O-arai Engineering Center, Power Reactor and Nuclear Fuel Development Corporation,
4002, Narita-cho, O-arai-machi, Higashi-Ibaraki, Ibaraki, 311-13, Japan

ABSTRACT

Creep fatigue behavior of SUS304 stainless steel in carburized sodium at 550°C was investi-
gated. Test duration was up to 6000 hours and the maximum carbon concentration at the sur-
face of the specimen was 0.46%. It was made clear that creep fatigue lives under the heavy
carburizing condition showed no life reduction compared with those in air environment. It
was implied that creep fatigue lives at low strain ragnes were governed by creep cavity nu-
cleation and growth inside the material rather than environmental effect which was restrict-
ed to the surface reagion of the material. Evaluation of creep fatigue life in carburized
sodium was shown to be possible based on the linear damage summation rule using the material
properties obtained in air environment.

KEYWORDS

SUS304; carburizing sodium; creep fatigue; environmental effect; linear damage summation
rule.

DJTCQDUCTION

In a secondary sodium loop of a fast breeder reactor which is composed of a steam generator
made of Cr-Mo steel and an intermediate heat exchanger made of austenitic stainless steel,
the material of the intermediate heat exchanger tends to suffer carburization during the
service period. In order to assess the integrity of the intermediate heat exchanger, one has
to evaluate creep fatigue strength of stainless steel under carburizing condition in liquid
sodium. Since the creep fatigue evaluation method for fast breeder reactors is constructed
on the basis of material properties obtained by experiments conducted in air environment, it
is necessry to confirm that creep fatigue strength in carburizing sodium is no less than
those in air environment.

Generally, in sodium, strucrural materials are subjected to less oxidization compered with
those in air environment and number of cracks initiated at the surface of the material is
also less than that in air environment. This makes the fatigue strength, which is mainly
goverened by propagation of cracks initiated at the surface of the material, increase in
sodium compared with that in air. On the contrary, creep strength and creep fatigue strength
which are goverened mainly by the nucleation and growth of cavities on grain boundaries in-
side the material, show little difference regardless of environment. However, in carburizing
sodium, there is a possibility that carburization accelerates the grain boundary damage near
the maetrial surface to cause a reduction of creep fatigue strength. In the present study,
the authors investigated the effect of grain boundary damage caused by carburization on the
creep fatigue strength of austenitic stainless steel SUS304 under carburizing condition in

291
292
liquid sodium.

EXPERIMENTAL PROCEDURE

Test Material and Test Facility

The material utilized in the present study was 304 stainless steel. The specimens were
machined from a plate with a thickness of 40 mm. The material was used in the solution con-
dition. Chemical compsition and mechanical properties of the material are shown in Table 1.

The configuration of the specimen is shown in Fig. 1. It is consisted of a normal creep

fatigue specimen used in air and a bellows which encloses the specimen. A spacer made of S45
C steel is placed in the inside of the bellows. This spacer decarburizes during creep fati-
gue tests and the specimen suffurs carburization. Test machine is an usual servo-hydraulic
creep fatigue test machine which is integrated into a sodium loop. In the present study,
static sodium was put into the bellows. Although carbon concentration in the sodium increas-
ed as the creep fatigue tests continues and decarburization of the spacer proceeds, change
of the cabon density could not be monitored with the appratus in the present study.

Strain was controled within an error of 5% by a LVDT attached to the two projections on the
shoulder of the specimen. Relationship between the strain and the displacement was obtained
by preliminary tests.

Test Conditions

Test temperature was 550°C. OxLgen density was kept less than lppm.

Triangular waveform with a strain hold time at a tensile peak was employed and experiments
were conducted under three conditions. The standard condition was a waveform at a strain
range of 1 % with a strain hold time of 1 hour. In order to investigate the effect of strain
hold time, a longer hold time of 10 hours was also introduced. For the purpose of obtaining
a longer duration creep fatigue data with a lower starin range, which seems to better re-
present the actual loading conditions encounterd in the fast breeder reactors, a waveform at
a strain range of 0.43% with a strain hold time of 1 hour was also employed. In all the
cases, the strain rate at loading/unloading portion was 0.1 %/sec.

Carbon Content Analysis and Visual Observation of Tested Specimens

Carbon penetration profile near specimen surface was determined for all the specimens after
the creep fatigue tests. Five thin foils with a thickness of 0.2mm were sliced from the
surface of the specimens. Those foils were sliced from the portion between the shoulder of
the specimen and the adjustment for the bellows.

Table 1. Chemical composition and mechanical

properties of the material
investigated. G LS 2 Portio
n of
displacemen
t
detec
t

c Si Mn P S Ni Cr
Portio
n of displacemen
t detec
t
0.05 0.60 0.87 0.026 0.002 8.94 18.59

(a) Specimen for testing ( b) Specimen for testing

0.2% Yield strength Tensile strength Elongation in air in sodium
'' ligf/mm* kgf/mm2 %
R.T. 23 64 63

550'C 12 39 40 Fig. 1. Specimen configuration.

 293
EXPERIMENTAL RESULTS

Carbon Content and Fracture Surface

Carbon content profiles near specimen surface after the creep fatigue tests are shown in
Fig.2. The depth of the carbon penetration is approximately 200//m. It seems that a longer
test duration leads to a deeper carbon penetration. The maximum carbon concentration of 0.46
wt% was observed on the spcimen at a strain range of 1% and a strain hold time of 10 hours.
The maximim carbon concentration expected in a fast breeder reactor whose secondary loop is
consisted of an intermediate heat exchanger made of 304 steel and a steam generater made of
2 l/4Cr-lMo steel is approximately 0.1% at the maximun assuming that the intermediate heat
exchanger and the steam generater are operated for 200,000 hours at 505 °C and 470°C respec-
tively. So, the carbon concentration in the sodium realized in the presentstudy is consider-
ably higher than is expected in practical conditions.

SEM observations of the fracture surfaces revealed that all the specimens showed inter-
granular fracture. Figure 3 shows an example of the intergranular fracture surface at a
strain range of 0.43 %.

Longitudinal sections of the specimens near fracture surface were observed by optical micro-
scope. A number of surface cracks were observed at a strain range of 0.94% with a strain
hold time of 1 hour and at a strain range of 0.98 % with a strain hold time of 10 hours. All
of those cracks were initiated on grain boundaries and propagated along them. On the
contrary, at a strain range of 0.43 %, despite that a number of intergranular cracks were
observed in the bulk of the specimen near fracture surface, only one surface intergranular
crack with a length of about two grain diameters was observed. Examples of longitudinal sec-
tions at a strain range of 0.43 % with a strain hold time of 1 hour and at a strain range of
0.94% with a strain hold time of 1 hour are shown in Fig.4.

From the above observations, we can obtain the following result regarding the creep fatigue
tests conduted in carburizing sodium. In the case of relatively high strain ranges and short
test durations, fracture occured by the propagation of intergranular cracks initated on the
surface of the specimens. On the contrary, in the case of lower starin ranges and relatively
longer test duration (approximately 6,000 hours), fracture occoured by the growth and coa-
lescence of intergranular cracks initiated in the bulk of the specimen.

Creep Fatigue Life

Result of the creep fatigue tests in the carburizing sodium is shown in Fig.5. Indicated in
Fig.5 are the presently obtained resluts (indicated by φ A ) »creep fatigue test results

0.6
*
(X)
k
(hr) *
(cyde)
* 11
(hr)
o 0.94 1 4SS 458 1
0.5 - Δ 0.43 1 631· 6333
a 0.9·
10 2S3 2531 |

~ 0.4

'w
| 0.3
\
c

hi\V
o
t 0.2
o
0.1
S=6=9
0 0.4 0.8 1.2
Distance from surface

Fig. 2. Carbon concentration after creep fatigue t e s t s .

294

Fig. 3. Example of intergranular fracture.

Fig. 4. Example of longitudinal sections.

in air (indicated b y O , Δ ) and creep fatigue test results in pure sodium (indicated by □ ) .
Dashed line in the figure represent the average fatigue strength of 304 steel in air envi-
ronment (Wada et al, 1987).

For the tests with a strain hold period of 1 hour, the creep fatigue strength in the carbu-
rizing sodium is almost the same as the strength in air irrespective of strain ranges. Bbr
the case of 10 hour strain hold, the creep fatigue strength seems slightly less than that in
air, but the difference is very small and it was condidered to be negligible. To sum up,
reduction of creep fatigue life did not occur even in a carburizing condition that was so
severe that the carbon concentration at the surface of the specimen reached more than 0.4%
at the end of the creep fatigue tests.

D Sodium (Fatigue, different heat)

o.i 1 ' ■ 1 ' > ■ 1
10 2 10 3 10 4 10 5
Number of cycles to failure (cycles)

Fig. 5. Creep fatigue strength in carburized sodium.

EVALUATION OF TEST RESULTS

Creep Fatigue Damage Evaluation

 295
Figure 6 indicates the creep fatigue damage calculated based on the stress-strain response
and the stress relaxation behavior obtained by the experiment. The line in the figure indi-
cates the criteria of Campbell. The present results are indicated by φ . The results in air
environment (indicated by O » Δ ) and the results in pure sodium (indicated by A ) are also
plotted in the figure. Fatigue damage per one cycle is calculated according to the following
equation,

1/N (1)

where Nf is fatigue life and calculated using the average fatigue strength in air (Wada et
al, 1987; Aoto et al, 1987; Wada et al, 1986; Yoshitake et al, 1986). Creep damage per one
cycle is calculated by the following equation,

th
J* dt/t (2)
0 r
where tr is creep rupture time and calculated using the average creep strength in air (Wada
et al, 1987; Aoto et al, 1987; Wada et al, 1986; Yoshitake et al, 1986). th is strain hold
time. Figure 6 shows that the result in the carburizing sodium is plotted closer to the
critera of Campbell than is the result in air environment. This result should be attributed
to the particular strain harding which is alledged to occur in sodium environment (Huthmann
et al, 1981).

Life Evaluation Based on the Linear Damage StTmmation Rule

The creep fatigue life in carburizing sodium was evaluated by the linear damage summation
rule based on the average fatigue strength and the average creep strength obtained in air
environment. Fatigue damage is calculated by Equation (1) as described above. Creep damage
is calculated as following. First, the stress at the begining of relaxation is obtained as a
half of a stress range calculated by the stress-strain relationship at half life correspond-
ing to a given strain range (Wada et al, 1987; Aoto et al, 1987; Wada et al, 1986; Yoshitake
et al, 1986). Next, stress relaxation curve is estimated by the average creep strain curve
in air (Wada et al, 1987; Aoto et al, 1987; Wada et al, 1986; Yoshitake et al, 1986) and the
strain hardening rule. Using thus obtained stress relaxation behavior, creep damage is cal-
culated by eaution (2) based on the average creep rupture strength in air. The result of
damage evaluation is shown in Fig.7. Figure 7 shows that the imaginary damage calculated
based on the fatigue strength and the creep strength in air is plotted closer to the
Campbell criteria than the damage calculated based on experimentaly obtained stress strain
response (see Fig.6). Predicted creep fatigue lives based on Fig.7 is shown in Fig.8. All of
the data are evaluated within an accuracy of a factor of 2. Those results made clear that,
as far as investigated in the present study, it was reasonable to evaluate creep fatigue
lives in carburizing sodium by the linear damage summation rule using the material proper-
ties obtained in air environment.

SUS304, 5 5 0 C SUS304. 5 5 0 C

\ Δ
O
o
o
o
o

• \ 0
* \
o

•oCarburising sodium
Air • Carburising (odium
o Air
A Sodium (Different haat) A Sodium (Different heat)
Δ Air (Different heat) Δ Air (Different heat)
1
0.01 0.1 , I
0.01 0.1
Creep damage D c Creep damage De

Fig. 6. Creep / Fatigue damage calculated Fig. 7. Creep / Fatigue damage calculated
based on experimental results. based on the method proposed in
the present study.
296
ιο4
SUS304. 550*C

z
&
Z 103
A
0)
υ
'•5
Φ
•
0
Carburising sodium
Air
|

▲ Sodium (Different heat) |

Δ Air (Different heat) |

102
V Ί03 Ί0 4
Observed life N (0 BS

Fig. 8. Prediction of creep fatigue lives in carburizing sodium.

Environmental Effect in Low Strain Reagion

The result of the observation of the fracture surfaces of the specimens tested in the car-
burizing sodium revealed that the fracture mechanism at relatively low strain ranges was
different from that at relatively higher strian ranges. That is, at relatively high strain
ranges and short test durations, fracture occurred by the propagation of intergrunular
cracks which were initatied on the surface of the specimens, while at relatively lower
strain ranges and longer test durations, fracture was caused by growth and coalescence of
intergranular cracks which were initiated on grain boundaries inside of the specimen. On the
other hand, since the degree of carbon concentration at the surface of the spcimens was
almost the same irrespective of test conditions (see Fig.2), it is implied that the degree
of grain boundary damage near specimen surface was also the same irrespective of test con-
ditions. Therfore it is inferred that fracture mechanism is determined by strain range
imposed provided the grain boundary damage near matrial surface is at the same degree. To
sum up, at low strain ranges, creep fatigue strength is governed by nucleation and growth of
creep cavity inside of the material rather than environmental effect which is restricted to
the surface of the material.

CONCLUDING REMARKS

Creep fatigue lives in carburizing sodium were almost the same as those in air environment,
althogh the maximun surface carbon concentration reached as high as 0.46%.

It was implied that environmental effect on the initiation of creep fatigue cracks on the
surface of a specimen was less pronounced at low strain ranges because cavity nucleation
inside of the material became more dominant.

As far as investigated, creep fatigue lives in carburizing sodium were reasonably evaluated
by linear damage summation rule based on the material properties obtained in air.

REFERENCES

Aoto, K., Y. Wada and R. Komine (1987). PVP, 123, 43.

Mrano, M., K. Kitao, I. Nihei and A. Yoshitake (1984). Liquid metal engineering technology.
BNES, London.
Huthmann, H. and G. Menken (1981). Conf. Mater. Behavior and Physical Chemistry in liquid
Metal Systems, Karlsruhe.
Wada, Y., K. Iwata, K. Aoto and Y. Kawakami (1986). Proc. Int. Conf. on Computational
Mechanics, 1, IV-25.
Wada, Y., Y. Kawakami and K. Aoto (1987). PVP, 123, 37.
Yoshitake, A, Y. Wada and M. Mrano (1986). Proc. Int. Conf. on Creep, 441.
WS6e8

CREEP LIFE ASSESSMENT OF AUSTENITIC STAINLESS

STEEL WELDMENT AT 873-1073 K.

V.M. Radhakrishnan and M. Kamaraj.

Metallurgical Engineering Department,
Indian Institute of Technology,
Madras - 600 036. India.

ABSTRACT

Investigations have been carried out to study the creep crack growth behaviour
in austenitic stainless steel weldments in the temperature range of 873 K -
1073 K. In the fully established creep deformation condition it is observed
that the energy rate line integral in the steady state region, C*s , can be
related to the rupture time t r in the form
C*s- t r = R
where R is a material constant. Based on this relation the creep life of
cracked material has been assessed. In the weldment formation of sigma
phase and other carbides provides the nucleation sites for crack propagation.

Keywords

Austenitic steel weldment; creep; energy rate line integral; creep crack
propagation; life assessment.

INTRODUCTION

Austenitic stainless steels are widely used in nuclear power plants and weld-
ing is normally employed for joining critical junctions. In order to incre-
ase the resistance to solidification cracking austenitic weld metals are
designed to contain a controlled amount of delta ferrite. Since this phase
is unstable at elevated temperature, several other constituents such as
chromium carbides and sigma phase can form during high temperature service.
Welding introduces a number of crack like defects such as lack of fusion,
lack of penetration etc., which will act as nuclii for crack initiation and
subsequent growth under creep conditions. The micro-structural changes due
to the transformation of delta ferrite will accelerate the process of creep
crack growth and final fracture of the component. The present investigation
has been undertaken to characterize the creep crack growth behaviour and
the precipitation morphology and its role in the structural degradation in
austenitic stainless steel weldments in the temperature range of 873 K to
1073 K.

297
298
EXPERIMENTAL
The materials used in the present investigation are (1) Types 316 and 304L
stainless steels annealed in vacuum at 1325K for 20 min. and (2) Type 308 Cb
stainless steel supplied by Messer. Grieshem and Co., Germany, containing an
initial delta ferrite of 4 FN. Welding in types 316 and 308L stainless steels
was made using electron beam welding. In type 308 Cb, autogenous weld metal
was obtained using microplasma welding. The ferrite number of the as-welded,
measured by ferritescope, has been found to be in the range of 3 to 3.5 FN.
Creep crack growth experiments were carried out in a constant load creep test-
ing machine at specimen temperatures of 873, 973 and 1073 K. Sheet specimens
of 0.5 mm thick, 15 mm width and 150 mm length were used with the weldment at
the middle. A starter crack of length 2.0 mm was used to localize the crack
nucleation and propagation in the weld metal. The load point deflection and
the crack length were measured at regular intervals of time with an accuracy
of 0.01 mm. The maximum test duration was 1200 hours. The crept specimens
were examined under optical microscope and STEM. The different phases that
formed during the creep deformation were identified using Philips PW 1050 X-ray
diffractometer. Details of the experimental procedure are given elsewhere
(Kamaraj, 1990).

RESULTS AND DISCUSSION

Crack Growth Characterization
It has been observed in all cases that in these tensile mode of creep deforma-
tion the creep crack growth always started when the entire material was creep-
ing and the deformation was in the steady state condition. Parameters like
stress intensity factor and net section stress have been tried to describe the
creep crack growth (CCG) rate, but the scatter was large (Kamaraj and Radha-
krishnan, 1989). The energy rate line integral, C*, given by the relation
(Webster, 1983)
n PAC
C* = — (1)
(n+1) B(W-a)

10
(kWh) 1
Fig.l. Relation between creep crack growth rate and C*.
Open symbols - base metal data and closed symbols-
weldment data.
 299
has been found to give a good correlation. P is the load, Ac is the load
point deflection rate due to creep ( Component due to elastic compliance has
been deducted from the experimental values of LPD rates). B is the thickness
and W is the width. 'a' is the crack length and 'η' is the creep stress
exponent. The relation between the CCG rate, da/dt, and the parameter C*
is shown in Fig.l. and is given by
da/dt = A (C*) (2)
where A is a constant and the exponent ! r' is almost equal to one in all the
cases. As the creep deformation was observed over the entire gauge length
when the crack starts growing, the Ct parameter (Saxena, 1986), applicable to
small scale creep zone, has not been tried. Further, in a tensile creep
when there is a small scale creep zone just ahead of the crack, this zone will
experience a stress relaxation as it is surrounded by an elastic zone and
hence free creep deformation cannot take place.

It has been observed that the rupture time, t r , is related to the steady
state energy rate line integral, C*s . The relation is shown in Fig.2., for
the three materials tested. The governing equation can be written in the form
C* . tT (3)
R is a constant whose value has been found to be 130, 55 and 140 kJ/m .h
for the three materials 316, 304L and 308 Cb stainless steels respectively.
The above relation is similar to the Monkman-Grant relation. Thus, knowing
the initial defect size and the value of the constant R of the material
used, the rupture time can be estimated if the loading conditions are fixed.
The energy input rate as a parameter for life prediction has also been
extended to high temperature low cycle fatigue with hold time effects
(Radhakrishnan, 1987).
301—

-10

+ «o
o
o · 316 SS
a . 308Cb
Δ
I * 304LSS

0-1
1
Rupture time t r (h)
Fig.2. Relation between steady state energy rate line
integral and the rupture time. Symbols same
as in Fig.1.
300

Fig.3. SEM Micrograph of as-welded

structure.

Fig.4. Carbide precipitation Fig.5. Sigma phase (dark) transform-

at 873 K. ed from ferrite at 1073 K.
Metallurgical Factors
The as-weld microstructure shown in Fig.3, consisted of austenite and delta
ferrite having a discontinuous vermicular morphology. The ferrite content of
the crept samples was found to be around 1 FN. The decrease in the ferrite
number in the weldment after exposure to elevated temperature has been attri-
buted to the formation of carbides and sigma phase (Kamaraj and Radhakrishnan,
1990, Edmond et al. 1978.). These transformation products have been detected
by STEM and X-ray analysis. Examination of thin foils by STEM reveals the
carbides and sigma phase. Typical carbide formation at 873 K and sigma phase
formation at 1073 K are shown in Fig.4 and 5 respectively for 316 stainless
steel weldment. At 873 K, the carbide M23C6 formed at the ferrite- aus -
tenite boundaries. The sigma phase formation accounted for most of the decr-
ease in ferrite content at 973 and 1073 K. At higher temperature the disso-
lution of delta ferrite is faster and the growth of sigma phase is rapid.

Typical crack growth and the microstructural aspects associated with cracking
are shown in Figs.6 and 7 for 316 stainless steel weld tested at 973 K. At
this temperature the predominant phase is sigma and the crack nucleation
starts at the interface between the primary sigma and austenite. At 873 K
carbide precipitation is pronounced and the crack growth is along the inter-
face between austenite and delta ferrite. At 1073 K the vermicular delta
ferrite breaks into spherical particles within a short time. Here also
 301

Fig.6. Secondary cracks ahead of Fig.7. Crack nucleation at the sigma

the macro-crack at 973 K. austenite interface at 973 K.

secondary cracks have been observed between sigma-austenite interface. Crack

propagation takes place by linking of these micro-cracks.
Life Estimation of Cracked Components
The product relation between the steady state energy rate line integral C*s
and the rupture time t r as given by equation (3) provides a good basis for
life estimation of cracked components subjected to tensile type of creep.
Taking the load point deflection rate due to creep as (Webster, 1983)
A c = C„Pn (4)
where C n is a measure of creep compliance, and substituting the same in eqn.
(1) and simplifying (Radhakrishnan et al. 1990), we get the relation between
the stress,CT^, the rupture time, t r , and the crack length, a/W, as
1 - a/W = (C ol / R ) 1 / ( n + 1 ) (f (tr ) 1 / ( n + 1 ) (5)
where C0i is a constant. Typical relation between the normalised crack
length, a/W and the rupture time, t for 304 L stainless steel is shown in
Fig.8. For a given crack length and the applied stress, the rupture time
will be longer if the value of the material constant R is higher. The above
procedure appears to be very simple and can be readily applied in the field
if the material constant R is evaluated experimentally.

CONCLUSIONS
From the investigations carried out to study the creep crack growth behaviour
of stainless steel weldments in the temperature range of 873-1073 K under
plane stress condition the following conclusions are arrived.
(a) The energy rate line integral C* can be used to correlate the creep
crack growth rate.
(b) The steady state value of the energy rate line integral, C*s at the time
of crack initiation correlates very well with the rupture time, t r given
in the form
C*s. t r = R
where the material constant R is a measure of the resistance of the
cracked component to creep failure.
(c) The above relation can be effectively used to predict the creep life of
cracked components.
(d) Delta ferrite in the weld metal gets dissolved when exposed to elevated
temperature. Carbides and sigma phase are formed. Crack nucleation
starts at the interface between the primary sigma and austenite. Crack
propagation takes place by linking of micro-cracks.
302

I* 5
i<r Rupture time (h)
10
Fig.8. Creep life estimation of cracked components with
different initial crack lengths.

REFERENCES
Edmond, D.P., D.M. Vadegriff and J. Gray (1978). in Properties of steel
weldments for elevated temperature pressure containment applications.
ASME MPC-9, 47-51.
Kamaraj, M. (1990). Some studies on creep crack growth behaviour of austenitic
stainless steels and their weldments. Ph.D. Thesis, I.I.T., Madras.
Kamaraj, M. and V.M. Radhakrishnan (1989). High temperature crack growth
in austenitic weld metals. Engg. Frac. Mechanics, 33(5), 801-811.
Kamaraj, M. and V.M. Radhakrishnan (1990). Structural changes and creep
cracking in type 316 stainless steel weldment. Trans. I.I.M., in press.
Radhakrishnan, V.M. (1987). Effect of hold time in high temperature low
cycle fatigue. Proc. ICM-5, 2, 1005-1011.
Radhakrishnan, V.M., M. Kamaraj and V.V. Balasubramaniam (1990). Life
estimation of cracked stainless steel components under creep conditions.
Trans. A.S.M.E., JEMT, in press.
Saxena, A. (1986). in Fracture Mechanics, ASTM STP 905, 185-201.
Webster, G.A. (1983). Crack growth at high temperature, in engineering
approaches to high temperature design, (eds) B. Wilshire and D.R.J. Owen.
Pineridge Press, Swansea, U.K., 1-55.
WS6e9

OPTIMIZATION OF A LIFE PREDICTION METHOD

FOR ENVIRONMENTALLY ASSISTED DAMAGE OF COMPONENTS
OPERATING AT HIGH TEMPERATURE

P. AGATONOVIC and N. TAYLOR

MAN Technologie AG, Munich, Germany

ABSTRACT
The life of high temperature components is limited by creep, fatigue and environmental
damage mechanisms. A comphrensive programme of creep-fatigue tests on Alloy 800H at
temperatures above those covered by existing design rules has shown that oxidation pene-
tration during the hold time accelerates crack initiation under cyclic loading. This defines an
important interaction mechanism which has to be considered for reliable component life
prediction. Based on these results a modified strain range partitioning life prediction meth-
od is proposed. The method has been verified for a wide range of literature data and also for
component stress-strain history simulation tests.

KEYWORDS
Creep-fatigue-oxidation interaction, life prediction, verification of life prediction method

INTRODUCTION
The sources of life exhaustion and damage accumulation limiting the useful life of industrial
components in service at high temperatures lie in the three main areas of fatigue, creep and
environmental damage. The general relationships between these and their interaction be-
come more and more complicated with increasing service temperatures, as are demanded
for high temperature components in advanced power generation, aerospace and engine
applications. However, as an example, the design of the conventional power plant compo-
nents has been based up to now essentially on proven rules and standards. These use simple,
conservative techniques, such as independent creep and fatigue life curves and linear dam-
age summation. Such conventional life assessment methods, involving simple addition of
the various contributions to the overall damage may prove inadequate for more arduous
conditions and cannot be recommended for the accurate evaluation of the life capacity of
novel components.
Furthermore for creep-fatigue situations the usual classification of the stages of damage
development, which is based on fatigue experience, is significantly complicated by the intro-
duction of creep mechanisms and their interaction with the fatigue processes. Creep defor-
mation involves grain boundary sliding with void nucleation and growth in bulk of the mate-
rial. The combination of local crack growth on the one hand and creep damage throughout
the material volume on the other makes the separation and corresponding treatment of
303
304
crack initiation and crack growth for the purposes of the life assessment extremely difficult.
Because of this, in the high temperature range the "local event" approach to life analysis, as
in the case of crack initiation, has to be extended to a more general approach based on dam-
age incubation and considering both, local crack development and early growth, as well as
bulk damage (Agatonovic and Taylor, 1990a). For this purpose identification of damage
mechanisms plays a very important role. Examination of creep-fatigue specimens indicates
that, for different combinations of cyclic inelastic deformation, creep and environmental
effects, different damage and failure mechanisms are possible. Obviously transfer of data
associated with a particular fracture mechanism to conditions where other mechanisms oc-
cur cannot be recommended if large inaccuracies are to be avoided.

SELECTION OF THE LIFE PREDICTION METHOD

With current life prediction technology, the different models available range from the pure-
ly phenomenoloeical to the physically based. A method of damage assessment based on mi-
crograph ically observable details, as discussed above, could potentially provide a more ac-
curate model for life prediction. With this goal in mind a cooperative project within the EC's
BRITE programme has been started. Based on previous experience and literature compari-
sons the Strain Range Partitioning (SRP) Method was initially selected. Among different
creep-fatigue life prediction
procedures SRP is most di-
rectly concerned with fati-
gue—with—dwell situations.
While it relates cycle life to
macroscopic parameters
such as the inelastic strain
range, it has as its foundation
the concept relating damage
development to microscopi-
cally observable details. It
was developed by Manson et
al (19??) after extensive te-
sting with different wave
forms. Between these, tensile
dwell CP conditions are the
most damaging, leading to a Fig. 1. Life prediction according to the SRP Method
reduction in life up to an or
der of magnitude compared to the pure fatigue PP life (Fig. 1). If under practical conditions
both PP and CP components of inelastic strain are present, it is logical to expect that the
life lie between these lines. For a maximum f^p = Ä€cp/A€jn = 1 the life corresponds the
CP line. Based on this the general relationships can be established:
J_ fpi
IZL Jcp ffpc fee
= (I)
Ni Npp(A€in) Ncp(Aein) Npc(Aeit1) Ncc(Aein)
Investigations of different materials by a number of researchers (including the method's
original proposers) show the necessity of considering a time effect at higher temperature.
For instance the reduction of creep ductility with increasing rupture life is well established
experimentally. To account for this Haiford et al ( as reported by Manson, 1982) proposed
the ductility-normalised SRP equation, which incorporates the creep rupture ductility as a
function of time. Using this correction the predictions can be improved. However according
to Day and Thomas (1985) it does not sufficiently improve correlation with experimental
data. Their tests showed substantial differences in test duration with different applied dwell
stress levels, and to compensate for this the CP life relationship was modified as snown here:
1 = J£E-
_L. fpp
· ^— (2)
Nt N,PP <-*">
 305

where the constant k is fitted from experimental results. Similarly in recent work Manson et
al (1987) have applied several forms of correction relating to the dwell or test time to the CP
life relationship.
ay
• » vocuum
S Δ 7<Xrc air
3
2 A " vacuum
CO.i
Δ j A** £ O 800 eC air
0^.0
3
• * vacuurr
A
I! ^ * Δ 700"C air AS
V^ A * vacuum
0.3
2xl02 l0
^L _
I0 4
0.1
2xl0 2 I04
MNpp
l0
Npc
(a) (b)
2.0, 2.0 — 5
s^ »"V
1.0 1.0

£0.5 20.5 PH.

N-l
O 8 0 D eC air \ rv
Ί
Sc
< • *
Δ 700'C air
vocuum O 800"C oir Γ '^
vacuum
□ 55C7C air Δ700·0 air
s
Ιιι air (aged) 0.1 =
J — JM ill
2
4x10 I0 5xl0 3
Ncp Ncc
(c) (d)

Fig. 2: The influence of environment on the cyclic life of SU 304 (Tokimasa, 1988)
These simple empirical modifications could improve predictions but their physical back-
ground was not clear. Moreover, the correction of the CP life relationship is not compatible
with the experimental results of Tokimasa (1988) shown in Fig. 2 presenting the life curves
for SUS 304 in air and va-
cuum. For both the CP
and PC data no effect was
observed. On the other
hand, in the PP and CC
tests a large difference is
found between air and va-
cuum, indicating that the-
se cycle forms are quite
sensitive to the air envi-
ronment. In fact, as shown
in Fig. 3, damage develop-
ment under CP conditions
occurs in the bulk of the
material, and therefore
cannot be influenced by
environmental effects.
Consequently the time
Fig. 3. Grain boundary cavitation in an Alloy 800H CP modification of CP life
specimen tested at 850 °C (x10). may not be correct.
TEST RESULTS
An advanced design method intended for high temperature should obviously follow the log-
ic developed in the preceding discussion with key attempt concerning interaction mecha-
nisms, their consideration is necessary to allow more precise life prediction. With this in
mind, an experimental investigation of the creep-fatigue behaviour of the austenitic Alloy
800H has been performed (Agatonovic and Taylor, 1990). The baseline PP and CP tests
were carried out at the relatively high temperature of 850 °C, chosen to be considerably
above that for which design standards currently exist for this alloy. Verification tests, incor-
porating a hold time at constant strain (relaxation), were then carried out to allow the pre-
dictions based on the PP and CP data to be checked. The test conditions were chosen to
306
produce significantly longer test durations compared to the basic PP and CP tests. After
analysis of the results of these tests, however, the necessity of performing further tests at
lower temperatures became obvious, and subsequent test series were performed at a ranee
of temperatures down to 750 °C. Besides recording the entire test histories for later analy-
sis, all specimens were metallographically examined.

Fig. 4: Verification test results plotted against Fig. 5: Comparison of the verfication test
the strain hold time. results with the PP and CP data.

Figure 4 shows the results of the verification tests plotted against the strain hold time and
compared with lifetime prediction. It can be seen that the relaxation period has a very strong
effect in reducing the cyclic life, and no trend towards saturation is observed with increasing
hold time. In Fig. 5 these data are compared with the PP and CP results. If the SRP model is
to be valid, the verification test results should lie between the PP and CP data loci (see Fig.
1). However they are found to lie closest to the CP results and with increasing hold times
tend to cross over the CP life line. Since the CP partition (fCP) in these tests is less than 0.4,
the SRP approach would jpredict lifetimes closer to the PP data. This indicates that the dam-
age occurring during the long time verification tests may be more severe than that produced
during the relatively short constant stress CP tests.
5
*10r 25.0 1 1 1

— o
3 0

15 0
I · Crack Initiation o
o
"I

& 10.0 -
^ o o ° 0° o0
ooo θ ο 0 οο ο ° 0° 0° 0 ο 0 θ° 0

5.0
r
0.0 I I I
2000 4000 6000 8000
Cycle No.
Fig. 6: The change in hold time mean Fig. 7: SRP predictions using ductility
creep rate during a CP test. normalisation and the CP crack initiati-
on criterion as in Fig. 6.
Before looking to improved methods, however, effort was firstly concentrated on improving
some features of the prediction procedure known to be less well defined or less reliable.
Determination of the mean creep rate during the stress hold period of each cycle in a CP test
allows examination of the change in this rate over entire test (Fig. 6). Initially the creep rate
 307
increase is practically linear, indicating that the number of the cavities is also increasing
approximately linearly. The non-linear increase in creep rate caused by accelerated cavity
growth, coalescence and cracking near the end of the test can define what we call damage
incubation and the subsequent transition used as a more accurate and sensitive criterion of
"crack initiation". The improvements in the life prediction afforded by introducing this cri-
terion proved, however, insufficient. Therefore it was found necessary to additionally in-
clude a ductility normalisation correction. In this way all but one of the results could be
predicted to within a factor of two (Fig. 7). The predictions nevertheless remain on the non-
conservative side and the error is seen to increase with increasing dwell time. As a conse-
quence for increased lifetimes, as may be required for real components, the applied correc-
tions may no longer be adequate. In summary, the trend of the present results cannot be
accounted for by these corrections, and some additional influences must be present.

METALLOGRAPHIC INVESTIGATIONS
The shorter than expected cyclic lives found for the verification tests made post-test metal-
lographic investigations of particular importance. Examination of longitudinal sections
provided evidence that surface cracks played a significant role in failure. While internal
damage in the form of grain boundary cavitation was also found, the results appear to pro-
vide clear evidence that enhanced surface cracking was responsible for the strong relaxation
hold time effect. As seen in Fig. 8, the cracks growing at surface grain boundaries appear
heavily oxidised. Due to the more rapid diffusiion and the sensitisation of the material adja-
cent to the grain boundaries areas for this alloy, oxidation penetration along grain bound-
aries is faster than into the bulk material. The chemistry of this process has been confirmed
by EDAX analysis of the composition of the affected regions. These grain boundary oxides
are brittle relative to the unoxidised material and fracture more easily. As a consequence
this type of oxidation accelerates fatigue crack initiation and growth at very high tempera-
tures. It emerges as an important damage mechanism and implies that the necessary time
correction to the SRP method should be applied not to the CP life portion but to the PP one.
This is in full agreement with Tokimasa's results shown in Fig. 4.

Fig. 8. Oxidised grain boundaries in a verfication specimen tested at 850°C (x200)

LIFE PREDICTION CONSIDERING AN ENVIRONMENTAL EFFECT

On the basis of the above discussion the following modified SRP formula is proposed, in
which a time parameter, a, is applied to the PP term:

N Npp a + Ncp (3)

Liu and Oshida (1986) have shown the effect of the embrittled surface region depends on
the size of affected zone or the exposed grain boundary length. Their expression for the rate
308
of oxidation penetration along grain boundaries leads to the following relation for the time
and temperature dependence of a:
a = a.xn-e-QIRT (4)
where Q is an activation energy. The verification test data was re-analysed to determine the
necessaiy a and n values needed to achieve accurate predictions (Fie. 9a). The temperature
dependence term was determined from the series ot relaxation dwell tests at different tem-
peratures but with the same strain range (Fig. 9b).

(a) (b)
Fig. 9. Evaluation of the environmental correction factor a.

(a) (b)
Fig. 10. Comparison of life predictions using (a) the standard SRP method and (b)
using the modified SRP method with an environmental correction term.
 309
VALIDATION OF THE METHOD
The validation of any design method requires a lengthy process, involving evaluation of test
and operational evidence, and consideration of a number of possible random influences,
such as charge-to-charge material variability, scatter of the basic data and component re-
lated effects. As a preliminary step a limited verification procedure was carried out by com-
paring the predictions with the available literature data for Alloy 800H. A broad search was
performed to find all relevant results, although these were restricted by the fact that only
tensile strain hold tests could be considered. The data found are detailed by Agatonovic and
Taylor (1990). Firstly the life prediction was performed using the conventional SRP method.
The results (Fig. 10) show large scatter and a trend to non-conservative predictions which
becomes even more critical as the total test time increases. On the other hand, the predic-
tions using the method developed above are seen to be very accurate, despite the fact that
the data comes from a number of different sources. Deviations are seen to be almost com-
pletely within a factor of two on life, and no trend with regard to test duration is evident. This
demonstrates the high extrapolation capability of the method.
For further verification of the method additional life tests to simulate component stress-
strain history has been performed. From the viscoplastic analysis of a plate-with-hole com-
ponent, described by Agatonovic and Taylor (1990b), the stress-strain hysteresis shown in
Fig. 11 was calculated at the critical notch root position. The key feature of this hysteresis is
the relaxation behaviour, which could be approximated by the generalised Neuber formula:
a' ep = const. (5)
where the exponent p has a value of 2. Depending on the conditions on the particular com-
ponent this exponent can also take different values. It was therefore decided to carry out a
series of cyclic tests incorporating a relaxation period of this type in which the Neuber
stress-strain relationship for different p values would be simulated. All the tests were per-
formed at 850 °C, for which oxidation conditions are the most pronounced for the range of
temperatures investigated.
Life prediction via the standard and modified SRP methods was carried out after partition-
ing the saturated hysteresis loops. These are compared with the experimental data in Fig.
12. (Also included are results of tests to simulate the stress-strain history at a critical point
on a turbine disk.) It is clearly seen that the modified SRP method provides accurate predic-
tions for all the tests, with the results falling within a factor of two of the predicted life. In
contrast the predictions made using the standard SRP correction are seen to be strongly
non-conservative. This tests therefore confirm the trend shown by the verification tests and
provide further evidence of the accuracy and reliability of the modified SRP model.
iau —i 1 1
Relax. Test 0 = Notch: SRP Method
J P = 2.0 (1.7) itf
100
1 P = ΐΤθ (0.9) " 0 = Disk: SRP Method
· = Notch: Modified SRP
...P.f.M &.3L. :
♦ = Disk: Modified SRP
' / '
2
50 Jy ^"**^fcJ >
/
0
/ " I io3 -t / ^
Vo 1
II
t ~_
= / j / >
(7) -50 -
? / /
100
^SBS- 102 £ y S Alloy 800H, 850°C _

.ιςη —L 1,,. . 1
5*101
-0.35-0.25 -0.15 -0.05 0.05 0.15 0.25 5*1θΊθ 2 10J 10'
Strain, ε % Predicted Life
Fig. 11: Hysteresis loops from tests Fig. 12: Life predictions for the compo-
carried out to simulate notch stress- nent stress-strain history tests.
strain histories..
310
CONCLUDING REMARKS
The combined effect of creep-fatigue and oxidation under cyclic and dwell time conditions
is found to be much more damaging than the creep-fatigue alone for Alloy 80ÖH at high
temperatures. Due to oxidation penetration during the hold time pure fatigue crack initia-
tion caused by the loading cycle is accelerated. This defines the main form of interaction
mechanism which has to be considered by the life prediction procedure. A modified SRP
method is proposed which accounts for this interaction in a physically meaningful way. Veri-
fication of the method on the basis of literature data and component stress-strain history
simulation tests has shown reliable life predictions for temperatures considerably above the
limits defined in the current standards to be possible. Since similar behaviour can be ex-
pected for a number other high temperature alloys whose environmental sensitivity over
long dwell times is well known the developed method may significantly contribute to the
progress in life prediction technology.

ACKNOWLEDGEMENTS
The support of the European Commission for this work through the BRITE programme
is gratefully acknowledged.

REFERENCES
Agatonovic, P. and N. Taylor (1990a). Establishing a Reliable Life Prediction Method for
Creep-Fatigue Interaction at High Temperatures. In: Creep and Fracture of Engineering
Materials and Structures, Institute of Metals.
Agatonovic, P. and N. Taylor (1990b). Computer Aided Predictive Methods. In: Advanced
Materials Technology International 1991. Sterling Publications, 212-214.
Day, M.D. and G.B. Thomas (1985). Fatigue and Fracture of Engineering Structures. 8.
p.33-46.
Kalluri, S., S.S. Manson, G.R. Halford (1987). Exposure Time Consideration in High Tem-
perature Low Cycle Fatigue. Mechanical Behaviour of Materials V. Pergammon Press.
Liu, H.W. and Y. Oshida (1986). Grain Boundary Oxidation and Fatigue Crack Growth
at Elevated Temperatures. Theoretical and Applied Fracture Mechanics. 6. 85-94.
Manson, S.S. (1982). A Critical Review of Predictive Methods for Treatment of Time-inde-
pendent Metal Fatigue at High Temperatures. Jn: Pressure Vessels and Piping Design
Technology. Ed. Zamrik, S.Y., ASME, p.203-225.
Tokimasa, K. (1988). Effect of Environmental Air on the Creep Fatigue Fracture Behaviour
of High Temperature Structural Materials. In: High Temperature Creep-Fatigue (Cur-
rent Japanese Material Research Vol. 3). Ohtani, R. et al (eds), Elsevier Applied Science.
WS6e10

ESTIMATION OF CREEP-FATIGUE INTERACTION OF 304 STAINLESS STEEL UNDER

NONPROFORTIONAL BIAXIAL CONDITIONS

T. ASAYAMA, K. AOTO and Y. WADA

O-arai Engineering Center, Power Reactor and Nuclear Fuel Development Corporation,
4002, Narita-cho, O-arai-machi, Higashi-Ibaraki, Ibaraki, 311-13, Japan

ABSTRACT

Biaxial creep-fatigue tests were conducted with 304 stainless steel at 550°C to examine
the effect of strain paths on fatigue / creep fatigue strength at low strain ranges near
elastic reagion. The waveforms employed included nonproportionl loading with a phase angle
of 90 degrees. The lowest strain range employed was 0.2%. It was shown that the effect of
strain paths on fatigue strength still existed at the lowest strain range investigated.
Evaluation of creep-fatigue strength was carried out with the linear damage summation rule.
Fatigue damage was calculated using a Mses type equivalent strain range which was based on
a total strain. Creep damage was calculated on the assumption that the biaxial stress relax-
ation behavior could be estimated based on the creep properties obtained under uniaxial con-
ditions. As a result, life prediction was possible within an accuracy of approximately
factor of 2, including the nonproportional loading.

KEYWORDS

SUS304; biaxial creep-fatigue; nonproportional loading; strain path; Mises type equivalent
strain range; linear damage summation rule.

INTRODUCTION

From the viewpoint of elevated temperature structural design, evaluation of fatigue / creep-
fatigue properties under nonproportional loading condition at low strain ranges are of par-
ticular importance. However, most of studies on multiaxial fatigue / creep-fatigue have delt
with relatively high strain reagion (Onami et al, 1985; Kandil et al, 1985; Ogata et al,
1988; Nakamura et al, 1989) and few studies have been reported regarding fatigue / creep-
fatigue strength at low strain ranges near elastic reagion. The authors carried out a series
of biaxial fatigue / creep-fatigue tests with 304 steel at 550°C in order to make clear
whether the effect of strain paths on fatigue / creep-fatigue life exist at the low strain
ranges near elastic reagion. The minimum strain range employed was 0.2%. Applicability of
the linear damage summation rule to the low strain reagion was examined.

EXPERIMENTAL PROCEDURE

Material and Specimen

The material utilized in the present study was 304 stainless steel from a hot rolled plate
(1000 x 1000 x 40mm) and was used in the solution anneled condition (1100 °C x 48min). The
chemical composition and the mechanical properties of the material are shown in Table 1.

311
312
Hollow cylinder specimens were machined after the heat treatment. Configuration of the
specimen is shown in Fig.l.

Test Apparatus

The tests were conducted with a hydro-servo axial-torsional fatigue test machine. Longitudi-
nal displacement and torsional angle were measured by an extensiometer directly mounted on
the specimen. The tests were conducted under strain controlled condition. It was possible to
control axial strain and torsional strain independently. It was also possible to hold both
axial strain and torsional strain simulutaniously at an arbitary moment in a creep-fatigue
cycle.

Test Condition

Test temperature was 550°C and environment was air. Axial and torsional strain was controll-
ed. Strain waveforms included proportional loading and nonproportional loading. Fatigue
tests and creep-fatigue tests were conducted. For a strain range of 0.2%, only a fatigue
test was performed.

For propotional loading tests, a ratio of torsional strain range Δ 7 and axial strain
range A f , defined by λ = Δ τ / Δ ε , took values of 0, oo, 1.7. Those values correspond
to pure axial loading, pure torsional loading and combined proportional tension-torsion
loading, respectively. For fatigue tests, triangular waveform was employed. The strain rate
was defined byeeq = A e e q / (r/2) where A £ e q and τ are ASME type equivalent strain
range and the frequency of cycling respectively. The strain rate took value of 0.1%/sec. For
creep-fatigue tests, in case of pure axial loading and proportional loading, a strain hold
period of 60 minuites was imposed at a tensile peak of axial strain. In case of pure
torsional loading, the same strain hold period was imposed at an extreme value of torsional
strain and sindusial waveform was employed.

For nonproportional loadings, sindusial waveform was employed. The strain ratio λ and the
phase angle φ were determined as 1.7 and 90 degrees respectively, in order to realize the
most severe loading condition (Oagata et al, 1988). Fatigue tests and creep-fatigue tests
were performed. In case of creep-fatigue tests, a strain hold time of 60 minuites was
imposed at a tensile peak of axial strain and torsional strain was held simultaneously. The
location of the strain hold was determined considering that the reduction of creep-fatigue

Table 1. Chemical composition and mechanical

properties of the material utilized. rAl

1100°CX48min WQ wt%

C Si | Mn P S Ni Cr Mo Ti AI N Nb+Ta
0.050 0.60 | 0.87 0.026 0.002 B.94 18.59 0.11 (0.002 0.013 0.019 <0.003

Yield Strength Tensile Strength Elongation

MPa MPa %
213.6 623.3 71.9

CO.5

T ZHS2 |
3.2S
jio.ol··— l·— 3 3 . 0 A
—

X = ].h *=90\ th=60min

Fig. 1. Specimen configuration. Fig. 2. Cyclic strain paths.

 313
life under uniaxLal condition was largest when a strain hold was imposed at a tensile strain
peak. The strain rate £eq was 0.1%/sec. Waveforms employed in the present study is sum-
marized in Fig. 2.

Fracture of specimen was determined as a number of cycles when the value of either an axial
stress or a torsional stress dropped to 75% of the stabilized value.

EXPERIMENTAL RESULTS

Fatigue / Creep Fatigue Life

Results of the fatigue / creep-fatigue tests are shown in Fig. 3. Figure 3 shows the
relationship between the ASME type equivalent strain range and the number of cycles to
failure. When axial strain Δ £ and torsional strain Δ 7 are imposed, the ASME type equi-
valent strain range A f e q is defined as follows,

2 2 1/2
Δε = (Αε +Δτ /3) (i)
eq
where Δ £ and Δ τ are axial strain and torsional strain respectively. First, regarding
the proportional loadings, the fatigue life was longer in the order of pure torsional load-
ing, combined proportional loading, uniaxial loading, although the difference was small. All
of those waveforms showed life reduction due to a strain hold time of 60 minuites at a
tensile peak ofaxial strain.

In the case of nonproportional loadings, fatigue life was reduced to approximately 1/5 to
1/7 of that of proportional fatigue life by a phase angle of 90 degrees. This tendency held
regardless of strain ranges. In another words, the effect of strain paths on fatigue life of
304 steel existed even at a strain range as low as 0.2% which was almost in elastic reagion.
A strain hold time of 60 minuites at an axial tensile peak reduced the creep-fatigue life to
1/2 to 1/5 of nonproportional fatigue life. The amount of the life reduction was almost the
same as the case of proportional creep-fatigue loading.

^ 10'
304 Steel, 550°C λ tn th(min)|
0
•Δ 0
60

£ 10° ▼ v · ■ *5·"ο^
A
u
CO

1 .7
0
°
60
o
60
■
o
V
T v o cÖtP-cL T 1 .7 90
60

/ U n i a x i al Fatigue 0.1%sec
ml
.'.!_.. i. ._L i 1 i 1
2 3 4 5
10 10 10 10 106

Number of Cycles to Failure n Cycles

Fig. 3. Biaxial fatigue / creep-fatigue strength of 304 steel at 550°C.

Stress Strain Response

Figure 4 shows the stress strain response obtained in the present study. In Fig.4, relation-
ship between the ΑΣΜΕ type equivalent strain range and Mises type equivalent stress range is
shown. Mises type equivalent stress range is defined as follows,

2 1/2
Δσ = (Δσ +3 Δ Γ ) (2)
eq
314
where Δ O and Δ Z are axial stress range and torsional stress range respectively. It is
observed from Fig.4 that an additionl strain hardening due to an nonproportionality of
strain path is evident particularly at relativly higher strain ranges. At lower strain
ranges, the additional hardening is not so evident but is still observed.

It was observed that stress relaxation during a strain hold period occurred proportionaly
toward the origin of the stress plane even under nonproportional creep-fatigue conditions.
An example of the stress relaxation behavior is shown in Fig.6.

ESTIMATION OF FATIGUE / CREEP-FATIGUE LIFE

Estimation of Stress Strain Response

It is widely recognized that the ASME type equivalent strain range is not adequate in evalu-
ating stress strain response under nonproportional loading conditions, because the addition-
al strain hardening can not be reasonably estimated. In the present study, Mise type equiva-
lent strain range obtained by strain path integration is examined. The Mises type equivalent
strain range A f p t h is definid by the following equation,

Δε S άε (3)
pth eq
where d£eq is Mises type total strain increment and the integration is conducted between
the extreme values of axial strain. Note that a total strain was used in the present study
instead of a plastic strain which was originaly used in the definition of Mises equivalent
strain range. Relationship between the Mises type equivalent strain range defined by Equa-
tion (3) and stress range defined by Equation (2) is shown in Fig.5. Figure 5 shows that the
additional strain hardening was relatively well evaluated using the M s e s type equivalent
strain range which takes into account the paths of strains.

800

7001-

600
Uniaxial Fatigue
4f\
^
, ' \ Uniaxial Fatigue
0.1%/sec v Of' Δ
\0.1%/sec
500 y/ A
s ■
1
400 / Δ 304 Steel, 550°C

300
λ ΦΠ th(min) ; ΦΟ th(min)
o 0 0 Ü
0 0
60
•Δ 0 •Δ 60
0
200 oo 0 oo 0
A 60 A 60
□ 1 .7 Q D 0
100 ■ 60 ■ 1 .7 60
V 0
T 1 .7 90
60
V
T 1 .7 90 o
60
0
0.5 1.0 1.5 2.0 0.5 1.0 1.5 2.0

ASME Type Equivalent Strain Range Aeeq % Path Dependent Equivalent Strain Range zJepth %

Fig. A. Additional strain hardening Fig. 5. Estimation of additional strain

due to nonproportionality of hardening using Mises type
strain path. equivalent strain range.

Damage Estimation Based on Uniaxial Material Properties

Experimental results obtained in the present study was evaluated based on the linear damage
 315
sunmation rule using material properties obtained under uniaxial loading conditions. Fatigue
damage and creep damage are defined by the following equations,

D = 1 / N (4)
f f

th
D = S dt/tr (5)
c 0

where Nf is fatigue life, tr is creep rupture time. For 304 stainless steel, following

Fig. 6. Proportionality of stress relaxation under nonproportional creep-fatigue

loading.

material properties are determined as best fit equations based on the average trend of uni-
axial properties (Wada et al, 1989; Aoto et al, 1987; Wada et al, 1986; Yoshitake et al,
1986) ; [1] strain range vs. number of cycles to failure; [2] strain range vs. stress range
at mid-life ; [3] stress vs. creep rupture time; [4] creep strain vs. time. Fatigue damage
defined by Equation (4) is obtained by the relationship between strain range vs. number of
cycles to failure. Creep damage defined by Equation (5) is obtained by determining the
stress relaxation behavior by the above material properties. That is, the initial stress of
stress relaxation is determined as a half of a stress range which corresponds to the strain
range detenrined from the relationship between strain range and stress range at mid-life.
The stress relaxation behavior is estimated by the relationship between creep strain vs.
time using the strain hardening law. With the relaxation behavior thus estimated and the
relationship between stress and creep rupture time, the creep damage in Equation (6) is
estimated.

In the present study, biaxial fatigue and creep-fatigue life were evaluated as follows.
Fatigue damage was obtained based on the Mises type equivalent strain range which takes into
account the strain paths (Equation (3)). For creep damage, the initial stress of stress
relaxation was determined by the relationship between strain range vs. stress range using
the Mises type equivalent strain range. The biaxial stress relaxation was assumed to be
estimated by the creep properties obtained under uniaxial conditions. In Fig. 7, fatigue
damage and creep damage thus obtained are plotted on the Campbell diagram. It is shown that
all of the data including the non-proportional loading are reasonably estimated, except
that the pure torsional creep-fatigue loading is estimated somewhat conservatively.

Result of life prediction based on the above damage evaluation is shown in Fig. 8. Although
most of the data are estimated within an accuracy of factor of 2, the pure torsional creep-
fatigue loading and the nonproportional fatigue loading at a strain range of 0.2% are esti-
mated somewhat conservatively. It seems that the effect of strain path is not so pronounced
316
SUS 304 Steel, 550°C / / \

Factor of 2 x
x
// / /
'' M

/"Yx / '
V o/ /p' * >/
/
L '' s *'
λ ΦΟ th(min)|
λ tn th(min) /oAk/ o 0 A
Rn
•▲ 0
οο 0
s> io •A oo 0 A
■ 1 .7
60 D
1 .7
6°
0
■ 60
τ 1 .7 90
6"0 I
V
\ T %/ ▼ 1 .7 90
ID-"
ιο-' 103 10* 105
Fatigue Damage Df Observed Life NfOBs cycles

Fig. 7. Estimation of fatigue / creep damage. Fig. 8. Comparison of observed lives with
lives predicted by the method
suggested in the present study.

at low strain ranges as at higher strain ranges. To sum up, the biaxial creep-fatigue lives
can be estimated approximately within an accuracy of factor of 2 with some coservativeness
by the method of life prediction suggested in the present study.

CONCLUSIONS

Biaxial fatigue / creep-fatigue tests were carried out at 550 °C with 304 stainless steel
and the following conclusions were obtained.

Nonproportional fatigue life was reduced to 1/5 - 1/7 of that of proportional fagigue life
compared under the same ASME type equivalent strain range, even at a strain range as low as
0.27„.

Life reduction occurred by introduction of a strain hold period at a tensile peak of axial
strain both under proportional loading and nonproportional loading. Under nonproportional
loading with a phase angle of 90 degrees, creep-fatigue life was reduced to 1/2 - 1/5 of
nonproportional fatigue life due to a strain hold time of 60 minuites. The amount of life
reduction due to a strain hold was almost the same as the case of proportional loading.

Fatigue life reduction including nonproportional loading, including that at low strain range
near elastic reagion, was reasonably estimated by Mises type equivalent strain range which
take into account of the strain paths.

Creep-fatigue life under nonproportional loading conditions were evaluated within an accura-
cy of factor of 2 by the linear damage summation rule assuming that the stress relaxation
behavior can be estimated based on the material properties obtained under uniaxial
conditions.

REFERENCES

Aoto, K., Y. Wada and R. Komine (1987). PVP, 123, A3.

Kandil, F.A., K.J. Miller and M.W. Brown (1985). ASTM 853, 622.
Nakamura, T., T. Ishikawa and Y. Asada (1989). PVP, 172, 69.
Ogata, T., A. Nitta and K.kuwabara (1988). Preprints of the 26th Symposium on Elevated
Ohnami, M., M. Sakane and N. Hamada (1985). ASIM STP 853, 651.
Temperature Strength, 70. (In Japanese)
Wada, Y., K. Iwata, K. Aoto and Y. Kawakami (1986). Proc. Int. Conf. on Computational
Mechnics, 1, IV-25.
Wada, Y., Y. Kawakami and K. Aoto (1987). PVP, 123, 37.
Yoshitake, A., Y. Wada and M. Hirano (1986). Proc. Int. Conf. on Creep, 441.
WS6e11

Cyclic stress-strain behavior and creep-fatigue

life prediction of perforated plates

Toshihide IGARI*, Masafumi YAMAUCHI*, Toshiro Matsubara*,

Shinichi NOMURA**
* Nagasaki R&D Center, Mitsubishi Heavy Industries, Ltd.,
Akunoura-machi 1-1, Nagasaki 850-91, Japan
**Nagasaki Shipyard and Machinery Works, Mitsubishi Heavy
Industries, Ltd., Akunoura-machi 1-1, Nagasaki 850-91,
Japan

ABSTRACT

Prediction methods of macroscopic and local stress-strain behavior of

perforated plates in plastic and creep regime are proposed in this paper.
Predicted results for macroscopic behavior are compared with the
experimental results for cyclic stress-strain behavior and relaxation
behavior. Creep-fatigue lives at around a hole of perforated plates are
predicted by using the local stress-strain behavior and are compared with
experimentally observed lives.

KEYWORDS

Perforated plates, creep, plasticity, creep-fatigue life, Hastelloy XR

INTRODUCTION

Stress analysis based on the equivalent-solid-plate concept is often used in

the design of high-temperature components containing perforated plates.
Prediction methods of both macroscopic behavior and local stress-strain
concentration around a hole are required in order to obtain macroscopic
deformation behavior and creep-fatigue damage around a hole. These methods
for the elastic analysis are shown in ASME Boiler and Pressure Vessel Code
A-8000. As for the elasto-plastic analysis, Uragami-Nakamura (1981)
proposed these methods by assuming the bilinear stress-strain behavior.

As for the creep analysis, on the other hand, Uragami-Nakamura (1981) and
Porowski-O'Donnell (1980) proposed these prediction methods when assuming
the Norton's creep law. Recently, Igari-Setoguchi (1986,1987,1988,1990)
have proposed advanced prediction methods in creep region which are
applicable to wider range of materials and temperature than previous works.
In order to predict the creep-fatigue life of perforated plates under cyclic
loading, however, a new proposal which can be applied to both plastic and
creep regime is necessary.

This paper describes a new proposal which extends the author's proposal to
plastic and creep regime involving cyclic loading, and describes the

317
318
application to the prediction of the macroscopic behavior and creep-fatigue
life of perforated plates.

PROPOSAL OF PREDICTION METHODS IN PLASTIC AND CREEP REGIME

Macroscopic behavior of perforated plates

Macroscopic behavior of perforated plates under uniaxial loading in plastic

and creep regime is expressed as follows in comparison with the behavior of
the base material composing the perforated plates.
E = Ee + Ep + Ec (Base material) (1)
E = Ee + Ep + 8c (Equivalent solid plate) (2)
, where the superfix * denotes the properties of the equivalent solid plate,
and Ee, Ep and Ec denote the elastic strain, the plastic strain and the
creep strain, respectively.

As for the creep strain of the equivalent solid plate, the authors (Igari
and Setoguchi, 198 6) had already proposed the prediction method as follows
for the case assuming the Norton's creep law.
Ec = A G n (Base material) (3)
Ec* = A*G* n (Equivalent solid plate) (4)
The equivalent-solid-plate property A* can be expressed by the following
equation.
Α*=(0.591/η+0.316)ΤΓ1·18η A (5)
, where T| is a ligament efficiency which defines a penetration pattern of
circular holes. Let us consider the creep behavior in the next form which
represents actual materials with both primary and secondary creep.
Ec = f (0,t) = C Gd t e + A O n t (Base material) (6)
A prediction method for macroscopic behavior using the effective stress has
been proposed (Igari and Setoguchi, 1990).
Ec*=f (Gnom,t)= C Gnom d t e + A Gnom" t (7)
, where Gnom is the effective stress which is defined by the next equation,
anom=(A*/A)1/nO* <8)
or simply defined by the next equation for a case of n from 5 to 10.
Onom=(E/E*)a* . (9)

Assume that the plastic strain of the base material and the equivalent solid
plate is expressed as follows.
Ep = Bö™ (Base material) (10)
Ep*= B*G* m (Equivalent solid plate) (11)
By considering the analogy between two materials with the stress-strain
behavior of eq.(3) and eq.(10) , the above-mentioned results for creep are
considered to be applicable to plasticity. That is to say, the next
relation
Β*=(0.59ΐΜ+0.316)η_1·18ιηΒ (12)
is obtained. For different types of equation, the concept of the effective
stress shown in eqs.(7) and (8) can be applied.
 319
Local stress-strain concentration
The maximum local strain around a hole can be expressed as follows.
£max = Eemax + Epmax + £cmax = K t Ee + K£ £p + K£ c £c* (13)
As for K£c, the following equations have been proposed by the authors (Igari
and Setoguchi, 1986) when considering the Norton's creep law.
K Ec = ecmax/ec*=(CKt) <2n/<n+1>> (14)
, where
C =(-1.359 log10Tl-0.551) (l/n-l)+l (15)
K t = E*Ymax/(ET|) (16)
, where K t is the elastic strain concentration factor and Ymax (=Gmax/(G /TJ) )
is the elastic stress multiplier shown in A-8000. Furthermore the
application of this method to the case with both primary and secondary creep
as shown in eq.(6) is reported by the authors (Igari and Setoguchi, 1988).

Plastic strain concentration factor K £ p is thought to be obtained by

considering the analogy between plasticity and creep as shown in the case of
macroscopic behavior.
K £p = Epmax/Ep* - (CKt) <2m/<m+1>> (17)
C = (-1.359 log10T|-0.551) (l/m-l)+l (18)
As for the stress concentration during creep or relaxation period can be
described by the next equation.
K 0 = amax/(G*/11)=T|(CKt) <2/<n+1>> (A*/A) 1 / n (19)
, where C, K t and A*/A are shown in eqs. (15), (16) and (5) respectively.

EXPERIMENT

Test method
Material tested is a nickel-base alloy, Hastelloy XR, and test specimens are
machined from a round bar with a diameter of 35mm. The perforated portion
is made in the flat part of the specimen. Two kinds of ligament efficiency,
0.5 and 0.7, are adopted by fixing the diameter of circular holes at 4mm.
Two kinds of loading direction are considered against the triangular
penetration pattern of circular holes, namely, X-load and Y-load. The width
of the flat part is 20.79mm and 20mm for X-load and Y-load respectively, and
the thickness of the flat part is 10mm.

The test specimens are heated up to uniform temperature of 950°C by high

frequency induction heating. Macroscopic strain is controlled by setting up
a gauge length of 40mm at the perforated portion. Test condition is
summarized in Table 1. Test condition is classified as follows : (i) Cyclic
loading without hold time period, (ii) Cyclic loading with hold time period,
(iii) Relaxation under constant strain. Macroscopic behavior of perforated
plates is mainly studied by (i) and (iii). Creep-fatigue life, on the other
hand, is studied by (i) and (ii).

Test results

Figure 1 shows the monotonic stress-strain curves of base material and

perforated plates. Stress-strain values of the tip of the hysteresis loop
at half life are also shown in this figure. Relaxation curve of base
320

250
Hastelloy XR 950°C

O
200

Δ B.M.
150
Monotonie 0.5X
P.P.
0.7X
D B.M.
Cyclic 0.5X
o·
&-' D

/HysteresisN P.P.
0.5Y 0
50 0.7X Δ A
Vtip ;
0.7Y V
Solid symbol: Strain-hold condition
5 10 15
Strain ε , ε * (x10-3mm/mm)

Fig.l. Monotonie and cyclic stress-strain behavior of

base material(B.M.) and perforated plates(P.P.),

200 Table L. Test c o n d i t i o n .

^^^^ Experimental Predicted
B.M. O Strain pattern η Load Δε, Δε* (x10" 2 mm/mm)
0.5X Δ Δε, Δε* B.M. 2.0,1.0,0.5
P.P.
0.7X D a
0.5 1.0, 0.5, 0.2 +
|Λ Λ t
X

Hastelloy XR 950°C
έ
[V V
=5x10-3 c-1
P.P.
0.5
0.7
Y
X
0.5, 0.2 +
1.0, 0.5, 0.2 +
( + : έ =1x10· 3 S" 1) 0.7 Y 0.5, 0.2 +

\
X
Δε, Δε* B.M. 0.2 (th=10mim)

y \ i \t 0.5 X 0.2 (th=10mim)

-1
έ ==1x10-3 s- 1 V*- P.P.
0.7 X 0.2 (th=10mim)

ε, ε* B.M.
\
0.5
XX
0.25

0.25
P.P.
0.7 X 0.25

Fig.2. Relaxation behavior of base

material(B.M.) and perforated
plates(P.P.).

^ 5.0i
Hastelloy XR 950°C P.P.
B.M.
0.5X 0.5Y 0.7X 0.7Y

10 urn 0 ΔΑ V
• OSolid
· symbol: Strain-hold
ω condition
* 0.5 Δθ?0· (th=10min)
ω
<
437

2 0.1

cö 0.05I
« 20 10 2 10 3 10 4 105
Number of cycles to failure N f

Fig.3. Creep-fatigue lives of base material(B.M.) and

perforated plates(P.P.).
 321
material and perforated plates are shown in Fig.2. Figure 3 shows the
failure lives in fatigue tests. Vertical axis is taken as Δ £ * for the
perforated plates. Failure lives are determined from the change of
macroscopic stress for the case of perforated plates. Crack length at around
the circular holes is around 0.3mm-0.8mm when the test is stopped.

COMPARISON BETWEEN PREDICTION AND EXPERIMENT

Macroscopic behavior

Monotonie and cyclic stress-strain behavior of perforated plates are

predicted by using the effective stress Gnom shown above. By using the
relation of eq.(8) together with the experimental results of "m=7.41" for
both monotonic and cyclic stress-strain curve, stress-strain behavior of
perforated plates are rewritten in Fig.4. Monotonic stress-strain curves of
perforated plates coincide well with that of the base material. And also
hysteresis tip of perforated plates at half life coincide well with those of
the base material. This fact shows the propriety of the prediction of
effective stress for case of plasticity.

Macroscopic relaxation behavior in Fig.2 is analized by using the relation

of eq.(7) together with the strain hardening rule. The obtained results are
shown in Fig.2 together with the experimental data. Analytical results
coincides well with the experiment. Prediction method which is originally
proposed for constant-load condition is found to be appliable to varying-
load like relaxation.

250 —

£ 200

E
| 150 B.M.
w Monotonie 0.5X
(A P.P.
Φ 0.7X
^ 100
Φ
B.M. o
Cyclic 0.5X D
>
50 /Hysteresis\ P.P.
0.5Y 0
S 0.7X Δ
to ) 0.7Y V

°0 5 10 15
Strain £, £* (x10-3mm/mm)

Fig.4. Monotonic and cyclic stress-strain behavior of

base material(B.M.) and perforated plates(P.P.)
in relation to effective stress.

Creep-fatigue life

First, fatigue lives of perforated plates are predicted. By applying above-

mentioned value of m to the eq. (13), the maximum strain range at around a
hole can be obtained. Figure 3 is rewritten in Fig.5 by taking the vertical
axis as AEmax for perforated plates. Failure lives of perforated plates
coincide well with those of the base material.

As for the creep-fatigue life prediction, the linear damage rule by Robinson
and Taira is used. Creep damage during hold time period is predicted by
322

D P.P. |

: X
B.M.
0.5X 0.5Y 0.7Χ|θ.7Υ |
O D 0 Δ V

1.0
0.5 5k

Hastelloy XR 950°C
: o.i
i 0.05
20 102 10 3 10 4 105 102 5x102 103
Number of cycles to failure N f Observed life Nfobs
F i g . 5 Creep-fatigue lives of base Fig.6. Life prediction for creep-
material(B.M.) and perforated fatigue test of base material
plates (P.P.) in relation to (B.M.) and perforated plates
predicted strain range. (P.P.).

assuming the initial stress at around a hole and by calculating the

relaxation behavior based on the creep property of base material. Predicted
results using the relation of "Df+Dc=l" are shown in Fig.6 in comparison
with experimental results. Predicted lives coincide with experimental
results.

CONCLUSION

(1) Macroscopic behavior of perforated plates including cyclic stress-strain

behavior and relaxation behavior is predictable by using the proposed
method in this paper.
(2) Creep-fatigue lives at around a hole can be predicted by using the propo
-sed prediction methods for stress-strain concentration around a hole.

REFERENCES

Igari,T. f Setoguchi,K. and Nomura,S. (1985). Simplified creep analysis of

perforated plates under steady creep condition. Nuclear Engineering and
Design. 97. 161-166.
Igari,T., Setoguchi,K.and Nomura,S. (1987). Experimental study on macro-
scopic creep behavior of perforated plates. Trans. SMiRT-9.L4/4 r 219-224.
Igari,T., Setoguchi,K., Matsumura,N., Hamaue,Y. and Kawaguty,K. (1988).
Experimental study of macroscopic and local creep behavior of perforated
plates. Proc. ICPVT-6 r Beijing China, 1093-1100.
Igari,T., Setoguchi,K. and Nomura,S. (1990). Prediction of macroscopic and
local creep behavior of perforated plates. To appear in Proc. of IUTAM
Symposium Creep in Structures IV. Cracow Poland.
Porowski,J.S., O'Donnell,W.J., Tanaka,T. and Badlani,M. (1980). Stress and
strain concentration in perforated structures under steady creep
conditions. J.Pressure Vessel Technol,102 f 419-429.
Uragami,K. Nakamura,K. Asada,K. and Kano,T. (1981). Simplified inelastic
analysis method of ligament plate. J.High Pressure Institute of Japan f 19f
57-65.
 WS7a1

CYCLIC FATIGUE-CRACK PROPAGATION IN CERAMICS AND CERAMIC COMPOSITES

R. H. DAUSKARDT and R. O. RITCHIE

Center for Advanced Materials, Lawrence Berkeley Laboratory,

and
Department of Materials Science and Mineral Engineering,
University of California, Berkeley, CA 94720, U.S.A.

ABSTRACT

Cyclic fatigue-crack propagation behavior is studied in transformation-toughened Mg-PSZ monolithic ceramics

(fracture toughnesses K c between 2.9 and 16 MPaVm) and a SiC-whisker reinforced alumina composite (K c
~ 4.5 MPaVm). Stress/life (S/N) data in Mg-PSZ, derived from unnotched cantilever-bend specimens, show
markedly lower lives under tension-compression compared to tension-tension loading; similar to metals,
"fatigue limits" approach 50% of the tensile strength of the material. Crack-growth results, based on studies
on "long" ( > 3 mm) cracks in compact-tension specimens, show fatigue-crack growth rates in both systems to
be markedly power-law dependent on the stress-intensity range, ΔΚ, with a threshold stress-intensity range,
A K f j j , of the order of ~ 5 0 % of K c . Conversely, for "small" ( < 2 5 0 μτή) surface cracks, fatigue-crack
growth is seen to occur at ΔΚ levels some 2 to 3 times smaller than the long-crack threshold, AKyjj. Possible
mechanisms of ceramic fatigue and the implications for safety-critical design criteria are discussed.

KEYWORDS

Ceramics, cyclic fatigue, crack propagation, Mg-PSZ, SiC-reinforced alumina, damage-tolerant design

INTRODUCTION

Recent studies have provided convincing evidence of the susceptibility of a wide range of ceramic and
ceramic-matrix composite materials to mechanical degradation under cyclic tensile loading. Extensive data
have now been reported indicating i) reduced lifetimes during stress/life (S/N) testing under cyclic compared
to sustained loads, and ii) accelerated cyclic crack-propagation rates at stress intensities less than required for
environmentally-enhanced crack growth (static fatigue) during fracture-mechanics testing; results exist for
zirconia, graphite and carbon, alumina and silicon nitride ceramics and LAS/SiCf and AI2O3/S1C composites
(Dauskardt et a/.,1987,1990a,b; Ewart and Suresh, 1986; Han and Suresh, 1989; Kawakubo and Komeya,
1987; Luh et al., 1990; Masuda et al., 1988; Reece et al., 1989; Ritchie et al., 1990; Swain and Zelizko,
1988; Ueno et al, 1990). While the precise mechanisms for such cyclic fatigue are still unclear, behavioral
characteristics are in general qualitatively similar to those of metallic materials. Typical (long-crack) data
showing the dependence of cyclic fatigue-crack growth rates, da/dN, on the applied stress-intensity range, ΔΚ,
for three zirconia ceramics, pyrolytic carbon, graphite and a SiC w -reinforced alumina composite, are shown in
Fig. 1; results are compared with those for steel and aluminum alloys. Similar to metals, the ceramic data
follow a Paris power-law relationship of the form:

da/dN = C ( A K ) m , (1)

where C and m are scaling constants; the exponent, m, however, varies between 15 to 60, which is far higher
than values of ~ 2 and 4 generally found for metals in this regime.

325
326
—i 1 1—

TS Mg-PSZ I
2091 Aluminum Alloy

Ovcragad Mg-PSZ

z
σ
-ö Pyrolytlc Corbon/ .'· « . , „ . ,, 7 D
Graphit· Composlt· / SIC.-Alumlne OQ/

σ
et:
• * / j ^· , ^ ' , j * High Strength St«*l

,0
%
o
! 1 / ) I
4 Cu li
Impregnated (v.
| Graphit«

1/3
Stress Intensity Range, ΔΚ (MPa m )

Fig. 1. Cyclic fatigue-crack propagation behavior for Mg-PSZ, pyrolytic carbon,

Cu-impregnated graphite, and SiC-reinforced alumina, compared with
metallic alloys. Data from Dauskardt et al. (1990b, 1991) and Ritchie et
al. (1990).

For structural design, cyclic fatigue in ceramic materials presents unique problems. In safety-critical
applications involving metallic structures, damage-tolerant design and life-prediction procedures generally rely
on the integration of crack velocity/stress intensity (v/K) curves (e.g., Eq. 1) to estimate the time or number
of cycles for a presumed initial defect to grow to critical size. Although such data are now available for many
ceramics, the approach may prove difficult to utilize in practice because of the large power-law dependence of
growth rates on K, which imples that the projected life will be proportional to the reciprocal of the applied
stress raised to a large power. For example, for a structure subjected to an alternating stress Δσ, where the
stress intensity K can be defined in terms of an applied stress σ and a geometry factor Q' as K = Q' σ V(7ra),
the projected number of cycles Nf to grow a crack from some initial size a 0 to a critical size ac is given by:
. -{{m-2)l2} -{(m-2)l2),
Nr *J (2)
(m-2) C(Q'Aa)m ττ'.(m/2)
*■ et c.

assuming a crack-growth relationship of the form of Eq. 1 (m 5* 2). For metallic structures where m — 2-4,
a factor of two increase in the applied stress reduces the projected life by roughly an order of magnitude; in
ceramic structures, conversely, where m values generally exceed 20 (and can be as high as 100), this same
factor of two increase in stress reduces the projected life by some six to thirty orders of magnitude!
An alternative procedure is to redefine the critical crack size in terms of the fatigue threshold, AKJJJ, below
which crack growth is presumed dormant; this in essence is a crack-initiation criterion where AK^JJ is taken
as the effective toughness, rather than the fracture toughness Kc. However, similar to behavior in metals
(Suresh and Ritchie, 1984), where cracks are physically small (typically of a length less than ~500 jim) or
approach the dimensions of microstructure or local crack-tip inelasticity, crack-propagation rates have been
recently shown to exceed those of "long" cracks (typically in excess of ~ 3 mm) at equivalent applied ΔΚ
levels, and more importantly to occur at ΔΚ levels less than AKyy (Steffen et al.> 1990; Cardona and
Beevers, 1990). Although results on small cracks in ceramics are limited, the observed sub-threshold crack-
growth behavior implies that conventional damage-tolerant design criteria may be highly non-conservative.
The objective of this study is therefore to investigate the cyclic fatigue behavior of both microstructurally-
small and long cracks in two toughened ceramics, namely a transformation-toughened Mg-PSZ monolithic
ceramic and a SiC-whisker-reinforced alumina composite, in the light of possible crack-advance mechanisms.
 327
EXPERIMENTAL PROCEDURES
Fatigue tests were performed on a precipitated partially stabilized zirconia, containing 9 mole% magnesia
(Mg-PSZ), chosen for its transformation-toughening behavior (Hannick and Swain, 1982). Sintering and sub-
eutectoid aging heat treatment resulted in a series of microstructures consisting of cubic ZrC>2 grains (diameter
— 50 μπι), with ~ 35-40 vol % lens-shaped tetragonal precipitates (maximum size ~300 nm) which can
undergo a stress-induced martensitic transformation to a monoclinic phase in the high stress field near the
crack tip. The resultant dilatant transformation zone in the wake of the crack exerts compressive tractions on
the crack surfaces which shield the crack tip from the far-field stresses (McMeeking and Evans, 1982). The
crack-tip stress intensity, Κ^ ρ , is therefore reduced from the applied (far-field) K by the shielding stress
intensity, Ks, which is dependent upon the volume fraction, / , of the transforming phase within the zone, the
width of the zone w, the dilatational component of the transformation strain ε , Young's modulus E,
Poisson's ratio v, and a constant A dependent on the frontal-zone shape:
K = K-K
tip s » (3)
Ks = A (E/l - ιϊ)εΊβνι/ι . (4)
Four microstructures in Mg-PSZ were examined with varying degrees of transformation toughneing, namely
peak toughness TS-grade (tensile strength a u = 400 MPa, steady-state K<. = 16.9 MPaVm), mid toughness
MS-grade (au = 600 MPa, K c = 11.5 MPaVm), low toughness AF-grade (ση = 300 MPa,
Kc = 5.5 MPaVm), and a pre-transformed overaged structure (au = 300 MPa, Kc = 2.9 MPaVm).
Also studied was a SiC-whisker-reinforced alumina, which was fabricated (Porter et al., 1987) by dispersion
processing, pressure filtration and hot pressing of high purity alumina powder with 15 vol% SiC whiskers.
The microstructure, which consisted of a uniform dispersion of < 1 μτα diameter SiC whiskers (aspect ratio ~
100) within a matrix of <5 μιη ΑΙ2Ο3 grains, had a tensile strength of 650 MPa and K<. = 4.6 MPaVm.
Fatigue-crack growth studies for through-thickness long ( > 3 mm) cracks were performed on 3-mm thick
compact tension C(T) specimens, cycled at a load ratio R (ratio of minimum to maximum loads) of 0.1 with a
frequency of 50 Hz (Dauskardt et al., 1990b). Following crack initiation from a wedge-shaped starter notch,
growth rates were determined over the range ~ 1 0 ' ^ to 10"^ m/cycle using computer-controlled decreasing
or increasing K conditions with a normalized K gradient of 0.08 mm'*. An electrical-resistance technique,
using - 0 . 1 μιη NiCr films evaporated onto the specimen surface, was employed to monitor continuously the
crack length to within ±5 /im. Stress/lifetime (S/N) tests were performed on 70-mm long polished or micro-
indented cantilever-bend specimens, cycled under tension-compression (R = -1) or tension-tension (R = 0)
loading. Data for Mg-PSZ are presented as cycles to failure, Nf, as a function of the maximum applied stress
on the outer specimen surface. Fatigue-crack growth data for small ( < 250 /im) surface cracks were
determined by optical examination of the top surface of the cantilever-bend specimens; tests were interrupted
after —100 cycles to ascertain damage accumulation during initial loading and then subsequently at ~ 10·^ to
10^ cycle intervals to measure crack-growth rates. Stress-intensity factors were computed from linear elastic
solutions (Raju et al., 1989) for three-dimensional semi-elliptical surface cracks in bending.

To examine non-steady-state crack growth, tests were also performed on long cracks subjected to variable-
amplitude cyclic loads. Block-loading sequences, comprising selected constant stress-intensity ranges, were
applied during steady-state fatigue-crack growth, and the transient crack-growth response following load
changes observed as a function of crack extension until steady-state growth was re-established.

RESULTS
Fatigue-crack propagation rates in Mg-PSZ are shown in Fig. 2a as a function of the applied ΔΚ; such long-
crack data conform to a conventional Paris power-law relationship (Eq. 1), with m varying between 21 and 42
and C scaling inversely with Kc. The value of the threshold ΔΚγρ, defined at —10'*" m/cycle, is ~50% of
Kc. Experiments at constant Kmax with varying K m m have established that such subcritical cracking is a true
cyclic fatigue phenomenon (Dauskardt et al., 1987; Ritchie et al., 1990). It should also be noted that the
transformation-toughened microstructures display the best fatigue resistance; the overaged material also
exhibits a similar power-law dependency, despite the absence of appreciable transformation "plasticity". In
marked contrast to metals, little discernable difference was apparent between monotonic and fatigue fracture
surfaces. Both fatigue and fracture surfaces in Mg-PSZ were primarily transgranular with crack paths showing
evidence of crack deflection, branching, and uncracked-ligament bridging behind the crack tip.

Resistance to fatigue-crack extension in Mg-PSZ is observed to increase with the degree of crack-tip shielding
resulting from increased transformation toughening (Fig. 2a). However, the crack-growth data for the four
microstructures can be normalized to a single curve (Fig. 2b) by characterizing in terms of the near-tip stress-
intensity range, ΔΚ^ ρ , which accounts for the shielding stress intensity Ks from transformation toughening:
328
ΔΚ,tip "" ^max " ^s » (5)
Methods for computing Ks using the integrated form
of Eq. 4 and Raman spectroscopy measurements of
the transformation-zone size are discussed elsewhere
(Dauskardt et al., 1989). An equivalent result can
be achieved by normalizing the crack-growth data in
terms of AKJKQ (Dauskardt et ah, 1990b).
S/N curves for MS grade and overaged material for
both tension-tension (R = 0) and tension-
compression (R = -1) loading are shown in Fig. 3.
Data from Swain and Zelizko (1988) for MS grade
tested at an R of 0 and -1 are included for
comparison; despite the scatter, results are
comparable. Similar to data on S13N4 (Kawakubo
and Komeya, 1987), cycling in tension-compression
is significantly more damaging than in tension-
tension. MS-grade Mg-PSZ shows evidence of a
fatigue limit of -300 MPa at 108 cycles (R = -1),
akin to behavior in steels where the fatigue limit is
- 5 0 % of the tensile strength. The overaged
material failed at much lower stress levels. The
more damaging nature of tension-compression
cycling is apparent from optical examination of
specimen surfaces in MS-grade material at R = 0
and -1 from an increased distribution of larger
microcracks at R = -1. Microcracks appear in
regions of surface uplift aligned primarily
orthogonal to the stress axis, although some cracks
form at angles of —45° to the stress axis at R = -1.
1/J
Stress Intensity Range, AK tip (MPa-m
Small-crack growth behavior, monitored from the
S/N samples, is shown in Fig. 4. Microcracks grow
at progressively decreasing growth rates with Fig. 2. Long-crack growth-rate data in
increase in size, until finally linking together as the overaged and transformation-toughened
density of cracks increases; the specimen then fails. Mg-PSZ, as a function of a) applied
Similar to data for A1 2 0 3 , S13N4 and LAS/SiCf stress-intensity range, ΔΚ, and b) near-
ceramics (Horibe, 1988; Hoshide et al., 1988; Luh tip stress-intensity range, ΔΚ*:0 =
et al., 1990) and metals (e.g., Suresh and Ritchie,
1984), small-crack growth rates (Fig. 4a) display a " m a x "s"
negative, non-unique dependency on stress intensity
and propagate at K levels well below Δ Κ ^ Η
(specifically at Km3LX levels of 1.6 MPaVm, a factor of seven less than Kc). The sub-threshold crack-growth
behavior for small cracks in Mg-PSZ can be explained by analogy to small-crack behavior in metals (Suresh
and Ritchie, 1984). Although the nominal stress intensity K increases with increase in crack size, the
shielding stress intensity Ks (in metals, resulting primarily from crack closure) is also enhanced as a shielding
zone is developed in the crack wake. The near-tip stress intensity (Eq. 5) and hence the crack-growth behavior
is thus a result of the mutual competition between these two factors; initially Kt:p is diminished until a steady-
state shielding zone is established, whereupon behavior approaches that of a long crack. In ceramics, such
decelerating sub-threshold crack-growth behavior has been modeled in a LAS/SiCf glass-ceramic, where the
predominant shielding results fromfiberbridging (Luh et al., 1990); with PSZ, however, the shielding results
from phase transformation. In fact, if the long-crack data are corrected for transformation shielding by
characterizing in terms of the near-tip stress intensity (from Eq. 5), the da/dN (Ktjp>max) curve corresponds
closely to that associated with the initial growth of the small cracks (Fig. 4b).
Similar behavior is observed in A^C^/SiC^. Long-crack data, plotted as a function of Km£LX (R = 0.1) in
Fig. 5, show a power-law dependency on the stress intensity with an exponent of 15; the threshold in this case
is —60% of Kc. Comparison of these data with other ceramics (Fig. 1) suggests that resistance to cyclic
fatigue-crack growth in ceramic materials in general is enhanced with increasing fracture toughness. Unlike
PSZ, however, the cyclic and monotonic fracture surfaces do show some distinction. Fatigue fracture surfaces
appear to be more textured and are rougher; at higher magnification, crack paths formed under monotonic
loading are predominantly transgranular, with a high incidence of cleavage steps and a flatter appearence. The
increased roughness of the fatigue surfaces is associated with an increasing proportion of intergranular
fracture, with limited evidence of abrasion and wear and a higher degree of SiC whisker pull out.
 329
600
Four-point Bend

50
-3
Q-
°
Σ
S 400
ω
C/5
-o
J> 300 Overaged
a (R = -1)
a Rotational
< Fatigue
| 200
O MS Condition (R = -1)
E • MS Condition (R = 0)
x D Overaged Condition (R = -1)
OT
2 100 5 5 ^ Four point Bend. MS Condition (R = 0) [Swain]

Rotational Fatigue, MS Condition [Swain]

i 11 mill uuil i 11 mill ι ι miiil

°10° 101 102 103 104 105 itf 107 10e
Number of Cycles to Failure, N f

Fig. 3. Stress/life (S/N) curves for overaged and MS-grade Mg-PSZ tested in
cantilever bend under tension-compression (R = -1) and tension-tension
(R = 0) cycling. Data are compared with results of Swain and Zelizko (1988)
on similar material under cyclicflexure(R = 0) and rotatingflexure(R = -1).

(a) Stress Intensity. K m ax (MPa-m"*)

Fig. 4. Small-crack growth-rate data in MS-grade

Mg-PSZ from cantilever-bend specimens,
as a function of Κ,,^χ at R = 0 and -1,
compared to corresponding long-crack
data as a function of the maximum applied
stress intensity in a), and b) showing
small-crack data compared to the near-tip
stress-intensity relationship for the long-
Stress Intensity. K m ax (MPa-m 1 ) crack data computedfromEq. 5.
330
Unlike results on the unindented PSZ samples, S/N data in the composite, derived from micro-indented
specimens at both R = 0 and -1, show that cycling in tension-compression is not more damaging. This may
be because fully reversed cyclic loading has a greater effect on initiating microcrack damage. Where defects
pre-exist (as micro-indents), lifetimes in tension-tension and tension-compression are comparable as crack-
growth rates are similar. However, in smooth specimens where microcrack initiation may account for a
significant proportion of the life, reduced lifetimes for tension-compression loaded specimens are apparent. By
computing growth rates from these tests, small cracks were observed to grow at progressively decreasing
growth rates; when plotted as a function of K m a x (Fig. 5), the growth-rate data display a characteristic
negative dependency on stress intensity. Moreover, small-crack growth rates are not a unique function of the
K m a x and appear to be sensitive to the level of applied stress. As noted above, small-crack effects can be
rationalized in terms of the mutual competition between the applied K and the development of a zone of crack-
tip shielding. In fact, a small crack is generally defined as being small relative to the size of the shielding
zone. With Al2C>3/SiCw, the primary shielding is from crack bridging by unbroken whiskers in the crack
wake (Dauskardt et al.y 1991). Specific analyses (Horibe, 19988; Hoshide et al.t 1988), however, introduce
additional crack-driving forces associated with the residual stress field surrounding the indent to model
behavior; in the present case, residual stresses account for the initial crack growth in thefirstfew cycles.

10

1 ■ 1 1
' < ' m yl
' ^J 10'5
SiCw reinforced A l 20 3 (Kc ~ 4 . 5 MPa
)
^
i
J ^
\
I* ΔΚ-5.48
1 AK « s ao
' ΔΚ-5.30 ΛΚ - s en UPI
' ΔΚ-δ.θΟΜΡβνΤτι

r-
°0
°
a

V '
m
0* J
f
1/. LDoa ntag- -Crack
■=

:1 I Mg-PSZ (MS)

%10"'
1
°
-io·"
= 0
·".<
li
. Δ* .
1
::
.
I,·
0
8
o 187 MPn1
o 195 MPa
» 197 MPa R --1.0
♦ 205 MPa
Small-Crack » *
Data
♦ 208
x 198
MPa'
MPal
-
• 226
»235
MPa
MPa
(a) Crack Extension, Aa (mm)
♦ 245 MPaJ :
min i i

Variable Amplitude Loading SKVAJ2O3 -

Maximum Stress Intensity Kmox ( M P a m ' )

Im111 ι

Fig. 5. Small-crack growth-rate data in the

Al203~SiCw composite, as a function :
of Kjj^x at R = 0.05 and -1, compared ■ ! 1 :

>.J I.·
1
to corresponding long-crack results.

: ϊ ί 1 ■»> i
=" I 1 1
t 3
In addition to constant-amplitude data, : 1 J

experiments were performed to examine the = K J

influence of variable-amplitude loading on Ξ
1 * C|
j »1
1 ]
steady-state fatigue-crack growth. Results for β - ^ Δ Κ . ί—
♦ΔΚ-3. . ϊ ΙΑΚ
both MS-grade Mg-PSZ and Al^CtySiC^ 1 1 1 1 1 1

subjected to high-low and low-high block (ΥΛ Crack Extension, Δα ( m m )

overloads are shown in Fig. 6. Behavior in

Mg-PSZ is similar to that widely reported in Fig. 6. Transient fatigue-crack growth
metals. In PSZ (Fig. 6a), a high-low block behavior showing variation in crack-
overload, from a ΔΚ of 5.48 to 5.30 MPaVm, growth rates following high-low and
is first applied; on reducing the cyclic loads, an low-high block-loading sequences in a)
immediate transient retardation is seen followed MS-grade Mg-PSZ and b) A1 2 0 3 -
by a gradual increase in growth rates until the SiC w composite. Predictions of
new steady-state velocity is achieved. transient crack-growth behavior for
Similarly, by subsequently increasing the cyclic Mg-PSZ in a) rely on steady-state
loads so that ΔΚ = 5.60 MPaVm (low-high crack-growth data (Fig. 2) and
block overload), growth rates show a transient transformation-zone size measurements
acceleration before decaying to the steady-state using Raman spectroscopy to compute
velocity. The increment of crack growth over AKtjp following load changes
which the transient behavior occurs is ~700 (Dauskardt et al., 1990a).
 331
μ\Ά, approximately five times the measured transformed-zone width of ~ 150 μιη. This is consistent with
zone-shielding calculations which compute the maximum steady-state shielding to be achieved after crack
extensions of approximately five times the zone width (McMeeking and Evans, 1982). In fact, predictions of
the post load-change transient crack-growth behavior have been obtained (dotted line in Fig. 6a) using a
mechanics analysis to account for the extent of transformation shielding following load changes (Dauskardt et
al., 1990a). In general, the significant variation in growth rates with small changes in ΔΚ is consistent with
the steep slope of the v/K curves (Eq. 1) in ceramics.

For Al2C>3-SiC w (Fig. 6 b ) , over the first ~ 1.2 mm of crack advance, the crack-growth rate remains
approximately constant at a baseline ΔΚ of 3.6 MPaVm. On reducing the cyclic loads to ΔΚ = 3.2 MPaVm
(high-low block overload), growth rates decrease by a ~ 1.5 orders of magnitude; by subsequently increasing
to a ΔΚ of 3.6 MPaVm (low-high block overload), growth rates increase to previous baseline levels. Note,
however, that unlike Mg-PSZ where marked transient growth-rate effects result from transformation-zone
shielding, the A^C^-SiC^y composite, which relies primarily on crack bridging, does not show such transient
behavior; the scatter in growth rates, however, does not allow precise resolution of this effect.

DISCUSSION

Mechanisms of cyclic fatigue in metals are based primarily on dislocation activity leading to crack advance via
such processes as alternating crack-tip blunting and resharpening. Accordingly, the refuted existence of a true
fatigue effect in ceramics has relied on the very limited crack-tip plasticity in these materials. However, it is
now apparent that other inelastic mechanisms may prevail; these mechanisms include microcracking and
transformation plasticity in monolithics such as PSZ, and frictional sliding at interfaces in composites such as
Al203-SiC w . Such deformation processes, like dislocation activity, contribute to fatigue damage due to their
irreversible nature, although the precise micromechanisms of crack advance are as yet unknown.

Despite uncertainty in the mechanistic nature of

ceramic fatigue, two general classes of mechanisms
can be identified (where failure involves a dominant
crack), specifically involving either intrinsic or
extrinsic m e c h a n i s m s , as i l l u s t r a t e d in F i g . 7 Mechanisms of Cyclic Fatigue Crack Growth in Ceramics
(Ritchie et al., 1990). Intrinsic mechanisms involve
the creation of a fatigue-damaged microstructure
ahead of the crack tip, and thus result in a crack- Intrinsic Mechanisms Extrinsic Mechanisms

advance mechanism unique to cyclic fatigue. This

could entail crack extension via alternating crack-tip
blunting and re-sharpening, as in metals, or through Y.S.
the formation of shear or tensile cracking at the tip 4FffR))
due to contact between the mating fracture surfaces
on unloading. In fact, fatigue striations have been
reported for cyclic failure in zirconia ceramics (Liu - cycli
c modificatio
n of x o n
· morpholog
y
and C h e n , 1 9 9 1 ) . Extrinsic mechanisms,
conversely, do not necessarily involve a change in
crack-advance mechanism compared to monotonic
fracture; here, the role of the unloading cycle is to 3. Crac
k Tip Bluntlng/Rasharpanin
g unbroka
n llga
r

affect the magnitude of the near-tip stress intensity

by diminishing the effect of crack-tip shielding.
Possible mechanisms include reduced shielding
through i) an enhanced forward transformation
zones in transforming ceramics, ii) a reduction in
c r a c k - t i p b r i d g i n g via the fracture of metallic
p a r t i c l e s w h i c h intersect the crack p a t h , or the
fracture and/or of buckling of brittle fibers, or iii)
the cracking and/or crushing of fracture-surface Relaxatio
n of Raaldua
l Strasaa
a

asperities which act as wedges or interlocking zones

between crack faces.

In reinforced ceramic-matrix composites, nonlinear

(irreversible) deformation behavior results primarily
from e x t e n s i v e m i c r o c r a c k i n g , c o n t r o l l e d Fig. 7. S c h e m a t i c i l l u s t r a t i o n of p o s s i b l e
crack-advance mechansisms during
debonding at matrix/reinforcement interfaces, or
c y c l i c f a t i g u e - c r a c k g r o w t h in
plastic deformation of the reinforcement phase itself
monolithic and composite ceramics.
(as in ductile-particle toughened ceramics), the latter
two p h e n o m e n a r e s u l t i n g in the formation of
bridging zones behind the crack tip ( e . g . , Cox,
332
1991). In fact, these factors are the prime reason for marked resistance-curve (R-curve) fracture-toughness
properties of ceramic composites, as both microcracking and bridging zones progressively develop (until
steady state) with increasing initial crack extension. Correspondingly, it is not unreasonable to hypothesize
that such nonlinear processes, together with progressive wear degradation of interfacial properties of the
matrix/reinforcement interface, may diminish the shielding under cyclic loads and provide the essential
inelasticity to cause cyclic crack extension.

CONCLUSIONS
Based on a study of stress/life (S/N) curves and cyclic fatigue-crack growth of long and small ( < 250 μπι)
cracks in Mg-PSZ ceramics and a 81(^-^203 composite, the following conclusions can be made:
1. S/N data for Mg-PSZ, derived from unnotched cantilever-bend specimens, indicate that fatigue lifetimes
are significantly reduced for tension-compression (R = -1) compared to tension-tension (R = 0) loading.
Similar to steels, the "fatigue limit" at 10° cycles (R = -1) approaches 50% of the tensile strength.
2. Cyclic fatigue-crack growth rates for long (> 3 mm) cracks were found to be power-law dependent on the
stress-intensity range, with an exponent m much larger than observed for metals (i.e., 15 in Al203>SiCw
and 21-42 in Mg-PSZ). In general, ceramics with the highest toughness exhibit the slowest growth rates.
Fatigue threshold AKJJJ values were approximately 50 to 60% of Kc.

3. Cyclic fatigue-crack growth rates for small (<250 /xm) surface cracks were found to occur at stress
intensities significantly smaller than the nominal long-crack threshold, ΔΚγρ. Similar to metallic
materials, small-crack growth rates showed a negative dependency on stress intensity and were sensitive to
the applied stress level. Such behavior is attributed to limited crack-tip shielding (primarily by
transformation toughening in Mg-PSZ and crack bridging in Al203~SiCw) with cracks of limited wake.

Acknowledgments: The work was supported by the Office of Basic Energy Sciences, Materials Sciences
Division of the U.S. Department of Energy under Contract No. DE-AC03-76SF00098 (for monolithic
ceramics) and the Office of Naval Research under Grant No. N00014-89-J-1094 (for composites).

REFERENCES
Cardona, D.C. and C.J. Beevers (1990). In: Fatigue 90 (H. Kitagawa and T. Tanaka, Eds.). Mat. Comp.
Eng. Publ., Ltd., Edgbaston, U.K. Vol. 2, pp. 1023-1029.
Cox, B.N. (1991). Acta Metall Mater., 39, in press.
Dauskardt, R.H., W.C. Carter, D.K. Veirsand R.O. Ritchie (1990a). ActaMetall Mater., 38, 2327-2336.
Dauskardt, R.H., M.R. James, J.R. Porter and R.O. Ritchie (1991). J. Am. Ceram. Soc, 74, in review.
Dauskardt, R.H., D.B. Marshall and R.O. Ritchie (1990b). J. Am. Ceram. Soc, 73, 893-903.
Dauskardt, R.H., D.K. Veirs and R.O. Ritchie (1989). /. Am. Ceram. Soc, 72, 1124-1130.
Dauskardt, R.H., W. Yu and R.O. Ritchie (1987). J. Am. Ceram. Soc, 70, 248-252.
Ewart, L. and S. Suresh (1986). J. Mater. Set. Lett., 5, 774-778.
Han, L.X. and S. Suresh (1989). J. Am. Ceram. Soc., 72, 1233-1238.
Hannick, R.H.J. and M.V. Swain (1982). J. Aust. Ceram. Soc, 18, 53-62.
Horibe, S. (1988). J. Mater. Sei. Lett., 7, 725-727.
Hoshide, T., T. Ohara and T. Yamada (1988). Int. J. Fracture, 37, 47-59.
Kawakubo, T. and K. Komeya (1987). J. Am. Ceram. Soc., 70, 400-405.
Liu. S.-Y. and I.-W. Chen (1991). J. Am. Ceram. Soc, 74, in press.
Luh, E.H., R.H. Dauskardt and R.O. Ritchie (1990). J. Mater. Sei. Lett., 9, 719-725.
Masuda, M., T. Soma, M. Matsui and I. Oda (1988). J. Ceram. Soc. Japan Inter. Ed., 96, 275-280.
McMeeking, R.M. and A.G. Evans (1982). J. Am. Ceram. Soc, 63, 242-246.
Porter, J.R., F.F. Lange and A.H. Chokshi (1987). Ceramic Bulletin, 66, 343.
Raju, I.S., S.N. Atluri and J.C. Newman, Jr. (1989). In: Fracture Mechanics: Perspectives and Directions
(Twentieth Symp.). ASTM STP 1020. Amer. Soc. Test. Matls., Philadelphia, PA, U.S.A., pp. 297-316.
Reece, M.J., F. Guiu and M.F.R.Sammur (1989). J. Am. Ceram. Soc, 72, 348-352.
Ritchie, R.O., R.H. Dauskardt, W. Yu and A.M. Brendzel (1990). J. Biomed. Mater. Res., 24, 189-206.
Steffen, A.A., R.H. Dauskardt and R.O. Ritchie (1990). In: Fatigue 90 (H. Kitagawa and T. Tanaka, Eds.),
Vol. 2. Mat. Comp. Eng. Publ., Ltd., Edgbaston, U.K., pp. 745-752.
Suresh, S. and R.O. Ritchie (1984). Intl. Metals Rev., 29, 445-476.
Swain, M.V. and V. Zelizko (1988). In: Advances in Ceramics, 24B Science and Technology ofZirconia III
(S. Somioya, N. Yammoto and H. Hanagida, Eds.). Am. Ceram. Soc., Westerville, U.S.A., p. 595.
Ueno, A., H. Kishimoto, H. Kawamoto and M. Asakwa (1990). In: Fatigue 90 (H. Kitagawa and T.
Tanaka, Eds.), Vol. 2. Mat. Comp. Eng. Publ., Ltd., Edgbaston, U.K., pp. 733-738.
WS7a2

STATIC AND CYCLIC FATIGUE OF SMOOTH TENSILE SPECIMENS AND CRACK GROWTH
IN GLASS AND SILICON NITRIDE

Hiroto SUGAWARA*, Akio OTSUKA** and Takehiko AMANO***

* Research Laboratory, Brother Industries, LTD.,

Mizuho-ku, Nagoya 467, Japan
-x-x Department of Materials Science and Engineering,
Nagoya University, Nagoya 464-01, Japan
■JHHfr Graduate Student, Nagoya University, Nagoya 464-01, Japan

ABSTRACT

Static and cyclic fatigue tests were made on glass and silicon nitride
under static tensile loading and tension-compression cyclic loading at
the stress ratios between R = -1 and 1, by using an apparatus specially
designed with a device to minimize the load eccentricity. Crack growth
tests were also made under static loading and cyclic loading in order to
obtain the crack growth rate da/dt, as a function of stress intensity factor
K. Test results on smooth round bar specimens show that almost no effects
of stress cycling were seen on silicon nitride A and borosilicate glass,
while appreciable degradation in strength due to cyclic loading was observed
on silicon nitride B. The relation, da/dt versus K, of small cracks
obtained from the tensile test on smooth round bar specimens showed much
higher values than those of large cracks obtained from the crack growth
tests. The increase in crack growth rate due to cyclic stress was observed
in both silicon nitride B and A, in the latter of which no effects of stress
cycling were observed in the tests on smooth round bar specimens.

KEYWORDS

Static fatigue; cyclic fatigue; tension-compression fatigue; crack growth;

silicon nitride; borosilicate glass

INTRODUCTION

Although it has recently been recognized that the strength of ceramics

sometimes shows appreciable cycle dependence as well as time dependence
(Kawakubo, T and K. Komeya, 1987; Kishimoto et al., 1987, 1989; Suresh,
1987; Ritchie 1988), the investigations on cycle dependence have been made
mostly on large cracks. To evaluate the actual strength of components,
however, not only the behavior of the cracked material, but also the
behavior of smooth specimens with fractures originated from small natural
flaws, may also be important. From this view, the present investigation
was made to find the correlations among the strength of smooth round bar
specimens, crack growth behaviors in these smooth specimens, and da/dt-

333
334
K relations of large cracks obtained by crack growth test, under the
conditions of static loading as well as under cyclic loading. Tests were
made on borosilicate glass and two kinds of silicon nitride.

EXPERIMENTAL PROCEDURE

Static tensile and tension-compression cyclic fatigue tests were made on

4mm diameter round bar specimens by using specially designed testing
apparatus (Sugawara et al., 1990; Otsuka et al., 1990) equipped with a
device to minimize the load eccentricity. Tensile tests were made under
the conditions of constant stress rates and constant stresses. Cyclic
fatigue tests were made under sinusoidal tension-compression loading at
various stress ratios between R = -1 and 1, at 10Hz and 0.1Hz. Crack growth
tests were made by constant moment method (Freiman et al., 1973) using
the apparatus shown in Fig. 1. Measurements of the crack opening in the
region near crack tip under unloaded and reloaded conditions were made
by the observation by SEM. All the tests were made in air at room
temperature. The materials used are two kinds of silicon nitride, SNA and
SNB, and borosilicate glass. SNA and SNB are gas pressure sintered and
pressureless sintered material, respectively, and borosilicate glass used
in this study is Iwaki 7740, equivalent to Pyrex 7740.

RESULTS AND DISCUSSION

Static and cyclic fatigue tests on smooth round bar specimens

Figures 2(a) and 2(b) show the fracture stress for constant stress rate
tests, constant stress tests (static fatigue tests) and cyclic fatigue
tests (R = -1 and 0) as a function of equivalent time to failure, teq,
on borosilicate glass and silicon nitride (SNA and SNB), respectively.
Here, equivalent time to failure under the varying stress conditions is
the time to failure of the material which is supposed to be subjected
statically to the maximum stress in the varying stress. The conversion
of the (actual) time to failure obtained by cyclic fatigue tests, t c , to
equivalent time to failure, teq t was made in the way given by Evans (Evans
and Fuller, 1974; Evans, 1980), assuming the relation da/dt = AK , where
the values of "n" used in this calculation are shown in Fig. 2. In the
present investigation, the ratios tc/teq of SNA, SNB and borosilicate glass
are 12.6, 13.8, 5.9 for R = 0, and 17.8, 19.8, 8.5 for R = -1, respectively.
It is noticed that borosilicate glass and silicon nitride A show no cycle
dependence, while silicon niride B shows pronounced strength degradation
due to the application of cyclic stress. Figures 3(a) and 3(b) show the
effect of stress range on the equivalent time to failure of SNA and SNB,
respectively. It is noticed that in SNA no degradation in strength due
to the application of cyclic stress is observed, while in SNB, a large
decrease in time to failure due to the application of cyclic stress is
observed in the region where the stress range is larger than approximately
195MPa, though in this region the degree of degradation does not vary
largely according to the amount of stress range. This difference in cycle
dependence between SNA and SNB of smooth tensile bar specimens seems to
be related to the difference in their fracture initiation processes. In
SNA, no flaw from which fracture was initiated was observed in the fracture
initiation area and fracture was initiated from the specimen surface by
slow crack growth, while in SNB, fracture was always initiated from
pre-existing flaws such as pores. A more detailed discussion has been
made elsewhere (Otsuka et al., 1990) related to the relation between the
 335
1000
—i T rjf—i ι 1 1 r-
900
800 ^ A ^ ^ k S1 N
3 4" A
700 A ^ffl*A A
600 • A->
b 500
Si3N4-B ft« € €>-^

(a)
I 1 1 ~~i r r 1
C v c l k atiaue
Const.fr
R=-1 R=0
Material Const^ n
10Hz aiHz 10Hz aiHz
S i l i c on N i t r i d e ( A) A A Δ A 50
S i l i c on N i t r i d e ( B)
• Q β » € 60

■ "■ Borosilicate Glass

■ y B OL E 11

%M
Borosiilcate
glass
■ ■:■
(b)
Fig. 1. Apparatus for crack 10"" 10"° 1 0 - ' 1 0 ' ' 10u 101 10' 10 J 10q 10 s 10b
growth test and Equivalent time to f a i l u r e t , sec
specimen
Fig. 2. Maximum stress versus equivalent
time to failure relation for
stress constant tests, stress
rate constant tests and cyclic
- '
1 1
-1
ΆΑ Si 3 N 4 -A
fatigue tests. Effects of
amax=785MPa
cyclic stress are shown.
0.5 1178
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en
0 -A JA 785 c

0.5 -\393 <υ

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IBorosilicate glassl
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Equivalent time' to failure t „, sec Q-l—'ιο

^ eq
L
Th
til c: J
*
■1 5· ip\

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Si 3 N 4 -B ΝΉ <-> -\

0.5 •
1
amax=392MPa
J 588 Ö
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o J
j-
co
1 "(b) 0
1 1 1 ·-* 10
6
£ i Λ-^""
Equivalent
^ time to failure teq , sec
10" 1 1 1 I I I !
0.2 0.3 0.1 0.6 0.8
Fig. 3. Effect of stress range, Δσ, on Stress intensity factor Κτ, MPa/Trf
the equivalent time to failure.
(a) s i l i c o n n i t r i d e A Fig. 4. da/dt - K relations in
(b) s i l i c o n n i t r i d e B borosilicate glass.
336

,[i
1 1 Ί 1— 1
3N4-BI $
| H
5
Ψ
HT'U L
Ö§ r /
**L
1 ^
6
L
Jo
7I
<D "1
π °>
6 II 0
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o
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ÜÜ

10" °L 1 1 ΠΊ 1 1
Ί 5 6 7 8 9 3 f 5 6 7 8 9
Stress intensity factor Kr, MPa/Ίτϊ Stress intensity factor Kj, MPa/¥

Fig. 5. da/dt - K relations in Fig. 6. da/dt - K relations in

silicon nitride A. silicon nitride B.

fracture initiation processes and cycle dependence.

Crack growth characteristics by constant moment tests

In Figs. 4, 5 and 6, crack velocity as a function of stress intensity factor

K is shown, where crack velocity in cyclic fatigue was defined by the
average velocity per cycle, namely, crack extension per cycle divided by
the period of one cycle, multiplied by tc/teq given in the previous section.
In these figures, crack growth data designated by "large crack" were
obtained from constant moment crack growth test specimens shown in Fig.l,
and those designated by "small crack" were obtained from the fracture stress
versus time to failure relation shown in Fig. 2, assuming the relation
da/dt = AK and the initial crack size (Evans and Wiederhorn, 1974). In
the above calculation, the value of the initial crack*size for borosilicate
glass was assumed to be 28ym from the fracture strength at highest stress
rate and fracture toughness, and for SNB, the value is assumed to be 70ym,
which is the mean size of flaws. It is seen that the growth rate of small
cracks obtained in this way is larger than the growth rate of large cracks.
If there is any initiation period, which is not considered in this
calculation, the growth rate of small cracks must be even larger. It is
interesting to notice that the acceleration effects of cyclic loading on
the crack growth rate in large cracks are observed not only in SNB, but
also in SNA, in which no degradation due to cyclic loading was observed
in the test of smooth round bar specimens. This result seems to mean that
the effect of cyclic stress is more pronounced in large cracks than in
small cracks, smaller than 100ym, for instance.

Crack opening behavior under unloaded state and reloaded state

In Figs. 7(a) and 7(b), the amount of crack opening, measured on SEM
 337

0.5 1.0 1.5 2.0

Distance from crack t i p x, mm

(b) Silicon nitride

Fig. 8. Schematic illustration

of crack opening under
unloaded and reloaded
states.
(a) b o r o s i l i c a t e glass
(b) s i l i c o n n i t r i d e

0.5 1.0 1.5 2.0

Distance from crack t i p x, mm

Fig. 7. Crack opening at various distances from the

crack tip under unloaded and reloaded states.
K-values during crack growth are given in figures,
(a) borosilicate glass (b) silicon nitride B

micrographs, is shown as a function of the distance from the crack tip

for borosilicate glass and silicon nitride B, respectively. In these
figures, crack openings are shown in unloaded condition and in reloaded
condition. Figure 7(b) shows that, near the crack tip in silicon nitride,
there is a region where crack does not open under reloading, while in
borosilicate glass, as seen in Fig. 7(a) there is no such a region. This
difference in behavior between borosilicate glass and silicon nitride B
will be assumed to come from the fact that in silicon nitride B, so-called
bridging stress (Fairbanks et al., 1986; Swanson et al., 1987) is acting
between the mating fracture surfaces near the crack tip, while in
borosilicate glass, fracture surfaces are completely smooth and flat and
there is no such interaction between fracture surfaces. These situations
are shown schematically in Fig. 8. The effect of cyclic stress on the
crack growth in silicon nitride seems to be related to the existence of
this bridging zone. The application of cyclic stress will promote the
pulling-out action of the bridging grains, and hence the acceleration
will occur. This mechanism will expain the result that borosilicate glass,
in which no bridging was observed, shows no effect of stress cycling, while
silicon nitride, in which bridging zone was observed, shows such effect
on crack growth.
338
CONCLUSIONS

The main conclusions obtained in the present investigation are as follows:

(1) Acceleration of crack velocity of large cracks was observed both in
SNA and SNB, while strength degradation due to cyclic stress in smooth
tensile bar specimens was observed only in SNB, and not in SNA. This result
suggests that the effect of cyclic stress is more pronounced in large cracks
than in small cracks.
(2) In borosilicate glass, no effect of stress cycling was observed either
in the tests of smooth tensile bar specimens or in the crack growth tests.
(3) Acceleration effect of cyclic stress on crack growth observed in silicon
nitride seems to be resulted from the effect of cyclic stress on promoting
the pulling out of bridging grains.
(4) Crack velocity of small cracks evaluated from the fracture stress versus
time to failure relation of smooth tensile bar specimens shows higher values
than the the velocity of large cracks obtained from crack growth tests.

REFERENCES

Evans, A.G. and E.R. Fuller (1974). Crack propagation in ceramic materials
under cyclic loading conditions. Met. Trans., 5, 27-33.
Evans, A.G. and S.M. Wiederhorn (1974). Proof testing of ceramic materials
- an analytical basis for failure prediction. Inter. J. Fracture, 10,
379-392.
Evans, A.G. (1980). Fatigue in ceramics. Inter. J. Fract., 16, 485-498.
Fairbanks, C.J., B.R. Lawn, R.F. Cook and Y.W. Mai (1986). Microstructure
and the strength of ceramics. In: Fracture Mechanics of Ceramics (R.C.
Bradt et al., Ed.) vol.8, pp.23-37. Plenum, New York.
Freiman, S.W., D.R. Mulville and P.W. Mast (1973). Crack propagation
studies in brittle materials. J. Mater. Sei., j$, 1527-1533.
Kawakubo, T and K. Komeya (1987). Static and cyclic fatigue behavior of
a sintered silicon nitride at room temperature. J. Am. Cerm. S o c , 70,
400-405.
Kishimoto, H., A. Ueno and H. Kawamoto (1987). Crack propagation
characteristics of sintered Si«N, under static and cyclic loads., 36,
1122-1127. (in Japanese)
Kishimoto, H., A. Ueno, H. Kawamoto and Y. Fujii (1989). Influence of
wave form and compressive loads on the crack propagation behavior of
sintered Si~N, under cyclic loads. J. Mater. Sei., Japan, 38, 1212-1217.
(in Japanese)
0tsuka,A., H.Sugawara and Y. Ishihara (1990). Static and cyclic fatigue
of glass and silicon nitride under tensile and tension-copression fatigue
tests, submitted to Eng. Fract. Mechanics.
Ritchie, R.0. (1988). Mechanism of fatigue crack propagation in Metals,
ceramics and composites: Role of crack tip shielding. J.Mater. Sei.
and Engng., A-103, 15-28.
Sugawara, H, A. Otsuka, Y. Ishihara and T. Amano (1990). Static and cyclic
fatigue charactristics of glass, glass ceramics and silicon nitride
under tensile and tension-compression tests. J. Mater. Sei., Japan (in
Japanese) (in printing).
Suresh, L.E.S. (1987). Crack propagation in ceramics under cyclic loads,
J. Mater. Sei.. 22, 1173-1192.
Swanson, P.L., C.J. Fairbanks, B.R. Lawn, Y.W.Mai and B.J. Hockey (1987).
Crack-interface grain bridging as a fracture resistance mechanism in
ceramics: I, experimental study on alumina. J. Amer. Ceram. Soc. 70
279-289. ~ —'
WS7a3

FATIGUE OF CERAMIC CUTTING TOOLS

R. Krishnamurthy

Department of Mechanical Engineering

Indian Institute of Technology
Madras-600036, INDIA.

ABSTRACT

During machining, a ceramic cutting tool experiences a state

of hydrostatic compressive stress due to thermo-mechanical
causes; the tool tends to relax during idling resulting in
stress reversal and consequent fatigue of bulk material.
Fatigue of ceramics resulted in spalling over the rake face.
Deformation of surface coating associated with thermal streses
resulted in occurrence of comb-cracking and spalling.

KEYWORDS

Ceramic tool - thermo-mechanical stresses - spalling - comb

cracking.

INTRODUCTION

Review on fatigue of ceramics

Rapid advancements in aerospace, nuclear and armament

industries have resulted in the large scale usage of difficult
to machine materials. Although several unconventional
machining methods have been developed to combat machinability
problems, traditional methods of machining with a cutting tool
harder than work material have come to stay. This is possible
largely due to the developments in ceramic cutting tools.
Developments such as micro-structure control, particulate and
whisker reinforcements, as well as introduction of newer class
of ceramic materials (Hatschek, R.L. 1983, Bergstrom, R.P.,
1986) have resulted in increased usage of ceramic cutting
tools even with moderate cutting velocities without chipping

339
340
or associated failures. The deformation energy due to
extensive plastic deformation ahead of the cutting nose, and
frictional energy due to severe frictional interaction at the
tool-chip and tool and first machined work surface interfaces
are converted into heat. A significant portion of the heat
concentrates over an extremely small area on the tool nose,
resulting in very high temperature. Under this conditions,
the cutting nose zone experiences a hydrostatic compressive
stresses during machining, followed by a relaxation during
idling. This stress alteration can result in wear of cutting
nose usually by a fatigue process. This problem would be more
acute and severe with cutting tool materials having poor
thermal properties such as ceramics. When a ceramic cutting
tool is cutting well and fails suddenly without any observable
changes in cutting conditions, then a fatigue failure is said
to have taken place. The cutting nose is subjected to both
static and cyclic stresses for a period of extended duration
before failure occurs. This suggests that internal structural
degradation occurs (King, A.G. et al., 1966)) prior to the
ultimate failure. Two different fatigue conditions exist on a
cutting tool material, the material at the surface is exposed
to processes of degradation different from those acting on
yhrbulk material. While deformational processes dominate over
the surface, deterioration sets-in over the grain boundary in
the bulk material. While the surface deformational fatigue is
usually of ductile mode, the bulk experiences brittle mode of
fatigue. For understanding the two types of fatigue,
machining trials have been carried out using oxide ceramics
and TiN coated cemented carbide tools.

EXPERIMENTAL

Machining trials have been carried out on Molybdenum alloyed

cast iron using oxide TiN coated cemented carbide tools in a
high speed precision VDF lathe as per specification listed in
Table 1. These machining trials are conducive for fatigue
failure of cutting tools. Both the types of cutting tools were
held under a high state of stress and temperature for an
extended time, superimposed with cyclic changes in stress due
to machine tool and chip induced vibrations. During the
trials at periodic intervals the tool was observed for the
types of wear associated with. The observations included tool
wear and corresponding work surface features.

RESULTS AND DISCUSSION

Fatigue of bulk material

During machining of cast irons, the ceramic tools exhibited

wear due to deformation (crater) and wear due to cracking and
spalling on the rake face. Typical cracking and spalling
observed on the while A 1 2 0 3 ceramic tool is illustrated in
Fig.l. It is seen that the crack originates from the secondary
cutting edge behind the nose and propagates into the bulk
material. During machining, the cutting tip experiences
higher order cutting temperature at three distinct places,
i.e., cutting nose, secondary grooving zone and depth of cut
 341
Table 1

Work material : Mo-Cr Alloyed cast iron

Total Carbon : 3%, Si 2%, Mo 0.75%, Cr 0.7%, Mn 0.83

P 0.35%

Hardness : 260 - 300 BHN

Tool : A 1 2 0 3 ceramics

Cutting condition : V = 400 m/min, S = 0.08 mm/rev

a = 0.5 mm

Work material : CFRP composite

Tool : TiN coated K type carbide substrate

V = 150 m/min, S = 0.05 mm/rev,
a = 1 mm

V = Cutting Velocity
s = Machining feed
a = Depth of cut.

line zone. The part of the tip behind the nose on the
secondary cutting flank portion experienced deformation
stresses at higher temperature. On cooling the deformed
material would tend to relax, thus experiencing stress
reversal. This would result in cracking of the material in
the secondary flank portion. Further, vibration of the tool
nose in the feed direction would have the effect of changing
the feed. This vibration would produce forces which when
exceed the fatigue limit of A 1 2 0 3 material, could initiate
fatigue cracking. Once initiated, the crack would propagate
into the material (as observed in Fig.l)) during subsequent
machining, depending on factors such as material resistance
and stress prevailing at the crack tip. If this stress
exceeds the resistance of the bulk material, then crack would
propagate further into material resulting in spall-out of
material as seen in Fig.l. It is well known that during
machining, the cutting nose is subjected vibration in
tangential and feed directions. Vibration in the tangential
direction would have the effect of varying cutting wedge
geometry and cutting speed; the cutting tool performance is
usually influenced only marginally by such vibrations.
However, vibration in feed direction could contribute
significantly to tool failure. Such vibration on the tool
nose could result in opening and closing of mouth of crack
over the secondary portion, facilitating propagation of the
crack into the bulk in the directtion of feed. This could be
seen in Fig.l.
Further propagation of cracking would be through the zone of
material over the rake face of the tool already degraded due
to thermal influences. This would result in spalling over the
342

Fig. 1 Crack originating at the secondary grooving portion and

propagating into the rake face material-the crack is seen to
form a boundary for subsquent spoiling

rake face. Typical spall observed on A 1 2 0 3 ceramic tools has

been illustrated in Fig.2. It could be seen that the crack
from the secondary portion propagating into the bulk, forms
the boudary of the spall on the rake face. During machining
the rake face material experiences maximum temperature over a
portion. This portion of the bulk material subjected to both
temperature and mechanical stresses, would deform platically.
Published literature on indentation of ceamics (Kim, C.H. et
al., 1973, Hockey, B.J., 1971) report that plastic deformation
during indentation is associated with high densities of
dislocations. Thus a sustained process of deformation during
metal cutting, would be associated with dislocation movement
causing large scale material gliding. On cumulative gliding,
the ceramic tool material experienced cracking and consequent
spalling over the rake face. This could be observed over the
spalled region in Fig.2.
 343

Fig. 2 Spoiling on the rake face of white cerdmic associated

with dislocation pile up and material gliding
Fatigue of Surface Material

It is well known that a cutting tool material has to meet

complex reguirements of resistance to both surface originated
wear and wear of substrate material. This could be achieved
by coating the substrate with a harder, wear resistant
material. Cemented carbides coated with thin layer of TiN
have been used for machining of CFRP (Carbon Fibre Reinforced
Plastics) composites. During machining of composites, owing
to temperature gradient due to frictional heating, the coated
layer would be thermally loaded. The thermo-mechanical
phenomenon associated with frictional heating could
significantly influence the wear of coating. A normal
influence of frictional heating would be cracking of the
coating called as thermo-cracking or heat checking. Fig.3
shows typical cracking observed over the coating. As seen in
the figure, the cracks are normal to the cutting edge on
primary flank, while they are parallel to the cutting edge in
the nose portion. The cracking was first observed near the
depth of cut line (primary grooving zone) and was observed to
occur in different zones towards the nose successively. The
occurrence of such parallel cracks normal to the cutting edge
has been termed as comb cracking.
344

Fig.3 Comb-cracking observed on TiN coated tools-CFRP machining

CONCLUSION

Thermo-mechanical stresses during machining, and stress

relaxation during idling caused cracking over the secondary
flank of A 1 2 0 3 ceramics.
Vibration in the feed direction, facilitated crack propagation
and consequent spalling.
TiN coated tools experienced comb cracking on the primary
flank during machining of CFRP composites.
REFERENCES
Hatscheck, R.L., (1983) New ceramics revolutionise upcutting
speed, American Machinist, Jan., 110-112.
Bergstrom, R.P., (1986) Getting a grip on cutting tools,
Manufacturing Engineering, Jan. 55-59.
King, A.G., Wheildon, W.M. (1966) Ceramics in Machining
Processes, Academic Press, New York.
Kim, C.H., Smith, W.C., Hastelman, P.H., Käme, G.E., (1973)
Evidence for dislocation controlled crater wear of
polycrystalline A l 2 0 3 cutting tools, Jl. App. Physics, 44,
5175.
Hockey, B.J., (1971) Plastic deformation of A 1 2 0 3 by
indentation and abrasion, Jl. American Cerm. Society, May,
223-231.
 WS7a4

FRACTURE MECHANICAL FATIGUE TESTS OF CERAMIC

MATERIALS BY NEWLY DEVELOPED LOADING AND MEASURING
DEVICES AT ROOM AND ELEVATED TEMPERATURES

M. KIKUKAWA and A. SAKAIDA

* Department of Mechanical Engineering, Fukui Institute

of Technology, Gakuen 3-6-1, Fukui, 910, JAPAN
** Department of Mechanical Engineering, Akashi College
of Technology, Nishioka, Uozumi, Akashi, 674, JAPAN

ABSTRACT

In order to investigate the fracture mechanical fatigue properties of

ceramics at room and elevated temperature, the following experimental system
was newly developed; one was eccentric compression loading method which
enables us to obtain stable crack growth ranges widely, and another was an
extended unloading elastic compliance method to detect the length and closure
behavior of fatigue cracks. After confirming the high performance of the
newly developed testing system by the experiments conducted on glass and
partially stabilized zilconia, the crack growth behaviors of silicon nitride
were investigated at elevated temperature up to 1673K.

KEYWORDS

Silicon nitride; partially stabilized zilconia; glass; fracture mechanics;

eccentric compression loading; cyclic fatigue; fatigue crack.

INTRODUCTION

To apply engineering ceramics as structural elements more widely, the

information on their mechanical properties including cyclic fatigue at
elevated temperature must be systematized for various loading and
environmental conditions. From this point of view, several studies on cyclic
fatigue crack growth behaviors were carried out for silicon nitride
(Kishimoto et^ aj^. , 1987) and zilconia (Dauskardt et_ aj^. , 1987) at room
temperature. But there are some difficulties in crack length measurement and
specimen gripping method in the fatigue test at elevated temperature.

In this study, a new fracture mechanical fatigue testing apparatus for

elevated temperature was developed, which facilitate the detection of fatigue
crack growth behaviors without optical measurement. An extended unloading
elastic compliance method was applied to detect length and closure behavior
of fatigue cracks. Fatigue crack growth behaviors of silicon nitride were
investigated at room temperature, 1373 and 1673K. The difference of fracto-
graphic patterns depending on the testing temperature was also discussed.

345
346
SPECIMEN, TESTING SYSTEM AND PROCEDURE

In order to determine the appropriate specimen shapes and loading conditions

applicable to elevated temperature, several computer-simulations were first
conducted on the basis of the calculated results of stress intensity factors
(Tada jejt JLL. , 1973) and the analyzed results of compliances (Okamura et_ a^.,
1975) for single edge cracked plates under tension and bending moment.

Figure 1 shows an example of simulation result for eccentric compression

loading with negative eccentricity e. The negative eccentricity means the
case where the outside of the specimen width W is compressively loaded as
indicated in Fig.l. Length Le means the equivalent gage length in the case
of the setting of measuring device for extensometer as shown in Fig.3(b), and
is corresponding to the gage length of strain gage as shown in Fig.2(c).

Three sorts of circular symbols in Fig.l show the values of stress intensity
factor obtained under the condition of constant angular displacement of
specimen ends, TH=2*10 . After the initial part corresponding to a chevron-
start notch, the stress intensity factor decrease slowly with the increase in
crack length, and stable crack growth is expected over the wide range of
crack length. The effect of loading position on the variation of stress
intensity factor is also small.

Three sorts of the square symbols (STH) show the normalized flexural
stiffness of cracked plate under eccentric compression loading, where the
flexural strain normalized by the compressive strain of the same plate
without crack under uniform compression loading. The STH-a/W curve seems to
vary almost linearly in the range of a/W larger than 0.3. It indicates that
the STH is the most appropriate variable for the estimation of crack length.

In order to investigate the performance of the testing system, fatigue tests

were conducted on PSZ and glass at room temperature. Subsequently,
experiments on a silicon nitride were conducted at room temperature, 1373 and
1673K. The specimens with chevron-notch were used in these experiments shown
in Figs.2 and 3.

10 DEP-e/w Ko STH
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compression loading with negative eccentricity.
 347

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Strain gage J jr-Strain gage (BF)

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f
ro Specimen-

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(a) Glass (b) PSZ I

(c) Testing apparatus

Fig. 2. Specimen shapes and set up of the testing
apparatus for room temperature.

Elastic suspension [
9
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/

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. 2 « ,J1 Pre-loading
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(a) Si 3 N A
(b) Testing apparatus

Fig. 3. Specimen shape and set up of the testing

apparatus for elevated temperature.

The setup of the testing equipment for elevated temperature is shown in

Fig.3. Eccentric loading position was determined by using elastic
suspensions, or ceramic cylindrical rollers. The elastic constraint moment
caused by the suspension increases the stable crack growth range. Ceramic
cylindrical rollers were also inserted between specimen ends and loading bars
to keep the loading position on the center line of specimen thickness. Super
kanthal cylinder was heated by a high-frequency induction heating apparatus,
and the temperature of the central part of specimen can be raised up to 1873K
in a short time and kept constant temperature automatically. Pre-loading
devices are applied to stabilize the compression loading condition and to
conduct a wide range fatigue test under pulsating and alternating stress with
arbitrary stress ratio.

Fatigue tests were performed with an electro-hydraulic servo type testing

machine with a capacity of 50kN operating at 5~6.67Hz under the conditions
of controlling the load or the relative angular displacement of both ends of
specimen. In the experiments at room temperature, crack length and closure
were measured continuously by the extended unloading elastic compliance
348
method using the COD strain gage and back face (BF) strain gage. And at
elevated temperature, the deformation of specimen was measured by
extensometer outside the furnace. As the on-line treatment, inevitable
signal noise induced by high amplification was eliminated by averaging the
signals of the same phase over a block of successive 100 cycles in the main
memory of the computer. Furthermore, in order to increase the accuracy and
availability of numerous hysteresis data, the successive hysteresis data were
compressed by using a newly developed computer software until statistical
significant difference was observed.

EXPERIMENTAL RESULTS AND DISCUSSION

Figure 4 shows the examples of subtracted hysteresis loops for glass (a) and
PSZ (b) at room temperature, where the notations COD and BF mean the data
obtained by COD strain gage and back face strain gage. These subtracted
hysteresis loops indicate that crack closure is not observed in these test
conditions, and the fracture surfaces of both specimens are flat and smooth
as shown later.

The comparison of crack length detected by the extended elastic compliance

method and that observed with a traveling microscope is shown in Fig.5. CUDC
is a compliance of the output from the COD strain gage normalized by
compressive strain of uncracked specimen under uniform compression loading,
and CUDB is that from BF strain gage. DP represents the change of virtual
loading position obtained by correction for the constraint moment of elastic
suspension, and which indicates that the change is negligible in this case.
STH is the stiffness of angular displacement of both ends of specimens, that
is, the reciprocal of sum of CUDC and CUDB. The calibration of crack length
was made by both initial equivalent crack length of chevron notch and the
final fatigue crack length observed on the fracture surface, and
interpolation between them was made by using the STH-a/W curve. It is
confirmed that the fatigue crack length detected with the extended unloading
elastic compliance method gave fairly good agreement with that measured by a
microscope.

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 349
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Ί
TmJ I ° i
02
CO J o
l· IJÄHT
o-3 Q 3 I I IcuDBfT/fHJ I I E
o
O
— — — — — I T — — — \ \ Λ e
-2 2 iQ.
0.1
-1
1
Ο^ I I I I I I I I I I I I
0, "4 6 8 10 12
a mm

Fig. 5. Experimental r e s u l t of Glass.

IOP IO"1-5.
I·
U
•I
o IO
(0
ro 1 £
Ö It ö
• I
10"f 6 • » A "

"Ό
* •7 II ^τί • a Qi

7 T3
5 1 II ^* · a
^ io' \ CD 1 1
i
T3
σ 1 11 *
10ΓΤ
411 1 *
•
>
•
IOΓ β 10"
3 4 5 6 0.2 0.5 I 2 3 4 5 10
ΔΚ MPatfn Kmax MPa/m
(a) PSZ (b) Si 3 N 4

Fig. 6. Relations between crack growth rate and

stress intensity factor.

Relationships between fatigue crack growth rates and applied stress intensity
factor obtained for PSZ and silicon nitride are shown in Figs.6(a) and (b),
respectively. The tests were carried out under the controlled condition of
the angular displacement, and the range of stress ratio R varied from 0.10
to 0.15 in the case of PSZ with the increase in the crack length. For
silicon nitride, the stress ratios at room temperature, 1373K and 1673K were
about 0.15, 0.36 and 0.56, respectively.

Examples of fracture surfaces at respective temperatures are shown in Fig.7,

which are obtained from static fracture under three point bending load after
fatigue tests. At room temperature, the fracture surfaces of PSZ (a) and
silicon nitride (b) are flat and smooth, and configurations of propagating
350

(a) PSZ (R.T.) (b) Si 3 N 4 (R.T.)

(c) Si 3 N 4 (1373K) (d) Si 3 N 4 (1673K)

Fig. 7. Examples of fracture surfaces at room and

elevated temperature.

fatigue crack front are clearly observed. The fracture surface of silicon
nitride at 1373K (c) is similar to that observed at room temperature. But,
morphology of fracture surface at 1673K becomes rough as shown in Fig.7(d).

CONCLUSIONS

The conclusions obtained in this study are summarized as follows:

1) New experimental system developed for cyclic fatigue tests of ceramics at
elevated temperature shows enough performance: Eccentric compression loading
method facilitates the fracture mechanical fatigue tests of ceramics with
wide stable crack growth range, and the extended unloading elastic compliance
method to detect the crack length and closure behaviors seems to gives
sufficient data.
2) The morphologies of stable fatigue crack growth area are flat and smooth
up to 1373K, however, it becomes rough at 1673K. Subtracted hysteresis loop
gives the information that crack closure is not observed in these tests of
PSZ and glass at room temperature.

REFERENCES

Dauskradt, R.H., W.Yu and R.O. Ritchie (1987). Fatigue crack propagation in
transformation-toughened zilconia ceramics, jJ. Am. Ceram. Soc., 70, C-248-
C-252.
Kishimoto, H., A. Ueno and H. Kawamoto (1987). Crack propagation characteri-
stics of sintered S13N4 under static and cyclic loads, J_. Mat. Sei. ,
Japan, 36, 1122-1127. (in Japanese).
Okamura, H., K. Watanabe and T. Takano (1975). Deformation and strength of
cracked member under bending moment and axial force, Eng. Fract. Mech., _7,
531-539.
Tada, H., P.C. Paris and G.R. Irwin (1973). Del Research Corp., In: The
Stress Analysis of Cracks Handbook, pp.2.10-2.15.
 WS7a5

FRACTURE OF CERAMIC MATRIX COMPOSITES

R. L. Brett and P. Bowen

School of Metallurgy and Materials / IRC in Materials for High Performance Applications,
University of Birmingham, PO Box 363, Birmingham, B15 2TT, UK

ABSTRACT

The fracture toughness of sintered silicon carbide (α-SiC) and silicon carbide reinforced with
paniculate titanium diboride (SiC/TiB2) has been evaluated using chevron notched bend
specimens at ambient and elevated temperatures. Significant differences in toughness are found.
A systematic investigation into the effect of chevron notch geometry on the resulting calculated
fracture toughness has been carried out. Recommended chevron notch geometries which give
consistent results are presented. Possible mechanisms which produce significant toughening in
the composite are discussed in this work.

KEYWORDS

Fracture toughness, ceramic matrix composites, elevated temperature, chevron notches, silicon
carbide, titanium diboride.

INTRODUCTION

Fatigue ^and fracture mechanisms are less well understood in brittle materials compared with
conventional alloys. Models of behaviour exist, but these are largely based on observations at
room temperature. One promising material is silicon carbide (SiC), but, although its maximum
operating temperature is very high, it has the disadvantage of having low toughness. It is
therefore likely that composite systems will be required, for instance, reinforcing SiC with SiC
fibres or using whisker reinforcement. A third option is the addition of a particulate
reinforcement phase, and although this has a less dramatic effect on the mechanical properties of
the material, it has the advantage of having much lower processing costs. An interesting system
is SiC/TiB2 in which the toughness is increased significantly compared with monolithic SiC
(McMurty, et al, 1987). This paper presents preliminary results in a study to quantify
micromechanisms of failure in such materials at ambient and elevated temperatures under
monotonic and cyclic loading. To date attention has been focussed on fracture toughness
determined in chevron notched bars (CVB) in bending.

351
352
EXPERIMENTAL

The materials studied in this work are commercially available α-SiC and SiC/TiB2 (supplied by
Carborundum Co., Niagara Falls, NY). The volume fraction of T1B2 in the composite material
is 16%. Bend bars of 6 mm x 3 mm x 50 mm were machined into which chevron notches of
different geometries were ground. The specimens were tested in three or four point bending on
an Instron 8501 servo-hydraulic machine at a constant stroke rate of 10 um/minute. The fracture
toughness, Kiev was evaluated using (Münz, et al, 1980):

Kicv = P T £ m i n (l)
where P m a x is the maximum load applied, W is the specimen depth, B the specimen thickness
and Y*min is the minimum stress intensity factor. This has been evaluated using the method of
analysis developed recently (Withey and Bowen, 1990).

The testpiece geometry is given in Fig. 1. The chevron notch included angle, Θ, was varied
between 40° and 120° for a constant ao of 0.3 and the depth, cto, was varied between 0.2 and
0.4 for Θ = 120°. In addition, two specimens of α-SiC with Θ = 60° and oto = 0.3 were slit to a
depth, a, of 0.44 which corresponds to the depth at which the minimum in the stress intensity
factor occurs, etc (Fig. 2). Testing was carried out at temperatures of up to 1200°C in air and
the specimens were held at temperature for an hour prior to testing.

Fractography was carried out using an Hitachi FEG SEM. The grain size of the SiC was
determined for both materials using polished specimens Optical sections of the fracture surface
were also prepared. The surface roughness of the fracture surfaces was evaluated using a Form
Talysurf, and the average roughness, Ra, was determined over a distance of 0.25 mm.

RESULTS

The effect of chevron notch geometry on the calculated value of fracture toughness is shown in
Fig. 3. It can be seen that there is little effect on KJCV as the notch depth or angle is varied.
However, an anomalous amount of scatter is observed in SiC/TiB2 when Θ = 40°. The geometry
used throughout the subsequent work in this study has been Θ = 60°, cto = 0-3. The specimens
which had been slit to etc prior to testing failed at higher loads than the normal specimens of the
same notch geometry (Table 1). There is a significant difference in toughness at the 99%
confidence level between the two materials tested, with the average value of Kiev increasing
from 2.5 MPaVm to 3.8 MPaVm (excluding the values obtained at Θ < 40°).

The effect of temperature on the toughness is shown in Fig. 4. The results are closely similar to
those obtained at room temperature, so at 1200°C there is no significant effect of temperature on
Kiev· There is fractographic evidence that the surface of SiC/TiB2 is attacked by oxygen at
1200°C (see Figs. 5a and b). The T1B2 particles on the fracture surface have obviously been
attacked, as shown by a change in their morphology. Examination of a fracture surface
produced subsequently at room temperature in the broken halves of the specimens tested at
elevated temperatures has shown this attack to have occured subsequent to failure since there is
no evidence of attack in the bulk of the specimen. Transgranular fracture was observed to have
occured in all the specimens. Both ot-SiC and SiC/TiB2 (Figs. 5a, 5b, 6a and 6b) appear to
have a greater amount of porosity on the fracture surfaces of the specimens tested at elevated
temperatures relative to the room temperature test-pieces. This can be explained by the oxidation
of free carbon (used as a sintering aid) which can be identified on the fracture surfaces resulting
from room temperature tests but is absent on the surfaces of the elevated temperature testpieces.
Such increased porosity is not observed to decrease the toughness as it occurs only at or near
the surface.
 353
The grain size of the silicon carbide was found to be 4.6 μηι in α-SiC compared with 3.7 μιτι in
SiC/TiB2. These results are from 200 grains measured in each material, with two readings from
each grain. This difference has been shown to be significant at a 99.9% level of confidence.

The surface roughness, Ra(0.25), has been found to be 0.9 μπι and 1.4 μιη for α-SiC and
SiC/TiB2 respectively. This increase is consistent with crack deflection around the T1B2
particles (Fig. 7) since there is an observed decrease in grain size in the composite matrix
material. It is interesting to note that the roughness of the surface of the α-SiC specimen tested
at 1200°C is reduced to 0.6 μιη while the corresponding value for SiC/TiB2 of 1.2 μιη is not
significantly lower than the specimens tested at room temperature.

DISCUSSION

The degree of scatter obtained at small chevron notch included angles is not fully understood, it
is considered in detail elsewhere (Brett, et al, 1991). In the present work it is sufficient to note
that there is a significant difference in toughness observed using this technique for SiC
reinforced with particulate T1B2. In addition, the tests on specimens with the notch ground to
the occ position did give significantly increased toughness levels, and this provides strong
support for the use of chevron notched bend specimens.

To date, it has not been possible to identify the critical parameter responsible for the toughening
of SiC/TiB2 composites. Possibilities include: microcracking, residual stresses (McMurty, et al,
1987) reduction in grain size and crack deflection (Seshadri, et al, 1987). Significant effects of
grain size have been found, but it is not generally accepted that this will definitely produce
toughening. Residual stresses appear not to be of primary importance since toughness values at
1200°C are closely similar to those measured at ambient temperature for the composite material.
Crack deflection has been shown to occur by the surface roughness results as Ra would be
expected to decrease with grain size and the larger value observed in this work indicates crack
deflection around the T1B2 particles. However, previous work (Seshadri, et al, 1987) has
predicted only a 6% increase in toughness due to crack deflection, therefore microcracking must
also be involved in the toughening mechanism. It is too early in this work to test models of
microcracking because of difficulties in estimating the size of the process zone (Evans, 1990).

Using a critical defect size of > 2 mm and values of Kiev as given above, operating stresses of
31 MPa and 48 MPa have been calculated for α-SiC and SiC/TiB2 respectively. Even though
this corresponds to a dramatic increase in toughness for T1B2 additions, these materials should
be primarily used in compression, or as lightly stressed tensile parts at best.

The use of the CVB geometry may be of interest for use at high temperatures since catastrophic
failure will take place at occ, some distance below the surface of the testpiece, compared with
degradation of rupture strength specimens.

CONCLUSIONS
Using chevron notched bend bars, values of the fracture toughness of α-SiC and SiC/TiB2 have
been determined to be 2.5 MPaVm and 3.8 MPaVm respectively.

No change in Kiev w a s observed between specimens tested at ambient temperature and 1200°C
and hence residual stresses have little effect on the toughness.

The increase in surface roughness values for SiC/TiB2 relative to α-SiC has been deduced to be
due to crack deflection around the T1B2 particles. This will undoubtedly contribute to the
increased fracture toughness of the composite material.
354
REFERENCES
Brett, R. L., P. A. Withey and P. Bowen, (1991). Chevron Notch Fracture Toughness Testing
in Brittle Solids, submitted to Mat. Sei. and Tech.
Evans, A. G., (1990). Perspective on the Development of High-Toughness Ceramics, / . Am.
Ceram. Soc, 73, 187-206.
Immerson, D., (1990). Private Communication.
McMurty, C. H., D. G. Boecker, S. S. Seshadri, J. S. Zanghi and J. E. Gamier, (1987).
Microstructure and Material Properties of SiC-TiB2 Composites. Am. Ceram. Soc. Bull.,
66, 325-329.
Munz, D., R. T. Bubsey and J. E. Srawley, (1980). Int. J. Fract. Mech.x 16, 359-374
Seshadri, S. G., M. Srinivasan, and K. M. Keeler, (1987). Numerical Computation of the
Toughening Increments Due to Crack Deflection in Paniculate Composites. Ceram. Eng.
Sci.Proc, 8, 671-684
Withey, P. A. and P. Bowen, (1990). Analysis of Chevron Notches in Pure Bending, Int. J.
Fract., 46, R55-R59

ACKNOWLEDGEMENTS

The authors would like to thank Dr. I. Thompson for useful discussions and Dr. A. Stathan for
surface roughness analysis. One of the authors (RLB) is supported by a SERC CASE award
with BP.

Table 1 Effect of incorporating a notch of depth occ into a CVB testpiece

Specimen Type Failure Load Fracture Toughness

(N) (MPaVm)
CVB Testpiece 55 2.6
ao = 0.3 47 2.2
Θ =60° 55 2.6
48 2.3
53 2.5
50 2.4
59 2.8
48 2.3
52 2.4
As above notched 64 3.0
to a = 0.44 (Fig. 2) 72 3.4
 355

Fig. 1 Geometry of CVB testpiece

(a) (b)

t aC
»

Fig. 2 Geometry of CVB testpiece (a) normal, (b) notched to occ

3 5
* , —
N

£ ~y
£4h * £ 4 -*
£ 4
■ Δ
VJ
O -»
c -) ■ o o
Up
o
H o
«j ~

o SiCao/W=0.3 3
O
• SiCao/W=0 o SiC
£ 1 Δ SiC/TiB2 ao/W=0.3
£1 Δ SiC/TiB2
A SiC/TiB2 ao/W=0
J_ _L :..i , . L. ... I

40 60 80 100 120 400 800 1200

Chevron Notch Angle (°) Temperature (°C)

Fig. 3 Effect of chevron notch geometry Fig. 4 Effect of temperature on Kiev

on Kiev (Θ = 60°, ao = 0.3)
356

Fig. 5 Fracture Surface of SiC/TiB2 (a) room temperature (BSE image), (b) 1200°C
(SE image)

Fig. 6 Fracture Surface of cc-SiC (SE image) (a) room temperature, (b) 1200°C

Fig.7 TEM micrograph showing crack deflection around TiB2 (Immerson, 1990)
 WS7a6

CRACK PROPAGATION BEHAVIOR OF SINTERED SILICON NITRIDE

UNDER CYCLIC LOADS

H.KISHIMOTO , A.UENO and H.KAWAMOTO

* Toyota Technological Institute, 2-12-1 Hisakata, Tempaku, Nagoya 468, Japan

** Toyota Motor Corp., 1 Toyota-cyo, Toyota 471, Japan

ABSTRACT

In order to clarify the crack propagation behavior of sintered silicon nitride under cyclic loads, a
series of research works using compact tension specimens, were carried out. Influence of stress
ratio, compression load, test frequency, and crack closure phenomenon on the crack propagation
rate were studied. One possible fatigue mechanism is proposed and discussed with some
evidence.

INTRODUCTION

Sintered silicon nitride is one of the best candidates for the structural ceramics. It is important to
know fatigue characteristics of the structural ceramics practically and also basically. We have
carried out a series of crack propagation tests of a sintered silicon nitride under cyclic loads
using compact tension specimen (Kishimoto et a/.,1987a,b,1989a,b,1990a,b; Ueno et
a/.,1990a,b). Many important fatigue behaviors became evident. The purpose of this paper is to
summarize all the important behaviors found in our studies in order to discuss fatigue
mechanisms in ceramics under cyclic loads.

KEYWORDS

Sintered Si3N4, Crack Propagation, Cyclic Load, Crack Closure, Bridging, Fatigue Mechanism

EXPERIMENTAL PROCEDURE

The material used in this study was a sintered silicon nitride doped with Y 2 0 3 and A1203. The
3-point bending strength σ b is 740MPa, Young's modulus E is 310GPa and mean fracture
toughness Kc is S.SSMPam1 . Fracture toughness Kc was obtained through indentation fracture
method using Niihara's equation.(Niihara et ed., 1982). The material used in this study was
357
358
composed of columnar /?-Si3N4 crystals whose average diameter was 0.48// m and average
aspect ratio was 6.8. Size and shape of test piece are shown in Fig.l. In cyclic fatigue tests,
sinusoidal stress wave form was employed. All tests were carried out at 25°C and in 60%
relative humidity.

Section A-A
0=O.25W (Chevron notch)

Fig.1. Configuration and dimensions of CT specimen.

TEST RESULTS

Influence of the Stress Ratio on the Crack Propagation RatefKishimoto etal.. 1989: Ueno etai,
1990a.b)

An example of the relation between maximum stress intensity factor Klmax and the crack

Kjhpx i k g f / m m
12 14 16 18 20
1.1
Ϊ10 Γ ffl
i p i|i . 1 |Ùà 1~Ί
Key f(Hz) R
1.0
I
r © 0.75
r o 50 0.85
3 T § J (off
0.9! SsS-a^^
I 10*L~o1 0.90
(1
Ä
F° - 100

fur 1 ^
v&H
* , 0-8 ig| .A
VK^/TW {·
■SI l3
c
° -in 8
IßtJm J 0.7
X*
+3 10 sj/Lpi /jT7
CO
1
5?
|£<r >

u
g.10 — &

I*
da/dN(m/cycle) ^fll
I Key
0.6 ισ'° 10"· 10-·

1
©
© * 99
50 ®
o D
Ξ
Δ
A
KHz)
10 ® H A
1 0 a A
Ü 1Ö 11|
0.5 I —1—
4 5 6 0.02 0.05 0.1 0.5 1.0
Stress intensity factor Κ ^ , MPa/m 1-R

Fig.2. Relation between daldt Fig.3. Relation between KImax

and K1mav. and 1-R.
 359
propagation rate daldt with various stress ratio R is shown in Fig. 2. Relation between daldN and
daldt is correlated as da/dt=da/dN Xf. It shows that even the cyclic stress of high stress ratio
accelerated the crack propagation rate as compared with that under the static load. The results
with positive stress ratio are shown in Fig.3. In this figure, abscissas is stress intensity factor
range A K divided by maximum stress intensity factor KImskx. A K is Klmax-Klmin. K* is the
stress intensity factor at the crack propagation rate 5 X 10"5m/cycle for each specimen. The crack
propagation rate did not change when the stress range decreased from 0.98 to 0.92, and the
crack propagation rate was equal to that under the static load. This means that too low stress
amplitude did not accelerate the crack propagation rate. When the stress ratio is below 0.92,
maximum stress intensity factir ^ Imax decreases consistently as the stress ratio decreases. The
effects of the cyclic loads on the crack propagation rate can be observed when R is below 0.92.

Crack ClosureiKishimoto era/.. 1989.1990a.b: Ueno etal.Λ990ζύ)

Crack closure was observed through unloading elastic compliance method as shown in Fig.4.
The crack opening load Popen decreased as R decreased.

R=0.1,K-decrease R— 2,K - d e c r e a s e
750
z
Q-" 5 0 0 II I i i
Hill
Ό
CO
5 250

vvvvv I
E
0
^

VXXYT
-250 -

-500 -
Z
oT -750 -
\ \ \ \ \

Aim
\ \ \ \ \
Ό
to
j -1000-

-1250-

-1500-

Fig.4. Examples of load-displacement curve.

The Influence of Compressive Load on the Crack Propagation RatefiCishimoto etal.. 1989)

The crack propagation test results with negative stress ratio is shown in Fig.5. The crack
propagation rate increased as the stress ratio decreased. The threshold stress intensity factor
KFSCC decreased as the stress ratio decreased. Figure 6 is reproduced from Fig.5. When R is
positive, ^ Imax decreases as R decreases. Whereas when R is negative KImax decreases slightly
as R decreases. This means that the compressive stress has little effect on the crack propagation
rate.
360

Figure 7 shows the relation between A K^KlmSiX and KlmJKc at three specific crack
propagation rate. A Keff is Klmax-Kopen. Almost linear relation is seen, and quite different from
Fig.6. From comparing these two figures, it can be said that A Keff is more effective factor as a
measure of amplitude than R in the crack propagation under cyclic loads especially when R is
negative. Thus we can conclude that the compressive load lowered opening load Popen, then A
Ke{{ increased, and finally the crack propagation rate increased as seen in Fig.5.

E 10" 79

|«·Ι
Φ
3 10

(0
D)
fM
'$&*?"^-U l ?r.
UN x«
ce Key R f(Hz)
' X*t da/dt(m/»*c)
-o- 10-
D 0.5 1 - O- 10 ■*

8· ioH n O 0.1 1
-«-
- β-
10"'
Δ -1 1 10"'
- Ö-

?
10"
V -2 1
J.—I.™ 1 -·- »"·
o -1 0
«/Kc Stress ratio R
i<r
0.4 0.6 0.8 1.0
Fig.5. stress
Normalized Relation between
Intensity daldt
factor K, m and Fig.6. Relation among daidu R
KlmJKCt mdKlmJKc.
and

Fig.7. Relation between Κ^Κ€ and AKJK^.

Influence of Frequency on the Crack Propagation RatefKishimoto et d.. 1989: Ueno et d.,
1990a.b)

Figure 8 shows the relation between maximum stress intensity factor Klimx and the crack
 361
propagation rate da/dt when/is within the range of 1Hz to 100Hz. Figure 9 is reproduced from
Fig. 8. With low Klmax which is lower than Klscc the crack propagated cycle-dependently, with
high Klmax the crack propagated almost time-dependently, and with medium Klmax the crack
propagated cycle-dependently and time-dependently. Klscc is the threshold stress intensity factor
under static load and is 5.1MPam1/2 as seen in Fig.8. For all of our test results, when the
frequency is within the range of 0.01 Hz to 100Hz, the crack propagated cycle-dependently with
^imax lower than Klscc and the crack propagated almost time-dependently with high KImax.

K ^ , kgf/mm3'2
_4 12 14 16 18 20

Ly°i Key Κ,„.,(ΜΡ8/Γη)

-Q-
-O-
-O-
5.50
5.25
5.00
4.75
-Φ-
-Q- 4.50
-<2>- 4.25
-♦- 4.00

f
4 5* 6 10 100
Stress Intensity factor Km™*, MPa/rn Frequency f , Hz

Fig.8. Relation between da/dt Fig.9. Relation between da/dt

and Klmax. and frequency/.

Controlling Factor of the Fatigue Crack Propagation

In this study, AKeff eq which is difined as A Keffeq = Klmax7' A ΚΐΠ1γ (Hojo et ed., 1987) was
determined experimentally as shown in Fig. 10. / ' is nearly 1, and it decreases from 1 to 0.9 as

c I 1 1 0.0
" '—9 ό ^ ^ n. )
1

0.5 0.5 i

0.0 1.0
10 - 10" 10"' 10° 10"
Crack propagation rate da/dN , m/cycie

Fig. 10. Relation between γ' and da/dN.

362
the crack propagation rate decreased from 10'5m/cycle to 10'9m/cycle. This means that at the
crack propagation rate 10" m/cycle, only Klm&x is important in the crack propagation under the
cyclic loads. At 10"9m/cycle, Klmax is again very important(90%) and A Kef( is a little
important 10%) in the crack propagation under the cyclic loads. Therefore, it is clear that the
crack propagation under the cyclic loads is mainly controlled by Κ1ηΛΧ and slightly controlled
by A Keff only in the case of very low crack propagation rate. Finally, the above mentioned
fatigue behaviors of the sintered silicon nitride under the cyclic loads seems to be merely stress
corrosion cracking phenomenon simply accelerated by the cyclic loads.

Fatigue Mechanism

The material used in this study was composed of columnar /?-Si3N4 whose average aspect ratio
was 6.8. In this material, fatigue crack propagated mainly intergranularly.(Kishimoto et cd.,
Submitted) Fracture surface was very rough. Figure 11 shows a crack pass which shows the
crack bridging due to the columnar ß -Si3N4 crystal as reported by Tanaka et.al.(\9S9) and
Grathwohl et.al.(\989). The crack bridging which occurs behind the crack tip shields the stress
at the crack tip and, as a result, the real stress intensity factor Ktip at th crack tip is reduced as
described in equation(l).

K ti ρ _
^Imax " & s (1)

Ks is the stress intensity factor shielded by the crack brigding.

Crack opening displacement of a semi-elliptical surface crack, which was made by Knoop
indentation and then about 50// m of the surface layer was polished off to remove the residual
stress, was measured at KY 3.1MPam (Ueno etal., Submitted). The first measurement was
done immediately after the surface polishing. Then 106 cycles of sinusoidal cyclic stress whose
^imax w as 3.9MParn z and R was 0.1 was applied. Afterwards, the crack opening
displacement was measured again at K1 3.1 MParn172. The results are shown in Fig. 12. It is
evident that the cyclic stress resulted in larger crack opening displacement. The larger C.O.D.
seems to be originated from the reduction in Ks. From the discussion on / ' in Fig. 10, it is
evient that Klmax is the most important factor for the crack to grow even under the cyclic
loads. Furthermore, upper part of Fig.3 means that Klmax at maximum load is essentially
important. We prefer a fatigue mechanism based on KlnuaL at maximum load. That is, Ks is
reduced by the cyclic loads, then Ktip increases under the cyclic loads as compared with ^ t i p
under the static load, and finally the crack propagation rate is accelerated under the cyclic loads.
Under the cyclic fatigue condition, cyclic back and forth action under cyclic loads is consider to
promote loosening at the bridging portion and then it reduces the bridging effect Ks. This
reduction in Ks is consider to increase as the amplitude of the cyclic stress increases. Figure 3
supports this mechanism. The horizontal line in Fig.3 when \-R is smaller than 0.08 may be
originated from Coulomb type of friction at bridging portion. As to this mechanism, effective
amplitude of the cyclic loads is given by A Ke{{ in all ranges of/? as seen in Fig.7, as contrast to
Fig.6 which shows different dependence of R on KlmjiX according to whether R is positive or
 363

Fig.l 1. Scanning electron micrograph of a crack path.

Bar indicates 3//m.

0.15
Key] Number ol cycles
oI 1
E
a.
•1 10'

- 0.10
1
vo Q,'
•
Q
O
Ü 0.05
CM o

A*
NN
0
-200 -100 0 100 200

Distance from center d , jjm

Fig. 12. Crack opening displacement at Kl 3.1 MPam1/2 measured on

the surface before stress cycling and after stress cycling of 106.

negative. The crack closure phenomenon increased Pmin of the cyclic loads to Popen, then it
decreased A KeW it prevented reduction of Ks under the cyclic loads and finally the acceleration
in the crack propagation rate. The cycle-dependent crack propagation phenomenon at ^ Imax
lower than Klscc as seen in Fig. 8 and Fig.9 is thought to mean that one stress cycle reduced Ks
the magunitude of which was determined by only A Kef{ and then increased Λ^ρ. As a result,
Ktip exceeded the threshold value for the crack growth under the static load. Cyclic fatigue
phenomenon as seen in this study is merely stress corrosion cracking accelerated by the cyclic
loads.

CONCLUSION

Crack propagation behavior of sintered silicon nitride under the cyclic load was investigated.
(1) The influence of the stress ratio, compressive stress, crack closure, and frequency on the
crack propagation rate were studied. (2) Controlling factor of the crack propagation was
evaluated. (3) A possible cyclic fatigue mechanism based on the crack bridging is proposed and
it is evaluated through the experimental results.
364
REFERENCES

Frei,H., Plappert, C. and Grathwohl,G.(1989). SEM In-situ Bending Experiments on High

Performance Ceramics. EURO-CERAMICS(GAe With,R.A.Terpstra and R.Metselaar,
Ed.),3, 3.115-3.119.
Hojo,M.,Tanaka,K.,Gustafson,C.G. and Hayashi,R.(1987). Effect of Stress Ratio on Near-
threshold Propagation of Delamination Fatigue Cracks in Unidirectional CFRP. Compos.
Sci.Technol.,29,273-219.
Kishimoto,H.,Ueno,A. and Kawamoto,H.(1987). Crack Propagation Characteristics of
Sintered Si3N4 under Static and Cyclic Loads. / . of the Society of Materials Science Japan,
36, 1122-1127.
Kishimoto,H.,Ueno,A. and Kawamoto,H.(1987). Crack Propagation Behaviors of Sintered
Si3N4 under Static and Cyclic Loads. Proc. of the 32th Japan National Symposium on
Stength,Fracture and Fatigue, Special Subject: Mechanical Behavior of Engineering
Ceramics, 32,61-67.
Kishimoto,H.,Ueno,A. and Kawamoto,H.(1989). Crack Propagation Behavior of Sintered
Si3N4 under Static and Cyclic Load. Proc. of the MRS International Meeting on Advanced
Materials(T.Kishi and M.Sakai, Ed.),_5, 531-536.
Kishimoto,H.,Ueno,A., Kawamoto,H. and Fujii,Y.(1989). The Influence of Wave Form and
Compressive Loads on the Crack Propagation Behavior of a Sintered Si3N4 under Cyclic
Loads. / . of the Society of Materials Science Japan, 38,1212-1217.
Kishimoto,H.,Ueno,A., Kawamoto,H.(1990). Crack Propagation Behavior of Sintered Silicon
Nitride under Cyclic Load -Influence of Difference in Material-. Trans, of the Japan Society
of Mechanical Engineers, A-56, 50-56.
Kishimoto,H.,Ueno,A., Kawamoto,H.(1990). Crack Propagation Behavior of Si3N4 under
Cyclic Loads -Influence of Difference in Materials-. Proc. of the 4th international
Conference on Fatigue and Fatigue Thresholds(H.Kitagawa. and T.Tanaka, Ed.), 2,
727-732.
Kishimoto,H. and Ueno,A., Fractographic Analysis of Fracture Stress of Sintered Silicon
Nitride Fractured under Static and Cyclic Load. Submitted to / . of the Society of Materials
Sciencejapan.
Niihara,K.,Morena,R. and Hasselman,D.P.H.(1982). /. of Materials Science Letters, 1, 13-16.
Steffen,A.A.,Dauskardt,R.H. and R.O.Ritchie.(1990). Cyclic Fatigue-crack Propagation in
Ceramics:Long and Small Crack Behavior. Proc. of the 4th International Conference on
Fatigue and Fatigue r/*ras/w/ifa(H.Kitagawa and T.Tanaka, Ed.),J£, 745-752.
Tanaka,T.,Okabe,N. and Ishimaru,Y.(1989). Fatigue Crack Growth and Crack Closure of
Silicon Nitride under Wedge Effect by Fine Fragments. / . of the Society of Materials
Sciencejapan , 38, 137-143.
Ueno,A.,Kishimoto,H., Kawamoto,H. and Asakura,M.(1990). Crack Propagation
Behavior of Sintered Silicon Nitride under Cyclic Load of High Frequency and High Stress
Ratio. /. of the Society of Materials Sciencejapan, 39, 1570-1575.
Ueno,A.,Kishimoto,H., Kawamoto,H. and Asakura,M.(1990). Crack Propagation
Behavior of Sintered Silicon Nitride under Cyclic Load of High Stress Ratio and High
Frequency. Proc. of the 4th International Conference on Fatigue and Fatigue Thresholds
(H.Kitagawa andT.Tanaka,Ed.),^, 733-738.
Ueno,A.,Kishimoto,H. and Kawamoto H., Static and Cyclic Fatigue Tests of Sintered Si3N4
with Small Semi-elliptical Surface Crack. Submitted to / . of the Society of Materials
Sciencejapan.
WS7a8

DAMAGE ACCUMULATION CAUSED BY CYCLIC INDENTATION

IN CERAMIC MATERIALS

E. TAKAKURA and S. HORIBE

National Research Institute for Metals, Tsukuba Laboratories,

1-2-1, Sengen, Tsukuba-shi, Ibaraki 305, JAPAN

ABSTRACT

Indentation fatigue in various ceramic materials was investi-

gated in terms of grain size, fracture appearance and
ionic/covalent bonding characteristics. It has been found that
there are two types of indentation fatigue behavior (Type I and
Type II). Type I is characterized by slight increase of damaged
zone size with increased number of indentation cycles, followed
by the abrupt chipping of a part of surface layer. Such Type I
behavior was observed in silicon carbide, silicon nitride and
sialon, which was considered to be caused by the continuous
growth of lateral cracks with indentation cycles. On the other
hand, Type II behavior, which was seen in magnesium oxide and
aluminum oxide, is characterized by pronounced enlargement of
indentation-induced damaged zone in early cycles. It is assumed
that this type of behavior is associated with plasticity and
microcracking characteristics of materials.

KEYWORDS

Fatigue; indentation; lateral crack; crack growth; ceramics;

grain size; plasticity.

INTRODUCTION
Indentation fatigue is the damage accumulation in the surface
layer of ceramics caused by local cyclic compressive loading.
It has been first reported by Guiu et al. (1986, 1987) that a
lateral crack propagates with indentation cycles, which results
in chipping behavior. This is supposed to be very important not
only from the view point of engineering practice such as con-
tact or fretting fatigue, but also for fundamentally under-
standing fatigue mechanism of the damage caused by crack-
asperity contact.

365
366
In this study, we attempted to systematize indentation fatigue
in terms of characteristics of materials and paid special
attention to the effects of grain size, fracture appearance
(crack path) and ionic/covalent bonding upon indentation fa-
tigue .

EXPERIMENTAL PROCEDURE

The tested materials are silicon carbide, silicon nitride,

sialon, aluminum oxide and magnesium oxide, which were produced
by sintering processes. Silicon carbide, silicon nitride and
sialon are highly covalent bonded materials, which are charac-
terized by brittle manner in fracture. Magnesium oxide is a
highly ionic bonded material and more ductile than silicon
carbide and silicon nitride. Aluminum oxide has medium nature
between the former and the latter.

Indentation fatigue tests were carried out by indenting repeat-

edly onto the same point of the specimen surface by using a
Vickers hardness tester. The surface crack behavior, the size
of damaged area and the number of cycles to chipping were
measured by an optical microscope. The fracture surface in the
chipping area was also observed by a scanning electron micro-
scope(SEM).

RESULTS AND DISCUSSION

General Tendency in Cyclic Indentation

Figure 1 shows the extending behavior of damaged area produced

by cyclic indentation. In silicon carbide, silicon nitride and
sialon ceramics with strong covalent bonding, very slight
increase of the damaged zone size was observed during cyclic
indentation for some tens of cycles, followed by the abrupt
extension of this area at a certain number of cycles (Fig. la).
We call this kind of damage Type I. Such behavior implies that
lateral crack propagation is caused by cyclic loading, which
results in the chipping of a part of surface layer. Figure 2
presents the relation between the indentation load and the
number of cycles required to produce chipping in silicon car-
bide and silicon nitride ceramics under cyclic indentation,
which corresponds to a S-N curve obtained by conventional
fatigue tests. From this figure, it is found that transgranular
fracture type materials tend to produce chipping more easily
rather than intergranular fracture type ones (Takakura and
Horibe, 1990).

As shown in Fig. lb, in magnesium oxide which has small but

significant plasticity attributable to ionic bonding, it has
been found that the damaged zone is pronouncedly enlarged in
early stages with number of indentation cycles. This kind of
damage was called Type II. It appears that aluminum oxide has
behaved in either way of Type I or Type II, depending upon the
grain size.
 367

(b)
Ο SiC(transgranular)
600 • SiC(intergranular) 600
Δ Si3N4(transgranular)
ε A Si3N4(intergranular) E
□ sialon(intergranular; 0.3 A m) a.
■ sialonjintergranular; 1.0/*m)
2
CO 400 400
Ό Φ
ω O)
ο> CO
η E
ε CO
•Ό
O MgO (10/im)
Ο 200 200 • MgO (25μνη)
8 D
■
Al2O3(10^m)
Αΐ2θ3( 2μπ\)
0) CO

10 20 30 40 10 20 30 40
Number of cycles Number of cycles

Fig. 1. Development of damaged area under

cyclic indentation; peak applied load
is 196N: (a)covalent bonded materials,
(b)ionic bonded materials.

40

O SlC(transgranular)
30 • SlC(lntergranular)
Δ Sl3N4(transgranular)
A Sl3N4(lntergranular)
3
20
Q.
O.
CO

CO
i? 10

Number of cycles to chipping

Fig. 2. Relation between indentation load and

number of cycles to chipping in sili-
con carbide and silicon nitride under
cyclic indentation.
368
Lateral Crack Propagation during Cyclic Indentation and Its
Mechanism (Type I)

Significant lateral crack growth and the resulting typical

chipping phenomena were observed in the materials with high
covalent bonding, such as silicon carbide, silicon nitride and
sialon ceramics, particularly in transgranular fracture type
ones. Figure 3 presents the SEM photographs of chipping area
produced in silicon nitride of transgranular fracture type. A
striped pattern is formed in chipping areas. The interval of
the stripes approximately corresponds to the lateral crack
growth rate (i.e., the size of chipping area divided by the
cycles to chipping). Therefore, such striped pattern was iden-
tified as a striation (Takakura and Horibe, 1990).

Continuous propagation of the lateral crack with increased

cycles of indentation is considered to be attributable to the
difference between the stress fields under loading and unload-
ing (Figure 4 ) . During unloading process after the first in-
denting, lateral crack is produced near the border between
plastic and elastic zones. The crack is supposed to propagate
also during the following loading, because in this process a
shear stress is produced at the crack tip, resulting in Mode
II cracking. Such lateral cracking under loading makes a new
residual stress field, followed by subsequent lateral crack
growth during unloading. It is assumed that the above sequence
is repeated. As a result, zigzag growth of a lateral crack is
produced, and observed as striations. The reason why the later-
al crack growth and the resultant chipping behavior are sup-
pressed in intergranular fracture type materials is presumably
that crack branching and microcracking more easily occur in
those materials so that the stress concentration at the crack
tip is relieved. In intergranular fracture type materials, Mode
II fracture is supposed to be restrained because of the rugged-
ness of crack surfaces. This might be another reason.

Effect of Plasticity
Around an indentation on magnesium oxide, many slip traces and
microcracks were observed. Indentation-induced cracking in
magnesium oxide is attributed to the reaction of dislocations,
which is reasonably explained by dislocation pile-up model
(Armstrong and Elban, 1985). Such cracking makes considerably
large damaged zone surrounding indentations. However, it might
be difficult for lateral crack to continuously propagate during
cyclic indentation in this material, because the residual
stress playing a role of driving force for lateral cracking is
easily relieved by plastic deformation or microcracking.

Effect of Grain Size

Grain size dependence of cyclic indentation behavior was exam-
ined by using sialon and aluminum oxide. From the results shown
in Fig. 1, it has been found that the effect of grain size in
sialon ceramics upon the cyclic indentation damage is insignif-
 369

Fig. 3. SEM photographs of chipping area pro-

duced in silicon nitride of transgran-
ular fracture type, (a)low magnifica-
tion, (b)high magnification.

jui ; L 2 ; u 2 ; L 3 : u 3 ; u i

Plastic deformation zone

Median/radial crack

Fig. 4. Lateral crack propagation mechanism.

(U^:unloading, L^:loading)
370
icant, but in aluminum oxide it appears to be considerable;
that is, coarse-grained aluminum oxide behaved in Type II,
whereas fine-grained one did in Type I. Since coarse-grained
aluminum oxide reveals R-curve behavior during crack extension
(Wieninger et al. , 1986), microcracks are expected to be easily
produced at grain boundaries or inside of the grains. Such
microcraking makes the damaged zone enlarge in early stages of
indentation cycles, but prevents the propagation of lateral
cracks during subsequent cycles in the similar fashion as
described on magnesium oxide.

SUMMARY
It has been found that damage is accumulated in surface layer
of ceramic materials by cyclic indentation. In terms of the
appearance and the extent of such damage, materials can be
classified into two groups; Type I and Type II. In the materi-
als of Type I, the apparent surface damage during cyclic inden-
tation is limited, but chipping tends to occur abruptly, which
is caused by cyclic propagation of lateral cracks. This type of
behavior is peculiar to the materials having high covalent
bonding, particularly in transgranular fracture type materials.
In the materials of Type II, indentation-induced damaged zone
is pronouncedly enlarged in early stages of indentation cycles.
This type of fracture is associated with plasticity and micro-
craking characteristics of materials.

REFERENCES

Armstrong, R.W. and W.L. Elban (1985). Dislocation aspects of

plastic flow and cracking at indentations in magnesium oxide
and cyclotrimethylenetrinitramine explosive crystals. In:
Microindentation Techniques in Materials Science and Engi-
neering, (P.J. Blau and B.R. Lawn, ed.), pp.109-126. ASTM,
Philadelphia.
Guiu, F. and D.A.J. Vaughan (1986). Crack propagation by fa-
tigue in tough ceramics. In: Processing of Advanced Ceramics,
(J.S.Moya and S.de Aza, ed.), pp.217-233. Arganda del Rey,
Madrid.
Takakura, E. and S. Horibe (1990). Indentation fatigue of
silicon carbide and silicon nitride. J. Jpn Inst. Met., 54,
611-616., in Japanese.
Vaughan, D.A., F. Guiu and M.R. Dalman (1987). Indentation
fatigue of alumina. J. Mater. Sei. Lett., 6., 689-691.
Wieninger, H., K. Kromp and R.F. Pabst (1986). Crack resistance
curves of alumina and zirconia at room temperature. J. Mater.
Sei., li, 411-418.
 WS7a9

EFFECT OF SURFACE FINISH ON FATIGUE STRENGTH IN SILICON NITRIDE

M.TAKAHASHI1, Y.MUTOH1, K.YANAGI1, H.OKAMOTO2 and T.OIKAWA2

1
Department of Mechanical Engineering, Nagaoka University
of Technology, Kamitomioka, Nagaoka, 940-21, Japan.
2
Advanced Technical Research Center, NKK Corp.,
Kawasaki-ku, kawasaki, 210, Japan.

ABSTRACT

Fatigue Tests of silicon nitride specimens with different surface finishes

were carried out. The effect of surface finish on fatigue strength was dis-
cussed using the surface shape parameters as well as the conventional rough-
ness parameters. A functional relationship between fatigue strength and a
certain grinding condition such as grade of abrasive grain, grinding volume,
etc., was hardly found. The surface shape parameters, which representing the
mechanical severity of valleys, gave a good correlation with the fatigue
strength. On the other hand, the conventional roughness parameters, which
informing the amplitude of surface roughness, did not satisfactorily
correlate with the fatigue strength.

KEYWORDS

Fatigue Strength; Surface Finish; Grinding Condition; Residual Stress; Sili-

con Nitride; Ceramics.

INTRODUCTION

It is known that embedded and surface defects have important influence on

strength of ceramic materials. Recent advance in processing technology
reduces size and number of embedded defects. It is also enable to reduce
size and number of surface cracks by surface finishing such as lapping.
However, for actual structural components, it will be physically and
economically hard to perform the high grade of surface finish to all the
surface of the component. Therefore, the components with as-sintered and/or
roughly-ground surfaces will be supplied for practical use.

Many studies on the effect of surface damage induced by the grinding on

strength have been carried out. It has been reported that the reduction of
bending strength is significant in the case that the direction of grinding
is perpendicular to that of tensile stress (Miyamoto et al. , 1989), and that
the compressive residual stress is provided on the ground surface(Tanaka et

371
372
al., 1987). However, studies on the effect of surface finish on fatigue
strength have been limited.

In the present study, fatigue tests of silicon nitride specimens with

several different surface finishes were carried out. On the basis of the
test results, the effects of surface finish and residual stress on fatigue
strength were discussed.

EXPERIMENTAL PROCEDURE

Fatigue Test

The material used is HIP-sintered Si3N4 with additives of A1 2 0 3 and Y 2 0 3 .

Mechanical properties of the material used are shown in Table 1. Fatigue

Table 1 Mechanical properties of the material used.

E Hv Of Kic
(OFtO (GRi) (Mfti) (Mft*fc)

S13N4 318 15.1 1120 6.4

Table 2 Grinding conditions.

Speciien Final grinding Setting depth Feed speed Uheel speed

wheel A (>im) li'iin) (■/■in)
SP-1 #1000 5-10 10 1700
SP-2 #80 5-10 10 1700
SP-3 #200 100 15 2000
SP-4 as-sintered
SP-5 notched
rough grinding : ιΊ4β-)Ι27β->Ι8ΒΒ (longitudinal direction)
final grinding : perpendiculer direction

F i g . l SEM p h o t o g r a p h s o f g r o u n d a n d a s - s i n t e r e d surface.
 373

angle of
r— P I quadratic inclination.e
function

cubic
N-2N function N+2
N-1 N N+ 1 ■
IN*. N*2
— N N
(a) The radius of (b) The area of (c) The angle of
curvature, p curvature, S inclination, Θ
Fig.2 Outline of the surface shape parameters.
test specimens with dimensions of 3 X 4 X 35mm were machined.

The specimen surfaces were ground under three different conditions shown in
Table 2. The final grinding of all specimens was conducted in the direction
perpendicular to the longitudinal direction of the specimen. The specimens
with as-sintered surface and with a U-shape notch, stress concentration
factor of which was a =1.7, were also prepared. Surface morphology of the
specimens used is shown in Fig.l.

Fatigue tests were carried out using a servohydraulic fatigue test machine
with a capacity of 4.9kN under four point bending with loading span of 10mm
and supporting span of 30mm. The sinusoidal wave form of loading with a
stress ratio of 0.1 and frequency of 20Hz was utilized in the fatigue tests.

Measurement of Surface Configuration

The maximum height Rmax and the center line average R a have been accepted as
a measure of surface finish. The notch sensitivity of ceramics is considered
to be high. Therefore, even if the Rmax value was low, the fracture strength
of a specimen with sharp valleys on the ground surface would be reduced. In
the present study, the following surface shape parameters proposed by Yanagi
et al.(Yanagi et al., 1991), which represent the sharpness of valley on the
ground surface, were used to evaluate the performance of ground surface. (1)
The radius of curvature, p (Fig.2(a)), (2) The area of curvature,
S(Fig.2(b)), and (3) The angle of inclination, Θ (Fig.2(c)). Small value of
p and S and a large value of Θ correspond to a sharp valley. The method
for evaluating these surface shape parameters was reported in detail in the
reference(Yanagi et al.,1991).

Measurement of Residual Stress

The residual stress on the ground surface was measured in the longitudinal
direction of the specimen. An X ray stress measurement cem was used. The
residual stress was evaluated by the sin2 φ method using the CuK a and CrK
a rays with an irradiation area of 4 X 2mm.

RESULTS and DISCUSSION

Fatigue Strength

A relationship between stress amplitude G a and number of cycles to failure

374

10 10' 10" 10" 10

Number of cycles to failure Nf

Fig.3 Relationship between stress amplitude and number of
cycles to failure.

Table 3 The surface shape parameters for the specimen

tested.

σΒ σ. Kaax R. P S Θ
(MW (Wk> <*■) <*■> (Mm) <*■■> (dee.)

SP-I 940 320 0.4 0.05 4.2 0.017 3,3

SP-2 735 220 2.6 0.32 3.1 0.038 4.1
SP-3 646 210 1.9 0.24 2.9 0.039 4.3
SP-4 409 ISO 40.0 5.00 0.9 0.090 13,0

Table 4 The surface shape parameters for SP-1 specimens

with different fatigue lives at the same stress
amplitude.

Stress Nmber of Riax Ra P S Θ

Specken amplitude cycles to (>um) (yum) (um) (/im 2 ) (deg.)
failure

SP-1 350 3000 0.480 0.048 3.795 0.0183 3.608

SP-1 350 2X10* 0.579 0.044 4.194 0.0164 3.317

Nf is shown in Fig.3. In the figure, the data at one cycle represent the
stress amplitude reduced by assuming that the maximum stress is equal to
bending strength. The fatigue strength a w at 2 X 106 cycles are shown in
Table 3. In the case of the U-notched specimen(SP-5), the fatigue strength
G w was around 180MPa, which was lower than that of SP-1 specimen by a
factor of 1.8. On the basis of the result, the fatigue strength reduction
factor ß was almost equal to the stress concentration factor a and the
notch sensitivity of ceramic materials was found to be very high. Since the
fatigue strength of the SP-4(as-sintered)specimen was lower than that of
SP-1 specimen by a factor of 2.1, the stress concentration factor of the
surface defects, which could be observed in Fig.1(d), seemed to be around
2.1.
 375
It was hard to find a functional relationship between fatigue strength and a
certain grinding condition such as grade of abrasive grain, grinding volume,
etc.

Surface Shape Parameters

Measured values of the surface shape parameters are listed in Table 3. The
values in the table are the average ones for all specimens tested. Values of
the conventional roughness parameters Rmax and Ra are also listed in the
table. From Tables 2 and 3, it seems that the value of R m a x depends on the
grade of grinding wheel regardless of other grinding condition and does not
always correlate with the fatigue strength. On the other hand, the surface
shape parameters, p, S and Θ, which represent the mechanical severity of
surface profile, seem to give a good correlation with the fatigue strength.

As can be seen from Fig. 3, the scatter of fatigue lives was relatively
large. The surface shape parameters were estimated for SP-1 specimens with
different fatigue lives at the same stress amplitude of 350MPa. The results
are shown in Table 4. It was found that the fatigue lives had a good
correlation with the surface shape parameters, while they did not correlate
to the conventional roughness parameters R ma x and Ra. The similar results
were also obtained in the different specimens.

On the basis of the foregoing results, the conventional roughness parameters

(Rmax, Ra) are not always appropriate to estimate the performance of ceramic
surface. The surface shape parameters ( p, S, Θ ) proposed by Yanagi et
al., which represent the mechanical severity of valleys, are preferable to
estimate the surface finish of ceramic materials.

It was reported that the pre-existing surface cracks, which initiate during
grinding processes, controlled the fatigue strength in ceramic materials
(Mutoh et al., 1991). The present successful results of the surface shape
parameters suggest that a large surface crack will be formed at the tip of a
sharp valley.

Residual Stress

The values of residual stress measured in the longitudinal direction using

an X ray stress measurement system are shown in Fig.5. The effective
penetration depths are 50 ~~ 80 μ m for CuK a ray and 14 — 25 ju m for CrK a
ray. Residual stresses were compressive for SP-1, 2 and 3 specimens with
ground surface. Although the grinding conditions of SP-1 and SP-2 specimens

Table 5 The residual stresses for the specimens tested.

Residual stress (Mft)

Specimen CuKa(323) CrKa(212)

SP-1 -11.8 -42.7

SP-2 -13.9 -57.9
SP-3 -28.0 -97.3
SP-4 14.8 52.7
376
coincided, the residual stress of SP-2 specimen, which was ground using a
grinding wheel with coarse grain, was larger than that of SP-1 specimen. The
residual stress of SP-3 specimen, which was severely ground, was larger
than those of SP-1 and 2 specimens by a factor of 2. For the as-sintered
specimen(SP-4), the residual stress was tensile.

On the basis of the measurements using two different X rays, the products of
penetration depth and average residual stress value almost agreed in the
same specimen. (For example, 65 μ m X 11.8MPa=767 and 18 μ m X 42.7MPa=769
for the SP-1 specimen) Therefore, it seems that the distribution of residual
stress is limited in a near surface region (less than 20 μ m from the
surface), where the residual stress will be steeply reduced. On the other
hand, using the bending strength and the fracture toughness Kic and assuming
a semicircular surface crack, the depths of the pre-existing surface crack
can be estimated to be 22 μ m for SP-1 specimen, 38 μ m for SP-2 and 50 μ m
for SP-3, which are deeper than the depth of the region where the residual
stress is distributed. Therefore, the residual stress may not have signifi-
cant influence on the fatigue strength.

CONCLUSIONS

The effect of surface finish on fatigue strength of silicon nitride was

investigated. The performance of ground surface was estimated using the new
surface shape parameters, which represented the mechanical severity of
valleys, as well as the conventional roughness parameters.

It was hard to find a functional relationship between fatigue strength and a

certain grinding condition such as grade of grinding wheel, grinding volume,
etc.

The surface shape parameters proposed by Yanagi et al. gave a good

correlation with the fatigue strength. On the other hand, the conventional
roughness parameter,,,which informing the amplitude of surface roughness, did
not satisfactorily give a correlation with the fatigue strength.

Since the residual stress was distributed in a limited narrow region near
surface, the effect of residual stress on fatigue strength seemed to be not
significant.

REFERENCES

Miyamoto, A., S. Usai, H. Okamoto, H. Miyasato and K. Nakano (1989). Effect

of high efficient grinding on strength of silicon nitride. NKK Technical
report, 127, 53.
Tanaka, K., T. Kurimura, E. Matsui and Y. Akiniwa (1987). X-ray measurement
of residual stress in sintered silicon nitride. J. Soc. Mater. Sei., 36,
817.
Yanagi, K., Y, Tsukada and Y. Mutoh (1991). A geometrical assessment of ma-
chined ceramic surface for estimating fatigue strength. Pre, of 5th Int.
Conf. on Metrology and Properties of Engineering Surface« Leicester Poly
technic, UK.
Mutoh, Y., M. Takahashi, T. Oikawa and H. Okamoto (1991). Fatigue crack
growth of long and short cracks in silicon nitride. Fatigue of advanced ma-
terials , ed. Ritchie and Dauskardt, MCEP, Ltd.
WS7a10

IN-SITU SEM OBSERVATION OF CRACK PROPAGATION BEHAVIOR

IN S13N4 AND SiC AT ROOM TEMPERATURE

Masaki Kitagawa and Yuhji Ohshima

Ishikawajima-Harima Heavy Industries Co., Ltd.
Research Institute
3-1-15 Toyosu, Koto-ku Tokyo 135 JAPAN

ABSTRACT

Crack propagation behavior of S13N4 and SiC was examined by scanning electron microscopy
applicable to fatigue testing at high temperatures. Cyclic crack propagation in S13N4 was found to
be accompanied by certain types of deformation near the tip of the crack. All cases of crack
propagation under cyclic tension and cyclic tension-compression load were similar in appearance.
The enhancing effect of moisture on crack propagation under a static load was confirmed by in-situ
observation. The effect of moisture under cyclic stress was not as apparent as under static stress.
Crack propagation under low stress level could be seen both in S13N4 and SiC. Based on stress
intensity analysis of an indentation cracked specimen, the cause of low stress crack propagation
was concluded to be weak link fracture in the ceramics. Cracks propagated under decreased load
when they did so under prior increasing stress.

KEYWORDS

Silicon nitride, Silicon carbide, in-situ observation, Crack propagation, Electron microscope, Cyclic
fatigue, Static fatigue

INTRODUCTION

Fine ceramics such as S13N4 and SiC are considered future structural materials for high
temperature components. Because of the low ductility of ceramics, a thorough understanding of
fracture behavior is essential. Direct observation of the fracture process should be useful for this
purpose (Kitagawa and Ohshima, 1990). The authors developed a scanning electron microscope
(abbreviated as SEM in the following) by which examination can be conducted at high
temperatures under various types of loading. This study was conducted to clarify fracture behavior
and devise a better design method based on the in-situ observation of this behavior. The results of
observation of the crack propagation behavior of two kinds of fine ceramics, namely S13N4 and SiC
at room temperature are presented.

EXPERIMENTS

A scanning electron microscope by which a specimen can be loaded at a temperatures as high as

1200°C during observation was developed (Kitagawa and Ohshima, 1990). A fatigue testing
377
378
Electron beam

(a) Tensile test specimen

S2_
29.0 12.0 . 29.0 |

/ ,... J. . ^'« ^tyr^'ll!'_ ^,Α ^ ~ R2 rst

S j
0ΗΞ
—.-
1ST
1
1 1
n

Λ^ Heat reflector/Thermal (b) Tension-compression

Heater coil electron trap test specimen
Fig. 1 Schematic diagram of apparatus
for ih-situ observation of ceramics at high Fig. 2 Specimen dimensions
temperatures

machine had a load capability of 3960 N (200 kgf), and the specimen could be observed at a
temperature as high as 1200°C. To observe high temperature behavior, a special heating device
was attached, as shown in Fig. 1.
The materials examined in this study were sintered silicon nitride and sintered silicon cabide.
Their dimensions are shown in Fig. 2. All specimens had an identation crack at the center.

Following loading conditions were used in SEM;

1. static and cyclic tensile load, and cyclic tension-compression load
2. static and cyclic tension load with and without moisture,
3. gradually increasing load
4. decreased load.

EXPERIMENTAL RESULTS AND DISCUSSION

Cracks produced by indentation and crack propagation under cyclic and static tensile loads

To examine crack propagation under typical loading conditions, an indentation crack was
introduced at the center of the specimen, and various levels of a cyclic load were applied. Each
specimen was subsequently loaded under an increasing static load.

Cracks in SiaNd. Figure 3 shows the appearance of an indentation crack and propagating crack
under an cyclic tensile load in S13N4. Figure 4 shows the crack propagation of the same specimen
under an increasing statis tensile load following the above cyclic load.

The indentation crack appeared as a wavy dark line as sohwn in the first photo of Fig. 3. The
fractured surface [Fig. 5a] showed fractures mainly on grain boundaries. Small holes on the
fractured surface were considered those of pulled-out grains. Fig. 3 also shows cracks propagating
under cyclic tension. The crack under cyclic tension first appeared as a white straight line,
indicating that before fatigue crack propagation, there are some factors which roughens specimen
surface. On the fractured surface, the crack appeared flatter than the indentation crack and
without any granular shape. The paths of crack propagation were thus considered to be mainly
transgranular.

Also of interest was the dark (mountain shaped) image in front of the propagating cracks, as shown
in 2nd through 4th photographs of Fig. 3. This dard image was wavy, implying the image to be
located on the grain boundary. Cyclic fatigue crack propagation requires stress redistribution on
 379

Indentation crack after

cyclic load of 3kgf-65kgf
for 12240 cycles
(no cyclic crack propagation)

After 2 560 cycles under

4kgf-68kgf

After 3280 cycles

Fig. 3 Appearance of a crack

produced by indentation and
by cyclic load

stress reversal. In metallic materials, plastic deformation is the mechanism for stress
redistribution. Production of the above white image or mountain-shaped image may be indication
of possible sources of plastic deformation in ceramics.

Fig. 4 shows cracks produced under static tensile load following cyclic loading. The crack was
wavier than the cyclic fatigue crack, indicating cracks under large static tensile load to propagate
again along grain boundaries.

All cases of cyclic crack propagation under cyclic tension and cyclic tension-compression were
essentially the same in appearance, i.e., straight.

Cracks in SiC. Since SiC is much more brittle than S13N4, crack propagation under a cyclic load
was difficult to detect. In-situ observation confirmed crack to actually propagate under the cyclic
load even in SiC. Crack propagation in SiC under indentation and cyclic loads was straight in both
cases. The fractured surfaces were flatter, similar in appearance and found to be transgranular.

Effect of moisture on crack propagation under static and cyclic loads

To examine the effect of moisture on crack propagation by in-situ observation in SEM, a specimen
380

Fig. 4 Crack growth during

a holding period of one hour
under 81.4 kgf following the
cyclic load indicated in Fig. 3

40

30 j 4
P = 62kg

20
1 0 0

JfP
10
4 \
0
40
51
P = 70kg
30

20 j 0; 0
J 4
1
0
10
0
50
1, m ,Up E*P W ■

40 P = 79kg
30 |w|
20 \
10-1 Fracture

0
\ 1 1 1 1 i 1 1—
1 2 3 4 5 6 7 8 9 8 9 10

Time, h Time, h
Fig. 5 Effect of moisture on crack propagation Fig. 6 Effect of moisture on crack propagation
in S13N4 under a static load ([W] indicates crack in S13N4 under a cyclic load ([W] indicates crack
propagation per hour during the first hour propagation per hour during the first hour
following moisturizing.) following moisturizing.)

was periodically (at two hours interval) removed from SEM, dipped in water for 30 min and then
examined in SEM.

Cracks in SJANA. Figure 5 shows the extent of crack propagation per hour in Silicon Nitride
(S13N4). [W] indicates that per first one hour after moisturizing. Cracks propagated only during
the first one hour following moisturizing except in the case of the 774N (79kgf) load. Crack
propagation just after load increase from 686N (70Kgf) to 774N was subcritical growth to be
described later in this paper. Moisture may have been evaporated during the first hour in the SEM
vacuum atmosphere. The absence of crack propagation during the second hour after moisturizing
should thus be attributed to lack of moisture on the surface. Crack propagation in S13N4 was
confirmed to increase by the addition of water to the surface, as has been shown by mechanical
testing results (Evans, 1972).
 381
The results of moisture effect under a cyclic load are shown in Fig. 6. Enhanced crack propagation
was less under the cyclic than static tensile load. The reason for this may be that under the cyclic
load, cracks propagate not only by a time-dependent SCC mechanism but also a mechanical fatigue
mechanism.

Cracks in SiC. The effect of moisture on crack propagation in SiC was confirmed by observation
but was less pronounced than in S13N4.

Crack propagation under increasing load

Figure 7 shows the relationship between total crack length (2C) and a applied stress in SiC. Cracks
propagated under a load much less than the final fracture load. Similar slow growing cracking was
also noted in S13N4 and the cause of which is discussed in the following.

Near the indentation crack, the stress intensity factor (K) decreased with increase in crack length
owing to the nature of stress caused by indentation. This decrease may terminate crack growth
after a certain extent, to possibly result in slow crack growth.

The stress intensity factor of the indentation crack under a static load may be expressed as follows
(Marshall and Lawn, 1979):

K=
*-£+2m °«&
where C is half the crack length(m), P, the indentation load(N), oR, applied stress (Pa) and χ and m,
material constants. According to Tanaka's experiments (ref. Tanaka et al, 1988), x = 0.058 and
m = 1.03 for S13N4. Using these values, K for S13N4 was plotted as shown in Fig. 8. The stress
intensity factor decreased with increase in crack length when crack size was small.

Owing to the above K trend in the small crack region, small cracks may propagate only up to a
certain extent, and propagate again when the load is increased to critical K for new crack length.
The stress intensity factor calculated from actual load-crack length of one experiment is also
plotted in Fig. 8. K for crack propagation was not constant. Subcritical crack growth in Si3N4 may
thus be concluded not caused by the effect of indentation residual stress but subcritical growth to
be due to variation in material strength.
401
SiC +Δ + ή
V

w 30-

^ Δ ^

- 20^

N#D
10·

0-φ
0 200 400
Crack l e n g t h , 2C, urn

□ TP42 + TP47 O TP48 Δ TP49 X TP51 v TP52 O TP53

Fig. 7 Crack propagation in SiC under increasing load

382

60·
15 98Ν (lOkgf)

50·
\ο\Κ ^
« 40·
1
' \ ^ ^'^^-^;^.^;;^.^:^v-^-·^·-^^" 7 -^ r,P3i
Ν
1\Ο Δ *-■

30 A—£=A—i -A —A—A —A—A" —Δ]

201
—Η—-Η ! 1 1 1 Η|

10 #==a==^
0.00003 0.00005 0.00007 0.00009 0.00011
Crack length, C, mn·

D 49MPa +98MPa O 147MPa Δ196MPa χ 245MPa V 2 94MPa

Fig. 8 Stress intensity factor for the S13N4 specimen with an indentation crack under
a tensile load and example illustrating the load-crack size relationship (TP No.31)

Takahashi et al (Takahashi et al, 1985) observed the critical stress intensity for fracture of
ceramics with small cracks such as few tens of microns generally to be much less than that for large
cracks. They found stress intensity factor of a small crack to be higher than that obtained from the
equation for a large crack. However, above subcritical crack growth should slightly increase actual
crack length at failure so that K is larger than that calculated based on original crack size. This
may explain the decrease in apparent critical stress intensity for smaller cracks.

Crack propagation during unloading period

Proof-tested ceramics materials often show failure at stress below the proof test stress. This is said
to be caused by crack propagation during the unloading period of the proof-test (Ishikawa, 1988).
To confirm crack growth during this period, crack propagation under decreased stress was
examined.

(n.5/i in)
7Γί κ
;^ 73.81*
( 1 0 . I /« i n ) χ Fracture
i)0 1 <K
1:.: ! 5 8 . Μκ
(Ομ in)

I (3.5;» m ) ^ p * 43.1kg .1.500101

14 51
Γ 35.3k K 3A.3h|t / · ' (10.4/1 m)
H ;—
15.5h (0/«m) Ii
(0 μ i n )

■'3.3l<g
Oh
(4.0/x m ) Time (arbitrary s c a l e )

Fig. 9 Crack propagation under decreased load (S13N4 at room temperature)

 383

First, the load was gradually increased up to the start of crack propagation and then decreased by
19.6 MPa (2Kgf/mm2) to see whether further crack propagation would occur. In some cases, the
load was decreased even when no crack growth could be detected during the loading period for
comparison. The results are shown in Fig. 9. Cracks propagate even at decreased loads. It is of
interest that crack propagation occurred only when cracks propagated during the preceding load-
increase period. This indicates crack growth to possibly be time dependent but only at week links.
Crack propagation thus soon terminates when a barrier is encountered.

As mentioned above, crack propagation during the unloading period is one cause of premature
failure of proof tested materials below the proof stress. The crack propagation under a decreased
load may perhaps be another mechanism for premature failure in proof tested ceramics, in addition
to time-dependent SCC failure. The extent of crack growth was few tens microns. This may
increase K value by few%. This the same order of the observed decrease in the strength of the proof
tests.

SUMMARY

Crack propagation in S13N4 and SiC was examined by in-situ observation under a scanning
electron microscope. The effects of cyclic load and moisture, and crack propagation under
increasing and decreasing loads were examined by in-situ observation of cracks. The significance
of the results in relation to macroscopic behavior are discussed.

ACKNOWLEDGMENT

This work was performed under the management of Engineering Research Association for High
Performance Ceramics as a part of the Fine Ceramics R&D Project of Basic Technology for Future
Industries supported by NEDO (New Energy and Industrial Technology Development
Organization).

REFERENCES

Evans, A.G., "A method for evaluating the time dependent fatigue failure
characteristics of brittle materials and its application to polycrystalline alumina", J. Materials
Science, Vol.7,1972, pp.1137-1146.
Ichikawa, M., "Reliability Aspects of Fracture of Ceramics", Proc. of Far East
Fracture Group Workshop", ICF, Nov. 1988, pp.109-116.
Kitagawa, Masaki, and Ohshima, Yuhji, "SEM with high temperature fatigue
testing capability and its application to crack behavior of S13N4", J. Society of Materials Science
Japan, Vol.39, No.440, May 1990, p.569-574.
Marshall, D.B. and Lawn, B.R., "Residual stress effects in sharp contact cracking:
part 1 Indentation fracture mechanics", J. Materials Science, Vol.14,1979, pp.2001-2012.
Takahashi, Ichiro et al, "The effect of defect size and notch root radius on the
strength of structural ceramics", Yougyou-kyoukaishi, No.93,1985.4, p.186-194.
Tanaka, Keisuke et at, "The effect of residual stress and applied stress on the
indentation crack in ceramics", Preprint of the 37th Symposium of the Society of Materials
Science, Japan, 1988, May, pp.349-351.
 WS7a11

FATIGUE CRACK FORMATION AND GROWTH IN SLIP CAST AND SINTERED

ZIRCONIA - CERIA ALLOYS

D.CCARDONA, P.BOWEN AND CJ.BEEVERS

School of Metallurgy and Materials/ IRC in Materials for High Performance Applications
University of Birmingham, U.K.

ABSTRACT

Studies on fatigue crack formation and growth in a zirconia - ceria alloy processed using die
pressing ( and sintering) and slip casting ( followed by heat treatment) routes have been carried
out.

Fatigue cracks in pressed and sintered material were formed both in association with pores and
within transformation bands while in slip cast material fatigue cracks were almost exclusively
observed within transformation bands.

The results of this study have shown that phase transformation band formation can play a
crucial role in both the formation and growth of fatigue cracks in these materials. Detail
analyses of the development of phase transformation deformation bands in both materials have
shown that the K m a x in the load cycle to sustain crack growth increases linearly with the
square root of the transformation band width. The relationship between band width and crack
extension results in such overall toughening that subcritical fatigue crack growth can occur
without instability to high K m a x values.

KEYWORDS

Fatigue, ceramics, zirconia - ceria alloys, short crack growth.

INTRODUCTION

The addition of cubic stabilising oxides modifies extensively the properties of zirconia. The
range of materials used as stabilising oxides includes not only MgO and CaO, but also specific
rare earth oxides, such as ceria, which result in substantial improvements in the toughness of
zirconia.

Zirconia (TZP) partially stabilised with Ce02 has been reported not only to exhibit a very high
fracture toughness for ceramic materials (Cardona et al., 1991a), but has also shown
outstanding fatigue crack growth resistance (Cardona and Beevers 1989,1990; Cardona et al.,
1990, 1991b). The response of the material to cyclic loading has been mostly attributed to
385
386

stress induced phase transformation, resulting in a very powerful toughening mechanism and
which has been modelled elsewhere (Cardona and Beevers, 1990; Cardona et al., 1991a).

The studies of fatigue crack growth of Ce-PSZ (TZP) published in the literature analyse
material manufactured by the die pressing and sintering route. The material has been found to
contain large sintering defects and pores, influencing perhaps the fatigue behaviour of the
material and undoubtedly the toughness. A batch of samples was therefore produced using slip
casting followed by heat treatment, in order to produce a more consolidated material. The
objective of this paper is to present a detailed description of the behaviour of short fatigue cracks
in Ce-PSZ (TZP) manufactured by slip casting and compare with that of material manufactured
by die pressing and sintering.

EXPERIMENTAL

Zirconia (tetragonal phase) partially stabilised with 12 wt % CeC>2 testpieces were used
manufactured by both slip casting followed by heat treatment at 1400°C and 1500°C and die
pressing followed by sintering at 1400°C, 1450°C and 1500eC. The sizes of the testpieces used
were: slip cast samples -50mm x 4mm x 4mm, die pressed samples -33mm x 13mm x 3mm.
Short fatigue cracks were all self formed, except for a die pressed sample sintered at 1400°C
which prior to testing had a spark eroded notch pit introduced onto its surface. The mechanical
properties of the material manufactured from die pressing and sintering had a rupture strength
and average grain sizes of 650MPa and 3.5μηι respectively when sintered at 1400°C; 500MPa
and 2.5μπι respectively when sintered at 1450°C; and 350 MPa and 1.7 μπι respectively when
sintered at 1500°C. The grain sizes obtained when etching the material manufactured by slip
casting and after heat treatment were very similar to those listed above, although the mechanical
properties of the material were not measured in detail.

Slip cast material was tested in all but one case in four point bending, the other test (for a sample
heat treated at 1400°C) was performed in three point bending. Die pressed material was tested
in three point bending.

Tests were all performed at room temperature, in air, at a frequency of 80 Hz. Crack lengths
were monitored using the replication technique. A load ratio, R, of 0.1 (where R =
C7
min/<Jmax) w a s usec * ^ every case.

RESULTS

Transformation bands were observed to appear on the surface of the samples where stress
induced phase transformation had taken place. These transformation bands were either
observed to be associated with crack tips or alternatively traversing the width of the sample in
the region of maximum stress. The transformation band width where crack tips were located
was observed to increase as the tests progressed.

a)Slip cast material -Fatigue cracks were in all but one case observed to form and grow
within transformation bands which traversed the whole width of the sample. Transformation
band formation was usually observed to take place simultaneously with fatigue crack formation.
Only one crack was observed to form at a large pore. Transformation bands were formed
subsequently at crack tips very soon after crack formation had taken place. In general fatigue
crack formation and growth were observed to take place readily, irrespective of microstructure,
with several short fatigue cracks forming and growing within one sample, although without
interacting with each other. A typical short fatigue crack is shown in Fig.l.
Variable crack growth rates were observed throughout the tests , and in many cases ( at least
once in every test), load increases were required to promote growth as the cracks experienced
arrest. The material manufactured by the slip cast route was expected to have less internal
defects and porosity than those present due to sintering in the die pressed material. Porosity
 387

was reduced in general but internal defects, when present (due to the casting process), were of
much larger size reaching 2mm diameter and 15mm deep. These large casting defects caused
most of the samples to fail prematurely at very low loads.

b) Die pressed material - Fatigue crack formation was observed to take place: either
within existing transformation bands which traversed the whole width of the sample; or at
pores or spark eroded notch pits, with transformation bands developing after crack formation at
the crack tips. Subsequent crack growth always took place within transformation bands. A
typical short fatigue crack formed within a transformation band is shown in Fig.2. The material
sintered at 1400°C presented the highest resistance to fatigue crack formation and growth,
requiring a spark eroded notch pit to be introduced onto the surface of the sample to create a
preferential fatigue crack formation site. Only a small amount of crack growth was
subsequently obtained before fracture occurred. In all but one case, the samples were observed
to fracture due to internal defects. A fatigue crack growing in a sample of the material sintered
at 1500eC reached a length of 1200μιη when the test was interrupted and the sample was broken
open to reveal a semicircular crack shape. Variable crack growth rates and crack arrest were
observed throughout the tests. Pore associated cracks required load increases for the
continuation of growth.

Crack growth rates and stress intensity ranges were calculated for all the samples tested (both
die pressed and slip cast material), and are plotted in Fig.3. From a large number of
observations it is found that the maximum stress intensity at the surface position, K max required
to promote continued growth increases linearly with the square root of the observed
transformation band width, Fig.4 (Cardona et al., 1991a). However, this work concentrates on
growth at short crack lengths where significant variation in this relationship is observed, Fig.5.

DISCUSSION

Two distinct modes of fatigue crack formation were observed in the die pressed and sintered
material. Fatigue cracks formed either in association with pores and in the absence of general
transformation, or within transformation bands after the formation of these bands. In general
fatigue crack formation within phase transformation bands occurred at a higher applied level of
stress than the formation of cracks in association with pores. On the other hand, in slip cast
material fatigue cracks formed almost exclusively in association with phase transformation
bands.

Fatigue crack growth took place at similar values of ΔΚ in both materials (1 to 7 MPaVm). The
irregularity in the crack growth rates was also common for slip cast and die pressed materials.
It is important to note that all the samples, but one die pressed and sintered at 1500°C, broke
due to internal defects. In the absence of such dominant internal defects, it was observed how
a "short crack" could grow from a length of about 300μπι (formed in the absence of
transformation bands, i.e., pore associated crack) to a length of about 1200μιη, after which the
test was interrupted. The transformation band formed associated with the crack tip was
observed to increase in width around the crack tip as the test progressed. This sample provides
experimental evidence of the fact that a "short crack" can grow up to the "long crack" regime (
in the absence of internal defects) as a result of stress induced phase transformation toughening
mechanism.

A model based on that proposed by McMeeking and Evans (1882) has been used previously to
analyse growth under cyclic loading (Cardona et al., 1991a, 1991b). In this paper the growth
of short cracks is considered in detail. The model predictions are also plotted in Fig.5. These
predictions are based on :

Kmax = ΔΚ € + Ki (1)
388

where the intrinsic toughness, K{, (in the absence of transformation bands) has been estimated
as 1.9 MPaVm (Cardona et al., 1991a), and the values of K m a x under cyclic loading, that are
expected to promote growth can be predicted by solving equation (2) (McMeeking and Evans,
1982):
T
V2h
AK c =0.22Ee ; -f (2)
11
ί2(1-υ)
where h is half the transformation band width, £ Ü T « 5% , f » 50%, E = 200GPa and υ = 0.21
( for this material). Note that 2h = H, which is the total width of the transformation zone.
Under steady state conditions, growth should not occur except for points defined by the
predictions of equation (2), Fig.5. Above the line, growth should be unstable and catastrophic
failure should result. Note that in Fig.5, the values of K m a x observed experimentally were
sufficient to promote crack growth, occurring at much lower values than predicted in most
cases. However, it is crucial to appreciate that the model predictions are based on steady state
toughening applicable only when the crack increment Aa, is large compared to half the
transformation zone width, h ( typically Aa /h>6 (McMeeking and Evans, 1982)). In the
present study, the total crack length a + Aa, is considered if growth occurs entirely within a
transformation band. For pore associated crack growth, Aa increments within the transformed
zone are considered only.

It is of interest to note from Fig.5 that crack growth within transformed zones can occur at
much reduced K m a x values than predicted. However although the cracks are growing they are
not near instability. This can be shown by plotting the locus of points during crack growth, as
indicated in Fig.5. Data is given in Table 1, where it can be rationalised solely in terms of the
crack growth resistance curve. It must be noted that the incremental crack growth fatigue
process allows the full toughening potential of the system to be realised, since toughening will
only occur as the crack penetrates the transformed zone (McMeeking and Evans, 1982). In deed
stable fatigue crack growth (long crack) has been obtained at K m a x values in excess of 22
MPaVm (Cardona et al., 1991a, 1991b).

Table 1. Crack growth data and related transformation band width

for a typical short crack sample

^max Crack Length Total Transformation (Aa +a)/h

2a Band Width, H,(H=2h) or Aa/h
MPaVm μιη μιη
5.84 317 40 7.92
3.93 139 38.4 4.0
3.02 82 31.3 2.61
1.88 80.8 23.3 3.47
1.7 66.2 17.4 3.8

CONCLUSIONS
1) Formation of fatigue cracks in the pressed and sintered material occurs in association with
either pores or preformed transformation bands, while fatigue cracks in slip cast material were
formed in association with pre-existing transformation bands.
 389

2) Fatigue cracks had transformation bands associated with them. The width of the
transformation bands was always observed to increase with increasing crack length.

3) An analysis of the variation of phase transformation band width with K m a x values at

growing cracks showed that the mode of crack growth in this material and in particular the
relationship between crack extension and band width, was such as to maintain extensive
subcritical crack growth without instability.

ACKNOWLEDGEMENTS

One of the authors (DCC) was supported in the course of this work by an SERC Quota award.
Thanks are due to T & N Technology LTD. for the provision of material.

REFERENCES

Cardona D.C. and Beevers CJ. (1989). Formation and growth of short fatigue cracks in a
Zirconia-Ceria alloy. Scripta Metall., Vol.23. No.6, 945.

Cardona D.C. and Beevers CJ. (1990). Fatigue behaviour of Zirconia - Ceria alloys. Fatigue
90, Honolulu, Hawaii,Conference Proceedings, Vol.2 J 023.

Cardona D.C, Bowen P. and Beevers CJ. (1990). Effects of non-uniform stress fields on
Fatigue crack growth in Zirconia-Ceria alloys, ECF 8, Torino, Vol.L 531.

Cardona D.C, Bowen P. and Beevers CJ. (1991). Mechanics of through thickness fatigue
crack growth in Ce-PSZ(TZP). Proceedings of the Mechanical Fatigue of Advanced
Materials. Sta. Barbara. To be published.
Cardona D.C, Bowen P. and Beevers CJ. (1991). The mechanical behaviour of short and
long fatigue cracks in Ceria - Zirconia (TZP). J. Mat. Sei. To be published.

McMeeking R.M. and Evans A.G.(1982). Mechanics of transformation-toughening in brittle

materials. J. Am. Ceram. Soc. 65Γ51. 242.

17 μπι 32 μπι

Fig.l Short fatigue crack Fig.2 Short fatigue crack

slip cast material die pressed material
(transformation band width (transformation band width
enclosed by arrows). enclosed by arrows).
390

Crack Growth Rate , da/dN vs Stress

Intensity Range, ΔΚ

lilllfit
MaximumStress Intensity ar the Crack tip o Short Crack 1300.»-1
,K m«x vs Square Root of the Transformation
Short Crack I500.J-2
Band Width, V2h
M 30-

0 * Short Crack 1450.*-2

■ Short Crack 1400.*-1
a Looi Crack 1 S 0 0 J 1»
* Loci Crack 13004-2

»=2.1500
* Long Crack 1430^-1
■ Loot Crack 14304-2
*=1.1400 K + Loot Crack 1 4 0 0 A- I
s=2,1400 K X * 0l - ■ Long Crack 1400,*-4f
■J&E»BQ
1=1,15001 i c
|£ X Loo« Crack 1400j-4b
Loai Crack 1450j-4f
»=1.15002 i c •5 SLDC M
1=1.15003 i c 2 ■ Loot Crack 1450j-lb
Short CrackWOOS.C.
0 10 20 30 O Short Crack 1400 2 S.C
Stress Intensity Range, ΔΚ ( MPa Vm) Squre Root of the Tnuufonnalioa B ud
Width. V2h ( -νμπι)
Short Crackl4O0 I S.C.
. Predicted V»lue,

Fig. 3 da/dN versus ΔΚ. Fig.4 Maximum stress intensity at the

surface crack tip versus square
root of the transformation band
width (after Cardona et al., 1991a.).

Maximum Stress Intensity K max vs Square

Root of Transformation Band Width ^2h
Short Crack Samples of Ceria - PSZ
u-
9- Short Crack 1500,s=l
8- v ^ o oo Short Crack 1500,s=2
Short Crack 1450,s=l
7- v/«£ o
s*.·· ·Τ
Short Crack 1450,s=2
6-
Short Crack 1400,s=l
5-
y I cP Slip Cast 1500,s=l
4- / ♦ #*** *° Slip Cast 1400,s=2
3-
2-
Xr°g%'~
B m
n ~ -I"·-*
Slip Cast 1400,s=l
• Predicted Values

1-
£ U o- 1
1 ' 1 ' 1
— i — i — i — r — i — | — i — | — i — | — « — | — i —
r

1 2 3 4 5 6 7 8 9 10
Suqare Root of Transformation Band Width
V2h,(Vnm)

Fig.5 Maximum stress intensity at the surface crack tip versus square
root of the transformation band width (doted line indicates a typical
growth locus of a crack).
 WS7a12

CYCLIC FATIGUE PROPERTIES OF SINTERED MULLITE CERAMICS

T.NISHIKAWA, K.OHYA*, H.KATAGIRI, M.TAKEDA and M.TAKATSU

Department of materials S c i e n c e and E n g i n e e r i n g ,

Nagoya I n s t i t u t e of Technology,Gokiso-cho,Showa-ku,Nagoya,Japan
*NGK Spark Plug Co.,Ltd.,Takatuji-cho,Mizuho-ku,Nagoya,Japan

ABSTRACT

Static and cyclic f a t i g u e t e s t s w e r e c o n d u c t e d on four t y p e s of s i n t e r e d mullite

ceramics, and r e s u l t s w e r e compared and s t u d i e d . S i n t e r e d mullite ceramics differ
from s i n t e r e d alumina in t h a t t h e y are h i g h quality materials t h a t do not exhibit
R - c u r v e e f f e c t and acceleration e f f e c t w h e n s t r e s s ratios are c h a n g e d . A s l i g h t
acceleration e f f e c t has b e e n o b s e r v e d in 25 vol% Z r 0 2 d i s p e r s e d mullite-zirconia
ceramics w h e n t h e s t r e s s ratio i s 0.1, h o w e v e r . Use condition and g u a r a n t e e d
f a t i g u e time were s t u d i e d .

KEY WORDS

Cyclic fatigue; mullite ceramics; m i c r o s t r u c t u r e ; acceleration effect; SPT diagrams

INTRODUCTION

S i n t e r e d mullite ceramics have drawn a t t e n t i o n a s h i g h temperature s t r u c t u r a l

materials due to t h e i r small thermal e x p a n s i o n c o e f f i c i e n t s , e x c e l l e n t h i g h
temperature s t r e n g t h and c r e e p r e s i s t a n c e p r o p e r t i e s . There has b e e n p r o g r e s s
r e c e n t l y in mass p r o d u c i n g h i g h p u r i t y mullite g r a n u l e s u s i n g t h e s p r a y
p y r o l y s i s method (S. Kanzaki et al., 1985) and s o l - g e l method (M.G.M.U. Ismail et
al, 1987). S t u d y c o n t i n u e s on controlling t h e grain s i z e , addition of s i n t e r i n g
b o o s t e r s and o t h e r composites to f u r t h e r application of s i n t e r e d materials.

In t h e p r e s e n t s t u d y , mullite with different m i c r o s t r u c t u r e s w e r e s u b j e c t e d t o

cyclic f a t i g u e t e s t s u n d e r variable s t r e s s ratio c o n d i t i o n s , u s i n g readily s i n t e r e d
mullite with MgO a d d e d a s a s i n t e r i n g b o o s t e r and zirconia-mullite s i n t e r e d
composite. The s i n t e r e d mullite with different m i c r o s t r u c t u r e s differed from
s i n t e r e d alumina in t h a t p r o n o u n c e d acceleration e f f e c t s w e r e not o b s e r v e d w h e n
t h e s t r e s s ratio c h a n g e d . On t h e o t h e r hand, t h e zirconia-mullite composite did
exhibit an acceleration e f f e c t at a s t r e s s ratio of 0.1.

EXPERIMENTAL

High p u r i t y mullite g r a n u l e s ( p u r i t y o v e r 99.9%) were p r o d u c e d b y s p r a y

p y r o l y s i s (specimen A) and s o l - g e l (specimen B) methods. A s i n t e r i n g b o o s t e r ,
MgO, was a d d e d t o specimen B to p r o d u c e readily s i n t e r e d mullite g r a n u l e s (C)
391
392
which were subjected to CIP forming, then sintered for 3 hr at 1650°C and formed
into a plate- shaped test sample. A mullite composite (M.G.M.U. Ismail et al., 1988)
containing 25 wt% commercially available Zr02 (specimen D) was added, and the 3X
4X45 mm specimen was lapped to mirror finish with ground corners.

Specimen hardness was measured with a Vickers tester, and modulus of elasticity
was measured by an ultrasonic pulse method. Mean bending strength was
measured by a three-point bending test to determine the Weibull parameter. The
critical stress intensity factor (KIC) was determined by the IF method, and bulk
density was determined by the Archimedes method. The sintered sample was
subjected to thermal etching and the microstructure was examined by scanning
electron microscopy (SEM). A piezoelectric bimorph acturator was used at stress
ratios (R=<r m l n / σ mex) of 1.0 0.7 and 0.1 with a frequency of 500 Hz one-sided
oscillation for a maximum of 10 e seconds.

Experimental results were normalized using the following equation (Takatsu et al.,
1988) which was derived from the empirical equation V = A(K,/Ki C ) n on the
subcritical crack growth.

log(^ m a x/Sr) =-log(t-r-g- , )/(n+l)+B (1)

where σ m a x is the maximum load stress, Sr is estimated bending strength, tt is

time-to-failure, and g _ 1 is a function of load-stress waveform. Fatigue properties
were expressed with another fatigue parameter A as the ratio of static fatigue
test value Ae and cyclic fatigue test value AQ (ΔΑ=Α 0 /Α β ). (Takatsu., 1990a):

logΔA = log{tτ}β-log{tr·g- 1 }o+log[(n ( a -2)/(no-2)]+(n 8 -no)log(σ m β χ/B) (2)

where n e and nQ are static fatigue and cyclic fatigue values n, and the calculation
approximate S=ST.
RESULTS

Table 1 shows the property value of each sintered mullite specimen. Bending
strength and other values did not depend on microstructure for these testpieces.
The Κισ value of mullite-zirconia composite (D) was large at 4.3. Photo 1 shows the
microstructure of each sintered specimen. In testpiece A the diameter of spherical
particles ranged from 0.1-0.5 /im, and elongated shapes of coarse mullite ranged
up to 5 jum. In testpieces B and C diameters were relatively uniform at about 1.5
/urn, while in testpieces D white Zr02 particles the same size as mullite particles
were dispersed throughout the testpiece.

Table 1. Relative density and mechanical properties of mullite ceramics

Specimen P R E Hv K IC Sf m Dp
(%) (GPa) (GPa) (MNnr 1 · 5 ) (MPa) (-) (M m)

A 97.3 217 11 2.5 284 9.3 0.81

B 98.3 219 11 2.5 245 8.1 1.67
C 98.3 217 11 2.6 302 9.3 1.66
D 99.5 219 10 4.3 316 11.2 1.33

p R : R e l a t i v e d e n s i t y , E r E l a s t i c modulus, H v : V i c k e r s
h a r d n e s s , K i c r F r a c t u r e t o u g h n e s s , S f : 3 - p o i n t bending
s t r e n g t h , m :Weibull modulus, Dp:Average p a r t i c l e s i z e
 393

Photo 1. SEM micrographs of mullite ceramics

Fatigue test results normalized by Eq. 1 are shown in Fig. 1. Static fatigue test
results are indicated by the solid line in the drawing, while the dashed line
indicates the range of standard deviation. Neither testpieces B nor C exhibited a
change in acceleration effect toward the short failure time side due to cyclic
fatigue . Fatigue parameter n of testpiece B was smaller than that of the other
testpieces, and the measurement point shifted toward the shorter failure time
side in the low load range compared to that of the high load range. This shift
indicates that testpiece B was susceptible to fatigue under low stress in these
tests.Cyclic fatigue test data for testpiece A at a stress ratio of R=0.7 clearly show
a shift to the long fatigue time side. Conversely, fatigue data for testpiece D at
stress ratios of R=0.1 and 0.7 show a shift to the short failure time side, and an
acceleration effect was noted. Using yttria partially stabilized zirconia in the
cyclic fatigue tests similarly produced a shift toward the short failure time side
(Takatsu et ah, unpublished data).

u 1
^; R n
o 1.0 2 0
- Δ 0.7 18
1.0
D 0.1 18
1 -

0.8 r B

I 1 1 1 I 1
0.6 \ R n

I 1.0 o 1.0 27
Δ 0.7 31
D 0.1 34
0.8 ctio ^ 1 J
D
r
0.6 1 L_ 1 » I
10° 102 104 10° Ί02 104
tf-g"*1 (sec)
Fig. 1. Analysis of cyclic fatigue properties on mullite ceramics by estimated
method on empirical equation on subcritical crack growth
Figure 2 shows the changes in ΔΑ indicated by stress ratio R for each specimen.
In the drawing, if logAA is positive the crack propagation rate acceleration in the
cyclic fatigue test. Just as in Fig. 1, shifts toward long failure time can be
quantitavely confirmed for testpiece A at a stress ratio of R=0.7, and a shift
toward the short failure time side is verified for testpiece E at R=0.7 and 0.1.
Examination of the fracture surface by SEM after cyclic fatigue testing disclosed
intra-granular fractures only in the mullite crystalline formations. In testpiece D,
inter-granular fractures were observed in the dispersed Zr0 2 portion.
394

-21—>-
0 0.5 1-0
R C-J
Fig. 2. Relations between applied stress ratio (R) and fatigue parameter (logAA)

DISCUSSION
Effects of Mullite Microstructure on Cyclic Fatigue Properties. Mullite granules of
testpieces B, C and D had mean diameters of 1-2 >um, which did not vary after
sintering. On the other hand, testpiece A had a mean starting granule diameter of
about 0.5 //m, and abnormal elongation of two to three times in side was observed
after sintering. The microstructure showed a slight shift of the starting mullite
granular structure to the silica side in stoic hiome trie composition (Kumazawa et
al.y 1988). Only sintered mullite with this microstructure showed an unmistakable
shift toward the long failure time side at R=0.7. This crack propagation retarding
mechanism remains as yet inadequately explained and requires further study.
Testpieces B and C had a narrow grain diameter distribution, and fatigue
parameters n and ΔΑ were virtually unchanged by stress ratio R. Fatigue time
was affected only by maximum stress in both static fatigue and cyclic fatigue .
Comparison of the two testpieces having similar microstructures,testpiece C,
having a small quantity of MgO added, had a larger n value. The addition of MgO
is thought to produce a solid solution or matrix phase of the mullite. Bending
strength was somewhat large, but a cumulative effect was not observed in the
cyclic fatigue. Cyclic fatigue data for alumina (Kamiya et ah, 1990) are shown in
Figs. 2 and 3 for purposes of comparison with mullite cyclic fatigue data. There
are differences in alumina and sintered mullite cyclic fatigue data. Some
acceleration effect was observed in 99% pure alumina, a pronounced acceleration
effect was noted in 92% pure alumina. In contrast, acceleration effect was either
nonexistent or only very slight in mullite. This factor is an important condition
for the development of materials resistant to cyclic fatigue.

Effect of ZrOg on Cyclic Fatigue Properties. Mullite composite with added Zr0 2
have improved strength and toughness, in cyclic fatigue tests, n increased

i1·0 α^&Η^,
0.8
GO

bE0.6 99%ΛΙ2θ3

10° 102 104 10° 10z 104

ti-g -1 (sec)
Pig. 3. Analysis of cyclic fatigue properties on alumina ceramics
 395

CXa (MPa)
Fig. 4. SPT d i a g r a m for mullite c e r a m i c s . T h e r mm a n d To a r e s h o w n for v a r i o u s
P a a n d (T P / o " a

somewhat, and the material was stable judging only by this fatigue parameter.
However, another fatigue parameter, ΔΑ, showed a shift toward the short failure
time side. Similar acceleration effect and i n t e r - g r a n u l a r fracture were observed
in Zr0 2 testpiece. Current ideas on the mechanism which reduces failure time and
acceleration of crack propagation under cyclic s t r e s s are expressed in the
following reports. 1) Residual s t r e s s is generated through differences in moduli
of elasticity between different granules or in the matrix phase, producing minute
surface cracks and reducing s t r e n g t h (Masuda et ai., 1989); 2) cracks open and
close due to mismatching of cracks and debris in the cracks, and a strong
drawing force is produced at the crack tip during s t r e s s relaxation as well as in
the compressive s t r e s s state (Tanaka et ai.,1989; Takatsu et al., 1990b).
Zr0 2 -mullite composites have a modulus of elasticity that is virtually identical to
that of zirconia and mullite, but since their thermal expansion coefficient is
nearly double residual s t r e s s is minimal. On the other hand, SEM disclosed
intra-granular fractures in mullite which had relatively low surface roughness on
the fracture surface, but the portion with dispersed Zr0 2 had inter-granular
fractures with surface roughness at least equal to the Zr0 2 grain size of 2 /zm.
Since an acceleration effect was observed when the oscillation width was large at
R=0.1, the fatigue mechanism of this composite is thought to be near the latter.
However, an indent effect at the convex regions stimulates acceleration of crack
propagation. The Zr0 2 content of this composite was 25% and the number of
indentations was at most 1/4 that of zirconia, but the reduction in failure time was
nearly the same. F u r t h e r study of these aspects is required

SPT Diagrams. The SPT diagrams shown in Fig. 4 was prepared using the
property values, and fatigue-test derived parameters n and A shown in Table 1 as
well and the equation of A.G.Evans et al. (A.G. Evans et ai., 1974) in order to
predict the guaranteed fatigue time of the various types of sintered mullite. The
minimum fracture time ( τ mm) was determined at proof s t r e s s σ Ρ during testing
using actual s t r e s s σ a from the fractures in the diagram. The dashed line in the
drawing forecasts failure probability P r for fracturing at time To under constant
s t r e s s without proof testing. In comparing the static fatigue results for each
testpiece, no disparities were found with the exception of testpiece B, which had
relatively low bending s t r e n g t h compared to the other testpieces and under
s t r e s s displaced r o toward the short failure time side. In cyclic fatigue tests,
396
comparing the SPT diagrams for testpiece A, which shifted to the long failure time
at a stress load of 0.7, and testpiece D, which shifted to the short failure time side
at a s t r e s s load of 0.1, with those of other testpieces showed testpiece A fracture
probability was reduced to more than one decimal plane. On the other hand, no
disparity was found for testpiece D and static fatigue data. Although the fatigue
parameter As increased, the n parameter also increased and negated each other in
the SPT diagram. Therefore, it is thought that using testpiece D as a structural
material under cyclic conditions will not present any particular problem from the
standpoint of failure time.

CONCLUSION

Four types of sintered mullite and composites were subjected to cyclic fatigue
tests with variable s t r e s s ratios at 500 Hz one-sided oscillation. The results are
listed below.
1) Sintered mullite did not exhibit an acceleration effect due from cyclic fatigue in
comparison with sintered alumina.
2) Sintered mullite with a mixed matrix of elongated coarse grain in the
microstructure exhibited a shift toward the long failure time side at a s t r e s s ratio
of 0.7 in comparison with static fatigue data.
3) Zirconia-mullite composite showed high fracture toughness and strength, but
the acceleration effect from cyclic fatigue was observed.
4) SPT diagrams were prepared for each type of sintered mullite based on fatigue
test results, and proof stresses and guaranteed failure times were calculated for
structural materials under cyclic stress.

REFERENCES

Evans,A.G. and Wiederhorn,S.M.(1974). Proof testing of ceramic material-

an analytical basis for failure prediction. Inter. J. Fracture Aty·, 379-392.
Ismail,M.G.M.U.,Nakai,Z. and Somiya,S.( 1987).Microstructure and mechanical
properties of mullite prepared by the sol-gel method. J.Am.Ceram. Soc. J0^ C7-C8.
Ismail,M.G.M.U. and Nakai,Z.(1988). Properties of zirconia-toughened mullite
synthesized by the sol-gel method. Adv. Ceram., 24, 119-125.
Kamiya,H.,Takatsu,M.,Ohya,K.Ando,M.and Hattori,A.(1990). Effect of microstructure
on cyclic fatigue properties of Al 2 0 3 ceramics and A1 2 0 3 composites. J.Ceram.Soc.
Japan, 98, 456-463.
Kanzaki,S.,Tabata, H.,Kumazawa,T. and Ohta,S.(1985). Sintering and mechanical
properties of stoichiometric mullite. J.Am. Ceram.Soc., 68, C 6- C 7.
Kumazawa,T.,Kanzaki,S.,Ohta,S. and Tabata,H.(1988). Influence of chemical
composition on the mechanical properties of Si0 2 -Al 2 0 3 ceramics.
J. Ceram.Soc. Japan,96, 85-91.
Masuda,M.,Soma,T.,Matsui,M. and Oda,I.(1988). Fatigue behavior of sintered Si3N*
under tension-compression cyclic stress.ibid.,96,277-283.
Okada,K.,Otsuka N.,Brook,R.J. and Moulson,A.J.(1989). Microstructure and
fracture toughness of yttria-doped tetragonal zirconia polycrystal/mullite
composites prepared by an in situ method. J.Am.ceram.Soc.,72,2369-2372.
Takatsu,M.,Kamiya,H.,Ohya,K.,Ogura,K. and Kinosita,T.(1988). Effect on vibrated
cyclic fatigue properties of ceramics from s t r e s s load condition. J.Ceram.Soc.
Japan,96,990-996.
Takatsu,M.,Takahashi,J.,Nishikawa,T.,Ohya,K. and Hattori,A.( 1990a) Cyclic fatigue
properties of piezoelectric ceramics, ibid.,98,1343-1348.
Takatsu,M.,Ohya,K. and Ando,M.( 1990b). The relationship between cyclic fatigue
properties and microstructures of sintered silicon nitride ceramics.
ibid. ,98,490-498.
Tanaka,T.,Okabe,N. and Ishimaru,Y.(1989). Fatigue crack growth and crack
closure of silicon nitride under wedge effect by fine fragments. J.Soc.Material
Sci.Japan,38,137-143.
 WS7al3

FATIGUE BEHAVIOUR OF NICALON / CAS COMPOSITE MATERIAL AT ROOM

AND ELEVATED TEMPERATURES

D.CCARDONA, P.BOWEN AND CJ.BEEVERS

School of Metallurgy and Materials/ IRC in Materials for High Performance Applications
University of Birmingham, U.K.

ABSTRACT

The fatigue behaviour of calcium aluminosilicate (CAS) matrix reinforced with Nicalon silicon
carbide continuous fibres, was studied at temperatures of up to 800°C. At room temperature,
no single dominant crack was observed and fatigue crack growth was characterised by a high
proportion of matrix-fibre interface debonding and crack tip bridging by fibres. At high
temperatures of 600° C and above a single dominant crack was observed, together with a
markedly reduced amount of matrix-fibre interface debonding and crack tip bridging. This is
consistent with changes in the interfacial bonding at high temperatures in air, and results in a
much reduced overall load bearing capacity of the composite.

KEYWORDS

Nicalon / CAS, fatigue, crack growth, elevated temperatures.

INTRODUCTION

The breaking strength of glass and ceramic materials is highly sensitive to the presence of
cracks. Toughness in brittle composites is derived principally from fibre-matrix interactions.
In particular, interface debonding and fibre pull-out can both deflect the crack and dissipate
energy, with the result that non-localised damage can be produced over a large volume of
material and significant toughness can be obtained (Cardona,1991).

Glass ceramics and ceramic matrix composites have great potential for use in high temperature
aerospace components due to their high specific strength and stiffness. It is crucial, therefore,
to assess such materials at envisaged operating temperatures. This paper concerns the
mechanical behaviour of a glass ceramic matrix (CAS) containing continuous SiC (Nicalon)
fibres under cyclic loading at room and elevated temperatures.

EXPERIMENTAL
Fatigue crack formation (short cracks) was studied using plane testpieces of length, depth and
thickness of 50mm x 5mm x 10mm respectively tested in four point bending. Tests were

397
398

carried out at room temperature, at a frequency of 60 Hz. The replication technique was used to
monitor the development of fatigue damage.
Fatigue crack growth tests were carried out using similar SEN testpieces, of dimensions length,
depth and thickness of 50mm x 10mm x 5mm respectively prenotched to a depth of 1.5mm, in
three point bending, with an overall span to depth ratio of 3.4. Tests were performed at room
temperature , 600, 700 and 800° C using a load ratio, R, of 0.1, at a frequency of 60 Hz.
Cracks were monitored at elevated temperature using an in-situ optical system fitted with a
photographic camera.

RESULTS

In plane testpieces, the initial stage of damage formation was characterised by extensive matrix
microcracking. Subsequently cracking of some of the fibre - matrix interfaces took place. These
were followed by the joining of matrix cracks with cracks along the fibre - matrix interfaces and
eventually resulted in final damage across the thickness of the sample. A typical example of
damage evolution is shown in Fig.l. No single dominant crack was observed.

Fig. 1. Self initiated damage evolution.

 399
At room temperature fatigue crack growth was always characterised by matrix cracks bridged by
fibres and/or crack deflection along the fibre - matrix interfaces. In general crack growth was
not sustained by the application of a constant cyclic load and continued load increases were
required. This particular feature is illustrated in Fig.2, with arrows showing where load
increases were applied. Note that load increases did not always result in increased crack growth
rates. Fatigue crack fracture surface was characterised by having a very high proportion of fibre
pull out ( and crack bridging), as shown in Fig.3.

Crack Growth Rate vs Total Crack Length

^ GMC - Room Temperature
7i 10-

a 20#C

ftf

t
Change in
40.8 MPa applied stress
s
a
10"
2000 3000 4000 5000 6000
u
Crack Length, a (μπι)

Fig.2. da/dNvsa at room temperature.

At temperatures of 600°C and above, it was observed that fatigue damage was much more
localised and resulted in a single dominant crack, growing mostly through both matrix and
fibres, although a small proportion of matrix-fibre interface debonding and crack bridging was
still observed. A typical example of the mode of crack growth at elevated temperatures is
shown in Fig.4. At 600,700 and 800°C it was observed that load increases were still required
to obtained continued crack growth, but most importantly the load bearing capacity of the
composite was observed to be reduced greaüy. A maximum load of 1.2 kN could be supported
at room temperature but at 800eC this was reduced to 0.6 kN. This may also be represented as
shown in Fig.5, where crack growth rate is plotted versus nominal applied stress intensity range
for tests at room temperature and 800°C. It is clear that in general elevated temperature
enhances crack growth rates. A K max of approximately 32 MPaVm sustained by the composite
at room temperature, at higher temperatures the maximum stress intensity that could be
sustained under cyclic loading was never greater than 16 MPaVm. Fatigue fracture surfaces at
elevated temperatures are characterised by having a very small proportion of fibre pull out as
shown in Fig.6.
400

Fig. 3. Fatigue crack fracture surface

room temperature.

0.5 mm

Fig.4. Mode of fatigue crack growth

at elevated temperature.
 401

GMC - ΔΚ vs da/dN
20°C and 800eC
10"

10 -5

10 - 6 Room Temperature
800'C
10- 7

10 _ 8 i

10" -n—
1 10 100
ΔΚ (MPaVm)

Fig.5. da/dN vs ΔΚ at room

temperature and 800*G

Fig. 6. Fatigue crack fracture surface

at elevated temperature.

DISCUSSION

The fatigue crack growth process was characterised at room temperature by multiple cracking of
the matrix and crack growth occurred by matrix-fibre interface debonding and matrix cracks
were bridged. The progressive reduction in crack growth rates observed throughout the tests
(often seen even after abrupt stress increases, see Fig.2) exhibited by Nicalon / CAS and also
402
seen in Ti fibre reinforced MMCs (Cotterill et al., 1990) is indicative that crack growth does
not dependent solely on static applied stresses but also displays features consistent with the
influence of alternating stresses. Such generic damage accumulation under cyclic loading is also
supported strongly by the short crack studies, Fig.l.

With temperature increase it was observed that damage was more localised with the
development of a single dominant crack, often growing in the direction of Mode I opening. A
reduction in the mechanism of crack growth by fibre bridging and in the extent of fibre pull out
were also exhibited by samples tested at high temperatures compared to those at room
temperature. This can be attributed to strengthening of the interfacial bonding between fibres
and matrix at high temperatures in air, as reported in the literature for similar systems (Cooper et
al., 1987) and subsequent embrittlement of the composite system.

Due to the mode of crack growth, some caution should be used in the application of fracture
mechanics parameters at room temperature. At higher temperatures however fracture
mechanics parameters can be used more accurately. Reduced values of K m a x observed prior
to crack instability at higher temperatures (Fig.5) may be taken to illustrate the important fact
that non-localised crack damage may be less potent in reducing the lifetime of a component than
damage localised to a dominant crack. If this can be shown in general, then it may provide an
opportunity for fracture mechanics to play a role in defining lower bound crack growth
resistance in such reinforced systems.

CONCLUSIONS

The key feature in the behaviour of Nicalon / CAS composite material under cyclic loading at
room and elevated temperatures is the behaviour of the fibre - matrix interface. In plane
surfaces, cyclic loading results in multiple damage rather than the formation of a single
dominant short crack. The process of damage evolution starts with matrix cracking, followed
by matrix-fibre interface debonding, and finally matrix cracks join to cracks growing along the
fibre - matrix interfaces.

At room temperature multiple long fatigue cracks were formed and grew by decohesion of fibre
- matrix interfaces and matrix cracks were bridged by fibres. At elevated temperatures a single
dominant crack growing mostly in the Mode I direction always characterised crack growth.
The load bearing capacity of the material was reduced greatly with temperature, consistent with
much reduced fibre-matrix interface debonding and reduced crack tip bridging by fibres.

ACKNOWLEDGEMENTS

One of the authors (DCC) was supported in the course of this work by an SERC Quota award.
Thanks are due to Rolls Royce pic. for the provision of material.

REFERENCES

Cardona D.C. (1991). Fatigue of Brittle Materials, Ph.D. Thesis, University of Birmingham.
Cooper R.F. and Chyung K. (1987). Structure and Chemistry of Fibre-Matrix Interfaces in
SiC Reinforced Glass-Ceramic composites : An Electron Microscopy Study.
J. Mat. Sei., 22, 3148.
Cotterill PJ. and Bowen P. (1990). Fatigue crack Propagation in a SiC Fibre Reinforced Ti
Based Metal Matrix Composite. Proceedings of the Fourth International
Conference on Fatigue and Fatigue Thresholds, Fatigue 90, Eds. Kitagawa and
Tanaka, July 1990, Vol.4. 2551-2556.
WS7b1

TENSILE AND FATIGUE FRACTURE BEHAVIOR AND WATER-

ENVIRONMENT EFFECTS IN SiC WHISKER/7075 COMPOSITE

K. Komai*, K. Minoshima* and H. Ryoson**

* Department of Mechanical Engineering, Kyoto University,

Yoshidahonmachi, Sakyoku, Kyoto 606, Japan
** SONY Co. Ltd., 6-7-35 Kitashinagawa, Shinagawa,
Tokyo 141, Japan

ABSTRACT

The mechanical strength except elongation and the fatigue strength in

laboratory air of SiC whisker/7075 composite were superior to an unrein-
forced 7075-T6 alloy. At lower stress level, water environment decreased
the fatigue strength of the composite. AE signal analysis and fracture
surface observation by SEM were conducted, thereby discussing fracture
mechanisms and environmental influence of water.

KEYWORDS

SiCw/7075; tensile strength; fatigue strength; water environment; AE

analysis; fractography

INTRODUCTION

Metal matrix composites (MMCs), have some advantages compared with polymer
matrix composites (PMCs). Many investigations on whisker reinforced metals
have been recently investigated, including strengthening mechanisms
(Aresenault, 1988a), fatigue behavior (Christman and Suresh, 1988b) and
also corrosion behavior in seawater (Aylor and Kain, 1985a). However, en-
vironmental influences on strength have scarcely reported (Yau and Mayer,
1986c).

In this investigation, we have conducted tensile and fatigue tests of a SiC

whisker reinforced high-strength 7075 Al alloy in laboratory air and in
water environments: the fracture mechanisms and environmental influence of
water are discussed.

EXPERIMENTAL PROCEDURES

The materials tested was a silicon carbide whisker reinforced high strength
7075 aluminum alloy (SiCw/7075). The composite materials was fabricated
with a powder metallurgy processing technique, and was heat treated to a T6
condition. The nominal volume fraction of the whisker was 20%.

403
404
M12

<w in

6
34
84

Fig. 1 Shape and dimensions of round smooth tension

specimens. All dimensions are in mm. Arrow
shows the extruding direction.,

Table 1 Mechanical properties of SiCw/7075 in laboratory air.

Elastic Modulus 0.2% Offset Yield Tensile Strength Elongation

GPa Strength MPa MPa %
122 740 844 1.6

Round smooth tension specimens shown in Fig. 1 were machined in the lon-
gitudinal direction, i.e., extruding direction. The mechanical properties
of the material are shown in Table 1.

Fatigue tests were carried out under a load controlled condition. The
axial stress wave form used was a triangular wave with a stress ratio R of
0.1 and a frequency f of 10 Hz. In water environments the frequency was
selected at 0.1 Hz. Tensile and fatigue tests were carried out in
laboratory air. Some fatigue tests were also carried out in ion-exchanged
water at 25 ± 0.5 °C. We also investigated the influences of cathodic
protection on fatigue strength. The environment used was 0.1N CH3COOH +
0.2N CH3C00Na solution, and a cathodic potential of 0.9 V vs. Ag/AgCl
electrode was applied to specimens.

Acoustic emission (AE) signals were measured in some tensile tests in order
to monitor damage initiation and progression (Komai et al., 1990). AE sig-
nals were acquired and processed with an AE acquisition and analyzing
system, Locan (Physical Acoustic Corp.). For some fracture surfaces, sur-
face roughness was evaluated through reconstructing its three-dimensional
shape using computer image processing technique (Komai and Noguchi, 1987b).

EXPERIMENTAL RESULTS AND DISCUSSIONS

Tensile Tests

Figure 2 shows a stress-strain curve together with changes in AE event

counts. The total number of event counts for SiCw/7075 was only about 180,
which was much fewer compared with a unidirectional carbon fiber/epoxy com-
posite (Komai et al. , 1990). The changes in AE parameter distributions
were analyzed by means of three-dimensional data processing; three dimen-
sional AE signal amplitude-, AE signal duration-, and C/D ratio- AE events
distributions against strain.

AE signal behavior was classified into four stages as is shown in Fig. 2,

which fairy well corresponded to the change of slope of the stress-strain
curve. First was a elastic deformation stage, Stage I, having small
 405

Fig. 2 Stress-strain curve of a ten- Fig. 3 Crack initiation site of a

sile test of SiCw/7075 together tensile test. Arrows in-
with changes in AE event count dicate whisker pull-out.
rates.

amplitude and short duration AE signals. These AE characteristics are

typically observed when a AE transducer catches electro-magnetic noises.
Second was the Stage II, when high-amplitude AE signals came out and elas-
tic modulus slightly decreased. In the case of CFRP, high-amplitude AE
signals are associated with fiber breakage. These AE signals might have a
relation with local breakage of whisker or whisker cluster. Finally was
the Stage III and the unstable fracture stage, Stage IV. In the Stage III,
AE signals with long-duration and relatively high amplitude came out.
These signals might be resulted from whisker pullout. In the final
unstable Stage IV, high-frequency (high C/D ratio), high amplitude AE sig-
nals, resulted from whisker breakage, and relatively long duration signals,
which might come out through matrix fracture, were observed.

Figure 3 shows a crack initiation site of a tensile test. Relatively

many whisker pullout can be seen, as was expected by AE signal analyses in
Stage III. A high stress, as nearly an ultimate tensile strength, being
applied, whisker pull-out occurred although interfacial strength between
aluminum matrix and SiC whisker is reported to be good. In fact close ex-
amination revealed that pullout whiskers were surrounded with matrix
material.

Fatigue Tests

The relationships between maximum stress and cycles to fracture both in

laboratory air and in ion exchanged water together with fatigue results of
a matrix aluminum alloy 7075 at R = -1 (Schwarman, 1986b) are shown in Fig.
4. Experimental results with * show the cases having inside sites of crack
initiation, the others being the cases having surface sites of initiation.
It is clear that strength of SiCw/7075 in laboratory air was superior to
that of the unreinforced matrix material. At lower stress levels, the
water environment decreased the fatigue strength, though the strength was
still superior to that of unreinforced 7075 alloy in laboratory air. Under
a cathodically charged condition, the fatigue strength reincreased up to
the fatigue strength of SiCw/7075 in laboratory air. This means that
cathodic protection gave a beneficial effect on fatigue strength in a cor-
rosive environment.
406

ΙΟΟΟι
- ο - Ι η air
• In water
ΘΟθί 9 E=-0.9V vs Ag/AgCI
— In air 7075-T6, R=0

600

400

200

. 1 . 1 , 1 , 1 . 1 . 1 i 1 i
10° 101 102 103 10* 105 106 107 108
Number of Cycles

Fig. 4 Relation between maximum stress and cycles to

failure in laboratory air and water environments.

Fig. 5 Surface site of fatigue Fig. 6 Inside site of fatigue

crack initiation in crack initiation in
laboratory air (omax = laboratory air (omax =
500 MPa). 400 MPa).

Figure 5 shows a fractograph of the surface site of crack initiation, and

the Stage II fatigue crack normal to principal stress was initiated
directly from the specimen surface. Figure 6 shows a fractograph of the
inside site of crack initiation. It shows that the crack was initiated at
a whisker cluster (Flom and Arsenault, 1987a). Fatigue loading gradually
caused debonding between whisker cluster and matrix material, which acted
as a crack starter. That is, a fatigue crack was initiated and propagated
when a size of debonded whisker cluster exceeded a critical size. The
critical stress intensity factor range above which a fatigue crack was in-
itiated and propagated, which was calculated using the debonded whisker
cluster size (Murakami, 1985b), was about 4 - 4.6 MPa'm17 .

The typical fatigue fracture surface 0.1 mm apart from the debonded whisker
cluster of the initiation site is shown in Fig. 7. The fracture surface
was very rough and we scarcely observed whisker. With the crack extension,
however, whisker pull-out and whisker breakage were observed (Fig. 8) and
surface roughness became smaller. This means that crack at low stress in-
tensity levels grew with avoiding whisker cluster (Christman and Suresh,
 407

Fig. 7 Fracture surface of fatigue Fig. 8 Fracture surface of fatigue

in laboratory air at a low in laboratory air at higher
stress intensity. The sur- stress intensity. The sur-
face was 0.1 mm from the face was 0.25 mm from the
initiation site (omax = 400 initiation site (omax = 500
MPa). MPa).

M -2
'^X J^o 0 0 0 0 0 «^^
30 60
X μτη

(b) Cross section along the A-A1 line on

the fracture surface

(a) SEM photograph

Fig. 9 Crack initiation site of fatigue in water

(omax = 400 MPa).

Table 2 Fracture surface area ratio of fatigue in laboratory air.

Maximum Stress Intensity 8

Factor (MPa'in 1/2 ) 10
Fracture Surface Area 1.85, 173, 1.64, 1.57: 1.65 1.63, 1.63, 1.50:
Ratio Average: 1.70 Average: 1.60

1988b), resulting in rough fracture surface; with increasing stress inten-

sity levels, crack propagated with whisker pull-out and whisker breakage.

Roughness of Fatigue Crack Path

The results are shown in Table 2 showing a tendency that a surface area
408
ratio was large when a stress intensity factor was low, whereas it became
smaller when a stress intensity factor was high. This corresponded with
the results mentioned above.

Influence of Water Environment

Figure 9 shows a crack initiation site of a fatigue specimen in water

at omax = 400 MPa. The figure also involves the cross section along the A-
A' line on the fractograph, which was calculated by using the three dimen-
sional image processing technique. The figure indicates that there was a
hole at the crack initiation site, and its mouth was covered with corrosion
products. This is considered to be brought about by pitting corrosion. In
monolithic metals, a pit mouth is widely opened, whereas the pit mouth of
the SiCw/7075 was closed and also covered with corrosion products, though
it was deeply hollowed out. Corrosion (pitting) concentrated on a high
density site of whisker, i.e., whisker cluster. This fairly well agreed
with the results by Aylor et al. (1985a). A galvanic couple between
whisker and the matrix material resulted corrosion especially around
whisker cluster. In this case the dispersoid (SiC whisker) is a noble
phase (Paciej and Argarwala, 1986a). The stress intensity factor range of
the corrosion pit obtained was 4.4 MPa'm 1 ' 2 which was the same as the
critical tJi for a crack to be initiated at whisker debonding.

The reason of a decrease in fatigue life in water was a corrosion effect,

which was also supported by the fact that fatigue life at the cathodically
charged potential was almost the same as that in laboratory air. At a
moderate cathodic potential, corrosion reaction on specimen surface was in-
hibited, and pitting corrosion no more occurred.

CONCLUSIONS

The mechanical properties other than elongation and the fatigue strength in
laboratory air of the SiCw/7075 were superior to an unreinforced matrix
material. Two kinds of fatigue crack initiation sites were observed, i.e.,
a surface site and an inside site. Fatigue crack path of the SiCw/7075
varied depending upon stress intensities. In water environments, corrosion
promoted crack initiation, resulting in a shorter fatigue life than that in
laboratory air.

REFERENCES

Arsenault, D.J. (1988a). Proc. 9th Ris Int'l Symposium on Metallurgy

and Materials Science, 279-284.
Aylor, D.M. and R.M. Kain (1985a). ASTM STP 864, 632-647.
Christman, T. and S. Suresh (1988b). Mat. Sei. Eng., A., JO2, 211-216.
Flom Y. and R.J. Arsenault (1987a). Proc. ICM-V, _2, 1253-1260.
Komai, K. and M. Noguchi (1987b). Trans. Iron & Steel Inst. Japan, 27,
658-663.
Komai, K., K. Minoshima and T. Shibutani (1990). Trans. Japan Soc. Mech.
Eng., 56, 1792-1799.
Murakami, Y. (1985b). Engng. Fract. Mech., 22, 101-114.
Paciej, R.C. and V.S. Argarwala (1986a). NASA STAR Technical Report.
Schwarmann, L. (1986b). Materials Data of High Strength Aluminum alloys
for Durability Evaluation of Structures, Aluminum-Verlag, Duesseldorf.
Yau, S.S. and G. Mayer (1986c). Materials, Mater. Sei. Eng., 82, 45.
WS7b2

FATIGUE OF ALUMINIUM-LITHIUM BASED MMCs AT

AMBIENT AND ELEVATED TEMPERATURES

P.D.Couch and P.Bowen

School of Metallurgy and Materials / I.R.C. in Materials for High

Performance Applications, University of Birmingham, P.O. Box
363, Birmingham, B15 2TT, United Kingdom.

ABSTRACT

Crack growth resistance under cyclic loading has been investigated at ambient temperature,
120°C and 250°C for a range of paniculate reinforcement sizes (at a constant volume fraction of
reinforcement) in an Al-Li (8090) base alloy. Crack growth resistance is increased at elevated
temperatures for all composites. Effects of pre-strain prior to ageing have been considered on
crack growth resistance at ambient temperature: pre-strain improves the crack growth resistance
of composites reinforced with fine paniculate (3 and 7μπι nominal sizes) but decreases that of
composite reinforced with coarse paniculate (20μπι nominal size). It is deduced that cracked
silicon carbide panicles are likely to reduce fatigue crack growth resistance. Despite this,
improved crack growth resistance, in general, is observed in composites reinforced with coarse
(20μιη) paniculate and the results are consistent with the controlling influence of matrix mean
free path: decreased matrix mean free path reduces fatigue crack growth resistance.

KEYWORDS

Metal Matrix Composite; Reinforcement Size; Crack growth resistance; Elevated Temperature
Properties; Interpanicle spacing.

INTRODUCTION

Future developments in the aerospace industry are directly dependent on the manufacture of
new materials with improved capability. To this end much emphasis has been put on metal
matrix composites for both their high specific stiffness and strength. Continuous fibre
composites attain the most spectacular improvements in specific properties but unfortunately
they have relatively poor transverse properties and high cost. Particulate composites, however,
exhibit isotropic properties, are easier to process and form into components and thus much
interest has also been shown in such composites.

The focus of this work is the reinforcement of an aluminium-lithium (8090) based matrix
material with particulate SiC at a constant volume fraction (16.6vol%) and with variation of
particulate phase size i.e. 3μπι, 7μηι and 20μπι. Previous work on effects of reinforcement size
(Shang et a/.,1988,Downes et al., 1990) has suggested that larger particulate size results in
modest increases in crack growth resistance compared with that for finer particulate sizes.
Effects can be more obvious on crack growth resistance in the near threshold region. A limited
amount of work has been conducted to identify the elevated temperature properties of metal
409
410

matrix composites (McDanels.,1985) covering basic mechanical properties alone and there
appears to be little fatigue data obtained at elevated temperatures in the literature.

EXPERIMENTAL

The material under investigation is an aluminium-lithium (8090) matrix (Al-2.4Li-l.2Cu-

0.9Mg-0.1Zr,wt%) with 3μιη, 7μπι and 20μπι nominal size particulate reinforcement phase at a
constant volume fraction of 16.6 vol%. These composites were produced by B.P. Metal
Composites Ltd using a powder metallurgy route including HIPping, forging, and rolling to a
plate thickness of =15mm.

Fatigue test specimens with the dimensions 100x21x12 mm were cut from these plates. These
blank test specimens were solution treated at 530°C for 1 hour followed by cold water
quenching and peak ageing for 12 hours at 150°C. A pre-ageing stretch was imparted to the
three composite systems in an attempt to remove the macroscopic residual stresses generated in
the quenching step. Pre-straining was performed in uniaxial tension to a nominal amount of 6%
plastic strain. A notch « 5mm deep was then cut in the L-T orientation to create single edge
notched (S.E.N.) bend specimens for fatigue testing. Constant load amplitude fatigue testing
was conducted in four point bend on an Amsler Vibrophore at a frequency of 90 Hz and at a
stress ratio of R=0.1 (where R=a m i n /a ma x). Fatigue crack growth was monitored using the
direct current potential difference (d.c.p.d.) technique. After pre-cracking, tests were performed
at a constant load range and hence increasing ΔΚ. The elevated temperature tests were
conducted in a purpose built Amsler Furnace, which gave a constant temperature of 120°C ±
5°C and 250°C ± 5°C with all of the tests concluded in approximately 5 hours.

Fractographic analysis was carried out using both an I.S.I. 100A and a Hitachi S4000 F.E.G.
scanning electron microscopes at an accelerating voltage of 20 kV.

RESULTS

Crack growth rates are presented on log da/dN versus log ΔΚ plots as shown in figs. 1 and 2
for all of the temperature and pre-strain conditions under investigation respectively. At room
temperature and 250° C the crack growth resistance of the 20μπι particulate reinforced
composites was better than that of the 3μιτι and the 7μπι particulate reinforced composites
(which present similar trends throughout). The influence of pre-strain on the composite systems
is different: the 20μπι composite system exhibits a reduction in fatigue crack growth resistance
with pre-strain, but both the 3μιη and 7μιτι composite systems show improved fatigue crack
growth resistance. It is clear from the fatigue data that composites reinforced with coarser
(20μπι) silicon carbide particulate are more resistant to crack growth than those reinforced with
7μπι or 3μπι particulate except after pre-straining. In addition, the elevated test temperatures
appear to have improved the crack growth resistance in all composites relative to their ambient
temperature behaviour.

The size of the reinforcement phase appears to control the mechanism of fatigue and fracture.
The finer 3μπι and 7μπι reinforcement phases produce solely matrix dominated failure surfaces
under all test conditions see fig. 3. The coarse 20μιη condition shows a more complex failure
with a dual matrix/reinforcement controlled process exhibited see fig. 4. The fatigue surfaces
become smoother as the test temperature is increased and the proportion of SiC observed tends
to zero at 250°C see fig. 5. It appears that the mechanism of fatigue and fracture encounters a
transition from a solely matrix dominated process to a dual matrix/reinforcement phase
controlled process as the size of the reinforcement phase increases from 3μιη to 20μπι.

DISCUSSION

The focus of this work is the fatigue resistance of the composite systems under investigation. It
is clear that there are a wide range of test variables (e.g. residual stresses, effect of pre-strain,
 411

temperature) in the work to date and a number of effects need to be isolated for the future.
Nevertheless, it is appropriate to consider trends in the experimental results and to attempt to
deduce possible controlling features for crack growth resistance. First, it is necessary to
recognise that although thresholds may sometimes be improved over the base alloy by
particulate addition, in general crack growth resistance decreases; and this appears to be the case
for the 8090 alloy under investigation.

The fractography would seem to indicate that the fatigue process for the 3μπι and 7μπι
reinforced composites proceeds by a matrix dominated process whereas that for the 20μπι
reinforced composite indicates evidence of the reinforcement phase on the fatigue surface.
However as the test temperature is increased to 250°C the proportion of SiC reinforcement on
the fatigue surface reduces markedly, but there is no apparent reduction in the fatigue crack
growth resistance of the 20μπι case. It is probable therefore that SiC particulate failure does not
improve the fatigue crack growth resistance. One possible reason for SiC cracking to be most
prevalent in the 20μπι reinforced composite is a direct consequence of their lower inherent
strength when compared with the smaller particulate reinforcement phases. Consider the
situation at the crack-tip. To a first approximation the peak level of tensile stress ahead of a
blunted crack-tip can be up to 5a y (Rice et a/.,1970, Tracey.,1976) in a monolithic material of
work hardening exponent, n « 0.2, and as the value of applied stress intensity increases, this
level of peak load stress remains unchanged, but it exists over a larger process volume
(occurring at approximately 1.96, where δ is the crack-tip opening displacement). If the matrix
yield strength is taken as 500 MPa at room temperature, then stresses of up to 2500 MPa are
possible, and if no stress relief occurs (due to growth in the matrix as the crack approaches the
particulate) then fracture of the particulate can occur only if their fracture stress is < 2000 MPa.
(Note that brittle fracture is controlled by tensile stresses and that neutron diffraction studies
have suggested that the silicon carbide particulate may be under a compressive residual stress of
= 500MPa). Even at room temperature, therefore, if the effective fracture stress of the finer
particulate reinforcements are > 2000 MPa then they can not fracture. At the higher test
temperature of 250°C, particulate fracture can be considered to be unlikely even for the 20μπι
reinforced composite, because the available local stresses may not achieve high enough stresses
(and the fracture stress of the particulate is expected to be independent of test temperature).
Fractographic analysis would suggest that SiC failure could be detrimental to the fatigue crack
growth resistance of the composite under investigation

The composites do not follow the trends of conventional alloys which tend to show a
deterioration in crack growth resistance with increase in test temperature, since they actually
present an improvement in crack growth resistance with temperature. Variations do exist,
however, between the three particulate sizes of reinforcement. The reduced presence of SiC on
the fatigue surface of the 20μιη reinforced composite would seem to indicate that the fracture
stress of the SiC is too high for the intensification of the reduced yield stress at the elevated
temperatures to cause failure and hence the fatigue process becomes more matrix dominated
(with some possible decohesion mechanism favoured as overageing at 250°C may reduce the
strength of the interfacial bond). In the 3μπι and 7μπι cases the crack growth resistance is
improved up to a temperature of 120°C plausibly because the microscopic tensile residual
stresses present in the matrix are reduced (Couch et al., 1990), and thus delay the failure
mechanism within the matrix. As this is evidently a matrix dominated process then it is clear that
factors which improve the fatigue crack growth resistance of the matrix will tend to improve the
fatigue crack growth resistance of the composite. However, the crack growth resistance at
250°C is not quite as good as at 120eC perhaps because precipitates will form at this
temperature which are deleterious to the mechanical properties of the matrix, thus outweighing
the improvement in crack growth resistance from further microscopic residual stress relief. In
contrast, the crack growth resistance of the 20μιη reinforced composite continues to improve up
to 250°C, at which temperature particulate cracking is not observed. It may be deduced
therefore that particulate cracking is detrimental to crack growth resistance.

The effect of pre-strain prior to ageing (many commercial product forms will be used in the pre-
strained condition) on the fatigue properties of the composites is of interest and supports the
above argument. The 3μπι and 7μιη reinforced composites appear to exhibit an improvement in
412
fatigue crack growth resistance with pre-strain, and the improvement appears to depend on the
extent of the pre-strain. The pre-strain will relieve some of the micro- and macroscopic residual
stresses but in addition there is a possibility that an increased dislocation density will be
generated. This could lead to a more uniform distribution of strengthening precipitates and thus
plausibly to improve the matrix resistance. In the 20 μπι case, however, there is a deterioration
in the fatigue resistance with pre-strain and this is assumed to be due to SiC damage during pre-
strain which would be expected to increase the proportion of SiC which could fail under the
stress conditions at the crack-tip. Fractographic evidence seems to identify an increased
proportion of cracked SiC on the fatigue surfaces, although a quantitative analysis is still to be
undertaken.

As the size of the reinforcement phase is reduced then the mean free matrix path can be
estimated by a simple calculation involving a cubic array of uniform spherical particles which
estimates the interparticle spacing to be 29.3μπι for the 20μπι reinforced composite, 1 Ιμιη for
the 7μπι system and 4.4jim for the 3μπι case. If crack growth resistance is controlled by a shear
localisation process in the matrix, then it is feasible that finer particulates might be expected to
promote this process, particularly as they are well bonded and thus these hard, elastic particles
will intensify strain in the matrix. It is of interest to note that the fatigue surface morphology
appears to show close similarities to the regions of fast fracture particularly for the finer
paniculate reinforced composites.

In the 20μπι composite reinforced system there is evidence of fatigue crack growth interaction
with the paniculate reinforcement phase. Some studies have suggested that cracked particles
might be beneficial in promoting crack growth resistance. While in near threshold regions this
might be possible due to increased surface roughness and hence increased crack closure it is not
clear why this should be the case at higher growth rates (note the area fraction of SiC in fatigue
regions appears independent of crack growth rate but final fracture surfaces exhibit a SiC
paniculate dominated failure mechanism). The detrimental effects of cracked SiC panicles is
deduced both from the effects of pre-strain where the crack growth rates are faster (than would
have been predicted from the results for the 3μπι and 7μπι conditions) and from the results
obtained at 250°C where crack growth rates are better than would have been predicted from
room temperature crack growth rates (and little evidence of cracked SiC panicles is observed on
fatigue regions produced at 250°C). The former observation can plausibly be explained if pre-
strain damages SiC panicles and the latter observation is consistent with the reduced levels of
local matrix tensile stress available to crack SiC particles at 250°C.

It is clear for a given volume fraction of reinforcement that there is an interdependence of its size
and the mean free path between the reinforcement i.e. as the reinforcement size increases so
does the mean free path. It therefore appears that the results are consistent with a crack growth
mechanism which is dependent directly on the mean free path between (reinforcing) paniculate.
Cracked silicon carbide paniculate is not considered beneficial for crack growth resistance. This
study would suggest a reduced crack growth resistance as the volume fraction of reinforcement
phase is increased.

CONCLUSIONS

This investigation indicates that composites reinforced with coarser (20μιη) paniculate are more
resistant to crack growth than those with (3μπι or 7μπι) particulates except after pre-strain prior
to ageing. In addition, the elevated test temperatures appear to have improved the crack growth
resistance in all composites relative to their ambient temperature behaviour. Both the 3μπι and
7μπι conditions exhibit improved crack growth resistance after a preageing stretch. The 20μπι
condition, however, exhibits poorer crack growth resistance after pre-straining and this is
deduced to occur as a consequence of SiC paniculate damage during pre-strain.

The fatigue process in the finer paniculate reinforced composite systems (3μιτι and 7μπι) is seen
to be matrix dominated under all conditions of temperature and pre-strain. For the coarser
(20μιη) reinforced composite system fractography indicates an involvement of cracked silicon
 413

carbide particulate during crack growth at room temperature, but at 250 e C few cracked silicon
carbide particles are observed. It is deduced that cracked silicon carbide particles are, in general,
likely to reduce fatigue crack growth resistance.

The results are consistent with the critical role of matrix mean free path: decreased matrix mean
free path reduces fatigue crack growth resistance.

ACKNOWLEDGEMENTS

Support for the author (PDC) with a S.E.R.C. C.A.S.E. award from B.P. Metal Composites
Ltd is gratefully appreciated together with the useful discussions with R.B. Newbery.

REFERENCES

Shang Jian Ku, Yu Weikang and Ritchie R.O. (1988). Role of silicon carbide particles in
fatigue crack growth in SiC-particulate-reinforced aluminium alloy composites. Materials
Science and Engineering Vol.102, pp 181-192.
Downes T.J., Knowles D.M. and King J.E. (1990). Effect of particle size and ageing on the
fatigue behaviour of an aluminium based metal matrix composite. European Conference of
Fracture 8, Vol. 1, pp 296-302.
McDanels D.L. (1985). Analysis of stress-strain, fracture, and ductility behaviour of aluminium
matrix composites containing discontinuous silicon carbide reinforcement. Metallurgical
Transactions A Vol. 16A. pp 1105-1115.
Rice J.R. and Johnson M.A. (1970), in "Inelastic Behaviour of Solids", edited by
M.F.Kanninen et.al., McGraw-Hill, New York p. 641.
Tracey D.M. (1976), Journal of Engineering Materials Technology. A.S.M.E. 98. p. 146.
Couch P.D. and Bowen P. (1990). Effect of temperature on fatigue crack propagation in SiC
particulate reinforced Al-base composites .Proceedings of the fourth Conference on Fatigue
and Fatigue Thresholds held 15-20 July, in Honolulu Hawaii, editors KKitagawa and T.
Tanaka. Vol. IV, pp 2545-2551.

, J , J , J n 1 , J r ■ ... , 1
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o
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4 6 8 10 12 14
ΔΚ (MPaVm)
fig.l The fatigue crack growth data for the composites
at ambient temperature, 120'C and 250'C.
414

. 1 ■ 1 ' I ' 1 ' 1 ' 1 ' II

o (a)
β

*°n ö
IG"4
■
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n

jD
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oo o flσ
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; o 20μιη
1 . 1 ■ 1 ■ 1 . 1 . 1 . 1
4 6 8 10 14
Δ K (MPaVm)

fig.2 Fatigue crack growth data at ambient fig.3 Typical fatigue surface for the 3μπι
temperature for the composites in the composite tested at ambient temperature,
pre-strained condition. (a) S.E.I, (b) B.E.L

(a)

(b)

fig.5 Typical fatigue surface for the 20μιη

composite tested at 250°C.

fig.4 Typical fatigue surface for the 20μπι

composite tested at ambient temperature,
(a) S.E.I., (b) B.E.I.
 WS7b3

SPECIMEN-GEOMETRY EFFECT ON FATIGUE CRACK PROPAGATION

IN SIC WHISKER REINFORCED ALUMINUM ALLOYS

Keisuke TANAKA

Department of Engineering Science, Kyoto University,

Yoshida-honmachi, Sakyo-ku, Kyoto 606, Japan

ABSTRACT

Fatigue crack propagation tests were conducted with compact tension (CT) and center-
cracked plate (CCP) specimens of 2024-T6 and 6061-T6 aluminum alloys reinforced with
20% volume fraction of SiC whiskers. For the cases of CT specimens, the crack
propagation path was curved, and the mismatch of the fracture surface roughness was
amplified by a mode II component of deformation. The threshold stress intensity
range was larger in SiC/2024-T6 than in unreinforced 2024-T6 because of a greater
amount of crack closure. For CCP specimens of SiC/2024-T6 and SiC/6061-T6, a crack
propagated straight. The increase in the crack propagation resistance near the
threshold in SiC/2024-T6 was very small in CCP specimens. On the other hand, the
threshold stress intensity factor was decreased in SiC/6061-T6 owing to the
refinement of the grain size by reinforcement.

KEYWORDS

Fatigue crack propagation; metal matrix composite; aluminum alloy; fracture

mechanics; crack closure; specimen-geometry effect

INTRODUCTION

Aluminum alloys reinforced with silicon carbide (SiC) whiskers have high stiffness
and strength as well as high wear resistance. Their good formability enables
secondary processing such as extrusion, rolling and machining. Extrusion introduces
whisker alignment in composites and then the mechanical properties become
anisotropic (Morimoto et al., 1990). In fatigue and fracture, the path of crack
propagation is very much influenced by the whisker orientation, specimen geometry or
loading mode. In the present paper, the effect of specimen geometry on the fatigue
crack propagation behavior in SiC whisker reinforced aluminum alloys was studied by
using compact-tension (CT) specimens and center-cracked plate (CCP) specimens, and
the propagation behavior was discussed on the basis of crack propagation morphology
and crack closure.

EXPERIMENTAL PROCEDURE

Two aluminum alloys, 2024 and 6061, reinforced with SiC whiskers were made by powder
metallurgy. The volume fraction of SiC whiskers is 20%. SiC whiskers are single

415
416
Table 1. Mechanical properties of materials.

Material 2024-T6 SiC/2024-T6 6061-T6 SiC/6061-T6

0.2% proof stress,

355 484 287 487
σ (MPa)
0.2

Tensile strength,
445 646 326 600
σβ (MPa)

crystals with a diameter of 0.1 to lym and a length of 5 to 50iJm. An extruded plate
of SiC/2024 and an extruded rod of SiC/6061 were heattreated under T6 conditions.
The specimens were cut from extruded-and-heattreated samples to have the L-T
orientation. Table 1 summarizes the yield strength and the tensile strength of
composites under tension along the extrusion direction, together with those of
unreinforced materials. The unreinforced materials were made by ordinary melting
and casting.

Ihe effect of the specimen geometry on the crack propagation behavior was examined
with SiC/2024-T6. CT specimens had a width of 40mm and a thickness, B, of 3 and
10mm; CCP specimens had a width of 20mm and a thickness of 3mm. An initial notch
was made perpendicular to the extrusion direction. The fatigue specimens of the
matrix material, 2024-T6, were of compact tension type and had B=10mm. For
SiC/6061-T6 and 6061-T6, the specimens used were CCP with a width of 14mm and a
thickness of 4mm, and had the L-T orientation.

Fatigue tests were conducted in a servo-hydraulic testing machine in air at room

temperature. The near-threshold propagation data were obtained by load shedding.
The length of a fatigue crack was measured with a travelling microscope at a
magnification of 200. The crack closure was measured with the unloading compliance
method. The load ratio, R, was 0.1 for SiC/2024-T6 and 2024-T6, and -1 for
SiC/6061-T6 and 6061-T6.

EXPERIMENTAL RESULTS AND DISCUSSION

Crack Propagation Morphology

For CT specimens of the composite (SiC/2024-T6), a crack propagated at about 30

degree from the direction of the initial notch for both thicknesses of 3 and 10mm.
The crack length measured was the one projected on the initial notch plane. On the
other hand, a crack grew in the initial-notch direction in CCP specimens (SiC/2024-
T6 and SiC/6061-T6). Albritton et al. (1989) reported similar crack curving in CT
specimens of SiC/2124 with the L-T orientation in fracture toughness tests, and also
straight crack growth in CCP specimens. The specimen thickness for their specimens
was 12.7mm. They also observed straight crack growth in CT specimens with a
thickness of 2.54mm, and ascribed straight growth to the plane stress state. The
thickness of 3mm is not enough to obtain the plane stress condition in the present
material. The difference in stability of the crack propagation direction was
discussed on the basis of the non-singular T stress (Tanaka et al., 1989). A
negative T stress in CCP specimens makes a slightly deviated crack back to the
original direction, while a tensile T stress in CT specimens helps the crack
curving.

An optical micrograph of a fatigue crack formed in a CT specimen (B=3mm, SiC/2024-

 417

(a) (b)
Fig. 1. Micrographs of a crack in CT specimen of SiC/2024-T6 (B=3mm).

(a) (b)
Fig. 2. Micrographs of a crack in CCP specimen of SiC/2024-T6.

T6) is shown in Fig. 1(a), and a scanning electron micrograph of Part A is in

Fig. 1(b). The crack propagated at about 30 degree to the initial notch direction
and stopped during load shedding. As seen in (b), the irregularity of crack growth
due to whiskers is evident, and whisker pull-out is observed. The mismatch of the
roughness of the fracture surface is amplified by a mode II component of
displacement resulted from crack deviation. Figure 2 shows micrographs of a crack
in a CCP specimen (SiC/2024-T6). The crack is macroscopically straight and
accompanied by microscopic irregularity due to whiskers. Pulled-out whiskers are
also seen. Because only mode I loading is operating, a horizontal displacement of
the surface zig-zag is not large. Similar morphology was observed with CCP
specimens of SiC/6061-T6.

Crack Propagation Behavior

The rate of crack propagation in both CT and CCP specimens of SiC/2024-T6 is plotted
against the stress intensity range, ΔΚ, in Fig. 3(a) and against the effective
stress intensity range, Δ Κ ^ , in Fig. 3(b). The results for the unreinforced
material were also shown in the figures. In the da/dN-ΔΚ relations, the crack
propagation rate in CT specimens is lower than the unreinforced material especially
near the threshold. The crack propagation rate is independent of the specimen
418
thickness. On the other hand, the crack propagation rate in CCP specimens is only
slightly slower than that of the unreinforced material near the threshold. In the
da/dN-AKgff relation, the relation is nearly identical for all the cases examined;
the increases in Young's modulus and strength due to whisker reinforcement do not
increase the intrinsic resistance to fatigue crack propagation. The whisker
reinforcement only increases the extrinsic resistance or the crack-tip shielding.
Figure 4 shows the change of the crack opening stress intensity factor K with the
maximum stress intensity factor K m a x . The K Q p / K m a x value is larger for composites

10" 10" -1—i i i i i i r—

L-T L-T
o SiC/Al (CT. B=10)
o SiC/Al (CT. B=10)
\ 10" Δ SiC/Al (CT. B=3) #
I· Δ SiC/Al (CT. B=3)
E v SiC/Al (CCP) E
v SiC/Al (CCP)
• 2024-T6 \
• 2024-T6
\ 10"

ω •^7o4 Vo
to * OO 10 -9 *7 Φ ·
"5 10" v
f
°o v v
>
10" 10"

10-11 Barred marks : 10"

Barred marks :
ΔΚ-increasing tests
ΔΚ-increasing tests
o
10-12 10 -12
^t
J I I L_l
■tv
2 * * *^ 10 15 0.5 ♦W1
X 2 5 10
Stress intensity range , ΔΚ ΜΡαΤπϊ Effective stress intensity range
AK eff MPa/rn

(a) da/dN v s . ΔΚ (b) da/dN v s . AK eff

Fig. 3 . Relation between crack propagation r a t e and s t r e s s

i n t e n s i t y range for SiC/2024-T6 and 2024-T6.

1.00 i τ 1 1 1
L-T O SiC/Al (CT. B=10)

%i
Δ SiC/Al (CT. B=3)
°^ •0.75 V o \
^ v SiC/Al (CCP)
φ- · 2024-T6

0.50 -
• ·
p 0.25 - : * H \ * % - , -
Barred marks :
ΔΚ-■increasing tests
1 1 1 1 1

0 5 10 15
Maximum stress intensity factor , K max ΜΡαΤττΓ

Fig. 4. Relation between stress intensity factor at crack

opening and maximum stress intensity factor.
 419
-1 1 ι 1—i—r- 10" T—i—i i i
L-T h L-T
o SiC/Al CP

10" • 6061-T6 \
2E
Λ o ·Φ·Φ •σ
o o 9+ \
10" Ί-9
o
ocP ►03
o

10 -10 10-10

10" 10" o SiC/Al

• 6061-T6
o
(J
10 -12
> 5
_l
*7
I I
10
l_
,o- U-d I I I I 1 1 L
4 * * 1 2 5
Stress intensity range , ΔΚ MPa/m Effective stress intensity range ,
AKeff ΜΡα/ίτΓ

(a) da/dN v s . ΔΚ (b) da/dN v s . AK e f f

Fig. 5. Relation between crack propagation rate and stress

intensity range for SiC/6061-T6 and 6061-T6.

than for the unreinforced material at all K m a x values. With respect to the geometry
effect, the value is larger in CT specimens than in CCP specimens, because of the
mode II displacement introduced by crack curving.

Figure 5 shows the results for SiC/6061-T6 and 6061-T6. With these materials, the
threshold stress intensity factor is much higher in 6061-T6 than in SiC/6061-T6,
while the relation between the crack propagation rate and the effective stress
intensity range is roughly the same. A large amount of crack closure in 6061-T6
resulted from excessive kinking and branching of a fatigue crack. This 6061-T6
material is made by ordinary melting and casting, not by powder metallurgy, and has
a coarse grain size about ten times larger than the matrix in the composite.

Effect of SiC Whisker Reinforcement

The reinforcement of SiC whiskers increases the Young's modulus, yield strength and
tensile strength nearly in accordance with the rule of mixture (Morimoto et al.,
1990). On the other hand, the fracture toughness is decreased by reinforcement
(Albritton et al., 1989). The threshold stress intensity range for fatigue crack
growth is increased by reinforcement as far as the matrix microstructure is not
largely changed. When composites are compared with unreinforced materials made in a
different process, the fatigue crack growth resistance can be lowered by reducing
the grain size in reinforcement. The upper threshold for unstable fatigue crack
growth is decreased by reinforcement (Hirano et al., 1989, Tanaka et al., 1989) like
the fracture toughness. It is important to note that the relation between the crack
propagation rate and the effective stress intensity range is not affected by
reinforcement, and that the intrinsic resistance of fatigue crack growth is
basically controlled by the matrix material. Therefore, the prediction of crack
closure due to reinforcement is essential for composite design. The present result
420
JC

o
-t-
0"
R p i n f ΠΓΓΡΗ
to CO
CO CO
ω - \ CD Unreinforced
1_
·+-
CO CO
TD -σ
N
"o
sz Unreinforced \ "o \
CO
ω
CO
ω \
H
f- 1-

Crack length , a Crack length , a

(a) SiC/2024-T6 (b) SiC/6061-T6

Fig. 6. Fatigue failure diagrams.

indicates that the amount of crack closure is also a function of specimen geometry
or loading mode. The fatigue strength of smooth specimens is increased by
reinforcement like the yield strength (Masuda et al., 1989). Figure 6 illustrates
fatigue failure diagrams of two materials examined, where the threshold stress is
plotted against the crack length. Normally, the reinforcement induces the expansion
of the safe region as shown in Fig. 6(a) by increasing both the fatigue limit of
smooth specimens and the threshold stress intensity factor. Even in this case, the
notch sensitivity of composites will be larger than that of unreinforced materials.

CONCLUSIONS

(1) For the cases of CT specimens, the crack propagation path was curved, and the
mismatch of the fracture surface roughness was amplified by a mode II component of
deformation. The threshold stress intensity range was larger in SiC/2024-T6 than in
unreinforced 2024-T6.
(2) For CCP specimens of SiC/2024-T6 and SiC/6061-T6, a crack propagated straight.
The increase in the crack propagation resistance near the threshold in SiC/2024-T6
was very small in CCP specimens. On the other hand, the threshold stress intensity
factor was decreased in SiC/6061-T6 owing to the refinement of the grain size by
reinforcement.
(3) The relation between the crack propagation rate and the effective stress
intensity range was nearly the same for unreinforced and reinforced materials.

REFERENCES

Albritton, J.R. and J.G. Goree (1989). Fracture of silicon carbide whisker
reinforced aluminum. In: Advances in Fracture Research, ICF7 (K. Salama et al.,
ed.), Vol. 2, pp. 889-896. Pergamon Press, Oxford.
H i r a n o , K. and H. Takizawa ( 1 9 8 9 ) . Evaluation of fatigue crack growth
characteristics of whisker reinforced metals. Trans. Jap. Mech. Eng., 55, 373-378.
^suda, C. and Y. Tanaka (1989). Fatigue fracture mechanisms for SiC whisker and
SiC particles reinforced aluminum composites. Trans. Iron Steel Inst. Jap., 75,
1753-1760,·
Morimoto, H., K. Ohuchi, and T. Minamide (1990). Effect of whisker volume fraction
on mechanical properties of SiC whisker reinforced aluminum composites. Kobe Steel
Eng. Rep., 40, 62-65.
Tanaka, K., M. Kinefuchi, and Y. Akiniwa (1989). In: Fatigue 90, (H. Kitagawa et
al., ed.), Vol. 2, pp. 857-862. Mater. Comp. Eng. Publ. Ltd., Birmingham, U.K.
 WS7b4

FATIGUE BEHAVIOR OF SiC/Al COMPOSITE MATERIALS

H. ISHII, K. TOHGO, H. ARAKI and K. OHSIMA

Department of Mechanical Engineering, Shizuoka University,

5-1, Johoku 3 chome, Hamamatsu 432, Japan

ABSTRACT

Fatigue strength and fatigue crack propagation behavior of SiC whisker

(SiCw) or particulate(SiCp) reinforced 6061-T6 aluminum matrix composite
fabricated by the high pressure infiltration method were studied. A
comparison was made with the properties of unreinforced 6061-T6.

KEYWORDS

Fatigue strength; fatigue crack propagation; SiC whisker; SiC particulate;

metal matrix composite; 6061-T6 aluminum alloy; orientation.

INTRODUCTION

Metal matrix composites (MMCs) of aluminum alloys reinforced with whisker

or particulate silicon carbide are types of material that have great
potential applications to various stiff and high-strength light weight
engineering components (Feest, 1986, Signorelli, 1989). The comparatively
low cost, high machinability and good workability, compared to the
continuous MMCs, are their other attractive attributes (Ohori et al., 1987,
Chandler, 1989). They possess, in general, increased Young's modulus,
increased yield and ultimate tensile strengths, and decreased ductility
when compared to their monolithic metallic alloys (Nair et al., 1985).
However, somewhat contradictory results are reported for the fatigue
properties of these MMCs and further investigations are necessary to
evaluate their fatigue performance. The object of the present study is the
characterization of the fatigue performance, i.e. fatigue strength and
fatigue crack propagation (FCP) behavior, of SiC whisker or particulate
reinforced 6061-T6 aluminum alloy.

EXPERIMENTAL PROCEDURE

Billets (200 mm diameter) fabricated by high pressure infiltration method

421
422
(Ohori et al., 1989) were hot extruded into the square bars (57 mm side
length) and then T6 treatment was applied. The SiC whiskers (SiCw) had
dimensions of 0.5 - 1,0 urn in diameter and about 7 urn in length. Randomly
oriented whiskers in the preformed stage became aligned in the longitudinal
(L) direction by the extrusion. The SiC particulates (SiCp) had the
dimension of A - 8 Mm in diameter. They were also forced to align in the L
direction by the extrusion. Volume fractions of the SiCw and SiCp were
estimated as about 25 % and 6 %, respectively. The longitudinal, L, and
the transverse, T, oriented dumbbell shaped tensile specimens (diameter of
7 mm and gauge length of 15 mm), L and T oriented circular taper dumbbell
shaped high cycle fatigue specimens (minimum diameter of 7 mm) and T-T, T-L
and L-T oriented CT type FCP specimens were machined mechanically from
these bars. By using a closed loop electro-hydraulic fatigue testing
machine and a cantilever type rotating bending machine (30 Hz), the
tensile, fatigue and FCP properties were obtained. For the determination
of FCP behavior of L-T oriented SiCw/Al composite, the CCT (center cracked
tension) specimens also were used because of their abnormal FCP path
(almost perpendicular to the initial notch) observed in the CT specimen.
Even by using the CCT specimen, FCP path gradually changed to the loading
direction as the crack length increased. The frequency employed to
determine the FCP rate, at a stress ratio R = 0.1, was 10 Hz. Near
threshold FCP rates were determined by load shedding method. The crack
closure level was measured from the elastic unloading compliance obtained
from a strain gauge mounted on the back surface of the CT specimen. No
measurement of the closure level was done in the CCT specimen of L-T
oriented SiCw/Al specimen.

EXPERIMENTAL RESULTS AND DISCUSSION

It was shown from the stress-strain diagrams of the L and T oriented

composites and matrix aluminum alloy of 6061-T6 that the yield and the
tensile strengths, as well as Young's modulus, increased and the ductility
decreased by SiC whisker or particulate reinforcing. However, a strong
orientation dependence of these properties appeared in the composites,
especially in SiCw/Al. In particular, a remarkable increase occurred in
the tensile strength of the L oriented SiCw/Al specimens. These results
are summarized in Table I.

Table I. Mechanical properties of the SiCw/Al and SiCp/Al

composites and unreinforced 6061-T6 aluminum.

Material Or ientati on 0.2* P.S. MPa U.T.S. HPa Elongation %

SiCw/Al L 400 603 2.2

T 292 373 1.7

SiCp/Al L 287 331 10.5

T 274 301 8.5

6061-T6 L 280 316 9.6

T 267 305 10.5

High cycle fatigue

Figure 1 shows the fatigue curves of the SiCw/Al and SiCp/Al composites and
the matrix aluminum alloy 6061-T6 of L and T orientations. Virtually no
 423

250

Σ 200

i
150

1
104 10° 10° 10' 10°
Number of cycles

Fig. 1 Comparison of fatigue curves for SiCw/Al and

SiCp/Al composites with unreinforced 6061-T6.

orientation dependence is observed in SiCp/Al and 6061-T6, but strong

orientation dependence exists in the SiCw/Al composite. The fatigue
strength of L oriented SiCw/Al composite, as well as its tensile strength,
was much higher than that of the T orientation. Their fatigue strengths at
10 cycles were around 40 pet. of their tensile strengths, irrespective of
the orientation. This fatigue strength is approximately the same as that
of the unreinforced 6061-T6. On the other hand, fatigue strengths of
SiCp/Al composite are lower than those of 6061-T6, irrespective of their
higher tensile strengths. Their fatigue strengths are around 30 pet. of
their tensile strengths. This lower fatigue ratio might result from the
nucleation of fatigue cracks at clusters of particulates located at the
specimen surface. The dimension of a cluster was around a few tenth
millimeter (and could be easily detected from the fractogtraphy). Fatigue
fractured surfaces were macroscopically perpendicular to the neutral axis
except for the L oriented SiCw/Al composite. Fracture surfaces of L
oriented SiCw/Al composites were slant; chisel edge and V shaped fracture
surfaces were formed in this composite. It is noteworthy that in the T
oriented SiCw/Al composite the crack nucleation always occurs on the
surface parallel to the whiskers direction.

FCP rate

Results of FCP rate, da/dN, plotted against the applied cyclic stress
intensity factor A K , or the effective cyclic stress intensity factor ΔKeff,
for the SiCw/Al and SiCp/Al composite together with 6061-T6 are shown in
Figs. 2 and 3, respectively. The stress intensity factors used in these
figures are for mode I loading. In SiCw/Al composites, the FCP resistances
for T-T and T-L orientations are essentially the same. They are much
smaller than that of L-T orientation when the comparison is made using A K .
When comparison is made with the unreinforced 6061-T6, it is clear that the
FCP resistance and the threshold of the T-L or T-T oriented SiCw/Al
composite is lower than those of 6061-T6. They are higher in the L-T
composite than in 6061-T6. On the other hand, when comparison is made
usingΔ Keff for the T-L and T-T orientations, essentially no difference is
observed between the SiCw/Al composite and 6061-T6 (except when the da/dN
424

»3
ISlCw/AII fSIcTTÄn
AK AKeff ΔΚ AKeff
L-T a ■ L-T a ■

: i-
T-L o · T-L o
T-T Δ A T-T Δ ▲ •
*f* ieoei-τβι I IfiÄbl&J ■i?
AK AKeff
L-T A , + L-T
ΔΚ
♦
AKeff
♦
>ol
T-L · · T-L ·
T-T V ▼ T-T v •
■ e#
5 10- 5
</
fr
i
'•*«* ·* ..*.'
■ *» ·
|
«Λ-6
10 *· * .* i- ' »* na *
• · 10 Ί -
ί
\ *1e
<e · .
z
* <·ψ f» " ■
«•^ ♦ ·
«% /» •A •
♦

A
4 A

w 7 "
0
A
•
*r»"8 -JL_I_I 1 1 I— i 1 iJ i 1 l l__ 1 1— i J 1- 11 1 1
2 5 10 20 50 2 5 10 20
ΔΚ AKeff (MPd/m) ΔΚ AKeff <MPo/m>

Fig. 2 FCP rate curves for Fig. 3 FCP rate curves for
SiCw/Al and 6061-T6. SiCp/Al and 6061-T6.

range is higher than 10"^ mm/cycle). The FCP resistance of the SiCp/Al
composite of L-T orientation is a little smaller than that of other T-L and
T-T orientations which exhibit the same resistance. The latter shows the
same resistance as the unreinforced 6061-T6. However, when comparison was
made using AKeff, the same FCP resistance is observed, irrespective of the
orientation or reinforcement. These results on the FCP rate vs. Δ K or
Δ Keff are summarized in Fig. A (with data points omitted).
Figure 5, which shows the change of normalized crack opening stress
intensity factor Kop/Kmax with the maximum stress intensity factor Kmax,
indicates that above mentioned difference in da/dN - Δ K results from the
difference in the crack closure (or opening) level. Note that the da/dN -
Δ Keff relation (except for the L-T oriented SiCw/Al composite) is the same
irrespective of orientation or reinforcement. It is reasonable to consider
that surface roughness induced crack closure is suppressed by SiCw or SiCp
reinforcing. This is confirmed from the fractographs of these composite
specimens. Reduced plasticity induced crack closure, resulting from high
yield stress caused by SiCw or SiCp reinforcing, might also be another
factor involved. Higher FCP resistance and threshold observed in the L-T
oriented SiCw/Al composite results from the deflected fatigue crack path.
Similar fatigue crack path morphology was also reported. Fractographs of
this orientation show relatively few whiskers and cavities. These results
indicate that whiskers act as strong obstacles to crack propagation and
that fatigue cracks propagate in the matrix by avoiding the whiskers. In
discontinuous reinforcement, like in the SiCw/Al composite, a crack path in
the matrix which does not pass through whiskers is possible by crack
deflection. Chisel edge and V shaped fracture observed in high cycle
fatigue specimen of L orientation is also the result of this crack path
deflection. When deflection of the path occurs, mode I loading condition
can no longer be maintained. The deflected crack should be treated as a
 425

2 5 10 20
ΔΚ or AKrff (ΜΡά/Fn)

Fig. 4 Comparison of FCP rate curves for SiCw/Al and

SiCp/Al composites with those for 6061-T6.

SiCw/Al ΓΤ-1 ·
L T -T 4

ΓΤ-L ·
*~ °° SiCp/Al T-T '
LL-T ■
[T-L o
■•..St *"V, 6061-TB

■ i*. "■*■K
s . · A*· ·

■ A O O
D O*

%_.
o o
- - ■ -- V♦ · .

1 1 1 1
15

Kmex (MPa/m)

Fig. 5 Variation of Kop/Kmax with Kmax for SiCw/Al and

SiCp/Al composites and unreinforced 6061-T6.

mixed mode loading crack. Comparison of the FCP rate data of the L-T
oriented SiCw/Al composite with that of other orientations, SiCp/Al
composite or unreinforced 6061-T6 using the mode I stress intensity factor
may have reduced significance. However, the fatigue crack threshold value,
426
which is obtained when the fatigue crack is not deflected, is unaffected by
these conditions.
In the T-L or T-T oriented SiCw/Al composite specimens no orientation
dependence in the FCP rate was observed when compared by K. Their FCP
resistance is inferior to that of 6061-T6. However, fatigue strength in T
orientation was higher than that of 6061-T6. This result indicates that
the fatigue crack initiation and/or small FCP stage was suppressed by SiCw
reinforcing. The FCP rate of the T-L or T-T oriented SiCp/Al composite is
the same and the fatigue strength of T oriented one is inferior compared to
those of 6061-T6. This result indicates that fatigue crack initiation
and/or small FCP stage is accelerated by SiCp reinforcing. Inferior FCP
behavior as well as fatigue strength in L-T or T oriented SiCp/Al composite
is caused by the aligned clusters of particulates that are produced by
extrusion.

CONCLUSIONS

1. Fatigue strength, as well as tensile strength, is increased by SiC

whisker reinforcing. On the other hand, although the tensile strength is
increased by SiC particulate reinforcing, the fatigue strength is
decreased. Low fatigue strength in SiC reinforced composite is caused by
aligned clusters of particulates.

2. FCP resistance and fatigue crack threshold of the L-T orientation is

enhanced, while those of T-L or T-T orientation is reduced, by SiC whisker
reinforcing. Inferior FCP resistance of T-L and T-T orientations results
from the reduced crack closure level.

3. FCP resistance and fatigue crack threshold of the T-L or T-T

orientation is unchanged, while those of L-T orientation is reduced, by
SiC particulate reinforcing. Low FCP resistance in the L-T orientation is
caused by aligned clusters of SiC particulates.

Acknowledgments - The authors greatly acknowledge Dr. Y. Kobayashi of

Mitsubishi Aluninum Co. Ltd. for supplying the materials.

REFERENCES

Chandler, H.E. (1989), Machining of metal-matrix composites and honeycomb

structures. In:Metal handbook 9th edition, 16, 893-901.
Feest, E.A. (1986), Metal matrix composites for industrial application.
Mater. Des., 7, 58-64.
Lee, E.U. (1990), Crack path morphology in silicon carbide whisker-
reinforced aluminum composite. Metall. Trans., 21A, 1783-1785.
Nair, S.V., J.K. Tien and R.C. Bates (1985), SiC-reinforced aluminium metal
matrix composites. Int. Metals Rev., 30, 275-290.
Ohori, K., H. Watanabe and Y. Takeuchi (1987), Silicon carbide whisker
reinforced aluminum composite - fabrication and properties. Mater. Sei.
Techno1., 3, 57-60.
Signorelli, R.A. (1989), Metal matrix composites. In: Concise encyclopedia
of composite materials (A. Kelly, Ed.), pp. 185-190.
WS7C1
CORROSION FATIGUE CRACK PROPAGATION
IN SQUEEZE CAST Al-Si-Mg-Cu ALLOY

Kazuaki SHIOZAWA*, Junnosuke MIZUTANI**,

Seiichi NISHINO* and Setsuo EBATA***

* Faculty of Engineering, Toyama University,

3190 Gofuku,Toyaraa 930, JAPAN
** Electronic Control Technology Department,
Toyama National College of Maritime Technology,
1-2 Ebie-Neriya, Shinminato, Toyama 933-02, JAPAN
*** Ishikawajiroa-Harima Heavy Industries Co.,Ltd.,
2-2-1 Oteraachi, Chiyoda-ku, Tokyo 100, JAPAN

ABSTRACT

Behavior of corrosion fatigue crack propagation in squeeze cast Al-Si-Mg-Cu

aluminum alloy, AC8A-T6, was investigated under the stress ratio of 0.1,
triangular waveform and testing frequency of 10Hz in 3.0Z saline solution
using the compact tension specimens with side grooves. Corrosion fatigue
crack propagation is affected by the initial stress intensity factor range,
ΔΚΐ, as the experiment was started. Path of crack propagation during
corrosion fatigue showed the dependency on the microstrueture consisted of
the dendrite and eutectic spheroidal silicon. Corrosion fatigue crack
propagated mainly along the eutectic structure and deviations in the path
were larger than those under the test in air.

KEYWORDS

Corrosion fatigue; squeeze cast aluminum alloy; crack propagation; crack

path; microstructure.

INTRODUCTION

Squeeze cast aluminum alloy is expected to apply to machine components

requiring high specific strength, reliability and toughness, because squeeze
casting is developed to obtain pore-free, fine-grained alloy components
having superior mechanical properties over those of conventional permanent
mold casting. Through there are many studies for the relation between
tensile properties and microstructure of squeeze cast aluminum alloy, few
studies about the fatigue strength and crack propagation behavior of this
alloy can be found (Fujii et al., 1984, Ishimaru et al., 1981). The aim of
this study is to clarify the behavior of corrosion fatigue crack propagation
in squeese cast Al-Si-Mg-Cu aluminum alloy.

427
428
MATERIAL AND TESTING METHOD

The material examined in this study was squeeze cast Al-Si-Mg-Cu aluminum
alloy, AC8A-T6. Sample was cast into a plate of 65mm in length and width and
13rara in thickness under 49MPa at 1033K with die temperature 633K, and then
underwent the T6 heat treatment; quenched at 783K for 8 hours, water cooled,
and aged for 8 hours at 433K. The chemical composition was 12%Si-1 .lXMg-
1.1Cu-1.3Ni and the balance with Al. Compact tension specimens with side
grooves were machined to the dimensions of 62.5mm(length) x 60mm(width) X
8mm (thickness). Any difference of micros true ture was not found in all
directions of the specimen. Fatigue tests were carried out using a servo-
hydraulic fatigue machine under a triangular waveform with frequency of 10Hz
and the load ratio, R, of 0.1. The corrodent is 3.0% saline solution
controlled at 298+2K and continuously circulated in a plastic reservoir
through the cell at a flow rate of about 30ral/min. The corrosion fatigue
crack propagation test was started, after making the pre-crack in air and
immersing in the corrodent for an hour without loading, in principle. Crack
extension was measured optically on the side face of the specimen by means
of a traveling microscope with xlOO magnification directed through a glass
window in the environmental chamber. The behavior of crack closure was
monitored by the unloading elastic compliance technique using the back face
strain gauge.

EXPERIMENTAL RESULTS AND DISCUSSIONS

Behavior of Crack propagation in air

The experimental results for fatigue crack propagation rates in air is shown
in Fig. 1 for tests carried out at an R ratio of 0.1. According to the
division of the fatigue crack growth rate curve followed well-established
patterns, Region Π was divided into the three regions, Region H A , Region
Π AB and Resion K B , by the transition points of T A and T B as shown in Fig.
1. In this study, the existence of another transition point was recongnized
at the low ΛΚ of Region Π Α · Therefore, Region Π A was also divided into two
regions of Region Π A and Region Π Α 1 at the point of T A f as shown in Fig.
1. This form pertaining to four lines may be caused by a difference of the
characteristics of crack propagation depending on the microstrueture of
metal.

Behavior of corrosion fatigue crack propagation

Figure 2 shows the experimental relationship between crack propagation rate,

da/dN, and stress intensity factor range, AK, under the test at a frequency
of 10Hz in 3.0% saline solution. The corrosion fatigue crack propagation
behavior was affected by the initial stress intensity factor range, AKi, as
the test was started, so that Fig. 2 was plotted with the parameter of AKi.
It can be seen from this figure that crack propagation rate under the test
 429
In air
1Ö5 1 1 ι 1—|—ι—i—i—r
AC8A-T6
° ΔΚ Λ f.10Hz.
# AKeff
R-0.1

ζ10'
"α
•Ό

10"

1Ö 3 b-

1Ö10I
7 8 9 10
ΔΚ JAPafiri
1 5 10
AKeff MPatfn
Fig.1. Experimental relations between da/dN and ΛΚ or
AKeff for AC8A-T6 aluminum alloy in air at R=0.1.

started at low ΔΚί was enhanced immediately after starting the test and
thereafter was decreased. After that in such retardation as crack propagate
independent on ΛΚ, crack propagated monotonously with increasing ΛΚ. On the
other hand, such enhancement and retardation could not be observed on the
crack propagation rate under the test started at high ΔΚί.

Figure 3 shows the relationship between accelerated crack propagation rate,

da/dN|ace, which occured immediately after starting the test and ΛΚ
corresponding to it. Because enhancement or retardation did not appear under
the test started at AKi=9.7MPam1/2, the initial crack propagation rate was
plotted in this figure instead of the accelerated one (marked * ) . It is
evident from this figure that da/dN|ace was almost constant and independent
on ΔΚ below AK=9MPam1/2. This region occured acceleration belongs to the
RegionΠA* under the transition point of T A * as shown in Fig. 1.

Behavior of crack closure

The relation between the crack opening ratio, U (= (Kraax-Kop) / (Kmax-Kmin)),

and ΛΚ is shown in Fig. 4. This behavior is also affected by AKi in the same
manner as da/dN-ΔΚ. From comparing with U-ΔΚ and da/dN-ΔΚ curves, U
increases with ΛΚ in the region where da/dN is decreased. This behavior is
the contrary tendency to be widely recognized. It is clear from these
experimental results that the decrease or retardation in da/dN can not be
explained by only corrosion product-induced crack closure.
430
In 3%NaCl
, -^ 1
ιυ = ' ' 1 ' · -
- ΔΚί MPa^m AC8A- -T6 -
- Ο 6.7 Ί
1
Δ 7λ
b
1ö 8.3 *g
- · 9.7
D/ D A

107 =-
• γ λ ΐ η air
& 4
~ r ^&Λ
/ N J a air J
■\
-<&
- <j*
^ C^A 4
r> O Δ /^W<^v>Ό Ί

1Ö8 "H
^ag

j
_ da/dN- AKeff da/dN-ΔΚ
1Ö9
MOHz q
R-ai -j
,η10 1 1 1 1 1
7 8 9 10 15
ΔΚ MPa vffi
1 5 10
AKeff MPavFn
Fig.2. Experimental relations between da/dN and ΛΚ or
AKeff for AC8A-T6 aluminum alloy under f=10Hz,
in 3.0% saline solution and R=0.1.

In 3%NaCl
υ10?
= f-10Hz
R-0.1 \
:

*io~' / / ■=

- Q
o /
10c - ■d

I \ l n air J

10 9 . 1 1 . . < '
7 8 9 10 15
ΔΚ MPa vffi

Fig.3. Relation between accelerated crack propagation

rate, da/dN|acc, and ΔΚ at f=10Hz in 3.0% saline
solution.

Shape of crack tip

Behavior of corrosion fatigue crack propagation is affected by not only

corrosion product but also blunting and raicrobranching at the crack tip by
dissolution. In order to explain the enhancement and the retardation occured
bellow AK=9MPam1/2, the optical microscopic observation of tested specimens
 431
In 3%NaCI
■- r i i i 1

ΔΚΐ MPa\/m f=10Hz I

o 6.7 R-0.1 1
0.8 - Δ 7.3 Ί

i. · 8.3 1
a 9.7 Π
0.6
3 1
t-

d ^ i
Γ M \In air
0.4
[
L £$v # AST*·Μ _
0.2 r $>r& Δ
-

1 i i i i 1 i 1 i

~6 8 10 12 14 16
ΔΚ MPav^m

Fig.4. Relation between crack opening ratio, U, and ΔΚ

at f=10Hz in 3.0% saline solution.

was carried out. It was observed that the secondary cracks formed under the
fracture surface at the ΔΚ region where da/dN retarded. And any secondary
cracks were not found above AK=9MPara 1/2 . Therefore it is expected that the
primary factor for the retardation of crack propagation is the decrease of
the stress intensity factor range at the crack tip due to the blunting by
the secondary cracks (Shiozawa et al.,1989).

Crack propagation path

In order to investigate quantitatively the dependency of microstrueture for

crack propagation path, we introduce the value of Sr defined as the ratio of
the sum of crack length along the eutectic structure to the total crack
length observed. Figure 5 shows the relation between Sr and ΔΚ obtained from
experiments in air and in 3.0% saline solution. If crack propagation is not
affected by the microstructure of specimen and propagate along straight
path, the value of Sr is 49.5%. It can be seen from the experimental results
obtained from the test in air that Sr is maintained constant up to
AK=9MPam 1 / 2 and path of crack propagation is independent on microstructure.
At the region of ΔΚ above 9 M P a m 1 / 2 , Sr increases with increasing ΔΚ and
crack propagate preferentially along the eutectic structure. On the other
hand, in the case of corrosion fatigue, change in the value of Sr in
relation to ΛΚ shows a similar tendency to that in air, but Sr is larger
than that in air. The corrosion fatigue cracks are apt to propagate mainly
along eutectic structure and deviation in the path is entirely larger than
that under the test in air because of the preferential stress-assisted
dissolution around eutectic spheroidal silicon (Seri et al., 1987).

CONCLUSIONS
432

100

CO

60

40 /Straight path Sr-49.5%

j L _J | I I
fcV
6 7 8 9 10 11 12 13 14
ΔΚ MPaVm

Fig.5. Experimental relation between Sr and ΔΚ

tested in 3.0% saline solution and in air.

(1) Crack propagation behavior under the test in air is affected by the
micros true ture of specimen and crack propagation rate diagram is divided
into four regions.
(2) Corrosion fatigue crack propagation behavior complexity depends on the
initial stress intensity factor range, AKi, as starting the test.
Enhancement and retardation of crack propagation are observed under the
condition of AKi below 9MPam 1/2 . The primary factor of the retardation is
the blunching by the secondary cracks.
(3) Enhancement of crack propagation rate is occured by the preferential
dissolution around the eutectic spheroidal silicon.
(4) Corrosion fatigue crack is apt to propagate along eutectic spheroidal
silicon, as compared with that in air.

REFERENCES

Fujii, N., M. Fujii, S. Morimoto and S. Okada (1984). Effect of eutectic

silicon size on mechanical properties of AC4C aluminum alloy castings.
IMONO , 56-7, 387-392.
Ishimaru, H. , J. Kaneko and M. Sugamata (1981). Effect of pressure casting
on properties of aluminum alloy castings. Jour. Jpn. Inst. Light Metal,
31-11, 712-719.
Shiozawa, K., T. Asaraoto and K. Miyao (1989). Crack propagation behavior
under low-cycle corrosion fatigue of A7003-T6 aluminum alloy. JSME Int.
Jour. Ser.I, 32-4, 572-580.
Seri, 0. and K.Tagashira , (1987). Effect of silicon in Al-Si alloys on
corrosion behavior in NaCl solution. Jour. Jpn. Inst. Light Metal, 37-3,
185-191.
 WS7c3

QUANTITATIVE EVALUATION OF EFFECTS OF IMHOMOGENEITY

PHASES ON THE FATIGUE STRENGTH OF Al-Si NEW ALLOYS

Y.MURAKAMI*, H.IKEDA** and T.TORIYAMA*

* Department of Mechanics and Strength of Solids,

Kyushu University,Fukuoka,812,Japan.
-x-x-TOYODA Automatic Loom Works,LTD,Aichi,448,Japan.

ABSTRACT

The effects of inhomogeneity phase(IP) such as Si and Al-Fe-Mn in Al-Si

eutectic alloys on fatigue strength are quantitatively evaluated. IPs are
necessary for wear resistance but behave like small defects or nonmetallic
inclusions in fatigue process. The fatigue strength prediction equation
proposed by Murakami et al is successfully applied to predict the scatter
band of fatigue strength of three kinds of Al-Si new eutectic alloys.
It is also suggested that the combination of the fatigue strength prediction
equation with the statistics distribution data on the square root of the
projection area of IPs, farea can be used for the quality control of
materials before the adoption for design.

KEYWORDS

Fatigue; Fatigue Strength; Al-Si Alloy; Imhomogeneity phase; Statistics

of Extreme.

INTRODUCTION

Aluminum alloys are finding increasing needs for machine components and
structures for their weight reduction and anti-corrosion. Particularly
for car industries, the weight reduction in cars is the crucial factor
for the improvement of mileage. Since conventional commercial aluminum
alloys do not have sufficient fatigue strength, it is difficults to replace
steels by them. However, recent development of new aluminum composite
materials is being expected to realize the weight reduction of car body
without decreasing the strength and function(Nakayama et al.,1990). It
is well known that the inhomogeneity phases in alloys cause a large scatter
and reduction in fatigue strength. However, the quantitative evaluation
of the effects of imhomogeneity phases on fatigue strength is considered
to be very difficult, because there are many complicated factors of
imhomogeneities such as shape, size, and location. In the series of previous
researches, Murakami(1989a,b,c), one of the authors, proposed the prediction
method of effects of small defects and nonmetallic inlusions on fatigue
strength of steels by using two crucial parameters, the Vickers hardness
Hv of the matrix and the square root of projection area (farea) of defects
or inclusions. This method has also been successfully used to evaluate

433
434
the upper and lower bounds of a large scatter in fatigue strength of high
strength steels by combining it with the statistics of extremes(Gumbel,1957)
of inclusion size. In this study, we analyze the fatigue strength of
aluminum alloys from the view point of the concept that inhomogeneity phases
in alunimum alloys are virtually equivalent to small defects as well as
nonmetallic inclusions in high strength steels and apply Murakami's
prediction method to Al-Si eutectic alloys which contain eutectic silicon
and Al-Fe-Mn as imhomogeneity phases.

MATERIAL AND TEST METHOD

The materials used in the present study are three kinds of newly developed
Al-Si eutectic alloys which have been recently adopted for piston components
of compressor of car-airconditioner. These are named materials A, B and
C respectively. Table 1 shows the chemical compositions of materials.
Material A was produced by extruded casting, B was produced by extrusion,
and C was by continuous casting. Figure 1 shows the examples of
micro-structures of the materials A, B and C. The primary compositions
of imhomogeneity phases are Si and Al-Fe-Mn. Table 2 shows heat-treatments.
Figure 2 shows the shape and dimension of the specimen for rotating bending
fatigue test. Table 3 shows the mean value of Hv at 10 points of the matrix
(Al) and the imhomogeneity phases (Si and Al-Fe-Mn) (The indentation load
25 g). Rotating bending fatigue testing machines of a uniform moment type
were used (Capacity 98 Nm, 2400 rpm). The maximum size of imhomogeneity
phases fareamax observed in 40 standard unit inspection area So in a
microscope are measured for statistics of extreme by automatic image
processor. The area So is fixed at 0.075 mm2 in the present study.
Table 1. Chemical composition. wt(%)

Sample No. Cu Si MR Zn Fe Mn Ni Ti Sn
A 4.73 13.17 0.60 0.01 0.63 0.52 0.02 0.01
B 3.94 11.55 0.66 0.06 0.26 0.20 0.01 0.01
C 4.30 11.65 0.64 0.05 0.24 0.24 0.01 0.01 0.01

Table 2. Condition of heat treatment.

Sample No. Heat treatment

A 495 "CX0.5 hr -► WQ -+ 230°CX50 min

B 495 °CX0.5 hr -♦ WQ -* 170°CX9 hr
C same as B

Sample A Sample B Sample C

Fig.l Typical examples of inhomogeneity phases.

iii
ΞΜΞ^

Fig.2 Shape and dimension of specimen.

 435
Table 3. Vickers hardness of Al-matrix and inhomogeneity
phases .

Sample No. Al-matrix Si-phase Al-Fe-Mn phase

A(Extrusion) 140 709 526

B(Extrusion) 165 same a s A same a s A
C(Continous 102 same a s A same a s A
casting )

IMH0M0GENEITY PHASES IN Al-Si ALLOYS AS THE FACTOR

INFLUENCING FATIGUE LIMIT

Recent investigations have revealed that fatigue limit of steels is not

the critical stress for crack initiation but the threshold condition for
propagation of cracks emanating from grain boundaries, slip bands or small
defects(Murakami,1989a). In case of nonferrous metals, the fatigue limit
is determined by the same reason as ferrous metals when initial fatigue
cracks start from small defects. Therefore, it is relevant to consider
that the fatigue limit of Al-Si eutectic alloys should be determined by
the threshold condition for propagation of cracks emanating from Si-phases.
Thus, we consider that the imhomogeneity phases are virtually equivalent
to initially existing small holes and small defects so long as the fatigue
limit is concerned. The concept described above has been successfully
applied to predict the fatigue strength of high strength steels containing
inclusions as fracture origin. According to Murakamifs(1989a,b,c) prediction
method, the fatigue strength prediction equations are given as follows
by using two parameters, Hv of matrix and farea of Si-phase.
[Surface inclusion]
a w = 1.43 (Hv+120)/(farea)1/6 (1)
[Inclusion just below surface]
a w = 1.41 (Hv+120)/(farea)1/6 (2)
[Interior inclusion]
a w = 1.56 (Hv+120)/(farea)1/6 (3)
»where the units of the quantities are σ w:MPa, Hv:kgf/mm and [area :μπι

THE DISTRIBUTION OF THE MAXIMUM SIZE OF IMHOMOGENEITY PHASES;

iarea max , IN STATISTICS OF EXTREMES
Predicdtion of farea max of Si-phase and its application

Figure 3 shows the cumulative frequency distributions of the maximum size

y
99.95, T
' 99.9 1000
61- 99.8 L 500 : S0=0.075mm2

99.5 - 200
I- 99.0 - 100

- 50 Q/

20 T = S / S0

- 10
/ o Ϊ

-
1 1
40 60 80 100 20 40 60
/ areamax Um) areamax (urn)
( a ) Sample A (b) Sample B (c) Sample C
Fig.3 Cumulative frequency of the maximum inhomogeneity
phases ((area™., ).
436
Table 4. Predicted value of faream<.x which is expected
to exist in constant area S .

fa reamn« (Mm)
Sample No.
S=l mm2 S=100 mm2
A 90.46 166.3
B 25.94 47.28
C 26.40 48.70

of imhomogeneity phases, i.e. the maximum size of eutectic silicon f area™a x

The linearity of the plotted data indicates that the distribution offarea™a,
of imhomogeneities obeys statistics of extreme. The value of fareamaxof
the Si-phase contained in N specimens with a definite test area S can be
predicted by estimating the return period T as T=NS/S0 in Fig.3(a), where
So is the unit inspection area So . Table 4 shows the predicted value of
fareamaxwhich is expected to exist in a definite area S=l mm2 and 100 mm2
for materials A, B and C. Material A has the largest Si-phase in the same
test area and J~areamaxfor materials B and C are approximately equal but
much smaller than A. Thus, the lower limit of scatter in fatigue strength
of N specimens or machine parts can be predicted with Hv of Al-matrix and
fareamaxOf Si-phase by Eq.(2) like the cases for small defects and
nonmetallic inclusions. The method mentioned above is also useful for
evaluating material quality without conducting fatigue tests.

The guideline for metallurgical size control of imhomogeneity phases in

material making process
Exsting data have shown that the upper limit of scatter of fatigue strength
of steels is approximately proportional to the matrix hardness and is
expressed by an empirical formaula Eq.(4).
o wu eil.6 Hv (4)
,where the units of quantities area wu :MPa and Hv:kgf/mm .
According to the authors * survey of data, Eq.(4) is also available for
nonferrous alloys with sufficient accuracy in practical use. Thus, the
guideline for controlling fareamax of Si-phase to obtain the ideal fatigue
strength of matrix is to refer the value offarea max ato w u = o wa(,i.e.
the upper limit = the lower limit). On the other hand, it must be taken
into consideration that there is another optimum size of Si-phase
appropriate for weare resistance.

RESULTS AND DISCUSSION

S-N curves

Figure 4 shows the S-N curves for materials A, B and C. There is little
300 r

Sample A (Hv-140)]
Sample B "(Hv»165) \ brol·
Sample C (Hv-102)J
o Δ α not broken

I ■ ■ ■ ■! ■ ■ ' ■■■■! I I I Mill

105 10 6 io 7

F i g . 4 S-N c u r v e .
 437
difference between the fatigue limits of material B and C regardless of
large difference in Hv. When a large scatter in fatigue strength or fatigue
life is observed in steels, the fracture origins are frequently at small
defects or inclusions. Therefore, it may be assumed that the scatter in
fatigue life of Al-Si alloys in the presant study should also result from
similar causes such as Si-phases. When there is a large scatter in fatigue
strength, it is unsafe for strength designers to adopt the fatigue limit
determined from S-N curve with limited number of specimens. This is because
the probability of fracture at lower stress level increases with the
increase in number of specimens or machine parts. The basic concept to
overcome the difficulty of this problem and to assure the safety in design
will be proposed in the next section.

Quantitative evaluation of a scatter band in fatigue strength

According to the previous study(Murakami,1990), the prediction method of

the lower limit of fatigue strength for rotating bending fatigue is as
follows. First, in order to predict the value of farea™ax contained in
a definite volume, the inspection unit volume V0 is defined by adding a
small amount of thickness h to inspection unit area So,i.e.V0=S0h. The
appropriate value of h can be calculated by Eq.(5),
h er Zfareamax. J / n (5)
j = I

»where n is the number of inspection area of farea max , say in this study
n=40. In the case of rotating-bending fatigue the test volume V exposed
to possible fatigue fracture involves empirically the part where the nominal
stress o o satisfies o ^ 0.9 # 0. Accordingly the specimen illustrated in
Fig.2 has the test volume V given by the following equation,
V = O.l/cdft (6)
»where d is the diameter of the test part and ß is the length of constant
diameter d. The return period T for N specimens having volume V is given
as follows.
T = NV/Vo (7)
The expected value of fareamax for N specimens is obtained by the procedures
indicated with arrows in Fig.3(a).
Table 5 shows the values of fareamax expected to exist in 10 and 100
specimens of materials A, B and C. The lower bounds of the scatter in
fatigue strength calculated by Eq.(2) are shown in Table 5. Figure 5 shows
the comparison of the experimental results with the lower bound of fatigue
strength. The preditions are in good agreement with the experimental
results. Although Hv of material B is different from that of C, there is
no large difference in S-N curves and fatigue limits for material B and
C. However, Fig.5 reveals substantial difference in fatigue fracture
behaviors between these two materials. Material B has relatively lower
fatigue limit than expected from Hv, because the matrix did not reach the
upper bound value of fatigue strength due to the detrimental effects of
Si-phase. On the ohter hand, material C, having lower Hv, reached the upper
bound value of fatigue strength, because Si-phase with approximately same
Table 5. Predicted values of farea,**, which is expected
to exist in 10 or 100 specimens.

Sample No. N: Number of T(N) faream«, (μπι)

specimens

A (Hv=140) 10 1.923X10^ 247.5

100 1.923X10;? 285.0
B (Hv=165) 10 4.807X10^ 74.34
100 4.807Χ10ς 84.92
C (Hv=102) 10 4.807X10^ 76.99
100 4.807X10° 88.05
438
size as B has no detrimental effects at low range of Hv. The same reason
causes a large scatter of fatigue strength in material B but almost no
scatter in C. Thus, it must be noted that even if the fatigue limits of
two materials are approximately the same, the basic fatigue mechanisms
are not necessarily the same.

CONCLUSIONS
(1) The imhomogeneity phases in Al-Si eutectic alloys behave similar to
small defects or nonmetallic inclusions, i.e. they become fatigue fracture
origins at high range of Hv.
(2) The maximum size of imhomogeneity phase (the maximum size of eutectic
Si)iarea max obeys the distribution of statistics of extremes.
(3) The lower bounds of scatter band in fatigue strength can be predicted
by combining the distribution curve of statistics of extremes of
imhomogeneity phases with the fatigue strength prediction equation for
small defects and inclusions. The predicted values are in good agreement
with experimental results.

• Sample A (Hv=140)
A Sample B (Hv«165)
■ Sample C (Hv=«102)
o Δ a not broken

The upper limit

£ 200

The lower limit of Sample A

fatigue strength
for N specimens Sample B.C
Prediction equation
owUl.41 (Hv+120)/(• aveamax )l,S
i I i i _i_
100 150

Vickers hardness Hv
Fig.5 Comparison of the predicted lower limit of fatigue
strength with experimental results.
REFERENCES

Gumbel, E.J. (1957), Statistics of extremes. Columbia University Press,

New York.
Murakami, Y. (1989a). Effects of small defects and nonmetallic inclusions
on the fatigue strength of metals (Review), JSME, Int.J. Ser.I, 32,
167-180.
Murakami, Y., Kodama, S. and Konuma, S. (1989b). Quantitative evaluation
of effects of non-metallic inclusions on fatigue strength of high strength
steels, I, Int. J. Fatigue, 11, No.500, 291-298.
Murakami, Y. and Usuki, H. (1989c). Quantitative evaluation of effects
of non-metallic inclusions on fatigue strength of high strength steels,
II, Int. J. Fatigue, 11, No.500, 299-307.
Murakami, Y.(1990). Manual for Material Evaluation by New Inclusion
Counting, (Dept. of Mechanics and Strength of Solids, Faculty of Engng,
Kyushu University, ed.).
Nakayama, S., Kurahashi, M. and Takenaka, K. (1990). Development of
forged aluminum alloy piston for automotive air conditioning. J. Jpn.
Inst. Light Metals, 40, No.4, 312-316.
 WS7C4

THE EFFECT OF ARTIFICIAL AGING ON FATIGUE BEHAVIOR IN A

DC-CAST A356 (AlSi7Mg) ALLOY.

J.A.Odegaard *, H.J.Roven ** and K.Pedersen *

* SINTEF, Div. of Metallurgy, Trondheim, Norway.

** The Norwegian Inst. of Techn., Metallurgy, Trondheim, Norway.

ABSTRACT

Fatigue life- and cyclic stress response curves for specimens in four different aging conditions
are obtained from a DC-cast A356 alloy. During aging a change in the precipitation structure
is observed, which affect the fatigue behaviour and the surface crack topography. In near
peak aged condition, coherent ß"-Mg2Si needles are observed. In slightly overaged condition
the precipitate structure consist of a mixture of ß"-needles and semi-coherent ß'-rods. In
overaged condition only ß'-rods were found. Also incoherent Si-precipitates are formed in
the slightly overaged and overaged conditions. These non-shearable Si-precipitates causes a
significant reduction in the slip band formation during cyclic deformation. While in the
underaged and the near peak aged condition coarse slipbands are formed extending through
the grains, only short slipbands adjacent to the primary silicon particles are formed in the
slightly overaged and the overaged condition. Also the fatigue crack growth mode changes
due to the secondary silicon particles. In the underaged and near peak aged condition, crack
growth occurs within PSB's while in the slightly overaged and the overaged condition the
crack growth occurs by debonding of the primary silicon /matrix interface.

KEYWORDS

Al casting alloy; heat treatment; precipitation; fatigue behaviour; initiation; crack growth;

INTRODUCTION

Cast aluminium alloys have a wide range of use as load bearing components in aircraft and
automobiles e.g. wheels, chassis components and suspensions. The demands on the
mechanical properties of these components require high static and fatigue strength combined

439
440

with good ductility. A commonly used alloy which fulfills these requirements and also has
good corrosion resistance is A356 (Honma and Kitaoka, 1984; Inguanti, 1985; Ozelton et
al.,1988). By optimizing the foundry techniques it is possible to reduce shrinkage defects and
the size of pores below which fatigue properties are dependent on the microstructure alone
(Inguanti, 1985). It has been found that fatigue cracks initiate at the silicon particles in the
interdendritic regions, generally at triple points (Odegaard et al., 1990; Plumtree and Shäfer,
1986). In precipitation hardened AlMgSil persistent slip bands (PSB's) are observed to play
an important role in both crack initiation and crack growth (Pedersen, 1986, 1989). The aim
of this paper is to show the effect of different aging conditions on fatigue crack initiation and
fatigue crack growth mechanisms in an A356 (AlSi7Mg) alloy.

EXPERIMENTAL PROCEDURE

Round specimens having 25 mm gauge length and 6 mm diameter were machined from a 150
mm industrially DC cast A356 billet. Table 1 shows the chemical composition of the alloy
(main alloying elements). Other elements are only present as trace elements, except Ti and
B which are used for grain refinement.

Table 1. Alloy composition in weight %.

Si Mg Fe Ti Al

6.1 0.35 0.12 0.17 bal.

The specimens were homogenized 5 hours at 525°C, quenched in cold water and stored at
room temperature for 1 hour before artificial aging in silicon oil bath for 5 hours at 160°C
to produce specimens in the near peak hardness condition and 9 days at 160°C to produce
specimens in slightly overaged condition. To produce specimens in the overaged condition
the specimens were aged at 200°C for 50 hours. Also specimens naturally aged at room
temperature for 1 week, the underaged condition, were tested. The grain size was 300pm,
DAS 20pm, and the average mean Si-particle diameter was 2pm. The material was nearly
free from pores, virtually no pores were observed neither at the specimen surface nor at the
fracture surfaces. After the heat treatment the specimens were mechanically polished with
4000 mesh grinding paper. For further details of the specimen preparation and testing
procedure see (Pedersen, 1986).

RESULTS

Figure 1 shows the hardness curves for specimen aged at room temperature, 160°C and
200°C. The dotted arrows indicate where on the curves the specimens are taken for tensile
and fatigue testing. As seen in Table 2, only a small difference in the yield strength and the
tensile strength is observed for near peak hardness and slightly overaged specimen. Figures
2 and 3 shows the internal microstructure in the peak hardness condition and slightly
 441

overaged condition. In peak hardness condition coherent ßM-Mg2Si needles are formed, while
in slightly overaged condition a homogenous distribution of secondary Si particles is also
found, as seen in Fig.3. The distribution of the Mg2Si- and the Si-precipitates were similar
in both primary aluminium dendrites and in eutectic aluminium. The S-N curves for
specimens given different heat treatments are shown in Fig.4. Slightly overaged condition
have superior fatigue life properties compared to underaged and overaged specimens. Also
the cyclic stress response shows different behaviour depending on aging condition, as shown
in Fig.5.

Specimens in the underaged condition show cyclic hardening until a saturation stress, A
tendency of softening is however observed at the end of the curves. In the near peak
hardness condition cyclic hardening to a peak stress followed by cyclic softening is seen.
Slightly overaged condition show moderate softening until failure. At Δερ=4·10"4 only a
reduction in peak stress of 30 MPa is observed after 17000 cycles. The overaged condition
show a constant stress level until cracks are initiated and failure occurs.

Table 2 - Tensile properties.

Condition Rp0.2 Am Am AB
MPa MPa % %

underaged 130 260 17 24

near peak hardness 230 315 11 16

slightly overaged 260 305 6 9

overaged 175 224 4 11

In both underaged and near peak aged conditions coarse PSB's are formed during fatigue,
while in the slightly overaged condition PSB's were more rarely observed and only adjacent
to the primary Si particles. In the overaged condition very few PSB's were observed.
However, crack initiation took place within PSB's adjacent to the silicon particles in the inter-
dendritic regions in all four aging conditions. In the underaged, and the near peak aged
condition three different fatigue crack growth mechanisms are observed. Fatigue crack
growth occurs within PSB's, by debonding of the aluminium/silicon interface and
perpendicular to the load direction. However, crack growth within PSB's seems to be the
most dominant, see Fig.6. In the slightly overaged and the overaged condition, crack growth
by debonding of the aluminium/silicon interface dominates, see Fig.7.

DISCUSSION

By DC casting of an A356 alloy a material nearly free from defects such as shrinkage and
gas porosities is obtained. It has therefore been possible to study the effect of microstructure
on crack initiation and crack growth without interference from coarse casting defects. The
observed difference in slipband morphology for the different aging conditions is probably due
442

to different precipitate structure. In underaged to peak hardness condition, coherent ß"-Mg2Si

is present. These are easily cut by moving dislocations, and localization of strain into PSB's
extending through the whole grain, occurs. The extensive softening observed in the cyclic
stress response curve also indicate localization of strain into PSB's. The presence of
homogenous distributed secondary Si-particles and semi-coherent Mg2Si precipitates in
slightly overaged and overaged conditions prevent formation of coarse PSB's in matrix. Only
short PSB's are found adjacent to the primary Si particles. The moderate softening observed
in the cyclic stress response for specimen in slightly overaged condition also indicates that
PSB formation is not that pronounced. The reason why the PSB's are formed in silicon
particle rich regions is unclear. One explanation, put forth by Inguanti (1985) for pressure
cast AlSi7Mg alloy, is that the formation of PSB's occurs at the silicon particle/aluminium
matrix interface because of weak precipitation free zones (PFZ) formed adjacent to the silicon
particles. Work carried out by Kvandal (1991), on the same material as investigated in this
work, shows that PFZ's around the silicon particles does not exist. Another explanation could
be that each silicon particle is surrounded by a stress field created during quenching due to
difference in the thermal expansion coefficient for silicon (3 · 10"6/°C) and aluminium
(23 · 10"6/°C). A third explanation is simply that, due to the difference in Young's modulus
between primary silicon (113 GPa) and aluminium (70 GPa), the applied stress gives stress
gradients in silicon particle rich regions which is high enough to cause slip in the material and
to form PSB's. A combination of these two latter theories are truly the mechanisms for
PSB's formation adjacent to silicon particles. The difference in fatigue life depending on the
aging conditions is probably due to the secondary Si particles. In underaged to peak aged
condition cracks are initiated from large PSB's. While in the slightly overaged and overaged
condition only small PSB's are formed adjacent to the primary Si particles. Thus, due to the
high density of incoherent secondary Si particles and semi-coherent ß'-rods, the crack
initiation become more difficult. Also the crack growth mechanism is affected by these
particles. Rapid crack growth at the surface within PSB's formed in front of the crack tip is
observed for specimens in underaged to peak hardness condition. An irregular surface crack
path is seen on the surface, while in the slightly overaged and overaged condition the crack
growth mechanism is debonding of matrix/Si particles and a smooth surface crack path is
formed. Since crack growth within PSB's occurs more rapid than crack growth normal to the
load direction this also increase the fatigue life for specimens slightly overaged.

CONCLUSIONS

An increase in fatigue life is observed for near peak hardness and slightly overaged condition
compared to the underaged and overaged condition. PSB's are observed in all aging condi-
tions at the silicon particles and are probably the mechanism for crack initiation. In
underaged and near peak aged condition fatigue crack growth occurs within PSB's, by
debonding of the aluminum/silicon interface and by growth perpendicular to the load axis. In
slightly overaged and overaged conditions the main mechanism of fatigue crack growth is by
debonding of the aluminium silicon interface. This difference in growth mechanisms can be
explained from the precipitate structure, where matrix in the underaged and the near peak
hardness conditions contains shearable ß"-needles. In slightly overaged and overaged
conditions the precipitate structure consist of non-shearable constituents like ß'-rods and
incoherent Si-precipitates.
 443

ACKNOWLEDGMENT

The authors would acknowledge the support from NTNF and the Norwegian aluminium
industry and their permission to publish this work.

REFERENCES

Honma, U. and Kitaoka, S. (1984). Fatigue Strength and Mechanical Properties of

Aluminium Alloy Castings of Different Structural Fineness, Aluminium 60,
Vol.12, 917-920.
Inguanti, P.C. (1985). Cast Aluminium Property/Microstructure Relationships.
Proc. 17th National SAMPE Technical Conference, Oct. 22-24.
Kvandal, S.(1991). Characterization of Hardening Structures in an Age-
hardenable AlSi7Mg Casting Alloy, M.Sc. Thesis (in Norwegian), The Norwegian
Institute of Technology, Dept. of Physics.
Odegaard, J.A., Hafsäs, J.E. and Pedersen,K.(1990). Fatigue Crack Initiation and
Growth in a DC-cast AlSi7Mg Alloy, proc. FATIGUE 90, Vol.1, 273-278.
Ozelton, M.W., Turk, G.R. and Porter, G.R.(1988). Relationships Between
Mechanical Properties, Composition and Microstructure of the Aluminium
Casting Alloy A357-T6, Techn. for Premium Quality Castings, 81-105.
Pedersen, K.(1986). The Effect of Microstructure on Fatigue Crack Initiation in
AlMgSi Alloys, proc. Aluminium Alloys Their Physical and Mechanical
Properties, Vol.11, 921-928.
Pedersen, K.(1989). Fatigue Crack Growth of Short Cracks in an AlMgSi Alloy,
proc. Advances in Fatigue Science and Technology, Vol.159, 773.
Plumtree, A. and Schäfer, S.(1986). Initiation and Short Crack Behavior in
Aluminium Alloy Castings", proc. The Behaviour of Short Fatigue Cracks,
215-227.

near peak hardness slightly overaged

10 100 1000 10000 100000

Time, (minutes)

Fig. 1. Hardness curves for the material aged at room temperature, 160°C and
200°C.
444

Figure 2. ß"-precipitates from Figure 3. β'- and Si-precipi

peak-aged condition at 200°C. tates from a slightly overaged
specimen (216hrs/160°C).

:
p
• Underage
d
280 -
• Nea
r peak hardnes
s
/^X··
260 -

—. 240 "
- Slightl
y overage
d
- Overage
d
:;;::;:;;:
Q)
X) 160 -
-·..
"Q. ,C
0

is - - ""
2 loo .
W oa - + -Underage
d
_ Δερ = 8 · 10-*
60 - ■ ■Nea
r peak hardnes
s
- · Δε„ = 4 · 10-"
o - Slightl
y overage
d

2 0- x -Overage
d

Cycles Cycles (thousands)

Figure 4. S-N curves. Figure 5. Cyclic stress

response curves.

Figure 6. Near peak aged Figure 7. Slightly overaged

condition. Growth in PSB's. condition. Growth mainly in
the interdendritic region.
WS7C5

Fatigue Notch Characteristics of Commercially Pure Titanium.

K.Takao and K.Kusukawa

Yuge Mercantile Marine College

Yuge, Ehime pref. 794-25 , Japan

ABSTRACT

Fatigue test were carried out on a notched specimen of an annealed commercial-

ly pure titanium under push-pull loading, in order to clarify fatigue notch
characteristics, especially the reason why the metal is extraordinarily insen-
sitive to notch in fatigue. The initiation and initial growth of a crack at
the notch root area were observed successively with optical- and scanning-
electron-microscopes using a replication technique. Observations have shown
that the main crack which leads to final fracture starts propagating only af-
ter one-grain-size cracks initiate at several neighboring grains and join with
each other. Measurements of the crack opening displacements(CODs) have shown
that CODs for cracks to be a starting point of fatigue fracture are small and
unchange almost before joining, however, after joining they vary abruptly and
increase monotonously with a number of cycles. It is suggested that a pure ti-
tanium has a very thick surface layer relating to crack initiation, leading to
extraordinarily low sensitivity to notch. The behavior is mainly attributed
to the strong constraint for microscopic plastic deformation between crystals
due to a few number of slip systems of the metal having hep crystal structure.

KEYWORDS

Fatigue; Titanium; Crack Initiation; Crack Growth; Successive Observation;

Notch Sensitivity; COD.

INTRODUCTION

A commercially pure titanium possesses a higher order of resistance to corro-

sion and is used for apparatus in various chemical plants and heat exchangers.
It is also used, for example, as structural members of deep-sea survey vehicle
and its demand may increase in the future. One of the authors has reported
fatigue characteristics of notched pure titanium specimens, which are (1)
notch sensitivity is extraordinarily low compared to usual metallic materials,
and (2) no non-propagating fatigue crack exists. These peculiar fatigue
characteristics have been explained by introducing the thickness of surface
layer relating to crack initiation (Takao et als..1986. Takao et al..1984 and
1987). A titanium has a very thick surface layer compared to other materials,
and this is the main parameter dominating low notch sensitivity. However, it
is not clear at this time what may happen actually in this surface layer.

In order to make clear the above reason qualitatively and quantitatively, fa-
tigue tests were carried out on a notched specimen of an annealed commercially
pure titanium under push-pull loading which is slightly higher than the fa-
tigue limit. The initiation and initial growth of a crack were observed suc-
cessively with optical- and scanning-electron-microscopes using a replication
technique. The fatigue crack initiation in pure titanium will be discussed.

445
446

MATERIAL AND EXPERIMENTAL PROCEDURES

The material is a commercially pure titanium(JIS TP 28, thickness 2mm). Chem-
ical composition is H;0.001, O;0.078, N;0.007, Fe;0.014, C;0.007, Ti;bal. wt%.
The geometry of a specimen is shown in Fig.l. The drill pit notch with 1.0 mm
in diameter and 0.5 mm in depth was machined. Specimens were annealed at 1073K
for 1 hr. in vacuum and were chemically polished before testing. The mechani-
cal properties after heat teatment are proof stress and UTS are 163 and 317
MPa, elongation 52.3%. An average grain size is 120 ^m.

Fatigue tests were carried out under push-pull loading (stress ratio R=-l,fre-
quency 20 Hz) on a closed loop servo-hydraulic fatigue machine. The stress am-
plitude is 115 MPa which is slightly higher than fatigue limit of unnotched
specimens, 110 MPa. Replicas of a notch root area were taken at pertinent in-
tervals during the test. At each interval, a specimen was kept under static
tensile stress of 25 MPa during replication. The replicas were observed suc-
cessively with optical- and scanning- electron-microscopes. In order to meas-
ure the microscopic crack opening displacement, some of the specimens were
scratched in a pattern of a square grids with a pitch of 0.05 mm and with an
angle of 45 degree to the loading axis in the notch root area. Crack opening
displacement with an accuracy of 0.05 > m can be obtained by measuring the
relative displacement of grid lines at both sides of the crack under the maxi-
mum and minimum stresses during a loading cycle (Nisitani et al . , 1981). The
fracture surface was inspected by SEM.

-1^ H Detail of hole

(a) (b)
Fig. 1. Dimensions of specimen and detail of notch.

RESULTS AND DISCUSSION

Successive Observation

Figure 2(a) shows an example of successive observations in the vicinity of the

notch root. Figure 2(b) are the enlarged SEM miclographs of the area boxed in
Fig.2(a). It seems that crack A (markedi ·) which initiates within one grain,
grows across grain boundary to B, C and D with increasing number of cycles and
the processes of initiation and propagation of a crack are the same as the
ones observed in the other usual metals (Nisi tani et al.. 1981). Detailed ob-
servations, however, indicate that crack A whose tip reaches the boundary does
not grow into the neighboring grain, but joins to another smaller crack in the
same grain, as shown in Fig.2(b). The similar behavior is observed also for
cracks C and D, on SEM. Cracks A and B which initiate independently at N=1.6x
10 join together at N=1.75xl0 . They have joined at N=l.75x10 s but not at N=
5 5

1.7x10s. After joining of cracks A, B, C and D at N=l.75x10 s , they start prop-

agating as a single crack. Therefore, the fatigue crack initiation process of
pure titanium is such that a few cracks which initiate independently at multi-
ple neighboring grains in the notch root region due to the cyclic slip, grow
in each grain and join together to be a starting stage of continuous growth.
Oth.er examples of observations are that cracks initiated at an edge of the
notch which locate much remote from the maximum stressed point,or at the mul-
tiple discrete locations near the edge. These observations suggest that pure
titanium has a thick surface layer relating to crack initiation, leading to
extraordinarily low sensitivity to notch.
 447

N = 1.7x10s N = 1.75x10s
5 pm
(b) SEM micrographs of box b in (a).

Fig. 2. Successive observations of crack initiation process.

Measurements of Crack Opening Displacement

Crack opening displacements were measured sucessively before and after the
crack joining on specimens which have grid pattern scratches at notch roots.
Figure 3 shows the area where crack joining occurs. CODs were measured at
three points, A, B and C as indicated in Fig.4. Figure 5 shows the results of
measurements and crack length versus number of cycles. In this figure, the
broken line indicates the situation before joining to be a single crack. The
steady propagation starts at N=3.5xl0 5 and joining of crack I and II occurs at
the same period. The COD is about 0.5 ßjn before joining and unchanges almost
with a number of cycles. Immediately after joining, however, it increases a-
bruptly and reaches 1.2 μπ\. CODs increase monotonously with number of cycles,
at the later crack propagation stage.
448

0.2 m m

Fig. 3. Measurement location of CODs before

and after joining of cracks.

Fig. 4. Micrographs for measuring COD, areas boxed in Fig. 3.

Number of cycles U10*)

Fig. 5. Variation of CODs and crack length before

and after of crack joining.

Surface-Layer-Thikness Relating to Crack Initiation

The maximum elastic stress at the fatigue limit of a notched member normalized
by the one of an unnotched mumber, has been demonstrated as the function of
the reciprocal of the notch radius as shown in Fig.6, in order to compare
notch sensitivity among various metals(Takao e t a l . , 1987) (Kt:stress concen-
 449
tration factor, Cwlicrack initiation limit and Ciw2:crack propagation limit).
The figure indicates that the more the normalized maximum stress increase from
the dashed horizontal line (maximum sensitivity), the less the sensitivity to
notch at any notch root radius. It is shown that the pure titanium is extraor-
dinarily insensitive compared to other materials. The reason why pure tita-
nium is extraordinarily insensitive, has been explained as follows by intro-
ducing the "surface-layer-thickness relating to crack initiation".

Figure 7(a) shows the schematic illustration of the cracking behavior at a

notch for pure titanium under cyclic stress of Cfwl as well as the curve for
the elastic stess distribution. Fig.7(b) is the similar one for a mild steel.

When a notched mild steel is subjected to the cyclic stress equal to its
fatigue limit (Twl, the fatigue crack which initiates in a grain at the notch
root, propagates into the neighboring grain and finally is arrested to be a
non-propagating microcrack. This cracking behavior is the same as the one for
an unnotched member, therfore, the elastic maximum stress Cfmax is a little bit
higher than CTwO near a notch root.. In other words, the average stress over
the definite region, ds, near a notch root where a crack initiate at tfwl,

1 /p , mm"1

Fig. 6. Comparison of notch sensitivity in fatigue of

metals ( Takao ^t_aL.,1989 ) .

<b>

Fig. 7. Schematic illustrations of Fig. 8. Crack at the start of growth

stress distributions near and the elastic stress
notch root at fatigue limit. distribution near notch root.
450
should be nearly equal to the one of unnotched member, tfwO. We call ds "sur-
face layer thickness relating to crack initiation". For titanium, however, the
fatigue crack does not start growing until joining of cracks in neighboring
multiple grains terminates as discussed earlierCsee Figs.2 and 5 ) . At the fa-
tigue limit, such a joining never occurs (Takao et al.. 1984). Therefor, (Jmax
is higher than ÖwO in order to fulfil the cracking condition at the region
where the stress gradient exist. In other words, the surface-layer-thickness
dt for a pure titanium should be considerably larger than ds for a mild steel.

The experimental results would be compared with above discussion. Figure 8

shows the trace of crystal grains and a crack at notch root area, when
N=1.75xl0 5 , in Fig.2, including a normalized stress distribution versus dis-
tance from notch root divided by notch radius(Noguchi et als.. 1988). A region
indicated by an arrow means where multiple cracks start propagating. The size
xO of the region is about 200 ju.m(x0/j> =0.4). The normal i zed» stress at x0/p=0.4
is about 1.2. On the other hand, for a mild steel S20C(Nisitani et al.. 1990)
G/CS m -1.8 at x/j> =0.4. Thus, it is suggested by this figure that pure tita-
nium has a very thick surface layer compared to a mild steel.

The peculiar behavior of crack initiation is due to the crystal stucture of

pure titanium, hep. Because its crystal structure has a few number of slip
systems, it is difficult to adjust the slip deformation between neighboring
grains compared to bec and fee. In other words, the effect on constraint of
localized strain is much remarkabe. This is a similar behavior to the one of
the material which has two phases, weak phase where crack initiats is sur-
rounded by a hard phase which resists the growth of slip bands or microcracks.
A typical example of two-phase metals is the induction hardened steel in which
martensite is studded with ferrite (Kunio et al., 1979).

CONCLUSIONS

The following conclusions were reached with regard to crack initiation be-
haviors of a notched member of a pure titanium under constant stress amplitude
slightly higher than fatigue limit.
(1) Fatigue cracks initiate nearby multiple grais, join together to be a crack
of a size of several grains,and finally the crack starts growing continuously.
(2) Crack opening displacements are less than 0.7^u.m and almost unchange wi th a
number of cycles before joining. At joining of cracks, however, it increases
abruptly up to about 1.2 )im. CODs increase monotonously with crack growth.
(3) The cracking behavior leads to a very thick surface layer relating to
crack initiation, and gives an explanation why a pure titanium is extraordi-
narily insensitive to notch. This is mainly due to a crystal structure of the
metal, hep, which has less slip systems and the effect on plastic constraint
is remarkable.

REFERENCES

Kunio, T. and K. Yamada (1978). Microstructual aspects of the threshold condi-

tion for non-propagating fatigue crack in mar tensitic-ferritic structures.
In: Fatigue Mechanisms (J.T.Fon, E d . ) , ASTM STP 675, pp. 342-361.
Takao, K. and H. Nisitani (1984). Fatigue crack initiation and notch Sensitiv-
ity of commercial purity titanium. Trans. of JSME., 50-A.453. pp.1049-1053
(in Japanese).
Takao, K., M. Sogoh and K. Matsumoto (1986). Effect of grain sizeon notch sen-
sitivity in fatigue of commercially pure titanium. Trans. of JSME., 52- A,
484, pp.2574-2578 (in Japanese).
Takao, K. and H.Nisitani (1987). Relation between the characteristics of crack
initiation of metals and their notch sensitivity in fatigue. Journal of the
Society of Materials Sience, Japan., 36. 409, pp. 1060-1064 (in Japanese).
Nisitani, H. and K. Takao (1981). Significance of initiation, propagation and
closure of microcracks in high cycle fatigue of ductile metals. Engineer-
i ng Fracture Mechanics.. 15. pp. 445-456.
Nisitani, H., T. Yakushiji and K. Kage (1990). Crack initiation process at a
place with stress gradient in fatigue. Trans. of JSME.. 56-A, 526, pp. 1354-
1359 (in Japanese).
Noguchi, H.,H.Nisitani and H.Goto(1988). Semi -infinite body with a drill hole-
shaped pit under tension. Trans.of JSME., 54-A,501, pp.977-982(in Japanese).
WS7C6

FATIGUE CRACK GROWTH OF AN Al-Cu-Mg ALLOY

IN VARIOUS ENVIRONMENTS

X. Su, H. 0- Guo and D. G. Cao

Institute of Aeronautical Materials, Lab 25
Beijing 100095, P. R. of China

ABSTRACT

Constant-amplitude cyclic loading tests were conducted on center-cra-

cked tension specimens of an Al-Cu-Mg alloy sheet materials of 3 mm
thick nominally. The test environments were: 3-5% sodium chloride salt
water, fog which was atomized from the same kind of salt water source,
fog with sulfur dioxide gas (8.7mg/m 3 ), moist air, and as well as labora-
tory air. Three different minimum to maximum stress ratios, 0.5, 0.1 and
-0.4, were applied.

The marked accelerations of fatigue crack growth rate caused by aggre-

ssive environments were manifested mainly over the lower stress in-
tensity factor ranges. The most detrimental environment tested was salt
water, which was followed by fog, fog with S0 2 , and with little or no in-
fluence of moist air.

Different stress ratios did not vary the effect of the environments on the
fatigue crack growth, in terms of the magnitude of the reduction of the
resistance to fatigue crack growth at given crack growth rates. Negative
stress ratio did not impede the attack of aggressive environments in this
alloy.

KEYWORD

Corrosion fatigue crack growth, Al-Cu-Mg alloy, stress ratio, salt water,
fog, sulfur dioxide, moist air
451
452

INTRODUCTION

Corrosion fatigue crack growth, as well known, is a complex phenome-

non. Many factors can affect the corrosion fatigue crack growth behav-
ior, such as environmental, metallurgical, mechanical and electrochemi-
cal variables.

In this experiment, the effect of two major variables, different environ-

ments and different stress ratios, on the fatigue crack growth of an Al-
Cu-Mg alloy was investigated.

EXPERIMENT PROCEDURE

Materials and Loading

The material tested was a 3 mm thick alclad Al-Cu-Mg alloy. The che-
mical composition was listed in table 1, and mechanical properties in
table 2.

Table 1: Chemical Composition (wt%)

Cu Mg Mn Fe Si Al
4A4 1.60 0.52 0.40 0.22 balance

Table 2: Mechanical Properties

σ ν (MPa) σ ττ (MPa) E (GPa) δ 1 Π ο , Heat Treatment

Y U 1U A
362 464 68 15 T3

Experiments were conducted on MTS 810 servo-hydraulic machine.

Loading frequency was set at 10 Hz in aggressive environments, while
the frequencies of 20-30 Hz were used in lab air. Three different mini-
mum to maximum stress ratios of 0.5, 0.1 and -0.4 were applied. Fatigue
crack lengths were measured by traveling-microscopes on both sides of
the specimens.
 453
Environments

The test sections were contained within sealed PMMA boxes which re-
tained localized environments. The various environments applied were
as follows:

Lab Air. Relative humidity was 30%-40% at 20 - 24 degrees Celsius.

Salt Water. 3.5% sodium chloride was dissolved in deionized water and
the pH values varied from 6.85-8.36. The salt water was pumped from
a reservoir and continuously circulated through a environmental box at
a constant velocity. The specimens were preexposed in salt water for 24
hours immediately before testing.

Fog. Fog was atomized from the same kind of salt water source as de-
scribed above. The condensed liquid volume on a 80 cm diameter collec-
tor was 1 - 2 ml/h. The fog was continuously pressed into a environ-
mental box, then went through a outlet to open air.

Fog with Sulfur Dioxide. Fog was mixed with sulfur dioxide gas first. The
sulfur dioxide content was approximately 8.7 mg/m^.

Moist air. Water evaporation method was used to produce a relative hu-
midity of 80% - 85% inside a environmental box at the temperatures of
20 -25 degrees Celsius. An electronic humidity meter was used through-
out tests to monitor the relative humidity conditions.

RESULTS AND DISCUSSION

Comparison of Fatigue Crack Growth Rates

Figure 1 shows the fatigue crack growth rate data in salt water and in
lab air. It shows the characteristics of the true corrosion fatigue.

The marked accelerations of the fatigue crack growth rate in salt water
environment were manifested mainly at lower ΔΚ ranges, say, below
the ΔΚ of 300 N / m m 3 / 2 . At AfC = 200 N / m m 3 / 2 , the crack growth rate in
salt water was 3 times as high as in lab air. As the ΔΚ increased, the me-
chanically governed fatigue crack growth processes gradually prevailed
and the data converged with that in lab air.

In other environments, although the magnitude of the accelerations of

454
fatigue crack growth rates was different from in salt water, the effect of
aggressive environments was mostly effective at lower ΔΚ values, as
same as in salt water.
10 "q A l - C u - M g Alloy R = 0.1
+ Lab Air f = 20 Hz
0 Salt Water f = 10 Hz

ci o-
■o
*\σ
•Ό

10"

10* "■ 1
10* 10 3
ΔΚ N/mm 3/2

Fig. 1. Comparison of fatigue crack growth rate in lab

and salt water.

Effect of Stress Ratio

Figure 2 shows the results in salt water and in fog with S02 under three
stress ratios. The moist air had no influence at R = 0.1 and -0.4 and lit-
tle influence at R = 0.5. The result in fog was similar to that in salt water.
Therefore, the results in salt water and fog with S0 2 were sufficient to
demonstrate the effect of stress ratio.

As shown in Fig. 2, the three different data sets at R = 0.5, 0.1 and -0.4
are basically parallel to each other along the X-axis. The phenomenon
was as same as in lab air, which showed the closure effect resulted from
different R ratios. The paralleled data means that at given fatigue crack
growth rate the magnitude of the reduction of resistance to fatigue crack
growth, in terms of ΔΚ /ΔΚ was essentially the same under the three
e a
stress ratios. Herein, ΔΚ and ΔΚ is the ΔΚ in aggressive environments
e a
and in lab air corresponding to a given crack growth rate, respectively.

The results explained that changing stress ratio did not vary the effect
of environment attack. The effect of stress ratio on corrosion fatigue
 455
crack growth in this alloy is negligible. And the closure behavior in ag-
gressive environments can be treated as in lab air by effective stress in-
tensity factor concept.

A l - C u - M g Alloy
A l - C u - M g Alloy 10 "'-a + Lab Air f = 2 0 - 3 0 Hz
+ Lab Air f 2 0 - 3 0 Hz 0 Fog + S02 f = 10 Hz
0 Salt Water f 10 Hz

R = 0.5
E E
io-
E
R=0.5 E10-

X»
R=0.1
^10 "

R = -0.4

R-0.1

io' 103
ΔΚ N/mm 3/2 ΔΚ N/mm 3 / 2

(a) (b)
Fig. 2. Effect of stress ratio (a) in salt water and
(b) in fog with sulfur dioxide.

Effect of Different Environments

Because the susceptiveness of the material to a given environment

under three stress ratios were basically the same, so we take the results
obtained under R = 0.1 for an example. As shown in Fig. 3, among the
environments applied, the most detrimental one was salt water, which
was followed by fog, fog with SCL, and with no influence of moist air.

It was interesting that the fatigue crack growth rate in fog with S0 2 was
lower than in pure fog, which was somewhat unexpected. It is generally
considered that the corrosiveness can be enhanced as the acidity of a
media increases. In this case, although it did show that with sulfur diox-
ide addition, the acidity of the condensed liquid increased. The average
pH value was 4.2, while it was 6.8 in pure fog. However, it did not cause
an additional increase of the fatigue crack growth rate and the results
were just contrary, lower than in pure fog.

In a recent experiment, the authors found that the different volume

content of sulfur dioxide in fog could play an important role in electro-
456
chemical reaction processes in this alloy. In that experiment, fatigue
crack growth rate in fog with less S02 (0.4mg/m 3 ) was evidently higher
than in fog with higher S0 2 content (8.7mg/m 3 ). There might be a tran-
sition of making a fresh fatigue crack tip area from active to passive.
However, to understand this problem needs further work.

10- 1 A1 -Cu-Mg Alloy

1 "
-] + Lab Air
j 0 Salt Water
1 X Fog
Δ
1
+*
10-H
Fog with S02
S
J n Moist Air

c 10-
\ 3
o
^
Zfa&i
10-

1
10 "3- T 1 1 I |
oo 22 10 3
3/2
ΔΚ N/mm

Fig. 3. Fatigue crack growth in various environments.

CONCLUSIONS

1. The marked accelerations of fatigue crack growth rate in aggressive

environments were manifested mainly over lower ΔΚ ranges in this Al-
Cu-Mg alloy.
2. Stress ratios did not vary the effect of the environments on the fa-
tigue crack growth, in terms of the magnitude of the reduction of the r e -
sistance to fatigue crack growth at given crack growth rates. Negative
stress ratio did not impede the environmentally caused accelerations in
this alloy.

3. The most detrimental environment tested was salt water, which was
followed by fog, fog with sulfur dioxide gas (8.7mg/m 3 ), and with little
or no influence of moist air.
 WS7d1

A PHENOMENOLOGICAL THEORY FOR TIME-DEPENDENT

FATIGUE CRACK PROPAGATION IN HIGH-STRENGTH SUPERALLOYS

K.-M. Chang
GE Corporate Research and Development, Schenectady, NY, USA

ABSTRACT
A set of mechanistic experiments were designed and performed in Inconel 718 super alloy
to investigate the time-dependent behavior of high temperature fatigue crack propagation.
In the fully time dependent condition, the fatigue crack growth rate appeared to be
equivalent to the sustained load crack growth rate. However, the formation of a damage
zone caused by environmental embrittlement under static stress intensity was found respon-
sible for the acceleration of crack growth under hold-time fatigue cycles. The kinetic of
such a stress oxidation cracking process was thermally activated following an Arhennius
relationship with temperature. A time dependent factor based on the characteristics of
damage zone formation was proposed to unify the fatigue crack growth rate.

KEYWORDS
Fatigue crack propagation, time dependence, sustained loading, Arhennius relationship,
stress oxidation cracking, damage zone, time-dependent factor.

INTRODUCTION
As proposed by Speidel, any difference in fatigue crack growth rate, da /dN, among materi-
als under a cycle-dependent condition, e.g., room temperature and vacuum, is mainly an
effect of elastic modulus. Normalizing the cyclic stress intensity factor, ΔΑΓ, by the elastic
modulus can unify fatigue crack growth rates measured from a wide variety of alloy systems
(Speidel, 1974). Testing parameters, such as fatigue cycle frequency and waveform, play a
negligible role in determining how fast the crack will grow for a fixed ΔΚ. In fact, da /dN
in the stage II, which is usually described by the Paris power law, da /dN = C x (ΔΚ)η, has
been considered to be insensitive to the variation of microstructure and alloy chemistry
(Fine et al., 1979).
When the temperature increases above 500°C , superalloys start to show time-dependent
fatigue crack propagation (FCP). AK is no longer the only decisive parameter for da /dN.
An acceleration of da /dN is observed for a given AK when the fatigue cycle frequency is
decreased below a certain value. Further decrease in fatigue frequency results m faster
da /dN. Eventually the crack growth becomes completely time-dependent with a constant
457
458
da Idt for the extremely slow fatigue cycles (Soloman, 1973). The onset of time-dependent
FCP is dramatically influenced by temperature.

In the present work, a set of critical experiments were designed and carried out to define
fatigue cracking behavior in premium grade Inconnel 718. An empirical theory is proposed
to interpret the phenomena of time dependent FCP observed in high strength superalloys.

EXPERIMENTAL

The superalloy used as the model material in this study is Inconel 718, which has a nominal
composition of Ni-19Cr-18.5Fe-3Mo-5.1Nb-0.9Ti-0.5Al-0.04C. All samples were machined
from a premium grade forging that was used for aircraft engine hardware. A standard heat
treatment: 1025°C/lhr + 720°C/8hr + 620°C/10hr, was applied to all sample blanks. The
one-hour solution treatment at 1025°C dissolved all intermetallic precipitates except iso-
lated MC carbide particles. Recrystallization and grain growth occurred during solutioning
to develop an equiaxed grain structure of ASTM 7 (35 μΐτι). Subsequent double-aging
formed coherent 7" (Ni 3 Nb, DO22 type) precipitates to provide alloy strength. The tensile
data measured at 650°C were as follow: .2% yield strength, 1020 MPa; tensile strength,
1185 MPa; elongation, 29%; and reduction in area, 45%.

Single-edge-notched (SEN) plate type specimens with a gage section of 1.9 mm thick and
10 mm wide were employed to measure crack growth rate. The dc potential drop tech-
nique was utilized to monitor crack length during the test. The measured potential drop
across the crack was recorded and converted into crack length by a microprocessor that
commands the servohydraulic system to control the load level for a specific stress intensity
on the specimen. Such a smart system permitted the FCP test to be run under a constant
stress intensity mode. The detailed experimental setup and the FCP testing procedure have
been reported elsewhere (Chang, 1987a).

Two types of crack growth testing were performed at temperatures from 500° to 700°C.
The first type was simply the sustained loading at a constant stress intensity to measure
da /dt at various temperatures. The static crack growth rate was an important reference
parameter for time dependent FCP. The second type consisted of the sinusoidal 3-second
fatigue cycle and different lengths of hold time at the maximum load. The time dependent
FCP behavior was characterized and compared with the sustained loading crack growth. In
all cases the_constant K mode was employed, and the maximum stress intensity was kept at
26.5 M P a v m . To examine the environmental effect, some specimens were tested in a high
temperature vacuum chamber. The vacuum system used a mechanical pump and a cryo-
pump to keep the vacuum better than 10"6 torr throughout the test.

RESULTS AND DISCUSSION

Sustained Loading Crack Growth

The static crack growth rate, da jdt, was measured at 540°, 590°, and 650°C in air under a
constant K. Every crack growth curve shows an incubation period before reaching to a
steady crack growth. As expected, a high value of da jdt is obtained at high temperatures.
The Arhennius relationship, da jdt - C x exp (-Q /RT), has been verified by plotting
log (da /dt) against 1/T in Figure 1, where T is the absolute temperature. The slope of the
line in Figure 1 corresponding to the thermal activation energy; the regression analysis
gives a Q value of 61.0 kcal/mole.

To consider the sustained loading da /dt as the creep crack growth is a mistake. A similar
test was performed in vacuum chamber following the same procedure as that in air. No
detectable da /dt was observed for a static loading up to 400000 seconds. At the highest
testing temperature 700°C, Inconel 718 may lose phase stability (Barker, 1970).
 459
790 650 6 0 550 50Q
E-5 F , ?
1' 1
|I_N 718| |

''0.
I
ίΕ-7
§,
5 t
OE-8
o a.
E-9 1 .1 1 _1 J_ ]_..I_J_I _l. _ I l___I
_ 1__ I 1 1 1 I I I ' .1 I

1.05 1.1 1.15 1.2 1.25 1.3

1/TEMPERATURE, 1000/K

Fig. 1 Constant K sustained loading crack growth rate in air.

Since the sustained loading crack growth, da /dt, only appears in air, environmental attack,
notably by oxygen, is believed to dominate the cracking process. Such an environment
assisted process can be defined by the term "stress oxidation cracking".

Time Dependent FCP

Figure 2 shows constant AK crack growth rate, da/dN, measured in air for various tem-
peratures and hold times. The hold times at each temperature were chosen to give crack
growth rates within a similar range. The degree of time-dependence at a given tempera-
ture increases gradually with the length of hold time. Eventually a linear relationship is
established when the hold time reaches above a critical value; i.e., the crack growth is fully
time-dependent.

E-4

r
: 0 811K /*
• X 866K f
|E-5
Q 1
El X 866K )·'
: + 922K
z
E-6 /x
σ +
(i
n UN 718
E-7 L__| 1 I Hill 1—l_l_LJMX 1—1 1 1 l l l l 1 1 t mnl 1 J _JIMU
I

0.1 10 100 1000 10000

HOLD TIME, s

Fig. 2 Constant AK fatigue crack growth rate in air.

460
Mathematically the da/dt data in Figure 1 can be employed to estimate da/dN in time
dependent conditions by a formula, da /dN - da /dt x At; At is the period of fatigue cycles.
The calculated results plotted in Figure 2 as broken lines indicate that time dependent FCP
has a good correlation with the sustained loading crack growth. However, there is no direct
evidence to conclude that the acclerated crack growth in fully time dependent conditions is
simply a consequence of sustained loading crack growth.
If a fatigue cycle consists of a long hold time, the monitoring microprocessor has enough
time to read the potential drop continuously and to calculate the instantaneous crack length
within one fatigue cycle. Figure 3 is an example of an air test with a 1000-second hold time
at the maximum load of each fatigue cycle. The testing temperature was 590°C. Under
this condition, the crack growth rate was measured about two order of magnitudes faster
than the minimum da /dN as seen in Figure 1. The crack length is plotted against the time
instead of cycle number so that the crack growth pattern within one fatigue cycle can be
examined. A stairway-like crack growth curve consists of the steady crack length for 1000-
seconds, and the abrupt jump in the crack length at every 1003 seconds. The sudden
increase in crack length is caused by the fatigue portion, i.e., unloading and loading, in one
cycle. The long hold time of sustained loading contributes a negligible part of total crack
growth.
The above observation overthrows the superposition idea of how the crack advances during
the hold time fatigue cycles. In the fully time dependent situation, the measured da /dN is
equal to the calculated value da /dt x At. Physical increment of crack actually occurs in the
cyclic portion of the waveform.
Damage Zone Model
The fast da /dN measured in air under a time-dependent testing condition can been satis-
factorily explained by the damage zone model (Chang, 1987b). The status of material
ahead of the crack tip where the cracking is to take place plays a dominant role in defining
the crack growth rate. Air environment interacts dynamically with the alloy through the
crack tip. Such environmental embrittlement generates a localized zone just ahead of the
crack tip, and the damage zone allows the crack to grow at an accelerated rate with subse-
quent fatigue cycles.
The kinetics of a damage zone formation ahead of crack tip have been successfully esta-
blished (Chang, 1988). The emperical size of damage zone developed under various
400 T
IN 718 +
590C/3+1000s/AIR
R = 0.05 -hinmHl
<o 300
!

"5)200+
c

S ioo+
da/dN = 4 E - 5 m/cycle

2000 -+-
4000 -+-
6000 -+-
8000 -+-
10000
TIME, s

Fig. 3 Crack growth behavior tested by hold-time fatigue cycles.

 461
Table 1. Comparison of the sustained loading crack growth rate, da /dt, and
the propagation speed oLthe damage zone, dD /dt, in Inconel 718
superalloy (26.5 MPav m in air).

Temperature: 540°C 590°C 650°C

-9 8
da/dt,m/s: 5.0 xlO 5.8 xlO" 4.8 xlO"7
6.9 xlO"8
dD /dt, m /s: 5.1 x lO'9 5.8 x 10"8 4.2 x lO'7
periods of sustained loading at different temperatures can be best fitted by the following
equation, D - Kxtxexp (-Q /RT), where K is a constant, t is the period of sustained load-
ing, and an Arrhenius relationship is used for the temperature. The activation energy, Q, of
58.7 kcal/mole obtained from a regression analysis is equivalent to the value measured
from the sustained loading crack growth, da/dt. An activation energy of 60 kcal/mole has
been reported for the oxidation of nickel-base superalloys at high temperatures (Rhee,
1970). This observation reconfirms that the time-dependent FCP in superalloys is indeed a
result of dynamic environmental embrittlement forming damage zones.
The data also suggests that the environmental damage is propagating at a constant speed,
dD /dt, at a given temperature. Table 1 compares the values of dD /dt and da /dt, the sus-
tained loading crack graowth rate, at various temperatures. Within the experimental accu-
racy, two sets of data are identical.

Phenomenological Theory
The formation of a damage zone in front of the crack tip is the key to understanding the
time-dependent cracking behavior in air. Consider hold time fatigue cycles applying on a
crack in air. During the hold time, the crack may or may not grow depending upon the
incubation period at the test temperature. Nevertheless a damage zone is built up in front
of the crack tip. The formation of damage zone is at a speed equivalent to the sustained
loading crack growth rate. After the hold time, the crack receives the subsequent cyclic
stress intensity (unloading and then loading). A substantial crack increment results from
fast crack growth in the damaged zone. The physical process of crack growth under time

E-4r

PEPENDENT
GOVERNED

E-7
-38 -36 -34 -32 -30 -28 -26
TD, ln(t)-Q/RT
Fig. 4 Crack growth rate normalized by the time dependent factor, TD.
462
dependent conditions includes damage zone buildup, accelerated cyclic crack growth, and
sustained loading crack growth, if there is any.
Define the time dependent factor as TO -In (t) - Q /RT, where Q is the activation energy
for the formation of damage zone, t is the hold time of fatigue cycle, and T is the absolute
temperature. Figure 4 replots the measured crack growth rate in Figure 2 against the time
dependent factor. All data fall on one curve, that is defined by two straight lines. The hor-
izontal line with a constant crack growth rate represents the cycle dependent domain.
Cyclic stress intensity, AK, is the predominant parameter. The other line obtained from
sustained loading crack growth data represents the time dependent domain. Static stress
intensity, Kmsx determines the growth rate.

CONCLUSION
A phenomenological theory based on stress oxidation cracking has been established to
characterize crack growth behavior of high strength superalloys in air. Fundamental con-
cepts verified by experiments are as follows:

1. Environmental embrittlement occurs at the crack tip through the formation of a

damage zone during sustained loading. Subsequent cyclic loading would cause a
large crack increment in the damage zone.
2. The propagation speed of damage zone is the same as the sustained loading crack
growth rate. Both follows the Arhennius relation with temperature.
3. Time dependent FCP, da jdN, can be correlated with the damage zone speed by sim-
ple multiplication with hold time.
4. Employing the time dependent factor, TD = ln(t)-Q/RT, can unify the crack
growth rate data in one curve.

REFERENCES

- Chang K.-M. (1987a) Time Dependent Fatigue Crack Propagation in Inconel 718
Superalloys. In: Mechanical Behaviour of Materials - V, Vol II (M.G. Yan, et. al., Ed.),
Pergamon Press, Oxford, 1139-1147.
- Chang K.-M. (1987b). Elevated Temperature Fatigue Crack Propagation after
Sustained Loading. In Effects of Load and Thermal Histories on Mechanical Behavior of
Materials (P.K Liaw et al, Ed.), AIME-TMS, 13-26.
- Chang K.-M. (1988). An Emperical Model for Environmental Damage at the Crack
Tip. In: Materials Stability and Environmental Degradation (A. Barkatt, et. al., Ed.),
Mat. Res. Soc. Symp. Proa, 125, 243-252.
- Fine M.E. and R.O. Ritch (1979). Fatigue-Crack Initiation and Near-Thresheld Crack
Growth. In: Fatigue and Microstructure (M. Meshii, Ed.), ASM, Ohio, 245-277.
- Rhee S.K. and AR. Spencer (1979). Oxidation of Commercial High-Temperature
Alloys. Met. Trans. A, I, 2021-2022.
- Solomon H.D. and L.F. Coffin (1973). Effects of Frequency and Environment on
Fatigue Crack Growth in A286 at 1100°F. In: Fatigue at Elevated Temperatures, ASTM
STP 520, 112-122.
- Speidel M.O. (1974). Fatigue Crack Growth at High Temperatures. In: High-
Temperature Materials in Gas Turbines (P.R. Sahm and M.O. Speidel, Ed.), Elsevier
Sei., New York, 207-255.
 WS7d2

THERMO-MECHANICAL FATIGUE OF A COATED AND

UNCOATED NICKEL-BASED ALLOY

J. Bressers*, J. Menigault^, and T. Rhys-Jones^

1. Institute of Advanced Materials, Joint Research Centre, CEC,

P.O. Box 2, 1755 ZG Petten, the Netherlands.

2. Now with Sollac-Dunkerque, CRDM, P.O. Box 2508, 59381

Dunkerque Cedex 1, France

3. Materials and Mechanical Research, Rolls Royce plc, P.O. Box 3,

Filton Bristol, BS 12 7QE, U.K.

ABSTRACT

Out-of-phase thermo-mechanical fatigue (TMF) tests on a coated and bare nickel-based alloy
were performed. Initial findings indicate that the nickel aluminide coating reduces the TMF life
of the high temperature alloy for applied mechanical strain ranges < 0.80 percent; for strain
ranges in excess of this maximum value the coating has little to no effect on the fatigue
resistance of the material. This result is a consequence of the differing modes of deformation
which are active above and below this critical value. Specifically, for mechanical strain ranges
> 0.80 percent the mode of deformation is heterogeneous; whereby the TMF life is controlled
by slip along glide planes and the cutting of the γ' phase. For applied strain ranges < 0.80
percent the alloy deforms homogeneously. Dislocations are not limited to glide planes, no
cutting of y is evident and fracture typically occurs in a direction perpendicular to the stress
axis. In addition, Manson-Coffin stress data reveals the existence of a fatigue limit at
approximately 550 MPa.

KEYWORDS

Thermo-mechanical fatigue, advanced nickel-based alloy, fatigue limit, mode of deformation,

stress-strain response, nickel-aluminide coating

© Rolls-Royce plc 1990

I. INTRODUCTION
Thermo-mechanical fatigue testing is currently being used to aid in the design of several gas
turbine engine components. Depending on the test system geometry, TMF testing is quite
successful in approaching the strain-temperature histories of critical volume parts in actual
systems; this salient point is crucial when attempting to identify and explain material behavior
during such combined cyclic profiles. Recent studies (Cook et al.y 1988; Marchand et al.,
1988) have elucidated upon the general feeling that isothermal fatigue (IF) testing, although a
viable technique, may not allow for a thorough materials analysis when attempting to predict an
463
464

alloys response to an actual in-service history. This feeling is sometimes expressed due to the
lack of versatility of the IF test itself. Two examples of such shortcomings are 1) the inability to
observe the effects of dephasing the temperature and mechanical strain as well as 2) the inability
to examine what effects the brittle/ductile transition of the coating has on the fatigue life when
the coated alloy is tested isothermally. Thus, the following TMF procedure was devised so as
to facilitate a better understanding of the advanced nickel-based alloys response to an
environment closely related to the one in which it must soon function without failure.

Π. EXPERIMENTAL PROCEDURE

II. a. Material

The material examined in this study is a single crystal, nickel-based alloy of gas turbine blade
quality. The main alloying elements are Co, Cr, Al, Ti, Mo, and V, respectively. The
orientation of the long axis of each test specimen is within 12° of the <100> direction. All
surface coatings are applied by a pack aluminizing process; initial work in this area (Goward et
aL, 1967: Redden, 1968) provides an excellent overview in relation to nickel-based
superalloys. The microstructure of the alloy consists of two different sized γ precipitates,
embedded in a γ matrix; the first Y morphology is typified by large cuboids (500 nm) whereas
the second type is characterized by small spheres whose radii are approximately 45 nm.

II. b. TMF Testing

The nickel-based alloy is subjected to simultaneous mechanical strain and temperature cycles.
The computer controlled variation of the temperature with time follows a triangular waveform
between 300 and 1050° C, increasing and decreasing between the two temperature limits in 30
and 60 seconds, respectively. The respective heating and cooling rates of 25° C/s and 12.5° C/s
are a compromise between an acceptable spatial temperature gradient on the one hand and high
linear rates of change of temperature approaching service conditions on the other hand. The
temperature at any one point of the 9.0 mm gauge length of the specimen is typically within ±
12° C of the average temperature, corresponding to a maximum thermal strain gradient of about
2 x 10~4. These temperature/thermal strain cycle conditions are achieved by means of a flat,
solid specimen with a rectangular cross section coupled with high frequency induction heating.
By means of a special coil design and forced air cooling, the system is optimized in order to
realize a hysteresis free temperature-thermal strain history. For the tests reported here the
mechanical strain is dephased -135° from the temperature resulting in a counter clockwise
diamond shaped mechanical strain-temperature relationship which simulates the history of gas
turbine blades during operation. The applied mechanical strains ranged from 0.55 to 1.40
percent. In each case the R value, or the ratio of the minimum to the maximum applied
mechanical strain, was set equal to zero.

ΠΙ. RESULTS AND DISCUSSION

III, a. Stress-Strain Response

A plot of log mechanical strain versus log number of cycles to failure (Nf) is shown in Fig. 1.
An initial inspection reveals that the response to the TMF history is parabolic in nature;
whereby decreases in the applied mechanical strain range of 0.20 to 0.30 percent yield drastic
increases in fatigue life. It is also seen that the material's ability to endure the applied thermo-
mechanical fatigue history is decreased by the presence of the coating; this characteristic
 465

Δ uncoated
A coated
bo

J Α.,,.,.,,,-rJ

] A Δ Δ
A

1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 I

100 1000 10000 100000

logNf

Fig. 1. Manson-Coffin plot of the mechanical strain range vs. Nf

is most prevalent when the mechanical strain range (Ae m ) is less than approximately 0.80
percent; above this level the nickel aluminide coating does not appear to affect the TMF life.

Due to the nature of the mechanical strain - temperature phasing, each sample realizes it's
maximum and minimum stresses at 487 and 862 °C, respectively. The evolution of these two
stress values varies relative to the magnitude of the applied mechanical strain, both in the coated
and uncoated conditions.

It is observed that when Ae m > 0.80 percent, both the maximum and minimum stresses are
typified by rapid changes early on in the TMF life; this is followed by a region of stability
known as the stress saturation regime or SSR. In particular at 487 °C the material undergoes
significant cyclic tensile softening, whereby the maximum and minimum stresses decrease by
approximately 20 percent in magnitude in the first few cycles. Once inside the SSR, stress
response stabilizes between the values of 570 and 680 MPa. At 862 °C the material exhibits
cyclic compressive hardening. Specifically, this minimum stress increases in magnitude by 85
to 100 percent, again within the first few cycles. Once within the stabilized stress region, the
minimum stress values range from -600 to almost zero MPa.

For Ae m < 0.80 percent, the observed maximum and minimum stress response is quite
different. Specifically, neither cyclic tensile softening nor compressive hardening is displayed,
respectively. Rather the maximum and minimum stresses remain relatively constant in the
portion of TMF life from 0.05Nf to 0.50Nf. Afterwhich there begins a gradual but persistent
degradation of their magnitudes up to about 0.90Nf. Failure then occurs by a rapid degradation
of the magnitudes of stress followed by catastrophic failure. These results are in general
agreement with recent findings (Malpertu and Remy, 1988) which indicate that the peak stress
amplitude remains relatively unchanged throughout the TMF life of the nickel-based superalloy
466

IN 100; this high temperature alloy was tested for mechanical strain amplitudes of 0.20 to 1.00
percent and in the temperature range of 600 to 1050° C.

Based on these findings it appears that a boundary exists, namely at 0.80 percent, which
separates two regions of quite different material response to the TMF history. This point will
be elucidated upon in the following sections.

1200
% 1o uncoated II
1100
1000 1 o
• coated

900 ~\ -vu- "J" — φ - O

800
• o
700
600 *■ w "1
o-^
500
400
300
200
100
0 I 1 ■ 1 1 ■ I 1 1 1 1 1 1 1 1 1 1 1 ■ 1 I 1 111

10000 100000

logNf

Fig. 2. Manson-Coffin plot of the stress range at mid-life vs. Nf.

Figure 2 shows the magnitudes of the stress ranges at mid-life versus Nf for both coated and
bare specimens. As is the case for the first Manson-Coffin plot, Fig. 2 reveals that the nickel
aluminide coating has a degradative effect on the TMF life of the alloy in question. This finding
is most prevalent for stress ranges below approximately 800 MPa; above this stress range, the
coating does not have much of an effect. The Manson-Coffin data above also reveals the
existence of a "fatigue limit" at approximately 550 MPa.

ΙΠ. b. Microstructural Analysis

Transmission electron microscopy (TEM) observations of thin foils taken close and parallel to
the fracture surfaces of the test samples reveal two distinct dislocation structures, giving
evidence of two different modes of deformation of the bulk. In both coated and bare samples,
which are tested at mechanical strain ranges of Ae m > 0.80 percent, the dislocation motion is
confined to {111} glide planes producing fracture surfaces parallel to the active (111) glide
plane, Fig. 3. This heterogeneous mode of deformation involves cutting of the γ particles
which produces dislocation pairs and stacking fault contrasts. The shear strains produced at the
interface of the glide planes and the coating causes the brittle coating to crack. Hence the origin
of the catastrophic failure is the heterogeneous mode of deformation. At mechanical strain
ranges of Ae m < 0.80 percent both the coated and the bare samples deform homogeneously.
 467

Fig. 3. Transmission electron micrograph depicting heterogeneous

mode of deformation. The applied mechanical strain range is
1.00 percent.

This is substantiated by the absence of dislocation cutting of the γ particles and by the
development of a dislocation microstructure which consists of dislocation networks wrapped
around theY particles, forming as the result of the homogeneous mode of deformation, Fig. 4.
The homogeneity of the deformation leads to fracture surfaces which are, in general, oriented
perpendicular to the stress axis. The change over in the mode of deformation and failure around
Ae m = 0.80 percent is also reflected in the steep increase in crack density beyond this strain
range.

The observations imply that the mechanism which controls the TMF life at Ae m levels in excess
of approximately 0.80 percent is the concentration of slip in planar {111} glide bands,
irrespective of the presence of the coating. Hence the coating itself should have no effect on the
TMF life, which is sustained by the experimental results. For strain ranges of A e m < 0.8
percent the coating brittleness promotes early crack initiation relative to the bare specimens.
Subsequent crack tip oxidation, which locally depletes the alloy of strengthening elements
(Boismier and Sehitoglu, 1990) and stress concentration drive the crack to catastrophic growth.
The presence of the coating hence reduces the cyclic life relative to the life of the uncoated
material.
468

Fig. 4. Transmission electron micrograph depicting homogeneous

mode of deformation. The applied mechanical strain range is
0.55 percent.

IV. CONCLUSIONS

Thermo-mechanical fatigue tests performed on a coated and bare advanced nickel-based alloy
yield the following results. The alloy exhibits a fatigue limit at a stress value equal to
approximately 550 MPa. It is determined that the nickel aluminide coating significantly reduces
the TMF life of the material below mechanical strain ranges of 0.80 percent; above this strain
range no effect on TMF is observed. This result is believed to be directly related to the various
modes of deformation active within each strain range. Specifically, for applied mechanical
strain ranges > 0.80 percent the mode of deformation is heterogeneous and the TMF life is
controlled by strain exhaustion on crystallographic slip planes. Below this range, however, the
material is seen to deform homogeneously, whereby the brittleness of the coating promotes
earlier crack initiation relative to the uncoated material.

V. REFERENCES

Boismier, D.A. and H. Sehitoglu (1990). Thermo-Mechanical Fatigue of Mar-M247: Part 1-

Experiments. / . of Eng. Math., 112. 68-79.
Cook, T.S., K.S. Kim and R.L. McKnight (1988). Thermal Mechanical Fatigue of Cast Rene
80. In: Low Cycle Fatigue, ASTM STP 942 (H.D. Solomon, G.R. Halford, L.R. Kaisand,
and B.N. Leis, eds.), 692-708, American Society for Testing Materials, Philadelphia.
Goward, G.W., D.H. Boone and C.S. Giggins (1967). Formation and Degradation
Mechanisms of Aluminide Coatings on Nickel-Base Superalloys. Trans, of the ASM, 60,
228-241.
Malpertu, J.L. and L. Remy (1988). Thermomechanical Fatigue Behavior of a Superalloy. In:
Low Cycle Fatigue, ASTM STP 942 (H.D. Solomon, G.R. Halford, L.R. Kaisand, and
B.N. Leis, eds.), 657-671, American Society for Testing Materials, Philadelphia.
Marchand, N., G.L. Esperance and R.M. Pelloux (1988). Thermal-Mechanical Cyclic Stress-
Strain Responses of Cast B-1900 + Hf. In: Low Cycle Fatigue, ASTM STP 942 (H.D.
Solomon, G.R. Halford, L.R. Kaisand, and B.N. Leis, eds.), 638-656, American Society
for Testing Materials, Philadelphia.
Redden, T.K. (1968). Ni-Al Coating-Base Metal Interactions in Several Nickel-Base Alloys.
Trans. Mettal. Soc. of AIME, 242, 1695-1702.
 WS7d3

MONOTONIC AND CYCLIC PLASTIC BEHAVIOUR OF

AUSTENITIC STAINLESS STEELS ALLOYED WITH NITROGEN

Suzanne DEGALLAIX, Abdelhamid SOUSSAN and Gerard DEGALLAIX

Laboratoire de Mecanique et Materiaux, (rattache au L.M.L.)

I.D.N., B.P. 48,59651 Villeneuve d'Ascq Cedex, F.

ABSTRACT

This paper summarizes certain results of our studies of interstitial nitrogen effect on the
monotonic and cyclic plastic behaviour of type 316L-316LN austenitic stainless steels at
room temperature. Nitrogen alloying leads to solid solution hardening, explained
essentially by a "pinning effect" as predicted by the Friedel model. The monotonic strain
hardening behaviour is correctly described by the modified Ludwik model proposed by
Ludwigson. The evolution of the numerical modelling with the nitrogen content is
explained by the strong interaction of nitrogen atoms with the dislocations. In low cycle
fatigue (LCF), the influence of nitrogen on the dislocation slip mode is the essential
parameter. Planar or at least simple slip favoured by nitrogen improves the dislocation
slip reversibility and consequently the strain reversibility, involving a better LCF life.

KEYWORDS

Austenitic Stainless Steels. Nitrogen. Monotonic Plasticity. Cyclic Plasticity.

INTRODUCTION

The current interest in "High Nitrogen Steels" is well shown by the success of the recent
conferences HNS 88 (Lille, France, 1988) and HNS 90 (Aachen, Germany, 1990). In the
particular case of the austenitic stainless steels, interstitial nitrogen alloying is used in
order to assure the metallurgical stability of the austenite phase and to improve the
monotonic mechanical properties, at room as well as at high and low temperature
(review papers, Degallaix et al., 1987,1988a). More recent studies (Degallaix et a\., 1989)
have shown that the cyclic mechanical properties of these steels are also improved by an
interstitial nitrogen addition, whatever the temperature. In the present work, we analyse
and try to explain the role of nitrogen solutes in the monotonic and cyclic plastic strain
behaviour of 316L-316LN austenitic stainless steels at room temperature.

469
470
MATERIALS AND EXPERIMENTAL PROCEDURES

We studied four type 316L-316LN austenitic stainless steels, noted respectively A,B,C
and D. The compositions and grain sizes are given in Table 1. It should be noticed that
their compositions are essentially the same, except for the nitrogen content, which varies
from 0.03 to 0.25 wt %.

Table 1. Chemical compositions (wt%) and grain sizes (urn).

steel C N Ni Cr Mo Mn Si grain size

A 0.020 0.029 11.50 16.90 2.02 1.66 0.51 45

B 0.026 0.080 11.54 17.10 2.19 1.54 0.62 135
C 0.014 0.120 13.13 18.84 3.35 1.72 0.38 110
D 0.024 0.250 12.98 17.01 2.62 1.59 0.65 100

Before machining, the hot-rolled, 25 mm square sectioned bars of the four steels were
solution treated for one hour at 1373K and then water-quenched. This heat treatment was
performed in order to have carbon and nitrogen as interstitials.

Tension and low cycle fatigue (LCF) tests were carried out on a servohydraulic testing
machine. The specimens were cylindrical and button-headed, and the total axial strain
was controlled with a strain-gauge extensometer, on a 10 mm diameter and a 10 (LCF) or
25 (tension) mm gauge length.

The tension tests were performed on steels B, C and D with a nominal total strain rate £ t =
4.10~3 s"1. The LCF tests were performed on the four steels in a fully reversed push-pull
mode, applying a triangular form signal. They were conducted with the same total strain
rate at the applied total strain ranges A£t = 6.10~ 3 ,10~ 2 ,1.6.10" 2 and 2.5.10"2 (two tests at
each level), up to rupture.

RESULTS AND DISCUSSION

Monotonie Plastic R o w Behaviour

The tensile mechanical properties of the steels B, C and D, yield stresses (YSQ.02%' ^$0.2%)
and ultimate tensile stress UTS, are plotted versus the nitrogen content in Fig. 1. They are
roughly linear functions of the nitrogen content. This is in good agreement with the
results of other works (Pickering, 1978; Norström, 1977). We previously explained this
linear effect (Soussan et ah, 1990) by the influence of nitrogen on the short-range stresses
acting on the dislocations, essentially due to a "pinning effect" in the FCC alloys (Friedel's
model, 1967), i. e. essentially due to short-range interactions between solutes and
dislocations.

From the recordings of loads and strains during the tensile tests, true stresses (σ) and true
plastic strains (ε) are calculated in the range 0.15% < ε < 20%, and then plotted on bi-
logarithmic coordinates in Fig. 2. The concave up shape of the resulting curves can be
taken into account by the Ludwigson modelling (Ludwigson et ah, 1971). Indeed this
 471

author supposes the existence, at low strain level, of a deviation Δ from the Ludwik
relation, defined as:
σ = K!. ( ε ) n i at high strain level (1)
σ = Κ^. (ε ) η ι + Δ at low strain level (2)
where Δ = K2.(e)n2*e.
The transition is defined as the oL-EL point at which Δbecomes very small in comparison
with the Ludwik term. It is here evaluated by r = A/iK^.E^) = 0.005 and a L = Κ ^ ε ^ ι .
The values of Kj, n j , K2, n 2 , oL and EL, for the steels B, C and D, are given in Table 2. The
directions of variation of these parameters are represented, in a simplified manner, in
Fig. 3. The following points can be observed in this figure : (i) at high strain level, the
plastic flow straight lines have the same slope n^ but undergo a vertical translation when
the nitrogen content increases; (ii) at low strain level, the deviation Δ from the Ludwik
model increases with the nitrogen content, and exists up to a strain level ε ^ all the higher
as the nitrogen content is high.
Table 2 . Parameters of the Ludwigson relation (2).
Coordinates of the transient point ( OL , ε ^ .
steel K a (MPa) Hi K 2 (MPa) - n2 eL G L (MPa)

B 1182 0.357 163 79.307 0.055 420

C 1302 0.353 193 68.096 0.064 494
D 1513 0.349 226 65.172 0.067 589

These results can be interpreted by the fact that at low strain level, the short-range
stresses predominate, all the longer as the nitrogen content is high, because of the strong
interactions between the dislocations and the nitrogen solute atoms. At high strain level,
the dislocation glide is multiple and the long-range stresses predominate.

Low Cycle Fatigue Behaviour

The LCF lives Nf of the four steels are plotted as a function of the total strain range in the
Fig. 4. The fatigue lives increase when the nitrogen content increases, all the more as the
strain level increases. This cannot be attributed to a lower dissipated energy per cycle
AWS; indeed Fig. 5 shows that the energy AWS, i. e. the area of the hysteresis loop at the
stabilized cycle (defined at 20 % Nf), is independent of the nitrogen content. Instead we
propose to explain this improved fatigue life by studying the reversibility of the cyclic
plastic strain. According to Abel's studies (Abel et ah, 1973), we characterize this reversi-
bility by the energy parameter ßg defined on the hysteresis loop in Fig. 6.a; a high value of
ßg corresponds to a better strain reversibility. Figure 6.b represents the parameter (^ at
the stabilized cycle as a function of the total strain range Δε4, for steels A, B and D. It
appears in this figure that at low strain level, the deformation reversibility decreases
when the nitrogen content increases, while at high strain level, it increases with the
nitrogen content.
Moreover, previous transmission electron microscopic observations (Degallaix et al,
1984, 1988b) showed that: (i) at low strain level, whatever the nitrogen content, the
dislocation slip is relatively simple during themain part of the life; (ii) at high strain level,
the dislocation slip is simple during the main part of the life in steel D, while it is multiple
472
early in the life in steels A and B, the nitrogen content of which being very lower than that
of steel D.
It thus appears that:
(i) at low strain level, the interstitial content - rather than the dislocation slip mode - is
essential in relation to the strain reversibility; this reversibility is all the more important
as the interstitial content is low;
(ii) on the contrary, at high strain level, the dislocation slip mode is the essential parame-
ter responsible for the strain reversibility; the higher the interstitial nitrogen content, the
more planar the dislocation slip, the better the strain reversibility.

We can therefore conclude that the planar dislocation slip favoured by the nitrogen
alloying is the essential cause of the good reversibility of the strain at high strain level,
and consequently of the better LCF strength of steel D. At low strain level, the reversi-
bility is better at low nitrogen content. However, the better LCF strength is still that of
steel D, even more so if the improvement is not very great.

ACKNOWLEDGEMENTS

The tests were performed in the "Laboratoire de Metallurgie Physique" of the University of Lille.
Professor J. Foct, director of this Laboratory, is gratefully acknowledged.

REFERENCES

Abel, A. and H. Muir (1973). The Baushinger effect and stacking fault energy. Phil. Mag.,27. n<3,
585-594.
Degallaix, S., RTaillard and J. Foct (1984). Role of Nitrogen interstitials in plastic fatigue of aust.
stainless steels. In: Fatigue 84 (C.J. Beevers, ed.), Vol. 1, pp. 49-59. Int. Ed. Panel, London.
Degallaix, S. and J. Foct (1987). L'azote dans les aciers inoxydables austenitiques; lere Partie :
influence sur les caracteristiques metallurgiques. Mem. Et. Sc. Rev. Met., 84, n°12,645-653.
Degallaix, S. and J. Foct (1988a). 2eme Partie : influence sur les caracteristiques mecaniques.
Mem. Et. Sc. Rev. Met., 85, n°2,111-123.
Degallaix, S. (1988b). Role of nitrogen on the monotonic and cyclic plasticity of type 316L SS at
room temperature. In: Basic Mechanisms in fatigue of metals (P. Lukas and J. Polak, eds.),pp. 65-
72. Academia, Prague.
Degallaix, S., I. Dickson and J. Foct (1989). The effect of nitrogen on the fatigue and creep-fatigue
behaviour of austenitic stainless steels. In: HNS 88 (J. Foct and A. Hendry, eds.), pp. 380-386.
Inst. of Metals, London.
Friedel, J. (1967). Dislocations. In: int. series of monographs on solid state physics. Vol. 3, Chap. XIII
and XIV.
HNS 88 (1989). Proc. 1st Int. Conf. (J. Foct and A. Hendry, eds.), Inst. of Metals, London.
HNS 90 (1990). Proc. 2nd Int. Conf. (G. Stein and H. Witulski, eds.), Stahl-Eisen, Düsseldorf.
Ludwigson, DC. (1971). Modified stress-strain relation for FCC metals and alloys. Met. Trans.,2,
2825-2828.
Norström, L.A. (1977). The influence of nitrogen and grain size on yield strength in type AISI
316L austenitic stainless steel. Met. Sc., 208-212.
Pickering, F.B. (1978). Physical metallurgy and the design of steels. Chap. 11. Appl. Sc. Pub.,
London.
Soussan, A. and S. Degallaix (1990). Effet combine de l'azote interstitiel et de la taille de grain sur
les contraintes d'ecoulement d'aciers inoxydables austenitiques type Z2 CND17-12. Mem. Et.
Seite;. Me*., 87,443-456.
 473

Tensile properties in MPa

800
UTS

6001

YS at 0.2 %
400 H

YS at 0.02 %
200

0.0 0.1 0.2 0.3

wt%N

steel C : (0.120 %N)

100 _J ■ ■ ' I '

1000
Fig. 1. Tensile mechanical pro-
perties YS a 0 2 % / YSQ.2%
and UTS as a function of
the nitrogen content. ♦ ♦♦♦

Fig. 2. Plastic flow curves :true steel D : (0.250 %N)

■ ' ■ ■ t 1 1 I I tl I ■ ■■■■■!
stress (σ) - true plastic 100
strain (ε). ·001 ·01 .1 , v 1
(ε)
jlogA

K,
[ON.
k 0 \sV %N4
\ y \ \.

s. ε
£L

Fig. 3. Schematic variation of plastic flow curves with the

nitrogen content:
a-Definition of K l 7 n l 7 GL a n d E L -
b - Definition of K 2 a n d n 2 .
474

ί* 5.
Γ I I " ' ■" ^
I

Γ ··
.·ί"·^?%ο ^ "I
"*··. °
" ■ ■ · ♦ .* . ^" ^^

St- l·-
'·····>. • ^ o ^ o » ♦ -j
< F J
er
• • steel A
ζ ·
< Γ * - steel B -\
er
ι- • - steel C
ο - steel D
<
I 1 Nf
Ο .1
10J 10* 1CT

Fig. 4. Room temperature low cycle fatigue life curves (A£tusNf).

AWS (J/cm 3 )
10

'j&^
^
• * j ^> — Steel A
— Steel B
Steel D
1 1 i i i 1
1 1 1
Δε t (%)
0.5

Fig. 5. Dissipated energy (at the stabilized cycle) AWS versus the
total strain range Ae{.
βΕ AT 2 0 % N R

I
\
i

^ ' ^ \
▲ steel A
• steel B
* steel D Δεχ (%)j

Fig. 6. Energy parameter β Ε :

a - Definition,
b - ßg as a function of the total strain range.
 WS7d4

FAILURE LIFE AND CYCLIC CONSTITUTIVE RELATION OF DIRECTIONALLY

SOLIDIFIED MAR-M247 SUPERALLOY IN CREEP-FATIGUE

T. HASEBE*, M. SAKANE" and M. ΟΗΝΑΜΓ

* Department of Mechanical Engineering, Graduate School of

Ritsumeikan University, 56-1 Tojiin Kita-machi Kita-ku
Kyoto, 603, Japan

** Department of Mechanical Engineering, Faculty of Science

and Engineering, Ritsumeikan University, 56-1 Tojiin
Kita-machi Kita-ku Kyoto, 603, Japan

ABSTRACT

This study investigates the effect of solidification direction on cyclic constitutive relation and
failure life of Mar-M247LC directionally solidified (DS) superalloy under creep-fatigue conditions.
Strain controlled low cycle fatigue tests with 10 and 60 min. hold-times in tension were carried
out for three kinds of specimens of which loading direction was 0°, 45° and 90° to the solidification
direction (DS axis). Step-up tests with a 10-min. tension hold-time were also conducted for these
specimens to develop a creep constitutive equation. An inelastic constitutive equation was
developed taking account of the anisotropy of Young's modulus and creep equation determined
from cyclic relaxation curves. Creep-fatigue life prediction was made based on the inelastic
analysis. The predicted life agreed with the exprimental life within a factor of two scatter band.

KEYWORDS

Creep-fatigue; anisotropy; constitutive equation; high temperature; DS superalloy; life prediction.

EXPERIMENTAL PROCEDURE

Test material used in this paper is Mar-M247LC Ni-base directionally solidified (DS) superalloy
of which chemical composition and heat treatment is published elsewhere (Hasebe et al., 1990).
Figures 1(a) and (b) respectively show the shape and cut-out direction of the specimen. Specimen
used was a cylinder with 5 mm diameter and 15 mm gage length. Three kinds of specimens were
employed; they were cut out from DS plates to provide three specimen axes of 0=0°, 45° and 90°
to the solidification direction. Width of columnar grain was between 5 and 10 mm.

An electric hydraulic servo-type uniaxial fatigue machine conducted total strain range controlled
creep-fatigue tests with a trapezoidal strain wave at 1173 K in air. Hold-times introduced at the
tensile peak strain were 10 and 60 minutes. Strain rate of the test was 0.1% /sec. A
high-frequency induction furnace heated the specimen. The number of cycles to failure, Nf, was
defined as the cycle at which the tensile stress amplitude decreases to 75 % from saturation. This
study also made cyclic step-up relaxation tests for three directions to obtain the stress rlaxation
475
476

(a) (b)

Fig.l. (a)Shape and dimensions of the specimen in milimeter, and (b)

cutout directions of the specimen of which loading axis is 0°,
45° and 90° to the crystal growing direction.

curves from various stress levels. The strain wave used for the test is a trapezoidal wave with 10
min. hold-time in tension. The strain amplitude was increased stepwisely and the stress relaxaion
was recorded during the hold-time.

EXPERIMANTAL RESULTS AND DISCUSSION

Creep-Fatigue life

Figure 2(a) compares creep-fatigue lives in 10 min. hold-time test with those in no hold-time test
(Hasebe et aL, 1990) for the three kinds of specimens. The open circle, cross and open triangle
show the fatigue data with no hold-time, while the solid circle, open circle with cross and solid
triangle indicate creep-fatigue lives of the 0°, 45° and 90° specimens respectively. The angle Θ
has a significant effect on creep-fatigue lives. The 0° specimen has the largest fatigue life, the 45°
specimen the smallest and the 90° specimen the intermediate creep-fatigue life. This trend is
similar to that in no hold-time tests. Life reduction due to the introduction of 10 min. hold-time
is about 55% for the 45° specimen and about 30% for the 90° specimen. The 0° specimen,
however, shows almost no life reduction by the hold-time.

Figure 2(b) shows the life reduction ratio with the introduction of hold-time, where the ordinate
is normalized by the failure life in no hold-time test. Life reduction of the 45° specimen is the
largest at tH=10 min., while that of the 90° specimen the largest at tH=60 min., which is almost
same as that of the 45° specimen. Since Ohta et al.(1989) have reported that the creep rupture
strength of the 90° specimen is the smaller than that of the other directioned specimens, hold-time
longer than 60 minutes may bring the largest life reduction to the 90° specimen.
 477

MAR-M247LC 1173K
1.4 i 1

MAR-M247LC 1173K
«MOV τττττη- Γττττπρ ΓΤΤΤΓΤΤρ
K 0=45'
• 0=0° (tH=10«ln) , A 0=90* J
LÜ
& 0=45°(tH-lOnln) 1.0 I
CD A 0=9O°(tH-lOiiln)
2
<C
S
\ A
* "'S.

<E
O 0-0* (tH-Oiln)
0.6
Λ "-._ \
X 0-45 β (ΐΗ-Ο·Ιη)
Δ 0=90*(tH-Oeln)
lO"1 I llllll . IMI.I ll n o I 1
10 10 2 10 3 IG4 10 5 0 30 60
NUMBER OF CYCLES TO FAILURE Nf HOLD TIME tH. mln.

(a) (b)

Fig.2. (a)Failure lives in 10 minute and no hold-time tests, and (b)

reduction of life ratio with increasing hold-time. Nf* is the
failure life in no hold-time test.

Stress relaxation curves and creep law

Figures 3(a), (b) and (c) show the stress relaxation curves during strain hold-time obtained in the
step-up relaxation test. For the formulation of the relaxation curve, we employ here the following
creep equation without taking account of the cut-out direction.
dec=aa"tm, (1)

where A, a and m are the material constants. Stress relaxation equation derived from eq.(l) can
be expressed as;
σ1-*=σ1ί-α+ΑΕ(θ,φ) ( α - 1 ) tm (a:MPa, t:hr.), (2)

where oi and Ε(θ,φ) are respectively the initial stress of relaxation and the Young's modulus. Θ and
φ are angles indicating the crystallographic orientation which is stated in the next section. Values
of the constants a and m are 8.9 and 0.7 respectively. In eq.(2), the material constant A depends
on the initial stress of relaxation, so A is assumed to have the following form.
-log(A)=R(ai)P, (3)

Constants R and/? have the values of 12.53 and 0.11 respectively. Solid lines in Fig.3 show the
stress relaxation curves calculated from eqs.(2) and (3). Calculated curves well express the
experimental results.

In the inelastic constitutive equation described below, eq.(2) is used to estimate the creep strain
occured during the hold-time. Material constants in the creep equation were determined from the
cyclic relaxation step-up tests.
478

MflR-M247LC H73K 000 MnR-11247LC 1173K „no MAR-M247LC 1173K

1
■ ' """I ' ' ' l""| ' ■ i HIHI 700 I ' ■ '|Mii| ni| 1 i > H'lij 700 I 1 i i |ini| 1 I I |ini| 1 i i null

TIME t . MIN. TIME t . MIN. TIME t . MIN.

(3)0=0° (b)0=45° (c)0=9O°

Fig.3. Stress relaxation curves obtained in cyclic step-up tests

with 10 min. strain-hold for (a)0=O°, (b)0=45° and (c)
0=90° specimens.

CYCLIC STRESS RESPONSE AND CREEP-FATIGUE LIFE PREDICTION

Inelastic Constitutive Relation

For the creep-fatigue life prediction, the estimate of stress amplitude is essential, since the damage
of DS superalloys is dominated by stress amplitude rather than inelastic strain amplitude. This
paper develops an inelastic constitutive relation taking account of the anisotropy of the Young's
modulus.

Total strain increment, de„ is assumed here to be a linear summation of elastic, dee, plastic, dep,
and creep, de^ strain increments:
det=dee+dep+dec, (4)

No interaction between plastic and creep strains is considered in this paper for the simplicity of
theory. In Mar-M247 DS superalloy, since Young's modulus has significant anisotropy due to the
crystallographic structure, the elastic strain component can be written as,
βθ=σ/Ε(Θ,φ), (5)

where Ε(0,φ) is the Young's modulus. Two angles, 0 and φ, respectively denote the angle between
specimen axis and [001] direction, and the rotation angle about [001] axis. The Young's modulus
is expressed as a function of 0 and φ as follows (Nye, 1957).
Ε{θ, φ) = lslx-2 ( s 1 ] L - s 1 2 - - s 4 4 ) x s i n 2 0 ( c o s 2 0 + i s i n 2 0 s i n 2 2 # ) ] -1, (6)

where s^ represents the elastic compliance. Eq.(6) clearly shows that the Young's modulus
significantly depends on 0 and φ (Hasebe et aL, 1990).

On the contrary to the Young's modulus, there is no anisotropic relation between plastic strain and
stress amplitude in experiments (Hasebe et al., 1990), so the plastic strain can be equated as,
 479
MAR-M247LC 1173K riAR-M247LC 1173K HAR-n247LC 1173K
1000 1000 ~r 1000

— Experimental — Experimentalj
—Caloulated —Caloulated

Oh

Z)£t=1.2% 4Bt-1.2%
ZlBt=1.2%
-1000 -1000 -1000
1 0 1 ι υ
"-1 0 1 ίυ
-1 0 1
STRAIN e. % STRAIN B. % STRAIN ε. %

(a)0=O° (b)0=45° (c)<9=90°

Fig.4. Comparison of the hysteresis loops between inelastic analysis

and experiments in 10 min. hold-time tests.

l/n
■(σ/Κ) (7)

K and n are the material constans having the values of 1008 MPa and 0.24, respectively.
Regarding the creep strain, this paper employs eq.(l) regardless the cut-out direction. Using the
strain components expressed by eqs.(l), (5) and (7), cyclic stress amplitude can be calculated for
a given total strain amplitude.

Cyclic Stress Response

Since DS superalloys show no clear yield behavior, this study employs no yield condition in the
constitutive equation. The elastic, plastic and creep strains are assumed to always occur for a given
stress amplitude. Stress response was calculated untill the hysteresis loop reached closed shape.

Figures 4(a), (b) and (c) compare the hysteresis loops obtained in experiments with those calculated
from the inelastic constitutive equation for 10 min. hold-time test. Solid lines express the
calculated loop, while broken lines the experimental loop at half life. The constitutive equation
developed in this paper quite well estimates the actual cyclic stress-strain relation.

As for the experimental results, the 0=45° specimen exhibits the largest stress amplitude, the 0=90°
specimen the intermediate and the 0=0° specimen the smallest. As usually seen in the hysteresis
loop of superalloys, the elastic strain is predominant in the hysteresis loop but the plastic strain has
a small percentage in the total strain. Thus, we can conclude that the difference in the cyclic stress
amplitude due to the cut-out direction is mainly resulted from the anisotropy of the Young's
modulus.

Creep-Fatigue life Prediction

We will make creep-fatigue life prediction using the cyclic constitutive relation derived above.
In predicting the creep-fatigue life, cyclic stress amplitude was calculated using the inelastic
equation and then the creep- fatigue damage was estimated based on the following equations.
480

10" F—i—i i 11 ιιΐ| 1—i i 11 ni| 1—i i^n

>^ lO.i. 60iii

0° •
45° Si *
LU 90° A ▲

Factor
of two -J
ω
CO
O

101 _i i i I mil i i i I mi
101 102 103 104
PREDICTED LIFE Nfp

Fig.5. Comparison of predicted creep-fatigue lives with experimental

lives.

Σ (Dc+Df) =D, (8)

Jc=l

where Dc and Df express the creep and fatigue damage per cycle. They are given as follows.

Dc=(tH(dt/tr(o)), <t>c=^Dc
C
JO ° Jc-i °
Df=l/N*f. φ,Λϋ,. (9)

Nf* and tr(a) are respectively the failure life in no hold-time test and the static creep rupture time
obtained from the Larson-Miller plot of Mar-M247 DS superalloy (Ohta et aL, 1989).

Figure 5 shows the comparison between the predicted and experimental creep- fatigue data. Most
of the data are within a factor of two scatter band so that the creep-fatigue life prediction based
on the inelastic constitutive relation taking account of Young's modulus is available to DS
superalloys.

REFERENCES

Hasebe, T., M. Sakane, and M. Ohnami, (1990). High Temperature Low Cycle Fatigue and Cyclic
Constitutive Relation of MAR-M247 Directionally Solidified Superalloy. Trans. ASME JEMT
(to appear).
Nye, J.F. (1957). Representation Surfaces and Young's Modulus. In: Physical Properties of Crystals
(Ridler, V. ed.), pp.143-145. Univ. Press, Oxford.
Ohta, Y., H. Hattori, Y. Nakagawa, and M. Yamazaki, (1989). Castability and Anisotropical High
Temperature Strength of Directionally Solidified Ni-base Superalloys. Tetsu to Hagane, 75,956.
WS7e1

SHORT FATIGUE CRACK GROWTH OF AUSTEMPERED NODULAR CAST IRONS

J.R. Hwang, J.L. Doong and P.J. Chung

Department of Mechanical Engineering, National Central University

Chung-Li, Taiwan 33054, R.O.C.

ABSTRACT

This paper studies the effects of austenitizing temperature, austempering

temperature and isothermal transformation time on the short fatigue crack
growth behavior of nodular cast irons. Differences between short and long
fatigue crack behavior are compared. The influence of stress ratio is also
investigated. Fracture surfaces are observed through a scanning electron
microscopy to understand the fracture mechanism. The results show that: (1)
For nodular cast iron with lower bainitic matrix, the short fatigue crack
growth rate increases with higher austempering temperature, while with the
upper bainitic matrix, it behaves contrarily. (2) The nodular cast iron
austenitized at 900°C for 1 hr and then austempered at 350°C for 30 min-4 hr
have better resistance to short fatigue crack growth. (3) The short fatigue
crack growth rate of austempered nodular cast iron increases with stress
ratio.

KEYWORDS

Nodular cast iron; bainite; austemper; short crack; fatigue; crack growth.

INTRODUCTION

Austempered nodular cast iron exhibits excellent strength, toughness, and

wear resistance. It has been used in application as diverse as crankshaft,
gear, connect rod and hubs of motor vehecle (Harris et al., 1970). Due to
the extensive applications, it is necessary to know how the manufacture
process affects the mechanical properties. Many documents on the tensile
properties (Cox, 1982, Dorazil et al., 1978), impact toughness (Voigt et
al., 1984) and fracture toughness (Doong et al., 1989, Lazaridis et al.,
1971) are available. However, there is limited information about the fatigue
crack growth behavior (Doong et al., 1988).

481
482

. r2
l·—2.3
~|
Mr 1
I J^ 22

i1 1
139.5

(a)

Fig. 1. (a) Configuration of fatigue specimen.

(b) Microstructure of as-cast nodular cast iron.

According to the crack length, the fatigue cracks are divided into long
fatigue crack and short fatigue crack. Many researchers have shown that
short cracks tend to propagate quicker than long cracks do (Miller, 1982,
Schijve, 1982). The life prediction based on long fatigue crack behavior is
not conservative in the case of short fatigue crack. In nodular cast iron,
the graphite nodules and microshrinkage pores may act as the potential sites
for crack initiation and propagation. Therefore, it is particularly
attractive to study the short fatigue crack. The short crack growth rate and
crack closure mechanism in as-cast nodular iron were investigated by Clement
etal. (1984) They also discussed the influence of three dimensional small
crack on the crack initiation. However, there is no literature on short
crack behavior in austempered nodular cast iron.

In the present study, the effects of various austenizing temperature,

austempering temperature and isothermal transformation time on the short
fatigue crack growth in austempered nodular cast irons are investigated.
Scanning electron microscopy was put to observe the fracture surface and
understand the fracture mechanism.

EXPERIMENTAL PROCEDURE

Nodular cast iron was melted in a high frequency induction furance,

magnesia-treated in a ladle, then cast into sand moulds. The chemical
composition is C 3.3, Si 2.33, Mn 0.36, P 0.04, S 0.01, Ni 0.48, Mo 0.03 and
Mg 0.02 in %wt. The microstructure of as-cast iron is shown in Fig. 1(a).
The ferritizing treatment was performed at 900°C for 2hr, cooled to 700°C
for 6hr, then cooled to room temperature in furnace to improve the
homogeneity of as-cast structure. To study the effect of various
austempering treatments, specimens were divided into three groups: (1)
austenitizing temperature 850-950°C, (2) austempering temperature 275-450°C,
(3) isothermal transformation time 9 min-4 hr. The details of the above are
referred to Table 1.

The mechanical properties were tested through a computerized MTS closed-loop

hydraulic servo-controlled machine. Configuration of fatigue specimen is
shown in Fig. 1(b). Fatigue precracking was performed by a load shedding
technique with a 10% decrease in load at each step. A sinusoidal load with
stress ratio R=0.01 and a frequency of 40 Hz were used. Crack length was
measured by a travelling microscope of resolution 0.01 mm along with
 483
Table 1. Austempering treatment conditions, mechnical properties
and retained austenite

Austenitizing Austempering Ultimate Yield Retained

Specimen temperature temperature strength strength e(%) BHN austenite
number (°C) and time (°C) and time (kg mm-2 ) (kg mm- 2 ) (%)

Al 850(lhr) 350(1.5hr) 104 85 4.2 290 13

A2 900(Ihr) 350(1.5hr) 102 84 6.2 270 18
A3 950(lhr) 350(1.5hr) 100 75 8.1 257 30
Bl 900(Ihr) 275(1.5hr) 146 .25 0.9 372 2
B2 900(Ihr) 300(1.5hr) 138 .16 1.6 327 6
B3 900(Ihr) 350(1.5hr) 102 84 6.2 270 18
B4 900(Ihr) 400(1.5hr) 105 75 12.8 248 20
B5 900(Ihr) 450(1.5hr) 100 71 5.2 239 18
Cl 900(Ihr) 350(9 min) 99 76 2.9 263 6
C2 900(Ihr) 350(30min) 102 80 4.8 283 8
C3 900(Ihr) 350(1.5hr) 102 84 6.2 270 18
C4 900(Ihr) 350(4 hr) 105 84 3.9 296 14

stroboscope. The specimens were precracked until crack length reaches 4 mm.
Then the lateral faces of specimens were machined to obtain the desired
short through crack specimen or long through crack specimen. These specimen
were tested under axial loading at 40 Hz with stress ratio R=0.01, 0.5 or
0.8. Crack length against fatigue cycle was recorded. Carck growth rate
da/dN was calculated by secant method. Stress intensity factor range öK was
calculated by ÖK=YÖOV1L, where the correction factor Y=1.99-0.41(
a/w)+1.87(a/w)2-38.48(a/w)3+53.85(a/w)4.

The volume fraction of retained austenite in the specimen was measured by

molybdenum X-ray diffraction method. A Rigaku diffractometer with a strip
chart recorder was put to scan the angular range (°2Θ) 30-39°, the rate was
0.01°/s. The amount of retained austenite was calculated by the method
(Rundman et al., 1982). The fracture surfaces were observed by a scanning
electron microscopy.

RESULTS AND DISCUSSION

Microstructures and Mechanical Properties

The metallographs of austempered nodular cast irons are shown in Fig. 2. The
microstructurs of Fig. 2(a) is lower bainite, that of Fig. 2(c) is upper
bainite, while that of Fig. 2(b) is a mixture of lower bainite and upper
bainite.

The effects of austenitizing temperature, austempering temperature and

isothermal transformation time on the tensile properties, hardness and
retained austenite are shown in Table 1. At higher austenitizing
temperature, more retained austenite is created along with the better
ductility, but the strength and hardness are worse, and vice versa. The
higher the austempering temperature is, the lower the strength and hardness
484

Fig. 2. Microstructures of austempered nodular cast

irons, (a) Specimen Bl, (b) specimen B3, (c)
specimen B5.

i- 950 -C - 270 -C »9. min

* 900 -C + 300 "C + 30 min
- 850 *C * 350 "C * 1. 5hr
B400 'C B4 hr
* 450 *C

(a) (b) (c)

10 100 1000 10 100 1000 10 100
ΔΚ (Kg m m " 3 ' 2 ) ΔΚ (Kg m m - 3 / ! ) ΔΚ (Kg m m ' 3 ' 2 )

Fig. 3. Effect of austempering treatment conditions on

short fatigue crack growth rate,
(a) Austenitizing temperature, (b) austempering
temperature, (c) isothermal transformation
time.

is, while the elongation and retained austenite is higher. But when the
austempering temperature exceeds 400°C, feather-like upper bainite is
formed, then the elongation and retained austenite decrease. With increasing
isothermal transformation time, the strength increases, while the elongation
and retained austenite increase, then decrease later on. The optimum
mechanical properties occur at 1.5 hr.

Short Fatigue Crack Growth Rate

The effect of austenitizing temperature on the short fatigue crack growth

rate at R=0.01 is shown in Fig. 3(a). The iron austenitized at 900°C has the
best resistance to short fatigue crack growth. It is more pronounced at
lower öK value. From previous discussion, the iron austenitized at 900°C has
better combination of mechanical properties in strength and ductility than
at 850°C or 950°C, it leads to higher resistance to crack growth. Fig. 3(b)
shows the effect of austempering temperature on the short fatigue crack
growth rate. For lower bainitic matrix, the resistance to short fatigue
 485

E-3
-0.35mm
+ 1.9 mm

rH
u
>,
O
•v.
E

E-6 L(b)
10 100 1000 10 100 1000
ΔΚ (Kg m t n - " * ) ΔΚ ( Kg „„,->•«,

Fig. 4. (a) Effect of stress ratio on short fatigue

crack growth, (b) effect of crack length on
short fatigue crack growth.
crack growth increases with the austempering temperature. However, it is in
the opposite case for upper bainitic matrix. The iron austempered at 350°C
has the best short crack growth resistance. Plots of da/dN vs. öK for irons
austempered at 350°C with various isothermal transformation time are shown
in Fig. 3(c). In general, the resistance to crack growth increases with the
isothermal transformation time. But there is no significant variation during
the time from 30 min to 4 hr.

Fig. 4(a) shows the plots of short fatigue crack growth rate at various
stress ratios. Specimens were austenitized at 900°C for Ihr, then
austempered at 275°C for 1.5 hr. It is apparent that the short crack growth
rate clearly increases when the stress ratio increases. To study the
influence of crack length, the irons were austenitized at 900°C for Ihr,
then austempered at 275°C for 1.5 hr. Plots of da/dN vs. öK for two
different crack lengths are given in Fig. 4(b). It shows that the short and
long fatigue crack growth behavior coincide at higher öK value.

Fracture surfaces of the short fatigue crack specimens are shown in Fig.
5(a)-(c). The feather-like transgranular fracture is observed from these
three irons. In the fracturing process, the bainitic ferrite is deformed
down the direction of applied load and extrudes out of the fracture surface.
When the loading continuously increases, the feather-like fracture region
extends, and the colensence of the different fracturs regions lead the crack
growth. It is seen that there are few differences among the fracture
surfaces of various austempering treatments.

CONCLUSIONS

1. For the nodular cast iron with lower bainitic matrix, the resistance to
short fatigue crack growth increases as the austempering temperature
increases, but with upper bainitic matrix, the resistance to short
fatigue crack growth decreases under the same situation.
2. The most optimum process of austempering treatment in the present study
is that austenized at 900°C for 1 hr, austempered at 350°C for the time
486

Fig. 5. Fracture surfaces of austempered nodular cast

irons, (a) Specimen Bl, (b) specimen B3, (c)
specimen B5.
from 30 min to 4 hr.
3. The short fatigue crack growth rate of austempered nodular cast iron
increases with the stress ratio.
4. The difference between short fatigue crack growth rate and long fatigue
crack growth rate is obscure at higher stress intensity factor range.

ACKNOWEDGEMENTS

The authors gratefully acknowedge the support of the National Science

Council of R.O.C. on the work through grant No. NSC79-0401-E008-03.

REFERENCES

Clement, P., J.P. Angeli and A. Pineau (1984). Short crack behaviour in
nodular cast iron. Fatigue and Fract. Engng Mater. Struct., 1^, 251-265.
Cox, G.J. (1982). Tensile properites of spheroidal graphit acicular irons.
Brit. Foundryman, 75, 1-7.
Doong, J.L and C.S. Chen (1989). Fracture toughness of bainitic nodular cast
iron. Fatigue and Fract. Engng Mater. Struct., 12, 155-165.
Doong, J.L. and S.L. Yu (1988). Fatigue crack propagation of bainitic
nodular cast iron. Int. J. Fatigue, 10, 219-226.
Dorazil, E., B. Barta, J. Crhak and E. Munsterova (1978). High-strength
bainitic cast iron with spheroidal graphite. Met. Sei. Heat Treat., 20,
532-535.
Harris, D.A., B. Tech and R.J. Maitand (1970). The products of isothermal
decomposition of austenite in a spheroidal graphite cast iron. Iron and
Steel, _2, 53-60.
Lazaridis, A., F.J. Worzalz, C.R. Loper and R.W. Heine (1971). Fracture
toughness of ductile cast iron. AFS Trans., 79, 251-360.
Miller, K.J. (1982). The short crack problem. Fatigue Fract. Engng Mater.
Struct., 5, 223-232.
Rundman, K.B. and R.C. Klug (1982). An X-ray and metallographic study of an
austmpered ductile cast iron. AFS Trans., 90, 499-508.
Schijve J. (1982). Differences between the growth of small and large fatigue
cracks in relation to threshold K values. Fatigue Threshold, 881-908. EMAS
Publ.
Voigt, R.C and C.R. Loper (1984). Austempered ductile iron process control
and quality assurance. J. Heat Treat., 12, 291-309.
 WS7e2

FATIGUE PROPERTIES OF TiN FILMS ON STEEL COATED BY DYNAMIC MIXING

R. Murakami*, T. Takeuchi**, T. Yano*** and M. Katsumura***

* Dept. of Mech. Eng., University of Tokushima,

2-1 Minami-josanjima-cho, Tokushima, Japan.
** Mita Cop. Ltd., Tamatsukuri, Chuo-ku, Osaka, Japan.
*** Goverment Industrial Research Institute, Shikoku,
2-3-3 Hananomiya-cho, Takamatsu, Kagawa, Japan.

ABSTRACT

The eight kinds of TiN thin films were coated on steel by using dynamic mixing method.
The structure of the coated thin films were analyzed by using X ray. It has been
found that the thin films were TiN structure alone and the mixed structures of TiN
and TioN. The fatigue life of thin film depends on an applied cyclic stress. When the
cyclic stress is high level, the thin film scarcely improves the fatigue life. At low
cyclic stress, the thin film markedly increases the fatigue life. Then, the fatigue
life of thin film increases with increasing the hardness of thin film. The enlarge-
ment of fatigue life of thin film relates with the process of crack initiation from
the coated TiN thin films.

KEYWORDS

Fatigue life; fatigue initiation; surface modification; ion beam method.

INTRODUCTION

The TiN thin film, which has higher hardness and the superior resistance to wear, has
been coated on the surfaces of tools. Such a ceramic thin film is generally coated by
CVD and PVD(Bryant, 1989, Rigsbee, 1989, Mchargue, 1989). Recently, dynamic mixing
method which mixes simultaneously metal vapor with ion implantation has been develop-
ed. The dynamic mixing method easily controls the composition and the structure of
the thin films and enlarges the adhesive strength. The coating of the TiN thin film
by this method has been applied to tools and its hardness and wear have been studied.
Then it is important to be clear the fatigue properties of coated ceramic thin films
on metal(Herman, 1891, Shiozawa et al., 1990).

In the present study, the eight kinds of TiN thin film were coated on the high ten-
sile strength steel by the dynamic mixing method. The fatigue properties of ceramic
487
488
thin films are studied, and then the effects of thin films on the fatigue life and
the crack initiation are discussed.

EXPERIMENTAL PROCEDURE

The substrate material used was 60kgf/mm2 grade high tensile strength steel having a
chemical composition(wt%); C 0.14, Si 0.31, Mn 1.30, P 0.015, S 0.012. The mechanical
properties of substrate were determined as; yield strength 461MPa, tensile strength
617MPa and elongation 32%. The fatigue specimens, 6mm thick with an area of 80mm X 20
mm were machined and were notched with a notch depth of 0.5mm and a notch tip radius
of 0.1mm. After machining, the notched fatigue specimens were electro-polished in the
solution of Perchloric Acid and Acetic Acid in the rate of 1:9.

The dynamic mixing equipment used was Hitachi IX-40-400. Nitrogen gas and pure tita-
nium were chosen to obtain the TiN thin film. The notched fatigue specimens have been
sputter cleaned for 0.6ks. in the nitrogen ion. The eight kinds of TiN thin films
were coated on the steel in the conditions as shown in Fig. 1. The thickness of TiN
thin films are about 5/zm. The notched fatigue specimen implanted nitrogen ion were
also prepared.

Three point bending fatigue tests were performed by using electro-hydraulic fatigue
testing machine at a frequency of 10Hz and a stress ratio of R=0. The stress varies
sinusoidally in the time. The fatigue initiation has been observed by the optical
microscope each N=10 5 cycles.

EXPERIMENTAL RESULTS AND DISCUSSION

The Structure and Hardness of TiN Thin Films

The structure of TiN thin film on the steel was analyzed by the X ray diffraction me-

I o 3kV
10 Γ 9 10kV Accelerating voltage
*E
<
\ 8

c 6,
•ωσ
+-
c
ω 4
l_

o
o <=-

O 1 2 3 4 5
Deposition rate / nm/s

Fig. 1. Coating condition of TiN thin film on steel.

 489
thod. Fig. 2 shows the X ray diffraction patterns of TiN thin films. The structure of
thin film is mainly TiN regardless of the coating conditions. Sample(b) includes T12N
in the TiN thin film. Sample(g) shows the broad X ray diffraction pattern and its
structure may be an amorphous like structure.

The micro-Vickers hardness of TiN thin films is shown in Fi. 3 as a function of ap-
plied load. The hardness value of TiN thin film decreases with increasing the applied
load and is strongly influenced by the deformation of substrate.

Fatigue Life of TiN Thin Film Coated On The Steel

The effects of TiN thin films on fatigue lives are shown in Fig. 4. At A a = 3 0 6 M P a ,
the fatigue life is greater for the samples(b), (c) and (e) than for the substrate.
While the fatigue lives for the samples(a), (d), (f), (g) and (h) are less than that
of the substrate. The greatest fatigue life is obtained for the sample(c). When the
cyclic stress increases to Δ σ =408MPa, the fatigue life of sample(c) is almost the
same as that of the substrate. Then, when the cyclic stress decreases to A(7=255MPa,
the fatigue specimen does not failure to 10 T cycles and this stress means the fatigue
limit. The sample(a) has the shortest fatigue life at Δ σ =306MPa among all of the
specimens. Furthermore, the decrease in the cyclic stress does not contribute to an
enhancement of fatigue life. Such a fatigue behavior for the samle(a) considerably
differs from that of sample(c). For the sample(i) implanted the nitrogen ion, the fa-
tigue life at Δ σ =306MPa is almost the same as that of the substrate. Similar re-
sults have been obtained by Herman(1981) for specimen implated nitrogen ion and unag-
ed. If the specimen is artificially aged, the fatigue life enhancement can be observ-
ed. Thus, the fatigue life strongly depends on the cyclic stress and the TiN thin
film. When the cyclic stress is high level, the TiN thin film little influences the

2000

-5»

Ä
1500

4000 r- ^
1000
18Λ Yv*
ΙΛ 2000 V
500
"vi
▲

HT60
1 J j.. J 1
50 60 0 10 25 50 100
2 Θ (degree) Applied load (gf)

Fig. 3. Effect of applied load

Fig. 2. X ray diffraction patterns on hardness of TiN thin
of TiN thin films. film.
490

500r

itf itf id" 10'

Number of cycles of f a i l u r e Nf

Fig. 4. S-N curves of TiN thin films coated on s t e e l .

fample(d) Δ-255ΜΡ0 fajlu//'

° Δ σ=306ΜΡ3

1000 2000 1.5 1.6 1.7 1.8 '"1.9 2.0

Vickers hardness Number of cycles (xlO,;;)

Fig. 5. Relation between fatigue Fig. 6. Variation of surface crack

life and hardness for length with number of
TiN thin film. cycles for sample(d).

fatigue life. At low cyclic stress level, the improvement of fatigue life results
from the TiN thin film except the sample(a). In this case, the fatigue life of TiN
thin film increases with increasing the hardness of the TiN.

The relations between the micro-Vickers hardness value and the fatigue lives at Δ σ =
306MPa and 255MPa are shown in Fig. 5. As described above, the TiN thin film results
from the increase in the fatigue life. But the fatigue life is sometimes reduced by
the coated TiN thin film. In both the cases, the relation between the hardness and
the fatigue life gives essentially straight lines. It is evident from Fig. 5 that the
fatigue life markedly depends on the hardness of TiN thin film.
 491
The Crack Initiation Process On Surface Of TiN Thin Film

The fatigue life of specimen coated the TiN thin film may be influenced by the crack
initiation process. For the sample(d), the relation between the crack length and the
number of cycles is shown in Fig. 6. The number of cycles to failure, Nf, at Δ σ =255
MPa is Nf=1. 96xlO b cycles. The number of cycles to crack initiation, Ni, is Ni=0.82Nf.
Micro-cracks of 0.1mm ~~ 0.5mm length were initialy observed on the notch root as
shown in Fig. 7. Similar crack initiation is observed for the other samples.

At A a = 2 5 5 M P a , the fatigue lives are greater for the samples(d) and (f) than for
samples(a), (g) and the substrate. For all of the samples, the crack initiates after
about half of fatigue life. However, the crack initiation process for the samples(d)
and (f) differs from those for the samples(a) and (g). The crack little grows with
increasing the number of cycles and drastically increases just before the final
failure as shown in Fig. 6. For the sample(f), a micro-crack is observed on the sur-
face of TiN thin film at the faigue limit. This crack grew through the thin film and
arrested in the substrate.

The fatigue crack initiation and propagation processes are schematically shown in Fig.
8. The crack initiation process can be clarified into two types; Type(A) and Type(B).
In type(A), the multiple cracks initiate from the surface of thin film because the
hardness of TiN thin film is lower and then the cracks grow through the thin film.
Thus, the fatigue life is less than that of the substrate. While, if the hardness of
TiN thin film is higher than that of Type(A), the crack initiation process is reveal-
ed from Type(B). A crack can initiate from an interface between the thin film and the
substrate and then grows to the substrate. Because the displacement of crack increas-
es with increasing crack length, the harder thin film can be mechanically failed.
In this stage, the internal crack emerges to the thin film surface. Because the de-
formation of substrate is constrained by the harder TiN thin film, the delay of crack
initiation gives rise to the enhancement of the fatigue life in Type(B).

Fig. 7. Micro-crack initiation process for sample(d),

N=1.7xl0,? cycles, Δ σ =255MPa.
492

Type A Type B

Stage 1

Stage 2

Stage 3

Fig. 8. Schematically crack initiation process

on surface of TiN thin film.

CONCLUSIONS

(1) The fatigue life of steel coated the TiN thin film depended on the applied cyclic
stress, the hardness and the structure of TiN thin film. At low cyclic stress
level, the fatigue life enhancement is obtained if its hardness value is greater.
In the case which the hardness of thin film is less, the fatigue life is less
than for the substrate. In the case which the hardness of thin film is higher,
the faigue life is greater than for the substrate.
(2) The crack initiation process can be clarified into two types; Type(A) where the
crack initiates from the TiN thin film surface and Type(B) where the crack initi-
ates from the interface between the thin film and the substrate. Such a crack in-
itiation process markedly influence the fatigue life enhancement by the the TiN
thin film.

REFERENCES

Bryant, W.A. (1989). Chemical vapor deposition. Surface modification engineering^.

Kossowsky, Ed.), Vol.I. CRC Press, USA, pp. 189-230.
Rigsbee, J.M. (1989). Physical vapor deposition, ibid, pp. 231-256.
Mchargue, C. J. (1989). Ion implantation and ion-beam mixing, ibid, pp. 257-284.
Herman, H. (1981). Surface mechanical properties-effects of ion implantation. Nuclear
instruments and methods, 182/183, pp. 887-898.
Shiozawa, K. and S. Ohshima (1990). The effect of TiN coating on fatigue strength of
carbon steel, Fatigue 90(H. Kitagawa and T. Tanaka eds.), Vol.1, pp. 299-304.
WS7e3
THE INFLUENCE OF APPLIED STRESS RATIO ON FATIGUE
STRENGTH OF TiN COATED CARBON STEEL

Kazuaki SHIOZAWA, Seiichi NISHINO

Faculty of Engineering, Toyama University, 3190 Gofuku,

Toyama, Japan.

and

Keiichi HANDA

Kawasaki Heavy Industries, LTD., 2-1-8 Wadayamadori,

Hyogo-ku, Kobe, Japan.

ABSTRACT

The influence of applied stress ratio on the fatigue strength of carbon

steel coated with TiN was studied on the bases of measurement of crack
initiation with D.C. potential method. Fatigue tests were performed under
the stress ratio of R=0 and -1 in air using the round notched specimens of
0.37%C steel normalized, JIS S35C, coated with TiN by PVD and CVD. From the
experimental results, increase of fatigue strength was observed in TiN
coated specimens under the tests of R=-l, as compared with that of uncoated
specimen. However, the fatigue life of coated specimens by PVD was
decreased under the tests of R=0, except for the region of low stress
amplitude. Also the fatigue life of coated specimens by CVD under R=0 was
smaller than that of the uncoated one. The difference of fatigue life with
applied stress ratio is explained by the fracture behavior of coating film
on the specimen surface.

KEYWORDS

Fatigue; TiN coated carbon steel; physical vapor deposition; chemical vapor
deposition; D.C. potential method; crack initiation; stress ratio.

INTRODUCTION

It is well known that the coating of TiN or TiC applied by the physical
vapor deposition (PVD) or chemical vapor deposition (CVD) for various kinds
of machine components improves the wear resistance, cutting ability or
cavitation-erosion resistance. This is due to the facts that these coatings
adhere well to steel substrate and that the surface hardness of these
coatings is much higher than that of conventional coatings. Recently, there
have been some studies on the role of surface coating in affecting fatigue
life. These investigations on the fatigue of steels coated with TiN or TiC
by PVD or CVD have reported fatigue lifetimes to be increased (Shiozawa et_
al., 1990), decreased (Hashimoto et al., 1990) or sometimes unchanged by the
residual stresses in the surface layer and substrate, hardness of coating

493
494
film and structural change in substrate with coating treatment. Also, it is
expected that the fatigue lifetimes are affected by the fracture behavior of
coating film during fatigue process. The various mechanisms by which
ceramics coating can affect the fatigue behavior have yet to be documented
in any systematic way. The aim of this investigation is to clarify the
fatigue behavior of steel coated with TiN by PVD or CVD, in order to apply
the ceramics coating to machine components and structures.

In this study, fatigue tests were carried out under two revels of stress
ratio using the specimens of 0.37% carbon steel coated with TiN by PVD and
CVD in order to study the influence of applied stress ratio on the fatigue
strength.

EXPERIMENTAL PROCEDURE

Testing Material and Coating Condition

The substrate material used in this investigation was 0.37% carbon steel,
JIS S35C, normalized at 1138K for 30min. The chemical compositions of this
steel is 0.37%C, 0.24%Si, 0.77%Mn, 0.019%P, 0.023%S, 0.1%Cu, 0.2%N and
0.4%Cr. Specimens were smooth bar with 10mm diameter and 100mm gauge length
for static tensile test, and round notched bar with 8mm minimum diameter, of
which stress concentration factor is 1.5 for fatigue test. Before TiN
deposition the substrates were polished with emery paper (grade #1000) and
electro-polished.

TiN coating was deposited onto the specimen surface by use of CVD and PVD
process. In CVD coating, specimens were inserted in a stream of mixed gases
of H -N -TiCl, under a reduced pressure of 3.37x10 Pa at 1223K or 1273K for
3 hours. Thickness and Vickers hardness of CVD coated layer were 5-6ym and
Hv(50gf) 2170, respectively. In PVD coating, the hollow cathode discharge
process was employed in vacuum to generate a glow discharge in nitrogen into
which titanium was evaporated at constant substrate temperature of 623K.
Its thickness was 2-3ym and Vickers' hardness was Hv(15gf) 1888.

Testing Method

Two types of fatigue tests were performed under stress controlled condition
in air using the electrohydraulic fatigue testing machine operated at the
frequency 20Hz; one was stress ratio, R=ö . /o =0, and the other was R=-
1. D.C. potential method was employed to observe the crack initiation in
substrate, which was supplied the constant current of 10A to the specimen
and detected the electric potential between the edges of notch. Cracks on
the specimen surface were measured by optical microscope on the replica
which was taken from the surface interrupted at various fractions of fatigue
life. Also cyclic deformation behavior of the specimen was measured by
extensometer.

EXPERIMENTAL RESULTS AND DISCUSSION

Static Tensile Tests

From the results of static tensile tests, PVD coated material has similar
mechanical properties to uncoated material. However, yield stress and
hardness of CVD coated material decreased significantly as compared with
 495

30 T 1 r

"20

? I5
'\n
c
a>
"° 10
σ
Ü 5

"0 0.5 1.0 1.5 2.0

Strain t , %
Fig. 1. Relation between flaw density on TiN coating film
and total tensile strain.

those of uncoated and PVD coated material, because microstructure of

substrate was changed during CVD process.

Figure 1 shows the experimental relation between flaw density on the coating
film and total strain obtained from the observation by optical microscope on
the replica which was taken from the surface interrupted at various strain
during the tensile test. It was found that flaws on PVD and CVD coating
film occurred at the total tensile strain of 0.38% and 0.87%, respectively.

Fatigue Tests

Figure 2 shows the experimental results obtained from the fatigue tests
under the stress ratio of R=0. It can be seen from this figure that the
fatigue life of coated specimens by PVD increased in the region of the
stress range below about 390MPa as compared with uncoated one. On the other
hand, that decreased for the region of high stress range. It is considered
that cyclic deformation behavior of the specimen affects the fatigue
strength, because the value of stress range of 390MPa is similar to the
yield stress of PVD coated specimen. From the measurement of cyclic
deformation behavior during fatigue process, ratchet strain was observed at
stress range over 390MPa, but it was not observed under 390MPa. Fatigue
limit of PVD coated specimen increased about 11%, as compared with uncoated
one. Fatigue strength of CVD coated specimen decreased significantly as
compared with that of uncoated specimen.

Figure 3 shows experimental results obtained by fatigue tests under the

stress ratio of R=-l. It can be seen from this figure that fatigue strength
of coated specimens increase under all of the stress amplitude revel as
compared with uncoated specimens, in contrast with the experimental results
mentioned above. About 18% and 4% increase of fatigue limit was observed in
PVD and CVD coated specimen, respectively, as compared with uncoated one.
In Fig.3, the experimental results obtained from the tests using the
specimen removed CVD coating film by electropolish are also shown. Fatigue
strength of this specimen is smaller than that of uncoated specimen,
because of structural change due to the high temperature during CVD coating
process. To discuss the effect of CVD coating film on the fatigue strength,
496
R=0. in air
500,

Number of cycles to failure Nf

F i g . 2 . S-N diagram under R=0 i n a i r .

in oir
300r™ 9-f'.

5(I0 4 I 0 5 I0 6 I07
Number of cycles to failure Nf

Fig. 3. S-N diagram under R=-l in air.

it is reasonable to compare the results obtained from the specimen coated by

CVD with those treated by same temperature as CVD process. From this point
of view, the fatigue limit of CVD coated specimen is improved about 37% as
compared with that of specimen removed the coating film.

Crack Initiation and Propagation Behavior

In order to discuss the crack initiation and propagation behavior, D.C.

potential method was employed. Table 1 shows the number of cycles to crack
initiation, N., and the number of cycles for crack propagation, N (N =N f -
N.)· Where N 1 was defined from the variation of D.C. potential, ^according
to the recommendation method by the Iron and Steel Institute of Japan(1989).
The values of N. of PVD coated specimen at stress range of 419MPa and CVD
coated one were decreased significantly as compared with that of the
uncoated one. However, the value of N. of PVD coated specimen at 385MPa
was increased significantly. Also N p of coated specimen was similar to that
of the uncoated one. It can be seen from these results that the TiN coating
on the specimen surface affects the crack initiation behavior but it does
not affect the crack propagation behavior.
 497
Table 1. N., N and N £ obtained from D.C. potential method.
i P f
2Ga Ni Np Nf
Material
(MPa) (Ni/N£ ) (Np/Nf )

419 1 .40x105 1 .48x105 2.88x10s

No-coating (0.49) (0.51)
(S35C,Normalizing) 384 4.90x10s 2.58x105 7.48x10s
(0.66) (0.34)
421 1 .50x104 1 .16x105 1 .31x10s
PVD coating (0.11) (0.89)
385 >7.03x106 <6.30x105 7.66x106
(>0.92) (<0.08)
CVD c o a t i n g 414 2.32x104 3.90x104 6.22x104
(1223K) (0.37) (0.63)

Fig. A. Macroscopic observation of fracture surface.

Figure 4 shows macroscopic observation of fracture surface of the tested

specimen. Under the condition that fatigue life is decreased, number of
ratchet marks on the fracture surface of coated material, which are the
results of multiple fatigue crack origins, are larger than that of uncoated
one. On the other hand, it was less than that of the uncoated specimen,
under the condition that fatigue life is increased.

Fatigue Crack Initiation Mechanism of Coated Material

From the experimental results and discussion, fatigue crack initiation

mechanism of coated material can be summarized as Fig.5. Under the testing
condition that large deformation occurs or accumulates during fatigue as
R=0, TiN coating film is fractured at the early stage of fatigue, because
it is too brittle to accommodate the film to substrate metal. Then many
cracks may be induced to initiate at substrate by flaws of coating film
(Fig.5(a)). On the other hand, under the testing condition without large
498

(a) Fatigue strength (b) Fatigue strength

decrease increase
Fig. 5. Schematic illustration of crack initiation of
TiN coated material.

cyclic deformation of the specimen, crack initiation is delayed by hard

coating film on the specimen surface which can act as barriers to egress of
dislocations (Fig.5(b)).

CONCLUSIONS

(1) Mechanical properties of coated material were not changed by coating

film. Flaw on the coating film of PVD and CVD was occurred at total
tensile strain of 0.38% and 0.87%, respectively, under the static
tensile test.
(2) The fatigue life of coated specimens by PVD was increased under the
tests of R=0, except for the region of high stress amplitude. Also the
fatigue life of coated specimens by CVD under R=0 was smaller than that
of the uncoated one.
(3) Increase of fatigue strength was observed in both of PVD and CVD coated
specimens under the tests of R=-l, as compared with that of uncoated
specimen.
(4) The difference of fatigue life of coated specimen with applied stress
ratio is due to the crack initiation behavior in substrate induced by
the rupture of coating film.

REFERENCES

Hashimoto,M., S.Nagashima and M.Shiratori(1990). An X-Ray on Residual Stress

and Fatigue Characteristics of TiC Coated Steels.J.Soc.Mat.Sei.,39,150-156.
Iron and Steel Institute of Japan(1989), D.C. Potential Method of Crack
Initiation Detection in High Temperature Low Cycle Fatigue -ISIJ Recommen-
dation-, pp.9. Iron and Steel Institute of Japan.
Shiozawa,K. and S.0hshima(1990). The Effect of TiN Coating on Fatigue
Strength of Carbon Steel. Fatigue 90, 299-304.
 WS7e4

LONG LIFE FATIGUE STRENGTH OF GAS-CARBURIZED STEEL

K. AS AMI

Department of Mechanical Engineering, Musashi Institute

of Technology, 1-28-1 Tamazutumi, Setagaya-ku, Tokyo 158,
Japan

ABSTRACT

The fatigue strength characteristics of gas-carburized Ni-Cr-Mo steels were

investigated with attentions paied to long life range up to 4x10 9 cycles
(about 3 years) and surface structure anomalies consisting of internal
oxides and nonmartensitic structure. Three kinds of carburizing conditions
were employed, and fatigue tests were conducted at room temperature in
laboratory air under rotating bending stresses. The specimens continued to
fail over 107 cycles and the S-N diagrams revealed some knees on the curves.
When surface structure anomalies were ground-off, the fatigue strengths were
improved in fatigue life range below about 105 to 109 cycles and no knees
were recognized on the S-N diagrams. Regardless the presences of surface
structure anomalies, no fatigue limits were found even at 4x10 3 cycles.
These reasons were discovered from view points of fracture origins and the
values of predicted fatigue limits were about 500 MPa to 650 MPa.

KEYWORDS

Fatigue; carburizing; S-N diagram; long life rang; fatigue limit; fracture
origin; internal oxides ; fish-eye; corrosion fatigue crack; moisture.

INTRODUCTION

Gas-carburizing is often used as a mean of obtaining high fatigue strength

in steels. The fatigue strength characteristics of gas-carburized steels in
the long life range over 107 cycles, however, have hardly been clarified
(Naito et al., 1984, Asami, 1985, Masuda et al., 1986, Asami and Emura,
1990). On the other hand, it is well-known that formation of surface
structure anomalies consisting of internal oxides and nonmartensitic
microstrueture can not be sufficiently avoided during gas-carburizing
process (Fischer, 1978) and causes reduction of fatigue strength in gas-
carburized steel (Naito et al., 1984, Asami, 1985).

499
500

(a) Carburizing and Quenching (I)t=870°C,T=1hr

(n)t=900°C,T=3hr
ITC)
840T
CDI) t=930°C#T=75hr

L0.25hr O.Q.

(b) Tempering

160T

A.C.

Fig. 1. Conditions of heat treatment.

This study, therefore, aims to clarify the fatigue strength characteristics

of low-alloy steel carburized in generated gas, with particular attentions
paid to long life range over 1 0 7 cycles and depth of surface structure
anomalies.

MATERIAL AND PROCEDURE

The steel used was JIS SNCM 420 steel containing 0.20 C, 0.30 Si, 0.55 Mn,
1.64 Ni, 0.53 Cr, 0.16 Mo by weight percent and was carburized in generated
gas with 0.8% carbon potential. Three kinds of carburizing conditions (types
j , 2 an( i 5Γ ) shown in Fig. 1 were employed in this study. The Vickers
hardness distributions after these heat treatments are given in Fig. 2. The
hardness values near the surfaces decreased, because of the presences of
surface structure anomalies consisting of internal oxides and nonmartensitic
microstructure. The internal oxides precipitated along grain boundaries and
the nonmartensitic microstructure was given rise to around them (see Fig.
3 ) . In type I of specimens, the depths of internal oxides and nonmartensitic
microstructure, the effective case depth (550 HV) and the total case depth
were about 5 um, 15 um, 0.3ramand 0.6 mmm, respectively. In types 1 and!
of specimens, they were about 8 um, 30 um, 0.8 mm, 1.6 mm and 15 um, 70 um,
1.3 mm, 2.0 mm, respectively.

The sand-glass type of fatigue specimens with a diameter of 8 mm were used

in this study. The surface layer of some carburized specimens was ground off
to a depth of 0.1 mm, in order to clarify the influence of surface structure
anomalies on the fatigue strength characteristics. The both specimens are to
be called "unground-off specimen" and "ground-off specimen1*, respectively.

Rotating bending fatigue machines of 98 N-m in load capacity and 2850 rpm in
cyclic speed were used for the fatigue tests, which were conducted at room
temperature in laboratory air. Then, the features of fracture origins were
observed by a scanning electron microscope.
 501

νυυ
SNCM420 Carburizing
_800 (I)B70*C-1hr
(Π) 900*C-3hr
ο (D 930*C-7.5hr
_» 700
>
- 600 \jl)
co
V)
\(Π)
■ο 500
3Ζ VilL
400
! 1 _ 1 _ 1 1

0.5 1.0 1.5 2.0

Depth below Surface (mm)

Fig. 2. Outlines of Vickers hardness distributions.

y
Non-martensitiCs
microstructure

Austenite grain boundary

Fig. 3. Schematic illustration of the surface structure

anomalies consisting of internal oxides and
nonmartensitic microstructure.

EXPERIMENTAL RESULTS AND DISCUSSIONS

Results of fatigue tests are shown in Figs, k to 6. The fatigue strengths

dropped even in long life range over 10 7 cycles. The S-N diagram of the
unground-off specimens carburized at 870°C for 1 hr revealed two knees, and
that of the unground-off specimens carburized at 900°C for 3 hr or at 930°C
for 7.5 hr three knees. On the other hand, no knees were recognized on the
S-N diagrams of the ground-off specimens. The improvements of fatigue
strengths by removing the surface structure anomalies depended on both
fatigue life range and carburing condition. That is, the effects were
discovered only in fatigue life ranges below 10 5 cycles of the specimens
carburized at 870°C for 1 hr and 109 cycles of the specimens carburized at
900°C for 3 hr or at 930°C for 7.5 hr. In other words, it is said that no
502

Number of Stress Cycles N

Fig. 4. S-N diagrams of rotating bending test

in SNCM 420 steel carburized at 870°C for 1 hr.

Number of Stress Cycles N

Fig. 5. S-N diagrams of rotaring bending test

in SNCM 420 steel carburized at 900°C for 3 hr.
 503

Number of Stress Cycles N

Fig. 6. S-N diagrams of rotating bending test

in SNCM 420 steel carburized at 930°C for 7.5 hr.

effect of removing surface structure anomalies can be expected in very long

life range over 10 9 cycles.

Observation results of fracture origins are added to test points in Figs. 4

to 6. The sites of fracture origins were divided into surface and subsurface
of specimens. When fracture origins were at surfaces of specimens, the
fatigue fractures in short life range initiated from the internal oxides
(see the mark "intergranular" in Figs. 4 to 6 ) . Then, those in long life
range also initiated from the intenal oxides, but corrosion fatigue cracks,
which were formed by interaction between corrosion due to moisture and
mechanical crack growth due to cyclic stress (Asami and Eraura, 1990), were
observed after the failed internal oxides (see the mark "featureless" in
Figs. 4 to 6). When fracture origins were at subsurfaces of specimens, the
fatigue fractures initiated from inclusions et al (see the mark "fish-eye"
in Figs. 4 to 6) (Asami and Eraura, 1990).

It is considered that the situations of fracture origins are different due

to both amount of internal oxides and level of cyclic stress. That is, in
the case that depth of internal oxides was shallow (below about 5 um), the
sites of fracture origins in high stress range became the surfaces of
specimens, while those in low stress range became the subsurfaces of
specimens (see Fig. 4 ) . In the case that depth of internal oxides was deep
(over about 8 um), the situations of fracture origin were different only in
intermediate stress range that corrosion fatigue cracks were observed as
mentioned above (see Figs. 5 and 6 ) . Such differences of fracture origins in
504
the unground-off specimens corresponded very well to the presences of knees
that were recognized on the S-N diagrams. On the other hand, when surface
structure anomalies were groung-off, all of the fracture origins shifted
from surface to subsurface. The S-N diagrams of the ground-off specimens
dropped linearly up to 4x10 3 cycles and no fatigue limits were found in this
experiment.

From these results, it can be said that the forms of the S-N diagrams shown
in Figs. 4 to 6 depend on the differnces of fracture origins. Then, In the
case that fracture origins were at subsurfaces of specimens, the fatigue
strengths of unground-off specimens were the same as those of ground-off
specimen. Therefore, fatigue limits of both specimens will be found in very
long life range over 4x10 9 cycles and the values, which is predicted by a
method reported previously (Asami and Emura, 1990), may be abou 500 MPa, 650
MPa and 500 MPa for specimens carburized at 870°C for 1 hr, at 900°C for 3
hr and at 930°C for 7.5 hr, respectively.

CONCLUSIONS

The Ni-Cr-Mo steels carburized in generated gas had surface structure

anomalies consisting of internal oxides and nonraartensitic raicrostructure.
The fatigue strength characteristics depended strongly on depths of internal
oxides and the S-N diagrams revealed two or three knees on the curves up to
4x10° cycles. The presences of knees could be explained by the differnces of
fracture origins. When the surface structure anomalies were ground-off, the
improvement of fatigue strenghs were recognized below 10 b cycles in the case
that the depth of internal oxides was shallow (below about 5 urn) and/or
below 109 cycles in the case that the depth of internal oxides was deep (
over about 8 urn). However, in fatigue life range over them, the fatigue
strengths of unground-off and ground-off specimens were the same. Therefore,
the effect of removing surface structure anomalies can be expected in long
life range. Regardless the presences of suface structure anomalies, no
fatigue limits were found even at 4x109 cycles and the predicted fatigue
limits might be about 500 MPa to 650 MPa.

REFERENCES

Asami, K. (1985). Long-life fatigue strength of tufftrided and carburized

steels. J. Jpn. Soc. Heat Treatment, 24, 123-128.
Asami, K. and H. Emura (1990). Fatigue strength characteristics of high-
strength steel. JSME Inter. J. Series , 33, 367-374.
Fischer R. C. (1978). Internal oxidation during carburizing and heat
treating. Metall. Trans. A., 9A, 1553-1560.
Masuda, C , S. Nishijima and Y. Tanaka,. (1986). Relationship between
fatigue strength and hardness for high strength steels. Trans. Jpn. Soc.
Mech. Eng., 52A, 847-852.
Naito, T., H. Ueda and M. Kikuchi. (1984). Fatigue behabior of carburized
steel with internal oxides and nonmartensitic microstructure near the
surface. Metall. Trans. A., 15A, 1431-1436.
 WS7e5

INTERGRANULAR FRACTURE OF CARBURIZED STEEL

N.MURAI
Kokura Steel Works Sumitomo Metal Ind.,Ltd.
Konomicho 1, Kokurakitaku, Kitakyushushi, Japan

ABSTRACT

Effects of Cr and B on fatigue and bending strength of carburized steels were studied. JIS SCR420
grades with varied Cr content and B added were examined. Specimens were carburized for two hours
at 1203K, quenched in brine and tempered at 443K for two hours. Fatigue limit and bending strength
were increased while intergranular fracture susceptibility of the carburized case was decreased by
decreasing Cr content and by adding B. Auger electron spectroscopy showed that intergranular
fracture was caused by carbide formation at austenite grainboundaries during carburising process.

KEYWORDS

Carburization ; intergranular fracture ; fatigue limit; chromium ; boron ; bending strength

INTRODUCTION

Carburized steel has long been used to produce high bending fatigue strength, surface strength and
good wear resistance for machine components. When cracks initiate from the surface of carburized
components under overloading or fatigue, it is generally thought that the life of the components is
affected by crack initiation in the case and crack propagation through the case. Therefore, fracture
modes of these stages have been studied.

Although there are many causes of cracks initiating in the case; internal oxidation (Namiki et al.,1986),
microcracks in high carbon martensite (Apple et al.,1973), and so on, L.Magnusson and T.Ericksson
(1979) have shown that austenite grainboundaries are important. Furthermore, with regard to crack
propagating through the case, the fracture mode is very often found to be intergranular (Marcus et
al.,1975). Thus, the susceptibility of prior austenite grainboundaries to fracture is important to both
overload fracture and fatigue of carburized components.

505
506
The causes of intergranular case fracture in carburized steels have also been studied. Recent studies
(Krauss,1978, Obermeyer et al.,1979, 1980) have shown that carbon and phosphorus are concentrated
above their bulk concentration in the austenite grainboundaries and carbon is present in the form of a
carbide by phosphorus segregation. In this paper, the effects of alloy element Cr and B on
intergranular fracture of carburized case, and its correlation with strength were studied because the
effects of alloy element on the intergranular fracture have not been well-known. The causes of
intergranular case fracture of carburized steels have been difficult to determine because there have
been no microstructual features identifiable by light or electron microscopy at prior austenite
grainboundaries, except for the correlation of intergranular fracture to well-developed cementite
networks produced in the high carbon potential atmosphere. Therefore, Auger electron spectroscopy
(AES) was used (Obermeyer et al.,1980) to analyze the chemical composition of a very thin layer of
the intergranular fracture surface.

EXPERIMENTAL PROCEDURE

The chemical compositions of steels are shown in T&blel. The steels were varied Cr content and
added B. Those steels were prepared by vacuum induction melting and hot forged to 30mm diameter
bars. Normalizing was carried out by holding the temperature at 1198K for one hour followed by air
cooling. The uniform moment rotating bending fatigue test specimens with a 1mm radius semicircle
notch and the three-point bending test specimens the configuration of which was 10mm square and
55mm long with a 2mm radius semicircle notch, were machined from the center of the normalized
30mm diameter bars. These specimens were carburized for two hours at 1203K under a controlled
atmosphere (carbon potential = 0.9%), quenched in brine and tempered for two hours at 443K. The
grips of the fatigue test specimens were ground in order to eliminate the thermal distortion. AES was
performed on the cylindrical specimens with a notch root of 1.6mm diameter. The specimens were
carburized for four hours at 1203K in the same atmosphere as that for the fatigue and bending test
specimens, quenched in oil and tempered for two hours at 443K. Then, they were broken under a
vacuum of lO^MO^torr and analyzed with an electron beam of lOkV / ΙΟΟηΑ.

Table 1. Chemical Compositions of Steels

Alloying Element (weight %)

C Si Mn P S Cr Ti solAl N O B

A 0.22 0.10 0.80 0.020 0.017 0.01 - 0.034 0.0096 0.0016

B 0.22 0.10 0.82 0.020 0.016 0.49 - 0.032 0.0097 0.0015
C 0.21 0.10 0.83 0.024 0.015 0.99 - 0.033 0.0107 0.0016
D 0.23 0.10 0.85 0.024 0.017 1.50 - 0.035 0.0115 0.0016
E 0.21 0.09 0.80 0.019 0.015 0.98 0.032 0.050 0.0056 0.0016 0.0025

RESULTS AND DISCUSSION

 507
Fatigue and Bending Test Results

The effects of Cr and B on the fatigue limit and the bending strength are shown in Fig.l and Fig.2,
respectively. The fatigue limit and the bending strength were increased by decreasing Cr content and
adding B. Scanning electron micrographs of the case fatigue fractured surface of each steel are shown
in Photo. 1. Intergranular fracture facets were smooth and flat, and precipitations were not observed
such as network cementite developed under the high carbon potential atmosphere. Intergranular
fracture was dominant in the case of 1.0% Cr steel, and the amount of it was decreased by decreasing
Cr content and adding B . It was concluded that the intergranular fracture susceptibility of the case
was decreased by decreasing Cr content and adding B, which was thought to result in the improved
fatigue limit and bending strength.

600 i 20
•
Q- °-^^_ I adding B

500 Pv
» 1.5
add ing B •^ z o
:>
400 ' ^<3
- i 1.0 °
o
^ ^ O re
ύ
300i 0.5
0 0 .5 10 1.5 0 0.5 1.0 1.5
Cr c ontent :wt%3 Cr content Cwt %3

Fig.l. Effects of Cr and B on fatigue limit Fig.2. Effects of Cr and B on crack initiation
for uniform moment rotating load for three-point bending test. The load
bending fatigue test. was applied with a strain rate of
0.33mm/sec. The support span was 40mm.

15um
i——-i
Photo. 1. Scanning electron micrographs of fatigue fracture surface at the
depth of 0.3mm from the surface, (a) is 0% Cr steel, (b) is 1.0%
Cr steel and (c) is 1.0% Cr - B steel, respectively.

Fatigue limit and bending strength are influenced by the case and core properties ; hardness profile
(Cameron et_aj.,1983, Diesburg et al.,1978, Furukawa et al.,1980), surface residual stress (Ebert,1978,
Cameron et al.,1983), prior austenite grain size (Urita et al.,1987) and depth of the internal oxidation
(Namiki et al.,1986). The case and core properties of each steel are shown in Table2. Surface hardness
and surface residual stress were not correlated with Cr content and B added in this investigation. On
the other hand, effective case depth, core hardness, austenite grain size and depth of internal oxidation
508
were correlated with Cr content and B added. Not only intergranular susceptibility of the case but also
these properties are thought to be related to fatigue limit and bending strength. The quantitative
contribution of intergranular fracture susceptibility of the case to the strength of the carburized steel
was not made clear by this investigation.

Table 2. Carburized Case and Core Properties

Surface Effective Core Residual Austenite Depth of

hardness Case Depth Hardness Stress Grain Size Internal
(JIS) Oxidation
Hv mm Hv MPa No. urn

A 698 0.59 282 -617 8.4 0

B 715 0.63 414 -932 8.1 2.1
C 720 0.61 435 -794 8.8 2.7
D 710 0.70 457 -776 9.1 3.4
E 744 0.59 441 -732 6.3 2.7

Surface hardness is defined as the hardness at the depth of 0.025 mm from the surface.
Effective case depth is defined as the depth of occurence of a hardness value of 550 Hv.
Residual stress is the peak value obtained from a residual stress gradient.

AES results

Differentiated Auger electron spectra from intergranular and transgranular fracture surface of 1.0% Cr
steel are shown in Fig.3 and Fig.4, respectively. The biggest difference in these spectra was the

ΙΛΚ—' "ir#mmi*Nr> Λ** yv^fp*ii ΊΠΤΤΠ

if r Cr' f l!
V
\

IFe FelFe

0 100 200 300 400 500 600 700 800 900 1000
Electron energy (ev)

Fig.3. Differentiated Auger electron spectra from intergranular

fracture surface of 1.0% Cr steel.
 509
increased carbon content on the intergranular fracture surface relative to that on the transgranular
fracture surface. Futhermore, the shape of the carbon peak of intergranular fracture surface indicated
that the carbon was present in the form of a carbide that was probably cementite. These results are
consistent with H.Obermeyer and G. Krauss's result (1980). Carbon is concentrated on the austenite
grainboundaries and formed cementite during carburizing process. The effects of Cr and B on the
peak height ratio of C to Fe are shown in Fig.5. Carbon content in the prior austenite grain

1 ***v
1 ii /

r
***** *wm
W\
A\Kcfi/ht

Γψ*
M li HI wjit m..u .« II. J
*ΡφΡΙΤ*ΥΡΙ · · ■ ' * l]

\
Cr If 1 1
z

!Fe Fe Fe

0 100 200 300 400 500 600 700 800 900 1000
Electron energy (ev)

Fig.4. Differentiated Auger electron spectra from transgranular

fracture surface of 1.0% Cr steel.

0.25

>0.20
c)
3
1 '
»V—ί \
p
0.15
t

Γ
^ ^ Λ add i ng B

0.10 p /
t
»

0.05

0.5 1.0 1.5 2.0

Cr content Cwt % ]

Fig.5. Effects of Cr and B on Auger peak height ratio (Ic/Ife) from

the intergranular fracture surface.
510
boundaries was decreased by decreasing Cr content and adding B. This tendency is consistent with the
susceptibility of intergranular fracture in the carburized case observed after the fatigue test. It is
thought that one of the reasons why fatigue limit and bending strength are increased by decreasing Cr
content and adding B is that the amount of carbide on the prior austenite grainboundaries decreases.

CONCLUSIONS

Fatigue limit and bending strength of the carburized steel are increased by decreasing Cr content and
adding B.

Intergranular fracture susceptibility of the carburized case is decreased by decreasing Cr content and
adding B, which is thought to result in the improvement of fatigue limit and bending strength.

AES results show that Intergranular fracture in the case is caused by carbide formation at austenite
grainboundaries during carburizing process, and that the amount of C at the austenite grainboundaries
is decreased by decreasing Cr content and adding B. This tendency is consistent with Intergranular
fracture susceptibility of the case.

REFERENCES

Apple,C.A. and G.Krauss (1973). Microcracking and fatigue in a carburized steel. Met. Trans., 4,
1195-1200.
Cameron,T.B., D.E.Diesburg and C.Kim (1983). Fatigue and overload fracture of carburized steels.
J.Met, 37-41.
Diesburg,D.E. and G.T.Eldis (1978). Fracture resistance of various carburized steels. MetTrans., 9A,
1561-1570.
Ebert,L.J. (1978). The role of residual stress in the mechanical performance of case caburized steels.
MetTrans., 9A, 1537-1551.
Furukawa,T., S.Konuma, H.Sakaniwa andT.Kasuya (1980). Effects of case depth and notch shape on
the rotating bending fatigue properties of carburized steel. Tetsu-to-Hagane, 65, 410-417.
Krauss,G. (1978). The microstructure and fracture of a carburized steel. MetTrans., 9A, 1527-1535.
Magnusson,L. and T.Ericksson (1979). Initiation and Propergation of fatigue crack in carburized steel.
Proceedings, Heat Treatment (1979), The Metal Society, London.
Marcus,H.L. and J.M.Harris (1975). Fracture of case-hardened steels. Scr.Metall., 9, 563-568.
Namiki,K. and K.Isokawa (1986). Effects of alloying elements on the rotating bending fatigue
properties of carburized steels. Trans.Iron Steel InstJpn., 26, 642-648.
Obermeyer,H.K., T.Ando and G.Krauss (1979). Fracture of high-carbon martensitic steel. Proceedings,
International conference Martensitic Transformation. 732-737.
Obermeyer,H.K. and G.Krauss (1980). Intergranular fracture of carburized steel. Proceedings,
International conference on heat treatment of materials. 209-224.
Urita,T., K.Namiki and T.Ikubo (1987). Effect of austenite grain size on mechanical properties of
carburized steels. Proceeding, The 114th ISIJ Meeting S1297.
 WS7e6
EFFECTS OF MICROSTRUCTURE ON LOW AND HIGH CYCLE FATIGUE
BEHAVIOUR OF A MICRO-ALLOYED STEEL

G. CHALANT* and B.M. SUYITNO**

*Professor, LM3 Laboratoire de Microstructure et Mecanique des

Materiaux, URA CNRS 1219, ENSAM, 151 Bd. de l'höpital
F-75013 Paris, FRANCE
**Engineer, Directorate of aviation safety, Jakarta, INDONESIA

ABSTRACT
The low and high cycle fatigue behaviour of a micro-alloyed steel have been studied with Bainitic
and ferrito-pearlitic microstructure obtained after hot rolling with different cooling rates.
Low Cycle Fatigue (LCF) experiments have been carried out under tension-compression (Re^-1)
loading, for low testing frequency (f<0.1 Hz), under Air atmosphere (few experiments were
carried out under vacuum), in the fatigue life range Nr=10 to 105 cycles.
High Cycle Fatigue (HCF) experiments have been carried out under tension-compression
(Ro=-l) and under alternate torsional (RT=-1) loadings, for high testing frequency (f=40-50 Hz),
under Air atmosphere, in the fatigue life range Nr=105 to 108 cycles.
All the results show that microstructure has a very little influence on the fatigue limit (high cycle
fatigue) for this steel. On the other hand, microstructural changes have strong influence on the
low cycle fatigue response in fatigue life and cyclic stress-strain behaviour.
This cyclic stress-strain behaviour can be rationalized taking into account for hardening
precipitate state and yield stress of both microstructure.

INTRODUCTION
Medium Carbon content range (0.2 to 0.5 %) steels, improved by heat treatments, are currently
used in mechanical industry. Those treatments are necessary to obtain good mechanical properties
such as, yield stress and fatigue limit, but are energy consuming.
Micro-alloyed steels (with Niobium and Vanadium content under 0.1 %) have been developed in
order to avoid such heat treatment, assuming that mechanical properties are good enough to suit
requirements for mechanical parts of structures.
It is easy to demonstrate that monotonic properties are quite good, but cyclic properties
comparison is more complex to deal with.
The purpose of this paper is to give some insight on low and high cyclic properties of a micro-
alloyed steel as compared to a more conventional quenched and tempered steel.
High cycle fatigue is investigated either under tension-compression and alternate torsion to
evaluate influence of microstructure and stress state on fatigue limit.
Low cycle fatigue is used to investigate microstructure influence on the cyclic plastic response.
It is worth noting that microstructural variation, due to difference of cooling rate during forging,
when thickness variations exist, can be encountered in structure parts. This observation is the
main reason for the investigation of microstructural influence on fatigue properties for this steel.
511
512

MATERIAL AND EXPERIMENTAL METHODS

Material

A micro-alloyed steel, Έ " was used for the experimental work. The steel was rolled from
starting temperature of 1250°C and cooled under Air atmosphere without any additional heat
treatment. Forged bars of 55 mm in diameter give a Ferrito-Pearlitic (EFP) microstructure, and
forged bars of 20 mm in diameter give a Bainitic (EBN) microstructure, with an average grain
size of 25 micrometers in both cases. A conventional steel (BQT) water quenched and tempered
(3 hours at 500°C), exhibiting a martensitic microstructure, was compared with micro-alloyed
steel. All compositions are given in Table I.

Steels C Si Mn S P N Zr Al V B Nb
EFP & EBN 4.55 3.0 15.0 0.38 0.21 0.20 0.10 0.41 1.16 0.08 0.42
BQT 4.45 2.6 15.7 0.33 0.14 0.13 — 0.27 — 0.02 —

Table I: Analytical composition of EFP, EBN micro-alloyed steels, and

conventional BQT quenched and tempered steel (10~3 weight).

The mechanical behaviour of the micro-alloyed steel can be adjusted through change of Vanadium
and Niobium content which give hardening precipitates (Charlier, 1985), and monotonic and
cyclic mechanical behaviour of conventional steel is given by heat treatments (Martin, 1983-a).
Monotonic mechanical properties are given in Table II (yield stress CJy, ultimate stress Qu,
elongation "A", section reduction "Z", average microhardness μΗν, rupture energy KCV).

Steels Qy Qu A Z μΗν KCV

MPa MPa % % vickers mJ/m2

EFP 771 1046 14 39 354 8

EBN 687 1005 11 27 313 13
BQT 882 998 15 48 —- 88

Table II: Monotonic mechanical properties of EFP, EBN micro-alloyed

steels, and conventional BQT quenched and tempered steel.
Experimental methods

High Cycle Fatigue (HCF) experiments have been carried out under tension-compression
(Ra=-1) loading, on an electro-mechanic machine, with testing frequency f=40 Hz, on a hour
glass shaped specimen (4 mm in diameter); and under alternate torsional (Rx=-1) loading, with
testing frequency f=50 Hz, on a cylindrical specimen (7.5 mm in diameter).
Experiments were conducted under load or torque control, at room temperature (20° C), under
laboratory Air, with moisture percent M=60 %, in the fatigue life range Nr=105 to 108 cycles.

Low Cycle Fatigue (LCF) experiments have been carried out on a servo-hydraulic testing
machine, under cyclic plastic strain range (Δερ) control, with strain ratio Re=-1 , at low testing
frequency (f<0.1 Hz), on a cylindrical specimen (6 mm in diameter).
Experiments were conducted at room temperature (20°C) under Air atmosphere, with moisture
percent M=60 % (few experiments were carried out under vacuum P<10 3 Pa), in the fatigue life
range Nr=10 to 105 cycles.
Flow stress have been continuously recorded during fatigue testing.
 513

RESULTS AND DISCUSSION

Fatigue life and fatigue limit

It can be seen, on Figure 1. that in the LCF region, conventional BQT steel (Martin, 1983-b)
takes place in between the two microstructural states EFP and EBN of the micro-alloyed steel.
This behaviour can be attributed to differences in material fatigue damage (or cyclic plastic
deformation) for a given stress level.
In the HCF region, micro-alloyed steel reach a unique fatigue limit (850-900 MPa), under
tension-compression loading, whatever microstructural state is considered, when the
conventional steel exhibit a higher (+25%) fatigue limit value (1100 MPa).
It can be seen, on Figure 2. that in the HCF region, under alternate torsion, micro-alloyed steel
reach an almost unique shear stress limit in fatigue (Δτ=600-610 MPa).

1 2 3 4 s 6 7 s
10° 10 10 10 10 10 10 10 10

Fig.l. LCF and HCF life curves under Fig.2. HCF life curve under torsional loading
tension-compression loading

Fatigue limit results are summarized in Table III, and comparison is done with monotonic
mechanical properties of materials.

Steels ΔσΡ ΔτΡ ΔσΡ ΔσΡ ΔτΡ ΔτΡ

MPa MPa 2.ay 2.au 2.ay 2.au

EFP 905 610 0.59 0.43 0.40 0.29

EBN 850 600 0.62 0.42 0.44 0.30
BQT 1100 0.62 0.55

Table III: Fatigue limits and ratios of EFP, EBN micro-alloyed steels,
and conventional BQT quenched and tempered steel.

For those steels, either under tension-compression and alternate torsional loadings, fatigue limits
looks pretty much like a mechanical property without any influence of the microstructural state.
One can see, on Table ΙΠ, that the ratio of fatigue limit over yield stress is almost constant (0.60)
for a Ferrito-Pearlitic, Bainitic and Martensitic steel as well.
On the other hand one must pay attention to differences in fatigue life, by a factor of ten, in the
LCF region, companng EBN and EFP micro-alloyed steels, and one must consider that BQT
martensitic steel lay in an intermediate position.
514

Low cycle fatigue behaviour.

In this LCF region, cyclic plasticity occur, and fatigue life comparison is not straightforward, and
is to be done taking into account for: flow stress, plastic strain and total strain under fatigue
loading.
Fatigue life variation with cyclicflowstress range (Δσ) has been already presented on Figure 1.
One can also use the cyclic plastic deformation (Δερ) to account for the fatigue behaviour in order
to compare fatigue resistance of EBN, EFP and BQT steels. It can be seen, on Figure 3 in a
Manson-Coffin diagram using Δερ as the fatigue parameter, that fatigue resistance of EBN is
better than fatigue resistance of EFP. This observation is in total contradiction with conclusions
drawn from Figure 1 whereflowstress is the fatigue parameter.
It must be noticed that in both cases conventional steel BQT lay in an intermediate position.

&p ί \ ' 1
1
EFP

^
fflN
\^v

Cycles |
1
10°
-i -■
10'
J*
2
10
3
10 10
4 5
10 10'
2
10
3
10
4
JO 10
5

Fig.3. LCF cyclic plastic strain Δερ Fig.4. LCF, cyclic total strain b£x
versus fatigue life Nr. versus fatigue life Nr.
Let remind that any fatigue experiment (and industrial problem as well) is successively composed
by three stages: -first, initiation of a microcrack (definition of which is still under discussion)
-secondly, propagation of the crack -thirdly, final rupture of the sample (structure part).
In the HCF region, thefirststage is, by far, of major importance (more than 90% of the life).
In the LCF region, initiation and propagation can be of equal importance, and relative proportion
of fatigue life can be 20%-80% for short life (Nr.=10 cycles) to 80%-20% for longer life
(Nr.= 104 cycles) for Initiation-Propagation life comparison.
But initiation is primarily govern by local (HCF) and global (LCF) plasticity, thus the larger
plastic deformation the shorter initiation life is.
On the other hand, propagation stage is primarily govern by local stress field at the crack tip
which is directly related to the applied cyclic stress.
Total cyclic strain range is a composite fatigue parameter where plastic strain andflowstress are
presents since one can write : b£\ = Δερ + Δσ / E.
Therefore, this parameter (Aet) can take into account for initiation (Δερ) and propagation (Δσ) at
the same time.
One can see, on Figure 4. in the LCF region, that fatigue behaviour of EFP, EBN and BQT is
very similar, and can be considered as identical, from the point of vue of total cyclic strain
range Δει, (Chalant, 1986-b) and (Suyitno, 1988).
 515

Cyclic stress strain behaviour

Different microstructures of the considered micro-alloyed steel are obtained through diameter
differences of the forged bars used in this study. Then there is a variation of Cooling rate
(Cr=20°C/mn for EFP and Cr=55°C/mn for EBN) after forging process, in the temperature range
800°C down to 500°C in which Niobium and Vanadium precipitate (Charlier, 1984).
Cooling rate change lead to two characteristics of the microstructural state of the steel:
- as a medium carbon steel, one obtain a Bainitic structure for the higher Cr (EBN) and a Ferrito-
Pearlitic structure for the slower Cr (EFP)
- as a micro-alloyed steel: -for higher Cr (EBN) afinehardening precipitation of Niobium takes
place (without Vanadium precipitate) -for slower Cr (EFP) a coarser hardening precipitation of
Niobium and Vanadium is obtained.
The consequences of this double microstructural state characteristics can be revealed by two
mechanical tests:
-For small monotonic plastic strain, Yield stress ay is sensitive to microstructural state of the
steel, and Table Π show that Bainitic structure (EBN) is softer than Ferrito-Pearlitic one (EFP).
-For cyclic plastic strain flow stress Δσ becomes very sensitive to the hardening precipitate state.
Figure 5 show that, for two levels of the applied constant cyclic plastic strain range Δερ, material
mechanical behaviour is completely different for the two alloy states EBN and EFP.

Fig.5. LCF cyclic stress range Δσ Fig.6. LCF rationalized cyclic stress-strain
variation of EBN and EFP curve for EBN and EFP
For EFP material with coarse hardening precipitate of Niobium and Vanadium, the cyclic stress
range Δσ increases with the number of cycles, and rapidly stabilize (after 5% of fatigue life) for
the applied cyclic plastic strain ranges Δερ.

For EBN material with fine hardening precipitate of Niobium, the cyclic stress range Δσ
increases, reach a maximum value then continuously decreases. This behaviour occur even for
very low applied cyclic plastic strain ranges Δερ.
One can consider that this behaviour is mainly due to dislocation multiplication and accumulation
against hardening precipitates.
When precipitates are too coarse to be sheared (EFP) a cyclic stress plateau is reached.
In the case of fine hardening precipitation (EBN) dislocation accumulation gives an increase of
cyclic stress range, as in the former case, then when then the critical shear stress is reached, for
the considerate precipitate, thus after a maximum value Aamax, the cyclic flow stress range Δσ
decreases during all the test (Thielen, 1976) and (Stoltz, 1978).
516

Therefore it has been considered that comparison of the cyclic stress-strain response of micro-
alloyed steels, for all microstructures, must be done taking into account for: -hardening
precipitate characteristics, thus ÄGmax is the intrinsic cyclic stress range -initial general
microstructure, thus cyclic flow stress must be normalized using monotonic yield stress Δσγ of
the material.
Then, Aomax I 2.Δσγ should be a good parameter in order to compare cyclic stress-strain
response of EBN and EFP steels (Chalant, 1986-a).
Actually it can be seen, on Figure 6, that cyclic stress-strain behaviour of micro-alloyed steels in
the two microstructural states is given by a unique curve representing experimental data.
Conclusions
On the fatigue phenomenon point of vue it can be said that micro-alloyed steels exhibit a
behaviour that can be successfully compared to more conventional Quenched and Tempered BQT
steels. Small fatigue limit differences are encountered, and microstructural natural variation after
forging of structural parts do not lead to variation of fatigue properties, either fatigue limit, or
fatigue life or cyclic stress-strain response of the material.

ACKNOWLEDGEMENTS
This work have been done in LMPM, Laboratoire de Mecanique et Physique des Materiaux,
URA CNRS 863, ENSMA, Poitiers, FRANCE.
The authors would like to thanks AFME for financial support, FIAS for Dr. B.M. Suyitno grant,
Dr. P. Charlier and SAFE for supply of micro-alloyed steel, Dr. P. Violan for Low Cycle Fatigue
testing under vacuum, and Dr. J. Petit for helpful discussions during this study.

REFERENCES
Thielen, P.N., Fine, M.E. and Fournelle, R.A. (1976). Acta Metallurgica. 24 (1976) pp. 110.
Stoltz, R. and Pineau, A. (1978). Material Science and Engineering. 34 (1978), pp.275.
Martin, J., Petit, J. and De Fouquet, J. (1983-a). "Cyclic behaviour of a medium carbon micro-
alloyed steel", Material Science and Engineering. 61 (1983), pp.237-246.
Martin, F. (1983-b). "Cyclic behaviour of medium carbon content micro-alloyed steels", these de
Docteur Ingenieur, Universite" de Poitiers, ENSMA, 1983, FRANCE.
Charlier, P. (1984). "Use of low alloying elements Nb, V, B, Al and Zr in a 0.45% C steel"
these de Docteur Ingenieur, Institut National Polytechnique de Lorraine, 1984, FRANCE.
Charlier, P. and Bäcker, L. (1985). 7th International Conference on Strength of Metals and
Alloys. ICSMA 7. \bl. II, pp. 1019-1024, Montreal, CANADA, August 1985, Pergamon
Press.
Chalant, G., Suyitno, B.M. and Petit, J. (1986-a). "Fatigue behaviour of micro-alloyed steels
with various microstructures", AFME report Nb 3.218.2768, February 1986.
Chalant, G., Petit, J., L'Alloret, P., Guimier, A., Charlier, P. and Bäcker, L. (1986-b).
"Developpement of micro-alloyed for mechanical industry". AFME seminar, Sophia-Antipolis,
FRANCE, may 1986.
Suyitno, B.M. (1988). "Fatigue behaviour of micro-alloyed steels" these de Doctorat, Universite
de Poitiers, ENSMA, 1988, FRANCE.
 WS7e7

Microstructual Effect on Extremely Low Cycle Fatigue

of Dual Phase Steel

Jun K0M0T0RI, Masato Υ0Κ0ΥΑΜΑ and Masao SHIMIZU

Department of Mechanical Engineering, Keio University
3-14-1, Hiyoshi, Kouhoku-ku, Yokohama, 223, Japan

ABSTRACT
Low cycle fatigue tests were carried out under the push-pull loading
condition for the steel with a ferrite-martensite duplex
mlcrostructure having various hardness ratios of martensite to
ferrite. Metallographic observation of a microfracture behavior
was also performed on the longitudinal section of the specimen after
a given number of strain cycles. It was found that a surface to
internal fracture mode transition in an extremely low cycle regime is
a typical phenomenon for the dual phase microstructure having a
relatively large brittle second phase and a ductile matrix. The
relation between a fracture ductility in the static tension test and
a fatigue live in the extremely low cycle regime where a final
fracture occurs in an internal fracture mode has also been discussed.

KEYWORDS
Fatigue; Low Cycle Fatigue; Fracture Mode Transition; Ferrite-
martensite Duplex Microstructure; Manson-Coffin Law; Ductility;
INTRODUCTION
It has been reported by the authors (Shimada et al.,1987, Kunio et.
al.,1988) that in an extremely low cycle fatigue regime where fatigue
life is less than about 10 2 cycles, a fatigue process is accompanied
by the static fracture mode and that a transition of surface to
internal fracture mode occurs with an increase in plastic strain
range Δ ε ρ in an annealed low carbon steel (See Fig.l). In this
regime, the final fracture occurs at a strain cycle count less than
that expected from the Manson-Coffin law applied to an ordinary low
cycle fatigue regime in which the development of small surface crack
leads to the fracture of a specimen (Kunio et al.,1988). In such a
situation, a fatigue life is determined by the competition between
two failure limit lines which correspond to the surface and internal
fracture modes respectively (Shimada et al.,1987). Fig.2 shows a
schematic diagram illustrating the above concept where the lines AB
and CD have been drawn as an indication of such failure limit lines.

However, a limited amount of knowledge has been obtained about the

effect of the fracture mode transition on the fatigue life of the
material with duplex microstructure other than ferrite-pearlite
microstructure.
517
518
The aims of present study are, (i) to make clear the damage and
fracture mechanisms of the steels having ferrite-martensite
microstructure with special attention to the role of a variation in
martensite hardness in fracture mode transition and (ii) to discuss
the relation between the fracture ductility and the fatigue life in
the extremely low cycle regime, in which the development of internal
crack leads to the final fracture.
Material and Experimental Procedure
The material used was a low carbon steel having a carbon content of
0.23%. Heat treatment shown in Fig.3 were performed to obtain a
ferrite-martensite duplex microstructure having various martensite
hardness. A typical feature of such a duplex microstructure is
shown in Fig.4, which will be referred to the Material MEF
(Martensite Encapsulated island of Ferrite)) here after. The
mechanical properties of the materials are given in Table 1 together
with the tempering condition (subscript of MEF shows the tempering
condition*). All experiments were conducted for the hourglass
shaped specimens with a dimension and geometry as shown in Fig.5.
After electropolishing the surface, strain controlled low cycle
fatigue tests were conducted under push-pull loading condition by
controlling the change in a minimum diameter of the specimen in a
servo controlled testing machine. Metallographic observation of a
microfracture behavior was also performed on the longitudinal section
of a specimen after a given number of strain cycles.

RESULTS AND DISCUSSION

Effect of the Hardness Ratio of Microstructures on the Fracture Mode
Transition and the Fatigue Life Properties
First, the micro-fracture behavior of a partially fatigued specimen
was examined on its longitudinal section to make clear the effect of
the hardness ratio ( strength ratio ) of microstructures on a
fracture mode transition. Fig.6 shows an example of the transition
from surface to internal fracture mode with an increase in plastic
strain range Δ ε Ρ for Material MEF3-2. Such a transition of
fracture mode was observed at a high level of plastic strain in the
material tempered at a temperature lower than 400°C, but not for the
material tempered at a temperature higher than 500 °C. Fig.7
illustrates a typical feature of the surface fracture mode which was
observed in the high strain extremely low cycle regime in Material
MEF6-2. In Table 2, the critical level of Δ ε Ρ for the surface to
internal fracture mode transition, the tempering condition and the
hardness ratio of microstructures are tabulated. It is found that
a critical level of Δ ε p for the transition becomes smaller with an
increase in the hardness ratio of microstructures. A reason for
this might be the following. As the hardness ratio becomes larger,
the micro-fracture of a martensite and the cleavage cracking of a
ferrite grain occur more easily inside the material and this has an
effect of accelerating the initiation and propagation of internal
crack. Fig.8 shows a typical feature of the micro-fracture of
martensite and the cleavage cracking of ferrite grain, which were
observed inside the material.

Next, the effect of such a fracture mode transition on the fatigue

life will be described. As an example, the results of low cycle
fatigue tests for Material MEF6-2, MEF4-2 and MEF2-1 are shown in

* For example, the subscript 2-1 of MEF2-1 denotes the

tempering at 200 C for 1 hour.
 519
Fig.9, where open and closed marks show the result for surface and
internal fracture modes respectively. The narrow horizontal bands
marked with the slashed lines in this figure show the lowest level of
Δ εp at which the internal fracture mode appears. It should be noted
that in Material MEF6-2 in which no fracture mode transition occurs,
fatigue lives can be expressed by a single Manson-Coffin curve over a
whole range of plastic strain levels. However, in MEF4-2 and MEF 2-1
in which the surface to internal fracture mode transition occurs,
the fatigue life curves are composed of the two straight lines with
different slopes, where a small slope arises from the internal
fracture mode and a large one from the surface fracture mode. As a
result, a fatigue life at a high Δ ε Ρ becomes shorter than that
expected from the Manson-Coffin curve at a low A e p , Such a reduction
of fatigue life can be observed at a smaller plastic strain range as
a hardness ratio becomes greater. This is caused by the fact that an
internal fracture mode appears more easily in the microstructure with
a greater hardness ratio as described before.

Relation between Fracture Ductility and Fatigue Life

The Mason-Coffin equation (Manson,1953, Coffin et al.,1954) relating
a plastic strain range Δ εP with the cycles to failure Nf, can be
written as
Δ ε p-Nr<* = C (1)
The constant C can be evaluated by considering that the upper limit
of the low cycle fatigue test is failure in the tension test, where
Δε ρ =2·ετ and Nf=l/4 cycle (Sachs et al.,1960)(See Fig. 10).
Taking a=0.5, the Manson-Coffin equation becomes

Δ ε ρ -Ν Γ β · 5 = ε r (2)
However,there is no general agreement between the fracture ductility
ε r in a tension test and the constant C of the Manson-Coffin
equation in the ordinary low cycle regime where the final fracture
occurs in a surface fracture mode (Landgraf,1970).
As the reason for this, it can be pointed out that the basic
mechanisms of a fatigue fracture and a monotonic tension fracture are
different each other. In addition to this, it has been proposed
that there are two failure limit lines which correspond to the
surface and internal fracture mode respectively in the materials in
which the surface to internal fracture mode transition occurs (See
Fig.2). Taking these into consideration ,the value of fracture
ductility ε r obtained from the static tension test should be compared
with the constant C of the Manson-Coffin equation taken from the data
of the specimens which had failed in the internal fracture mode.
In Fig.11, a comparison has been made between the constant C of the
Manson-Coffin equation for internal fracture mode and the fracture
strain ε t in monotonic tension test. It is obvious that a good
correlation is obtained between the values of ε r and C. This
suggests that the fatigue life in the extremely low cycle regime
could be predicted using the value of fracture ductility in monotonic
tension test. Fig.12 shows that the predicted fatigue life curves
obtained by eq.(2) are in good agreement with the experimental data
of fatigue life only for the specimen failed in the internal fracture
mode. From these results, it could be concluded that,in a large
plastic strain range where a specimen fails in the internal fracture
mode, the constant C of the Manson-Coffin equation is closely related
to the true fracture strain et obtained from the tensile tests.
520
CONCLUSION
Low cycle fatigue tests were carried out under push-pull loading
condition for the steel with the ferrite-martensite duplex
microstructure having various martensite hardness. On the basis of
the results of raetallographic observation of micro-fracture
behaviour, discussions were made on the effect of second phase
hardness on the fracture mode transition and on the characteristic of
fatigue life in extremely low cycle regime with special attention to
the relation between fracture ductility in static tension and fatigue
lives. The results obtained can be summarized as follows:
(1) A transition of the surface to internal fracture mode was
observed to occur with an increase in plastic strain range for the
steel having ferrite-martensite duplex microstructure. Such a
transition shows a remarkable dependence upon the hardness ratio of
martensite to ferrite.
(2) No fracture mode transition appears in the extremely low cycle
regime for the dual phase steel having a low hardness ratio of
martensite to ferrite.
(3) In a large plastic strain range where final failure occurs in the
internal fracture mode, the constant C of the Manson-Coffin equation
is closely related to the true fracture strain ε r obtained from
tensile tests. The fatigue life curve can then be written in the
form Δ εΡ·ΝΓΒ·5 = ε r .

REFERENCES
Coffin, L.F., Jr., N.Y. Schenectady (1954). A Study of the Effects
of Cyclic Thermal Stresses on a Ductile Metal. Trans. ASME, 76, 931.
Kunio T., M. Shimizu, N. Ohtani and T. Abe (1988). Microstructural
Aspects of Crack Initiation and propagation in Extremely Low Cycle
Fatigue. ASTM, STP 942, 751-764.
Landgraf R.W.,(1970). The Resistance of Metals to Cycle Deformation
ASTM, STP 467, 3-36.
Manson S.S., (1953). Behavior of Material under Conditions of Thermal
Stress. NACA TN 2933.
Sachs G., W. W. Gerberich, V. Weiss and J.V. Latorre (1960). Low
Cycle Fatigue of Pressure Vessel Materials. Proc. ASTM, 60, 512-592.
Shimada k., J. Komotori and M. Shimizu (1987). Fracture mode
transition and damage in extremely Low Cycle Fatigue. In: Low Cycle
Fatigue and Elasto-Plastlc Behavior of Materials (K.T. RIE, ed.),
pp. 680-686. Elsevier Applied Science,London.

Table 1 Mechanical properties of test materials.

Tempering Condition Proof s t r e s s Ult imate t e n s i le F r a c t u r e due t i I i ty
rCxhr) (Mpa) stress (Mpa) ε f
M E F 2-1 2 0 0 x 1 4 0 8 8 3 0 0 . 2 0
M E F 2-2 2 0 0 X 2 3 7 2 8 0 3 0 . 2 4
M E F 3-2 3 0 0 x 2 3 6 7 7 2 9 0 . 3 8
M E F 4-2 4 0 0 X 2 3 2 2 6 6 1 0 . 5 4
M E F 5-2 5 0 0 X 2 3 1 6 5 5 4 0 . 7 4
M E F 6-2 6 0 0 X 2 2 8 9 5 2 0 1 . 0 8

Table 2 Surface to internal fracture mode

transition level of Δ a p
Fracture Mode T r a n s i t i o n Micro-Vickers Hardness (25g)
Level of Δ ε ρ Martensi te Ferrite Ratio
M E F 2-1 0 . 0 1 5 4 7 5 1 1 7 4. 1
M E F 2-2 0 . 0 2 3 9 2 1 0 3 3. 8
M E F 3-2 0 . 0 3 3 3 4 1 1 0 3. 0
M E F 4-2 0 . 0 7 3 3 2 1 1 4 2. 9
M E F 5-2
- 2 6 5 1 1 8 2. 5
M E F 6-2
- 2 4 1 1 2 3 2. 0
 521
[Increase In Plastic Strain R a n g e d

(Section)
B°8°3° (Section)
Surface Fracture Mode Internal Fracture Mode
Fig.l Schematic representation of fracture mode transition.

Internal Fracture
Mode

Fracture Mode
Transition
D

Surface Fracture
Mode

Log Nf
Fig.2 Schematic diagram illustrating the two
failure limit lines.

1200°Cx3hr 600°Cx2hr
79Q°Cx1hr 200°Cx1hr
^ A3
ö Ai
d»
Q.
E Io M

JLi
Annealing Normarizing ω
cω Q.
D E
a
Time
Fig.3 Heat treatment processes. Fig.4 Microstructure
of material.

90
45

Wf\
Fig.5 Specimen geometry.
\M14x1
522

MEF3-2 Δ £ ρ =0.005 ,1mm, MEF3-2 A8p=0.1 ,1mm ,

Fig.6 Transition from surface to internal fracture mode

with an increase in plastic strain range.

MEF6-2 Δερ=0.3 J mm

Fig.7 Typical feature of surface fracture mode

observed in extremely low cycle regime.

(a) MEF3-2,A εp=0.05, n=60 (b) MEF2-2,Δ ε ρ =0.05, n=30

Fig.8 Typical feature of (a) microfracture of martensite and
(b) cleavage cracking of ferrite grain.
 523

α 1
CJ ο MEF6-2
<3 Δ MEFA-2
■\β *^Α Ο
D MEF2-1
§10"
C ~ ^ . - ^ ^ 0

ιο 2
'ϋ

I"
Ö
GL

ισ 3 1 10 102 103 1(f

Cycles to failure Nf
Fl g.9 Effect of fracture mode transition
on low cycle fatigue behaviors.

Fatigue test Tension test

0.1 0.5 1.0
Monotonic fracture ductility tf
Fig.10 Schematic diagram illust- F i g . 1 1 C o r r e l a t i o n between
rating the relationship ε r and C.
between fatigue test and
monotonic tension test.

10 1 10 10' 10-
Cycles to failure Nf
Fig.12 Comparison of Eq.(2) with fatigue test results.
 WS7e8

Effect of Microstmcture on Fatigue Properties

in Low and Ultra-low Carbon Steels

T. YOKOMAKU*, M. KINEFUCHI* and T. IWAI**

♦ Mechanical Engineering Research Laboratory, Kobe Steel, Ltd.

*♦ Kakogawa Works, Kobe Steel, Ltd.
5-5, Takatsukadai 1-chome, Nishi-ku, Kobe, Japan

ABSTRACT

Ultra-low carbon s t e e l containing phosphorus and copper (P-Cu steel) has

both a higher fatigue limit and b e t t e r crack propagation r e s i s t a n c e than
conventional low carbon s t e e l s with the same t e n s i l e s t r e n g t h . The
e x c e l l e n t fatigue limit in P-Cu s t e e l can be a t t r i b u t e d to solution hardening
caused by phosphorus and p r e c i p i t a t i o n hardening caused by c-Cu. On the
o t h e r hand, the superior r e s i s t a n c e t o fatigue crack propagation was caused
by grain coarsening which occurs with reduction of carbon content, leading
e v e n t u a l l y to roughness-induced crack closure.

KEYWORDS

Fatigue limit; Crack propagation; Small crack; Crack closure; Microstructure.

INTRODUCTION

It is g e n e r a l l y thought t h a t the fatigue limit of s t e e l s is only s l i g h t l y

affected by the microstructure if the s t a t i c s t r e n g t h of the s t e e l s is
identical in each case. It has also been reported, on the o t h e r hand, t h a t
the t h r e s h o l d s t r e s s i n t e n s i t y of long fatigue crack propagation, A^th, is
g r e a t l y affected by the microstructure. Grain refinement, for example,
improves fatigue limit through an increase in t e n s i l e s t r e n g t h , but decreases
AKth in general. It is t h e r e f o r e difficult to improve the fatigue limit and
the crack propagation resistance at the same time. It will be demonstrated
in this paper, however, t h a t ultra-low carbon s t e e l containing phosphorus
and copper has both a higher fatigue limit and b e t t e r crack propagation
r e s i s t a n c e than conventional low carbon s t e e l s with the same s t a t i c
s t r e n g t h . The mechanism for improving the fatigue p r o p e r t i e s of these s t e e l s
is discussed on the basis of microscopic observations by e l e c t r o n microscope
and measurements of crack closure behaviour for small and long fatigue
cracks.
525
526
EXPERIMENTAL PROCEDURE

MATERIALS
Two h o t - r o l l e d s t e e l sheets (P-Cu and C-Mn s t e e l s ) , shown in Table 1, were
used in t h i s experiment. Fatigue t e s t s were conducted on a s - r o l l e d (fine
grain size) and annealed (coarse grain size) materials. The two s t e e l s have
almost identical t e n s i l e s t r e n g t h of 450 MPa in the a s - r o l l e d condition.

FATIGUE AND FATIGUE CRACK PROPAGATION (FCP) TEST

High-cycle fatigue t e s t s were conducted using plane bending smooth
specimens at the s t r e s s r a t i o , R (= a m in/a m a x )= -1 and a t t h e frequency, f =
60Hz.
The FCP r a t e for small cracks was measured by t h e r e p l i c a t i o n method on
axial load smooth specimens, which were t e s t e d under a c o n s t a n t load
amplitude a t R = -1 and f = 20Hz. The crack closure behaviour was recorded
with a l a s e r interferometric displacement gauge (Sharpe, 1971, Kinefuchi
e t a l . , 1990).
The FCP t e s t s for long cracks were performed using single-edge-notched
specimens, under a constant load amplitude and a s t r e s s i n t e n s i t y range
decrease a t R = 0.1 and f = 10Hz.

RESULTS AND DISCUSSION

FATIGUE LIMIT OF SMOOTH SPECIMENS

The fatigue limit, aw, of the plane bending specimen and t h e endurance r a t i o ,
aw/T.S., a r e l i s t e d in Table 1. The endurance r a t i o of a s - r o l l e d P-Cu s t e e l is
equal t o 0.71, which is much higher than t h a t of C-Mn s t e e l and t h e r e p o r t e d
values of 0.45 to 0.55 for conventional low carbon s t e e l s .
The r e l a t i o n between fatigue limit and grain size is shown in Fig.l. The d a t a
of o t h e r C-Si-Mn s t e e l s (Steel C, D, and E) and a low carbon s t e e l (Steel F),
r e p o r t e d by different r e s e a r c h e r s , a r e also p l o t t e d in Fig.l (Nakai e t a l . ,
1981, Abe e t a l . , 1984, Akiniwa, 1989). The r e l a t i o n s h i p can be expressed as:
aw= aQ + k ' d " 1 / z
= , 215 MPa (P-Cu steel) (1)
wnere Oo 1 1 3 Q ± 2Q M p a (other s t e e l s )
k = 0.3 - 0.4 MPa-m 1/2

Table 1 Chemical compositions and mechanical p r o p e r t i e s of a s - r o l l e d

materials
Chemical c o m p o s i t i o n s (wt%) Y.S. T.S Fatigue Endurance
Steel limit ratio
C Si Mn P Cu (MPa) (MPa) aw (MPa) aw/T.S.

P-Cu 0.003 0.26 1.26 0.089 0.32 333 451 315 0.71
C-Mn 0.090 0.02 0.76 0.012 309 442 238 0.55
 527
The value of k is almost independent of materials. On t h e o t h e r hand, t h e
value of (Jo in P-Cu s t e e l is much higher than t h a t in o t h e r s t e e l s . The value
0Ό, which is supposed t o be t h e friction s t r e s s on slip bands, depends on t h e
hardening mechanism, such as solution-hardening, precipitation-hardening,
and p e a r l i t e - h a r d e n i n g , e t c . A number of fine p r e c i p i t a t e s of 6-Cu was
observed in P-Cu s t e e l as shown in Fig. 2. The solution hardening by
phosphorus (Takada e t a l . , 1982) and t h e p r e c i p i t a t i o n hardening by £,-Cu a r e
thought t o lead t o a higher 0Ό value and then superior fatigue s t r e n g t h in
P-Cu s t e e l . The p e a r l i t e - h a r d e n i n g in C-Mn and C-Si-Mn s t e e l s had l i t t l e
effect on t h e value of 0To.

FATIGUE CRACK PROPAGATION PROPERTIES FOR SMALL CRACK

At s t r e s s l e v e l s above t h e fatigue limit, a major p o r t i o n of fatigue life is
t h e crack propagation life, and t h e r e f o r e t h e evaluation of small fatigue
crack propagation behaviour will help us t o understand t h e difference in
fatigue s t r e n g t h between P-Cu and C-Mn s t e e l s . In Fig. 3, t h e crack
propagation r a t e s for small cracks in smooth specimens of two s t e e l s a r e
compared as a function of ^K c a l c u l a t e d for t h e semicircular surface crack.
It is indicated t h a t P-Cu s t e e l has a significantly higher crack propagation
r e s i s t a n c e than C-Mn s t e e l .
The load vs. crack opening displacement curves for fatigue cracks of 0.1mm in
length, measured with t h e interferometric displacement gauge, a r e shown in
Fig.4. In P-Cu s t e e l , only a small c y c l i c a l l y p l a s t i c deformation was
observed and t h e crack c l o s u r e load remained a t high l e v e l s . On t h e o t h e r
hand in C-Mn s t e e l , t h e s t r e s s condition is f a r beyond t h e small scale
yielding condition because of t h e low yield s t r e n g t h of t h e f e r r i t e phase. I t
can be concluded t h a t a superior fatigue limit and fatigue s t r e n g t h in P-Cu
500 I 1
plane
Δ A (P-Cu steel) Ending
n O B(C-Mn steel)

I I I I I
0 100 200 300 400
Inverse square root of grain size,
1//d rrr1/2
Fig. 1. Relation between fatigue limit and
inverse square root of grain size.
528
s t e e l is a t t r i b u t e d to a high friction s t r e s s on slip bands and a high
r e s i s t a n c e t o small fatigue crack propagation, which a r e caused by the
solution- and precipitation-hardening in the f e r r i t e phase.

FATIGUE CRACK PROPAGATION PROPERTIES FOR LONG CRACK

In addition t o superior high-cycle fatigue p r o p e r t i e s , P-Cu s t e e l had a
higher t h r e s h o l d s t r e s s i n t e n s i t y for long cracks, /\Kth, than C-Mn s t e e l of
t h e same t e n s i l e s t r e n g t h (for example, 5.7 M P a m 1 / 2 for a s - r o l l e d P-Cu s t e e l
and 4.8 MPa-m 1/2 for a s - r o l l e d C-Mn s t e e l ) .
The /\K*h a n ( i t h e effective s t r e s s intensity, l K e f f , t h for P-Cu, C-Mn and
o t h e r s t e e l s are shown in Fig. 5 as a function of grain size. The ßKth is
expressed as:
Δ Κ ^ = ΔΚο ♦ h d 1 / 2 (2)
Unlike t h e d a t a for the r e l a t i o n between fatigue limit and grain size in Fig.l,
a l l t h e d a t a in t h i s case f a l l on the narrow band:
ΔΚο 2.8 h 0.9 MPa-m 1/z (3)
h 660 MPa
The effective s t r e s s intensity, _K e ff, t h is only s l i g h t l y dependent of the
grain size and the material system and i t is approximately equal t o J\,K0.
Therefore, the crack closure s t r e s s i n t e n s i t y range, /\K c i is given as:

TO"7 ffa MPa (R=-1]

• BS-3A 196
A BS-3B 196
■ BS-4B 186
o GDI
▼ BS-4C 186

10" C-Mn Steel " ■

Δ
ΔΔ

A Δ
m
- > * W A Δ
Δ
<%Y Jm Δ
2 10" A f T Δ

■ W? ΔΔ

^Δ P-Cu Steel
,o
o
io- h <Ja MPa
D VÜ AS-1A 284
CO
W HUÜ AS-3A 314
o AS-5B 284
ÜD7
AS-5C 284

10"
^rrrrr 10 20
Stress intensity range, ΔΚ MPaJni
Fig. 2 Transmission e l e c t r o n Fig. 3 Small fatigue crack propagation
micrograph of P-Cu s t e e l . r a t e of P-Cu and C-Mn s t e e l .
(Crack length 0.1 ~~ 1.6mm)
 529
P-Cu Steel
AS-5B
i7a=284MPa
2 a = 1 03/tfn
4K = 5.57MPa7S

- Closure point
(a) P-Cu s t e e l

s
0.2 -0.1 0 0.1 0.2 0.3 0.4
Crack opening displacement, COD μπ\
C-Mn Steel
4.5
BS-3A
tfa=l96MPa
3.0 2 a = 101 /im
4K = 3.80MPa/m
1.5

(b) C-Mn s t e e l 0

-1.5

-3.0
- Closure point
-4.5i , -,
-0.8-0.6-0.4-0.2 0 0.2 0.4 0.6 0.8
Crack opening displacement, COD //m

Fig. 4 Load vs. crack opening displacement curves for small cracks
of P-Cu and C-Mn s t e e l s , (crack length = 0.1 mm)

<b Δ A (P-Cu steel) R=0.1

c _12 O B (C-Mn steel)

2 ic • C(S20C)
£10 * D(SM41B) **\h
\

in ~.
<1> Ϊ"
I!. V
ts <J
Ό
O JZ
*:
Φ <j

8 10 12
3_1/2
Square root of grain size, Z3" *10 m
Fig. 5 Relation between threshold stress intensity range
for long cracks and square root of grain size.
530
ΔΚαΐ= Δ Κ ^ - A K e « . t h = h - d 1 / z (4)
That is, the crack c l o s u r e behavior of long fatigue cracks is affected only
by grain size. Because of the u l t r a - l o w carbon content, t h e l a r g e grain size
can be obtained in P-Cu s t e e l with t h e same h o t - r o l l i n g and h e a t - t r e a t m e n t
conditions as in C-Mn and C-Mn-Si s t e e l s , which is a major cause of roughness
induced crack closure.
Reducing the carbon content will lead t o grain coarsening and then decrease
the t e n s i l e s t r e n g t h . In t h e case of P-Cu s t e e l , though, t h e degradation of
t e n s i l e s t r e n g t h caused by reducing the carbon content is offset by t h e
solution hardening r e s u l t i n g from t h e addition of phosphorus and by t h e
hardening brought about by the p r e c i p i t a t i o n of £,-Cu. This micromechanism
will r e s u l t in the improvement of both fatigue limit and fatigue crack
propagation resistance.

CONCLUSIONS
(1) Ultra-low carbon s t e e l containing phosphorus and copper (P-Cu s t e e l ) has
a higher fatigue limit and b e t t e r crack propagation r e s i s t a n c e than
conventional low carbon s t e e l s even though they have t h e same t e n s i l e
strength.
(2) Fatigue limit, Ow, is c o r r e l a t e d with grain size, d, as:
aw = σ 0 + k - d " 1 / 2
The value (Jo is dependent on materials and a high 0Ό value in P-Cu steel can
be attributed to the solution hardening caused by phosphorus and the
precipitation hardening by &-Cu.
(3) On the load vs. crack opening displacement curves for small cracks in
P-Cu steel, only a small cyclically plastic deformation is observed and the
crack closure load remains at high levels. These effects result in high crack
propagation resistance for small fatigue cracks in P-Cu steel.
(4) Threshold stress intensity, Δκ**ι» *s correlated with grain size, d, as:
Δκ*ΐι= Δκο + h d 1 / 2
AKo and h a r e almost independent of materials. A high ΔΚ*ΐι value in P-Cu
s t e e l is thought t o be caused by roughness-induced crack c l o s u r e because of
a l a r g e grain size in comparison with conventional low carbon s t e e l s .

REFERENCES

Abe, T., Sampei, T., Osuzu, H. and Kozasu, I. (1984). J. Iron and Steel Inst.
Japan, 70, 1459
Akiniwa, Y. (1989). Doctor's Thesis, Kyoto University
Kinefuchi, M., Akiniwa, Y. and Tanaka, K. (1990). Trans. Japan Soc. Mech.
Engrs., 56, 251
Nakai, Y., Tanaka, K. and Nakanishi, Y. (1981). Eng. Fract. Mech., 15, 291
Sharpe, J r . W.N. (1971). Int. J. Nondestructive Testing, 3, 59
Takada, H. Sudo, M., Tsukatani, I., Takai, D.,Hase, A. and Tsuji, K. (1982).
J. Iron and Steel Inst. Japan, 68, 1398
This paper will be presented at the 6th International Conference on Mechanical Behavior of Materials, ICM 6,
29 July - 2 August 1991, Kyoto, Japan, and will be published in the proceedings.

WS7f1

PROPAGATION OF DELAMINATION FATIGUE CRACKS IN

UNIDIRECTIONAL CF/PEEK LAMINATES

Masaki Hojo*, Keisuke Tanaka**, Claes-Göran Gustafson***,

and Kiyoshi Kemmochi*

* Industrial Products Research Institute, AIST, ΜΓΠ, Higashi, Tsukuba 305, Japan
** Dept. of Engineering Science, Kyoto University, Sakyo-ku, Kyoto 606, Japan
*** Div. Materials and Processes, The Norwegian Institute of Technology,
7034 Trondheim-NTH, Norway

ABSTRACT

The effect of the stress ratio on the near-threshold growth of delamination fatigue cracks was
investigated with unidirectional laminates made from ICI APC-2 thermoplastic prepregs
(AS4/PEEK). Tests were carried out under mode I opening loading by using double cantilever
beam specimens. The crack growth rate under different stress ratios was a unique function of
the equivalent stress intensity range proposed by the authors. The fatigue crack growth rate near
the threshold was mainly controlled by the stress range rather than by the maximum stress. The
resistance of CF/PEEK laminates against fatigue crack growth was much higher than that of
conventional CF/epoxy laminates even near the threshold region. This increase of resistance,
however, was smaller than that of fracture toughness. The difference in growth behavior
between CF/PEEK and CF/epoxy laminates was discussed on the basis of the mechanism
consideration.

KEYWORDS

Fatigue; fracture; composite materials; CFRP; PEEK; delamination; crack propagation; DCB
specimen

INTRODUCTION

Carbon fiber reinforced plastics (CFRP) have already been used for the primary structures of
commercial aircraft, and composite structures used as primary structures require performance
reliability based on damage tolerance. Conventional CFRP laminates made of brittle epoxy
matrix have very low interlaminar strength, manifested as a low threshold of delamination
fatigue crack growth and a low static fracture toughness (Wilkins, 1981; Bathias and Laksimi,
1985; Hojo et al.y 1987a). Hence, the improvement of the delamination strength of CFRP
laminates is of current interest in their structural applications.

Polyetheretherketone(PEEK) is a new semicrystalline thermoplastic matrix resin which is

expected to improve significantly the interlaminar strength. The interlaminar fracture toughness
of CF/PEEK laminates was reported to be 3 to 4 times higher than that of conventional

531
532

CF/epoxy laminates (where the toughness is expressed in terms of the stress intensity
factor)(Leach and Moore, 1985). On the other hand, very little is known about the effect of
cyclic loading on the delamination growth behavior in CF/PEEK laminates. Although Prel et
al. (1989) carried out mode I and mode II delamination fatigue crack growth tests by using DCB
and CBEN specimens, they dealt only with crack growth at very high rates. Recently,
0'Brien(1988) found in edge delamination tests that the delamination onset in CF/PEEK
laminates under fatigue loading occurred at significantly lower strain levels than its delamination
onset under static loading was.

In the present study, the effects of the stress ratio (the mean stress) on the near-threshold growth
of delamination fatigue cracks were investigated. The results were compared with our previous
results for CF/epoxy laminates(Hojo et al, 1987a, b).

EXPERIMENTAL PROCEDURE

Material and Specimen

The laminates were made from prepregs of ICI APC-2 (AS4/PEEK). The unidirectional
laminates (thickness=6mm) were fabricated by ICI Wilton. The degree of crystallinity was 34%
by using DSC (Differential Scanning Calorimetry). Tests of delamination fatigue crack growth
were carried out under mode I opening loading by using double cantilever beam specimens
(width=20mm) with a special loading device(Hojo et al, 1990). The distance between the center
of the pin and the specimen surface was designed to be 3mm in order to minimize the
geometrical nonlinearity. Crack opening displacement on the load line was measured by an
extensometer attached to the loading apparatus.

Fatigue Tests

Tests were carried out with a computer-controlled fatigue testing system established by the
authors(Hojo etai, 1987a, b). The energy release rate, G and the stress intensity factor, K,
were also calculated by the same procedure as before. In each test, the stress ratio, R, of the
minimum to the maximum load was kept constant to be 0.2 or 0.5. A normalized gradient of
energy release rate, 2C=(l/G)dG/da, was also controlled between -0.3 to -0.8 mm_1(Hojo et al,
1990). The frequency of stress cycling was 10 Hz. The testing environment was air of 50%RH
at 23 c €. The length of a crack was computed from the measurement of the compliance of the
specimen(Hojoeifl/., 1987b).

EXPERIMENTAL RESULTS AND DISCUSSION

Effect of Stress Ratio

Figure 1 shows the relation between the crack propagation rate, da/dN, and the stress intensity
range, ΔΚ, under R=0.2 and 0.5, where ΔΚ = K max - K m i n (K max and K m i n are the maximum
and minimum values of the stress intensity factor corresponding to the maximum and minimum
loads). For each case of the stress ratio, da/dN is expressed as a power function of ΔΚ in the
region where da/dN is larger than about 10' 10 m/cycle. Below this region, da/dN deviates to the
lower rate, and there exists a growth threshold for fatigue cracks. When compared with our
previous study on CF/epoxy (Hojo et a/., 1987a), the downward deviation in the da/dN vs. ΔΚ
 533
APC-2
I 1 1 1 1 | 1

23eC Air

/Oo
ooo -
o or
- oo°
V7 <*°/° ^
Ψο/ ZllO
Θ o uoo 1
9 ° o°

<?8>Ä. . °
CP&& o -
■ «ξ o -
<V
cP R
O 0.2
o 0.5

1 1 1 . 1 1 1 .
1.0 1.5 2.0 200 500 800
Stress intensity range, AK(MPam,/2) Maximum energy release rate, Gmax(N/m)

Fig. 1. Relation between crack propagation Fig. 2. Relation between crack propagation
rate and stress intensity range. rate and maximum energy release rate.

relation is not so clear near the threshold region.

However, the slope is steep enough to suggest the
existence of the growth threshold in practical applications.
The exponent of the power function and the R-dependence
on da/dN are smaller than those for CF/epoxy. Crack
closure was not detected in the present tests.

In Fig. 2, the growth rate is plotted against the maximum

energy release rate, G max . The difference in the crack
growth rate due to R values becomes larger than that in
Figure 1. When compared at the same G n da/dN
decreases with increasing R value. Thus, the effect of R
on the da/dN-G max relation is reversed in comparison with
that on the da/dN-AK relation.

For the case of CF/epoxy laminates, the growth rate under

different stress ratios was fairly well correlated to the
energy release rate range, AG, where AG = G m a x - G m i n
(^max anc* ^min ^0 t n e m a x i m u m a n d minimum values of
the energy release rate corresponding to the maximum and
minimum loads) (Hojo et al.t 1987a). Thus, da/dN is
plotted against AG in Fig. 3. The R-dependence is larger 200 500 800
than that on the da/dN vs. ΔΚ relation. Energy release rate range, AG(N/m)

Fig. 3. Relation between crack

Controlling Fracture Mechanics Parameter propagation rate and
energy release rate range.
In our previous analysis of the near-threshold crack growth
534

(Hojo et al., 1987a), we proposed the following

ZU
.... ., ι ' ' ' ' I
ΔΚ=ΔΚο(1- R ) r
equivalent stress intensity range, ΔΚ , as a da/dN=10"10m/cycle ο-""!
controlling parameter for fatigue crack growth under
various R values: 1.0 ^°^^
ΔΚ αι = ΔΚ(1-Κ)-Ύ : ΔΚ(μΎ)Κ Ύ (1) ΔΧ
/ 1
where γ indicates a relative contribution of the 05
maximum stress to the cyclic stress in determining the
crack growth rate. ΔΚ_ can be regarded as an
equivalent parameter of ΔΧ at R=0 to which the R . V
dependency of ΔΚ is converted. ο APC-2 0.36
Δ 9UC 0.85
0.?
In Fig. 4, ΔΚ at da/dN=10 -10 m/cycle is plotted
1 > ι . ι _
0.2 0.5
against a stress ratio parameter, (1-R), in order to Stress ratio parameter, 1-R

determine γ values. The results of the CF/epoxy Fig. 4. Relation between stress
laminate (T300/914) are also shown with the triangle intensity range and stress ratio
marks in this figure (Hojo et al., 1987a). The parameter at da/dN=10"10m/cycle.
exponent of a straight line fit of data gives the γ
values. For the case of CF/PEEK laminate, the γ
values is 0.36. This low value of γ suggests that the mechanism of fatigue crack propagation is
mainly controlled by the stress intensity range (ΔΚ) like in metallic materials. On the other hand,
the results of CF/epoxy laminate fit to the line at the slope of 0.85. This slope means that the
contribution of the maximum stress intensity factor (K max ) is larger than that of stress intensity
range (AK)(Hojo et al., 1987a). The influence of the stress ratio on the growth resistance is
completely different between CF/PEEK and CF/epoxy. SEM observation showed the difference
between the fracture surface of static fracture and of fatigue fracture for CF/PEEK laminates

9UC/APC-2
Π—i i i i i i · · i i «

10 23°C Air

Ί0

p6 12p7
-SIO*

no
R 91AC APC-2
°-10 h
0.2 ♦ o
0.5 · o
10
0.5 ** 1.0 1.5 2.0 2.5 3.0
Equivalent stress intensity range, AKeq(MPam 1/2)

Fig. 5. Relation between crack propagation rate and equivalent stress intensity
range for CF/PEEK(APC-2) and CF/epoxy(914C) laminates.
 535

Φ ——1 1—1 1—1 1 1- 1 ' 1 ■

(Hojo etal, 1990). On the other hand,
c ■ CF/epoxy(914C)
no significant difference was observed (0
between fracture surfaces of fatigue D CF/PEEK(APC-2)
1.5 -j
fracture and of static fracture for
CF/epoxy laminates(Hojo et ah, 1987a).
These facts agree with the difference of ^π- j
the contribution of ΔΚ and K max . 1.0 ^ ^ J
The open marks in Fig. 5 shows the ^*^
relation between da/dN and ΔΚ for it 0.5 \
CF/PEEK laminates. The influence of
the stress ratio is minimal for the whole
region. It can be concluded that ΔΚ is
00
the controlling fracture mechanics . 1 1 1 i 1 L.

parameter for APC-2 laminate. 1

1/2v
Fracture toughness, K ic(MPam "*)
Fig. 6. Variation of fatigue threshold with fracture
Comparison with CF/epoxy toughness.
As mentioned above, the γ values in Eq. (1) are different between CF/PEEK and CF/epoxy
laminates. While ΔΚ of CF/PEEK laminate is only 1.8 times that of CF/epoxy laminate under
R=0, the difference in ΔΚ is much larger at higher R values as shown in Fig. 4. In Fig. 5, the
relation between da/dN and ΔΚ for 914C (CF/epoxy) laminates is also shown to compare
with the relation for APC-2 (CF/PEEK) laminates. The resistance of APC-2 laminates against
fatigue crack growth is much higher than that of 914C laminates. When compared at the same
growth rate, ΔΚ value for APC-2 laminate is about twice as much as that for 914C laminate.
When compared at the same ΔΚ_, da/dN for APC-2 laminates is about 4 orders of magnitude

APC-2/9UC 1
1 ' 1 ' 1 ' 1 ' 1 ' 1 '
♦
10 - R APC-2 91 AC
- 0.2 O ♦ ooo
0.5 o •
^10 -
. · ;

¥
E $ o
- Jf
-g 10 V
ο^° ♦ ^

■10 c$f
V
Ϊ
Φ
V<P
^
•
L
10 %
♦

♦
1 i i 1 i I M 1 I 1 I 1 I 1 I
10
0.3 0.5* 0.7 0.9
Normalized equivaleni stress intensiiy range,AKeq/Kic

Fig. 7. Relation between crack propagation rate and normalized equivalent stress
intensity range for CF/PEEK(APC-2) and CF/epoxy(914C) laminates.
536
lower than that for 914C laminates. The exponent of the power function for APC-2 laminates
reduced to three fourths. Figure 6 shows the relation between the fracture toughness, K IC , and
ΔΚ Λ , where ΔΚ Λ is the ΔΚ value at the crack growth threshold. It should be noted in the
figure that the remarkable increase in fracture toughness, K IC , for APC-2 laminates contributes
only 50% to the increase in fatigue crack growth resistance near the threshold region. In. Fig. 7,
da/dN was plotted as the function of the normalized equivalent stress intensity range, AK^TKjp.
This figure clearly shows that the normalized delamination growth resistance and the threshold
value under fatigue loading decrease with increasing toughness. This fact indicates that the
contribution of fatigue is very important in damage-tolerance design for laminates with
toughened matrix systems. A similar tendency was found by Mall et a/. (1989) with toughened
matrix systems in the high growth rate region .

CONCLUSIONS

The crack propagation rate under different stress ratios was expressed as a unique power
function of the equivalent stress intensity range at the growth rates above about 10"1" m/cycle.
Below this region, there was a growth threshold. The contribution of the stress range was
higher than that of the maximum stress.

CF/PEEK laminates are more resistant to fatigue crack growth, showing a higher growth
threshold, lower crack growth rates and a lower exponent in the power relation. On the other
hand, the ratio of the the fatigue threshold to the fracture toughness in the CF/PEEK laminates
decreased in comparison with the CF/epoxy laminates. The increase in fracture toughness by
improving matrix toughness is not translated directly into the improvement in delamination
resistance under fatigue loading.

REFERENCES

Bathias, C , and A.Laksimi (1985). Delamination threshold and loading effect in fiber glass
epoxy composite. ASTM STP 876 , 217-237.
Hojo, M., K.Tanaka, C.-G. Gustafson, and R. Hayashi (1987a). Effect of stress ratio on
near-threshold propagation of delamination fatigue cracks in unidirectional CFRP.
Composite Sei. Tech., 2 ^ 273-230.
Hojo, M., C.-G. Gustafson, K. Tanaka, and R. Hayashi (1987b). Mode I propagation of
delamination fatigue cracks in CFRP. In: Advanced Materials for Severe Service
Applications (K. Iida and A. J. McEvily, ed.), pp. 353-372. Elsevier, London.
Hojo, M., K. Tanaka, K. Kemmochi, and R. Hayashi (1990). Propagation of delamination
fatigue cracks in CF/PEEK laminates. Proc. 10th Tsukuba General Symposium, 57-63.
Leach, D. C , and D. R. Moore (1985)., Toughness of aromatic polymer composites
reinforced with carbon fibres. Composite Sei. Tech., 2 ^ 131-161.
Mall, S., K. T. Yun, and N. K. Kochhar (1989). Characterization of matrix toughness effect
on cyclic delamination growth in graphite fiber composites. ASTM STP 1012, 296-310.
O'Brien, T. K. (1988), Fatigue delamination behavior of PEEK thermoplastic composite
laminates. /. Reinforced Plast. Compos., 7, 341-359.
Prel. Y. J., P. Davies, M. L. Benzeggagh, and"F. X. de Charentenay (1989). Mode I and mode
II delamination of thermosetting and thermoplastic composites, ASTM STP 1012,
251-269.
Wilkins, D. J., J. R. Eisenmann, R. A. Camin, W. S. Margolis, and R. A. Benson (1981).
Characterizing delamination growth in graphite-epoxy. ASTM STP 775, 168-83.
WS7f2

A Fatigue Failure Criterion of Notched Plates of FRP

H. HYAKUTAKE, T. HAGIO and T. YAMAMOTO

Department of Mechanical Engineering, Fukuoka University,

Nanakuma, Jonan-ku, Fukuoka 8lU, Japan

ABSTRACT

Plane bending fatigue tests were carried out on the notched specimens
of fiber glass/epoxy laminates for a wide range of notch-root radii.
Our attention focussed on the damaged zone near the notch root of
specimens. The process of fatigue damage was studied by measuring the
luminance at the limited spot near the notch root. Closer observation
by using a scanning electron microscope revealed that the initiation
of micro cracks at the notch root was accompanied with the decrease of
the luminance near the notch root. The experiment shows that the
number of cycles to failure is determined by both the maximum elastic
stress at the notch root and the notch-root radius. On the basis of
the concept of severity near the notch root, the experimental results
were elucidated clearly. Applying the fatigue failure criterion
derived here, we can make an accurate estimate of the fatigue life
prediction for notched specimens of FRP.

KEYWORDS

Fatigue; reinforced plastics; notch; stress concentration;

life prediction; damage; fatigue failure criterion; luminance.

INTRODUCTION

There is considerable literature on the fatigue fracture for notched

specimens of fiber composites. The attention in these studies is
mostly to reveal the fatigue damage and the mechanism of damage
development at the notch root (Bakis and Stinchcomb, 1986; Itsutsuji
et al., 1985; Maekawa et al., 1986; Shimokawa and Hamaguchi, 1983).
Our goal is to elucidate the fracture behavior of composite laminates
containing stress concentrations in various notch geometries and to
develop a limiting condition for predicting the fatigue life of

537
538

notched bars of composite materials.

Studying of stress analysis near the notch root, we have obtained a

fracture criterion for notched bars in static load (Hyakutake and
Nisitani, 1987). The criterion is based on the concept of severity
near the notch root and experiments have shown that the criterion is
applicable to notched bars of FRP over a wide range of notch
geometries and dimensions of specimen (Hyakutake et al., 1989a;
Hyakutake et al., 1989b). The aims of the present research are to
provide the experimental evidences of the validity of the fracture
criterion for the fatigue failure of notched plates of FRP.

EXPERIMENTAL PROCEDURE

The material used was a commercial sheet of FRP which was a fiber
glass/epoxy laminate. The dimensions of FRP sheet were 1 m wide, 1 m
long, and 2 mm thick. The sheet is made up of eight layers of glass
cloth, and the diameter of glass fiber is about 0.01 mm. All
specimens having a width of 10 mm were notched in an U-shape on both
sides at the mid point of their length. The notch-root radii were
varied from 0.15 to 2 mm. The notch depth was 1.5 mm in all
specimens. The range of the value of geometrical stress concentration
factor K-t is 1.33 to 2.67. Fatigue tests were performed on a plane
bending testing machine at frequency l6.7 Hz. The luminance near the
notch root was measured successively during tests to evaluate the
fatigue damage.

RESULTS AND DISCUSSION

Figure 1 shows the S-N curve for notched FRP plates in plane bending
fatigue tests. It can be seen from Fig. 1 that there is little effect
of the notch-root radius p on the fatigue life Nf. Maier et al.
(1987) showed the decrease of notch sensitivity in fatigue tests on
carbon fibre-reinforced polyimides.

An example of the process of fatigue damage growth on the surface of

specimen is shown in Fig. 2. Usually fatigue damage appeared near the
notch root in the early stage: it takes 5-10 % of the fatigue life as
shown in Fig. 2(a).

To evaluate the fatigue damage near the notch root, we measured the
luminance at the limiting spot located a fixed distance of 0.U mm from
the notch root. Figure 3 shows the relative luminance decrease during
fatigue test for the specimens having the notch-root radius p = 1 mm.
The photographs of the surface damage on the specimen for the point a,
b, c and d on the curve of on = 118 MPa in Fig. 3 are shown in Fig.
2(a), (b), (c) and (d), respectively.

It can be seen from Fig. 3 that the relative luminance decreases

rapidly at the point as shown by the arrows in Fig. 3. The value of
relative luminance of these points are about 0.9 in all specimens for
which ön = 118-177 MPa. At the point as shown by the arrows in Fig.
3, a few micro cracks appear near the notch root as shown in Fig. k.
 539

200 ο Ρ = 0.15
A 0.25
σ • 0.5
α. $\ Δ 1
Σ
/*7CkO □ 2
150 ν Smooth
ν ζ · ck \α

o«*aA
*** I *
100
Τν
,η 4*
ι ii —ι—t-pü

50 I I I I III I I I I I II ll I I I I I I II
5
10' 10 10 e
107
Cycles to failure Nf

Fig. 1. S-N curve for notched FRP plates in plane

bending.

(α) (b) (c) (d)

Fig. 2. Fatigue damage development on the surface

of specimen for which notch-root radius
p = 1 mm, nominal stress on = 118 MPa and
fatigue life Nf = 3.73 * 10 6 : (a) N/Nf =
5 %i (h) N/Nf = 21 %i (c) N/Nf = kO %', and
(d) N/Nf = 80 %.
540

1. 1 r
P=1
u 1.
c °r
o °απΠ*- ΔΔ
··
f^r-o< 0 .
ΚΛΓ^Μ
.E 0. 9 d
E I
■2 0. 8 r /
/ 157 137 118
■i °,7h σ η = 177ΜΡα
o
"5 0. 6 h
0.5 ι ι mil i mil i i M mil ι ι ι
10 3 10 4 Ί05 10 6
Number of loading cycles N

Fig. 3. Relative luminance decrease near the notch

root of FRP specimens for which p = 1 mm
and on = 118 - 177 MPa.

I 1
(a) (b) 0.02 mm
Fig.- k. Micro cracks near the notch root at Nrf for
the specimens showing in Fig. 3: (a) on =
118 MPa; (h) on = 177 MPa.
 541

From the experimental results mentioned above, we can determine the

fatigue damage N^ which is the number of cycles to the point where the
value of relative luminance is about 0.9·

Based on the concept of severity near the notch root, the fracture
criterion for a notched bar in static load is expressed as:

°max ~ °maXj c \ P)» (1)

where omax is the maximum elastic stress at failure and is determined

by the product of the nominal stress in the notch section on and the
geometrical stress concentration factor K^m The parameter omax c on
the right-hand side of (l) is the material constant, which is governed
by the notch-root radius p only and is independent of other notch
geometries and specimen size.

In view of the concept of severity near the notch root, it seems

appropriate to discuss the fatigue failure criterion for notched
specimens in terms of a combination of the maximum elastic stress
°maX9 notch-root radius p and the fatigue damage N£, It is assumed
that the fatigue failure criterion for a notched bar in cyclic load is
expressed as:

500

400
o
Σ
300
x
O

200

3
100 I I I I I I III I I I I I I I ll I I I I I I III

103 10 A
10 5
106
Cycles to damage Nd

Fig. 5· Effect of notch-root radius p on the

relation between the maximum elastic
stress omax and the number of cycles to
damage Nrf.
542

°max'(®d)m = C(p), (2)

where m is the material constant. The parameter C on the right-hand

side of (2) is the material constant, which is governed "by the notch-
root radius p only and is independent of other notch geometries and
specimen size. For Nrf = 1 in static load, (2) reduces to (l).

Figure 5 shows the relation "between omax and Nrf for a constant notch-
root radius p. There are five kinds of p. Each experimental point
falls in close proximity to a characteristic straight line for which p
is constant and five characteristic straight lines are pararell to
each other, as can "be seen from Fig. 5· From the experimental results
mentioned above, we will confirm the validity of the fatigue failure
criterion (2) "based on the concept of severity near the notch root.

CONCLUSIONS

The fatigue fracture "behavior of notched FRP plates was studied over a
wide range of notch-root radii. The fatigue damage evaluation
measuring the luminance near the notch root is used to determine the
damage development and fatigue life. From the standpoint of the
concept of severity near the notch root, a fatigue failure criterion
is determined in terms of a combination of the maximum elastic stress,
notch-root radius and the number of cycles to failure. Appling the
fatigue failure criterion derived here, the experimental results were
elucidated clearly.

REFERENCES

Bakis, C.E., and W.W. Stinchcomb (1986). Response of thick, notched

laminates subjected to tension-compression cyclic loads. ASTM STP
907 (H.T. Halm, ed.), pp. 31^-33^.
Hyakutake, H. and H. Nisitani (1987). Conditions for ductile and
brittle fracture in notched polycarbonate bars. JSME Inter. J., 30,
29-36.
Hyakutake, H., H. Nisitani and T. Hagio (1989a). Fracture criterion
of notched plates of FRP. JSME Inter. J., 32, 300-306.
Hyakutake, H., T. Hagio and H. Nisitani (1989b). Fracture of FRP
plates containing a circular hole under tension. Trans. Jpn. Soc.
Mech. Eng., 55, Ser. A, 112-117.
Itsutsuji, S., T. Fujii and Z. Maekawa (1985). The fatigue damage
process of FRP laminates with U and V type notches. Trans. Jpn.
Soc. Mech. Eng., 51, Ser. A, 2198-2202.
Maekawa, Z., S. Itsutsuji and T. Fujii (1986). Study on the low-cycle
and high-cycle fatigue strengths of FRP laminate with a notch.
J. Soc. Mater. Sei. Jpn., 35, 636-61*1.
Maier, G., H. Ott, A. Protzner and B. Protz (1987). Notch sensitivity
of multidirectional carbon fibre-reinforced polyimides in fatigue
loading as a function of stress ratio. Composites, 18, 375-380.
Shimokawa, T. and Y. Hamaguchi (1983). Distributions of fatigue life
and fatigue strength in notched specimens of carbon eight-harness-
satin laminate. J. Soc. Mater. Sei. Jpn., 32, 1050-1056.
 WS7f3

Fatigue Damage of Composite Laminate

under Biaxial Loads

Ippei Susuki

Airframe Division,
National Aerospace Laboratory
7-44-1 Jindaiji Higashi-machi Chofu, 182
Tokyo, Japan

ABSTRACT

This paper deals with the fatigue behavior offiber-reinforcedcomposite laminates under in-plane
biaxial loadings. An attempt is made to find the optimum configuration of cruciform type
specimen to obtain desired biaxial stress states in the gauge area and avoid failures at the arms.
The central region which makes the gauge area is consisted of a reduced section of uniform
thickness, and connected by transition surroundings to the full thickness of the arms.

Stresses and strains of cruciform type specimen are analyzed and evaluated by a two-dimensional
finite element method. Laminates used in this report are [0/45/0/-45]s symmetric three-directional
laminates of graphite/epoxy and glass/epoxy composites.

Numerical calculation results indicate the possibility of the difference in fatigue damage modes and
reduction of fatigue strength if each cyclic load has out-of phase. Limited experimental results
show that the fatigue strength of composite laminates are reduced drastically under out-of phase
loading conditions as our previous analyses pointed out.

KEYWORDS

Composite material, Laminate, Biaxial stress, Fatigue, Strength

INTRODUCTION
Composite materials have increasingly expanded their application fields in severe service
environments, particularly where weight is at a premium. Laminated plates of fiber reinforced
composites are generally used in strength or stiffness critical applications in those structures.
Composite laminates do not only have the advantage that they possess high specific strength and
stiffness but also their mechanical properties can be tailored throughfiberorientations, ply
thickness ratios, and stacking sequences.
This capability gives a designer an additional degree of flexibility to obtain the desired strength or
stiffness if fundamental ply data such as tensile, compressive and shear strength along and across
thefiberdirection, are reliable. However, most composite laminates in an actual structure may be
subjected to a biaxial loading condition, most available static and fatigue data are based on uniaxial
stress state(l).
543
544
There does not seem to be a well established data base on the biaxial fatigue damages of laminates
nor method to determine those from uniaxial strength data(2). In this research, fatigue properties
of [45/0/-45/0]s laminate are studied under the in-phase and out-of-phase biaxial loading
conditions.

STRENGTH OF LAMINATES UNDER COMBINED STRESS STATE

The usual assumption of the symmetrically laminated plate theory is used. The laminate is so thin
that the laminate strains are equel to ply strains, and therefore they are constant across the laminate
thickness. Analytical procedures followed in this study are in Ref.(3). The laminate strength is
determined by the first-ply-to-failure(FPTF) envelope. The quadratic failure criterion(3)(4) is
adopted to estimate the strength of each ply. Ply properties used in this study were taken from
Ref. 1, and repeated in Table 1.

It has been proved by our previous investigations(5)(6) that any combination of in-plane stresses
can be expressed as a point of one of the normalized stress regions. Figure 1 shows a map of the
best ply groups of APC2 laminate in the normalized tension dominated stress region. This map
indicates that the three directional laminates of 0,45, -45 degreefiberorientations can build up the
optimum laminate which covers a wide range of tension-tension and tension-compression biaxial
stress combinations in higher strength. The static and fatigue strength were investigated for a
three directional laminate of [45/0/-45/0]s in this study.

Table 1 Material properties

Elastic Properties Strength Properties [MPa]
Ex Ey Major Es 1 Longitudinal Transverse Shear
MATERIAL [GPa] [GPa] Poisson's [GPa] MATERIAL
Ratio Tensile Compressive Tensile Compressive

ALUMINUM 1 ALUMINUM
(2024-T3) 72 72 0.30 27.7 (2024-T3) 345 345 345 345 199 1
Graphite/Epoxy
Graphite/Epoxy
181 10.3 0.28 7.17 1 (T300/N5208)
1500 1500 40 246 68
(T300/N5208)
Graphite/PEEK
Graphite/PEEK
(APC2) 134 8.9 0.28 5.10 (APC2) 2130 1100 80 200 160
AS4/PEEK
1 AS4/PEEK

S6 APC2
S 1=1

[0p/-45s]

[0p/45r/-45s]
[0p/90q] S2
- 1 .0 -0.5 [010 0.5 1 .0

Fig. 1 Territorial map of optimized ply-groups for APC2 laminate

in Tension Dominated region
 545
STRENGTH CHARACTERISTICS OF [45/0/-45/0]s LAMINATE
UNDER BIAXIAL LOADS

Ply strength ratios(R) were calculated to evaluate each ply strength for a normalized given set of
stresses(5). The variations of each strength ratio with S2 are represented in Fig. 2 for APC2
[45/0/-45/0]s laminate under the condition of Sl=lMPa, where SI and S2 are normal stress
components parallel to the 0 degree and 90 degree fiber axes respectively. These components
represent laminate stresses which are obtained by averaging the actual ply stresses.

It is observed that the strength ratio of 0 degree ply is always higher than that of 45 and -45 degree
plies in S2=-1.0~0.2MPa stress combinations. Both ratios are increasing with increase of S2
component up to approximately S2=0.13 where the strength ratio of 0 degree has the maximum
value. The strength ratio of 45 and -45 degree plies, they are always the same under no shear
stress condition, have more strength than the 0 degree ply for S2=0.2 0.4MPa stress
combinations. Therefore the laminate strength, as we adopt FPTF assumption, is controlled by 0
degree ply for the range of S2=0.2~0.4 MPa stress combinations, and other combinations by 45
and -45 plies.

The strength curves under |S2|>|S 1| stress conditions are investigated by an alternative approach as
shown in Fig.3. We can figure out the strength characteristics of [45/0/-45/0]s laminate under
|S2|>|S1| stress conditions by the strength curves of [45/90/-45/90]s laminate in the normalized area
of Sl=lMPa and the range of S2 is S2=-l to 1 MPa. The strength is low and not sensitive to the
value of S2 stress component so much.

Y
R APC2
Sl=1.0MPa(S6=0) [45/0/-45/
Type A

) P
«J
■1000 \
v X
^—'
/—^ ^~·\
l<=& V / ■500 \ \ 4 5 ' -45° )
^^-^0*

1
8 0^
1 ,1 ._ . „ _ 1 1
-0.5 1.0 _2^
MPa ■*
S2 9>

Fig. 2 Ply strength of APC2 [45/0/-45/0]s laminate

under tension dominated biaxial stresses
Type B

R Ä1PC2
Sl-1.0MPa(S6=0) [45/90/-45

^ fc
01 fl
■1000
^ ^

500 45'-45" , 80 -
^^__9£l___
200

-1.0 -0.5 () 0.5 1.0 Fig. 4 Cruciform specimen

S2 MPa
configuration used in stress
Fig. 3 Ply strength of APC2 [45/90/-45/90]s laminate distribution analysis
under tension dominated biaxial stresses
546
STRESS DISTRIBUTIONS IN CRUCIFORM SPECIMENS

A number of different type of cruciform specimens have been proposed and investigated for
characterizing the mechanical properties under biaxial static and fatigue loads( 1). However,most
of the specimens have been designed for metal alloys or conventional isotropic materials. For
testing such anisotropic materials as composite laminates, and finding suitable cruciform
configurations, the computer aided design system is strongly required and under way in several
laboratories(7) including ours.

Table 2 Variation of engineering constants in a cruciform specimen

[45/-45]n Thickness Engineering Constants (GPa)
n (mm) E1 E2 E6 Poi 21 Poi12
0 1.00 76.815 22.229 19.880 0.675 0.195
1 1.50 57.244 24.408 24.806 0.713 0.304
2 2.00 47.433 24.622 27.270 0.727 0.377
3 2.50 41.540 24.343 28.748 0.735 0.431
4 3.00 37.610 23.941 29.733 0.739 0.471
5 3.50 34.802 23.530 30.437 0.742 0.502
6 4.00 32.695 23.146 30.965 0.745 0.527
7 4.50 31.055 22.796 31.375 0.746 0.548
8 5.00 29.745 22.483 31.704 0.748 0.561
9 5.50 28.672 22.203 31.972 0.749 0.580
10 6.00 27.778 21.952 32.195 0.750 0.592
11 6.50 27.021 21.727 32.386 0.750 0.603
12 7.00 26.373 21.525 32.548 0.751 0.613
13 7.50 25.811 21.342 32.689 0.752 0.621
14 8.00 25.319 21.177 32.812 0.752 0.629

kgf/m 0*10=10 kgf/mm2

0*20= 0 kgf/mm2

.01 on l - a x i s

σ2

Fig.5(a) A-type Fig.5(b) B-type

Fig. 5 Stress distributions on the center line along
0 degree direction under uniaxial tensin load

kgf/mm2 ΟΊ 0=10 kgf/mm2

120 0*20= 0 kgf/mm2
σο<$^ > σ»
80
:\°ί
40
01ο
on 2-axis

;-"σΓ 50 100 150 2C 0 mm

-40

-80

Fig. 6(a) A-type Fig. 6(b) B-type

Fig. 6 Stress distributions on the center line along
90 degree direction under uniaxial tensin load
 547
The effect of shoulder geometry on the stress distribution in a gage area was investigated first. As
specimen configuration is shown in Fig.4, two kinds of shoulder geometry A-type and B-type
were compared. The central regions of both which make the gage areas are the same geometry,
and consisted of a reduced section of uniform thickness, and connected by transition surroundings
to the full thickness of the arms. A two dimensional finite element method including pre- and
post-processors was developed to analyze stress and strain distributions in gage areas. The results
of the analysis of the A- and B-type configurations will be presented here for a [45/0/-45/0]s APC2
graphite/PEEK laminate in gage area and surroundings are added the same materials of [45/-45]s
plies to make a smooth and linear change of thickness to the arms. The material properties used
are shown in Table 1. Engineering constants in each thickness was represented in Table 2.

Stress distributions on the center line along 0 degree fiber direction under uniaxial tension were
shown in Fig.5(a) for A-type specimen and Fig5(b) for B-type specimen. Similarly, stress
distributions on the center line along 90 degree fiber direction were shown in Fig.6(a),(b)
respectively. The magnitude and direction of principal stress distributions were represented for
B-type specimen in Fig. 7. Our limited analyses indicated that the A-type geometry has no
significant advantage to B-type.

σι/σο = ι
σ2/σο =
σι/σο = ι
σ2/σο =-ι

Fig. 7 Principal stress analysis by

two dimensional FEM

Material: APC2
Laminate: [0/45/t)/-45]s
SI: 200MPa(R-1)
S2: OMPa(R-l)
Phase: 0 deg

Fig. 12 Fatigue damage by in-phase or

out-of-phase biaxial fatigue test
Fig. 8 Variation of laminate strains Material: glass/epoxy
(el,e2) and strength margin (Q-G-112-2800)
during uniaxial fatigue test
548

EFFECT OF BIAXIAL LOADING PHASE ON FATIGUE PROPERTIES

The effect of loading phase on fatigue damage, mode, and strength was investigated analytically
and experimentally. In-plane orthogonal cyclic loads are applied to a cruciform specimen. The
wave form of applied stress is assumed to be complete tension/compression sine wave in this
study. Figure 8 shows a history of laminate strain el and e2 along the 1- and 2-axis which
coincides with 0 and 90 degree fiber direction in the [45/0/-45/0]s laminate under uniaxial SI cyclic
stress. The history of 0 and 45A45 degree ply strength ratio(R00,R45) are analyzed. The
strength ratio was decreased to the minimum about R00=2.5 when SI reached the maximum
compressive stress level. Figure 9 to 11 show the results of laminate strain histories and strength
ratios when biaxial S1 and S2 stresses were applied. The phase between S1 and S2 made a big
differences in the histories of laminate strains and consequently the minimum values of strength
ratios during one cycle of biaxial stresses. In the case of in-phase stress condition shown in
Fig.9, the strength ratio has the minimum value of about 4.5. But the phase between S1 and S2
reached to the 180 degree (Fig. 11), the strength ratio is decreased to less than 2. However it may
not be clear to discuss the fatigue properties directly from the difference of the strength ratios, the
acceleration of fatigue damage can be expected from these results.

The effect of biaxial loading phase on fatigue properties was also investigated by fatigue tests.
The cruciform specimen has the same [45/0/-45/0]s laminate but glass/epoxy plies are used to
observe the fatigue damages during the test directly. As seen in Fig. 12, the fatigue damage under
the 180 degree out-of-phase condition was much severe than that of in-phase stress condition.
CONCLUSIONS

An attempt was made to develop a tool for designing cruciform specimens of composite materials.
The importance of biaxial loading phase for estimating fatigue strength was pointed out by
analytical and experimental results.
« r ^ ™ ™ Beaver, P.W. (1984) ARL-STRUC-R-410, Ref. 1
REFERENCES Makinde,L., Thibodeau,D., Neale,K.W. and Lahoud,A.E. (1989). Proc. 1989
SEM Spring Conf. onExpr. Mech.,112-116, Ref.7
Susuki, I. and Tsai,S.W. (1984) Material System, 3, 99, Ref. 5
Susuki, I. (1985) Proc. 30th National SAMPE Symposium, 1179, Ref. 6
Swanson, S.R., Christoforou, A.P. and Colvin, G.E.,Jr. (1988). Experimental
Mech.,243, Ref. 2
Tsai, S.W. and Wu,E.M. (1971) J. Comp. Mat., 5, 58, Ref. 4
Tsai, S.W. (1988) Composites Design,4th edition, Ref. 3

Material: APC2
Laminate: (0/45/0/-45]s
SI: 200MPa(R-1)
S2: 40MPa(R-1)
Phase: 180 deg

Fig. 9 in-phase biaxial Fig. 10 out-of-phase (90deg.) Fig. 11 out-of-phase(180 deg.)

Variation of laminate strains(el,e2) and strength margin(R00,R45) during biaxial fatigue tests
 WS7f4

Impact Fatigue and Characteristics of S1O2

Fillers in Epoxy resin

M. Niinomi*, T. Kobayashi*. K. Uwai*, T. Ohishi*

and T. Higashihara**
* Department of Production Systems Engineering, Toyohashi
University of Technology, Toyohashi 441, Japan
'* Takaoka Chemical Co., Ltd.,
Jimokuji-cho, Ama-gun 490-11, Japan

ABSTRACT
Impact fatigue tests and tensile tests were carried out on epoxy resins filled
with various types of SiO? particles. The effect of the characteristics of SiO?
particle fillers on impact fatigue strength and tensile strength characteristics or
epoxy resins was investigated. The effect of silan coupling treatment which was
considered to be effective for preventing water infiltration on impact fatigue
strength and tensile strength of epoxy resins was also investigated. The S1O2
fillers used in this study were coarse, fine and very fine milled ones, and very
fine molten and coarse molten globular ones. Siian coupling treatment was
conducted with some of the epoxy resins filled with coarse milled S1O2
particles.
Relationship between maximum impact cyclic tensile stress, σ^ and cumulative
duration time, (Nf-Te) was able to be described by the following equation for
each epoxy resin:
of(Nf-Te) m =D
where D is a constant which is a measure of a material's strength, and m is a
constant which reflects the amount of strength lost due to the accumulation of
impact fatigue damage.
Impact fatigue strength of the epoxy resin conducted with silan coupling
treatment decreased slowly with suction time of water while that of the epoxy
resin without silan coupling treatment decreased rapidly.

KEYWORDS
Impact fatigue strength; tensile strength; epoxy resin; S1O2 fillers;
water suction; silan coupling treatment.

INTRODUCTION
Epoxy resin filled with S1O2 particles is used widely as a high voltage insulator
because it is superior in various electrical characteristics. Traditionally, great
importance has been attached to the electrical properties of insulators while
mechanical strength has received less attention in the design of insulating
549
550
structural materials such as epoxy resin filled with S1O2 particles. However, the
strength characteristics and the fracture mechanism under impact loading
conditions should be considered because insulators are often subjected to
impact stresses.
Epoxy resin filled with S1O2 particles is often used for the structural materials in
high voltage switches (Kamata et al., 1981). In such usage, in particular,
impact stresses are cyclically loaded on them. Therefore, impact fatigue of
epoxy resin filled with S1O2 particles is coming up to be important problem.
Various types of SiO? particles are used for fillers of epoxy resin. They are, for
example, "milled, molten and molten globular ones, respectively. It is also
important to investigate the strength of epoxy resin filled with various types of
Si02 particles under cyclic loading conditions.
Silan coupling treatment is, in general, conducted with epoxy resin filled with
S1O2 particles in order to prevent water infiltration for outdoor usage.
The effects of the characteristics of S1O2 particle fillers such as coarse, fine and
very fine milled ones, and very fine molten and coarse molten globular ones,
ana silan coupling treatment on the static tensile fracture strength of epoxy
resins and impact fatigue strength were investigated in this study. The
microfracture mechanisms of impact fatigue were also examined.

EXPERIMENTAL PROCEDURE
Test materials were epoxy resin filled with various types of S1O2 particles. The
S1O2 particles used were coarse, fine and very fine milled ones, and very fine
molten and coarse molten globular ones. Some of the epoxy resin filled with
coarse milled S1O2 particles were conducted with silan coupling treatment. The
weight percentage of S1O2 particles was 60 wt% in each epoxy resin.
JIS K 7113, No. 3 specimens were made by casting in a vacuum to inhibit the
formation of fine gas bubbles and voids. These specimens were used for both
impact fatigue tests and static tensile tests.
Static tensile tests were carried out according to the tensile test method of hard
plastics (JIS K 7113) at a cross head speed of 5 mm/min using an Instron type
machine at room temperature. Impact tensile fatigue tests were carried out
under cyclic tensile loading at a frequency of 10 cycles per second (c.p.s.) at
room temperature using fne newly developed impact tensile fatigue testing
machine by one of the authors (M. Niinomi et al.t 1990).
Water suction tests were carried out according to the water suction test method
of hard plastics (JIS K 6911) on the impact fatigue test specimens with and
without silan coupling treatment, which were made of epoxy resins filled with
coarse milled SiÖ2 particles. Tensile strength tests and impact fatigue tests
were also carried out on water sucked specimens.

EXPERIMENTAL RESULTS AND DISCUSSION

Static tensile strength
The static tensile strength of epoxy resins filled with various types of S1O2
particles are shown in Fig.1. The static tensile strength is greatest in epoxy
resin filled with very fine molten SlOo particles and smallest in one filled witn
coarse milled S1O2 particles when without silan coupling treatment. The static
tensile strength of epoxy resin filled with S1O2 particles tends to increase with
decreasing tne size of SiO? particles. The epoxy resin filled with molten S1O2
particles snows greater static tensile strength than one filled with milled Si02
particles. Silan coupling treatment decreases tensile strength of epoxy resin
 551
filled with S1O2 particles.
120
«3
Q.

C/)

(a) (b) (c) (d) (e) (0

Specimen mark
Fig. 1 Static tensile strength of each test specimen.
(a) Coarse milled S1O2 particles (silan coupling treatment)
(b) Coarse milled S1O2 particles (non treatment)
(c) Fine milled SiO? particles (non treatment)
,d) Very fine milled S1O2 particles (non treatment)
;e) Coarse molten globular SiO? particles (non treatment)
(f) Very fine molten S1O2 particles (non treatment)
Impactfatiguestrength
Effects of the size and types of SiQ2 particles. The relationships between the
amplitude of the impact stress, at, and the cumulative duration time, (Nf-Te)
where Nf is the number of impact stress cycles to failure and Te is the loading
time, that is, S-(Nf-Te) curves in epoxy resins filled with coarse, fine and very
fine milled SiO? particles, and very fine molten and coarse molten ones without
silan coupling treatment are shown in Fig.2. Each relationship between a\ and
(Nf-Te) was round to be expressed by the following equation (Okabe et al.,
1985) (Nakayama etaL, 1985):

ov(NfTep=D (1)
where D is a constant which is a measure of a material's strength, and m is a
constant which reflects the amount of strength lost due to the accumulation of
impact fatigue damage.
The impact fatigue strength seems to be greater with increasing the size of
S1O2 particles in lower (Nf-Te) region while that seems to be greater with
decreasing the size of S1O2 particles in higher (Nf-Te) region when the milled
S1O2 particles are used.
S-(NfTe) curves of epoxy resins filled with coarse milled and coarse molten
globular S1O2 particles clearly cross at a point where impact fatigue stress is
round 50 MPa.
The impact fatigue strength of epoxy resin filled with very fine molten S1O2
particles is greater than that of the epoxy resin filled with very fine milled ones,
and is greatest among others.
Effect of the silan coupling treatment. S-(Nf-Te) curves of epoxy resins filled
with coarse milled S1O2 particles with and without silan coupling treatment
before water suction are shown in Fig. 3. Impact fatigue strength is greater in
epoxy resin without silan coupling treatment than in that with silan coupling
treatment. Since the slopes of both lines in Fig. 3 are almost same, that is, m of
552

both lines are almost same, the difference of impact fatigue strength in this
case is considered to be depend on D in equation (1). Therefore, this difference
in impact fatigue strength is resulted from the difference in static tensile
strength.
100r
a.

u
a.
E
1 10 102 103 104
Cumulative duration time , (Nf -Te) ; sec
Fig. 2 Effect of the size and types of S1O2 particles on
cumulative duration time (Nf -Te) for epoxy resin filled
with S1O2 particles under the condition of cyclic
triangle impact tensile stress pattern.
(a Coarse milled S1O2 particles
b) Fine milled SiO?particles
(c) Very fine milled 01O2 particles
(a) Coarse molten globular SiO? particles
(e) Very fine molten S1O2 particles
100 1
1 1 I I 1
o_ — • — W i t h silan coupling treatment
| «s
.
—A--Without silan coupling treatment

" ^1 ' "^w

V)
ω 50 ^J 1 -• ^ 1 " A
^ 1 >A.
^ < 1· ^ > A

^·v f ^
20
1 10 10 2 103 104
Cumulative duration time, (Nf-Te) ; sec
Fig.3 Effect of silan coupling treatment on cumulative duration
time (Nf -Te) for epoxy resin filled with S1O2 particles
under the condition or cyclic triangle impact tensile
stress pattern.
S-(Nf-Te) curves of epoxy resins filled with coarse milled SiO? particles with
and without silan coupling treatment after water suction are shown in Fig. 4
Suction time of water is 40 hours in this case. The impact strength of the epoxy
resin without silan coupling treatment is still greater than that o f the epoxy resin
with silan coupling treatment at a smaller ( N f l e ) than round 70 sec. However,
 553
the difference of the impact fatigue strength between epoxy resin with silan
coupling treatment and that without silan coupling treatment is smaller
compared that before water suction in this (NfTe) region. The impact fatigue
strength of epoxy resin with silan coupling treatment is greater than that of
epoxy resin without silan coupling treatment at a larger (NfTe) than round 70
sec. Therefore, silan coupling treatment is effective for preventing a decrease
in impact fatigue life of epoxy resin filled with S1O2 particles in wet conditions. It
was also confirmed that silan coupling treatment was effective for preventing a
decreasing in static tensile strength in wet conditions.

Γ
80
GL I V
1 ^
1 »N

'Z 50

• V ^L

1 ^ x
— # - W i t h silan coupling treatment ^ 1 1
—A--Without silan coupling treatment ^
Q.
E
10 11 11 ii M
1 10 102 103 104
Cumulative duration time , (Nf -Te) ; sec
Fig. 4 Effect of silan coupling treatment on cumulative duration
time (Nf -Te) for epoxy resin filled with SiO? particles
under the condition of cyclic triangle impact tensile
stress pattern after water suction for 40 hr.
Relationship between impact fatigue life and fracture surface morphology
The impact fatiaue crack propagation path is schematically shown in Fig. 5 in
coarse milled S1O2 particles. The fracture surface is composed of stable and
unstable crack growth stages. The fracture surface of the stable crack growth
stage was macroscopically smooth. The stable crack growth stage was
relatively longer in the specimen which showed longer impact fatigue life. On
the other hand, this stage was confined to a relatively small area very near the
crack initiation region in the specimens which showed lower impact fatigue life.
The fracture surface was very rough, and secondary crack was also observed
in this stage. In the stable crack growth stage, crack propagates along the
epoxy resin-SiC>2 particle interface. On the other hand, crack propagates
through the large S1O2 particles in the unstable crack growth stage. However,
crack did not propagate through SiO? particles even in the unstable crack
propagation stage when S1O2 particles were fine and very fine milled and
molten ones.
The direction of crack propagation

Stable fracture Unstable fracture

Fracture surface S1O2 particle

.—*\ \

I <?
Fig. 5 Schematic diagram of impact fatigue crack propagation
path in coarse milled S1O2 particles.
554
CONCLUSIONS
The effects of the characteristics of S1O2 particle fillers and silan coupling
treatment on impact fatigue strength and tensile strength characteristics or
epoxy resins were investigated. The microfracture mechanisms of impact
fatigue were also examined. The following conclusions were obtained.
(1) Static tensile strength increases with decreasing the size of the S1O2
particles. Static tensile strength in molten S1O2 particles is greater than that in
milled S1O2 particles.
(2) Relationship between the impact stress, o\f and cumulative duration time,
(Nf-Te) is able to be described by the following equation :
Gf(NfTe)m = D
where m and D are impact fatigue characteristics parameters.
(3) The impact fatigue strength tends to increase with decreasing S1O2 particle
size in higher impact fatigue life region while opposite trend is observed in
lower impact fatigue life region in milled S1O2 particles. The impact fatigue
strength in molten S1O2 fillers is greater than that in milled ones in higher
impact fatigue life region while a opposites trend in observed in lower impact
fatigue life region.
(4) The fracture surface is composed of stable and unstable crack growth
stages. In the stable crack growth stage, crack propagates along the epoxy
resin-Si02 particles interface. In the unstable stage, crack propagates through
the S1O2 particles when coarse milled S1O2 particles are used. Crack
propagation through S1O2 particles is not observed even in unstable crack
growth stage when fine, very fine milled S1O2 particles and molten ones are
used.
(5) Silan coupling treatment decreases impact fatigue strength and tensile
strength of epoxy resin filled with SiO? particles. However, this treatment is
effective for preventing a decrease in static tensile strength and impact fatigue
strength in wet conditions.

REFERENCES
I.Kamata and N.Okabe (1981). J. Japan Inst. Electricity, 43., 101
M.Niinomi, K.Uwai, T.Kobayashi and A.Okahara (1990). Impact fatigue
of epoxy resin filled with SiO? particles. Engng. Frac. Mech. , in press
N.Okabe, T.Yano, I.Kamata and TtMori (1985). Impact fatigue strength
and reliability for filler reinforced epoxy resin castings under the
condition of high temperatures. J. Soc. Mater. Japan, 24, 333-339
H.Nakayama and T.Tanaka (1985). Impact fatigue. J. Soc. Mater. Japan,
24, 1483-1489
WS8a1

ADVANCES IN THE POTENTIODYNAMIC REACTIVATION

METHOD

V. CIHAL

University of Mining, Faculty of Metallurgy and

Materials Engineering, 708 33 Ostrava; National
Research Institute of the Protection of Mate-
rials, 190 11 Praha 9, Czechoslovakia

ABSTRACT

The paper briefly describes the early phases of the development

in the electrochemical potentiodynamic reactivation method for
measuring the degree of sensitization or structural transformat-
ion in stainless steels.

By using the reactivation procedure from the full passivity or

transpassivity region one can assess the tendency of the res-
pective type of steel and alloys for intercrystalline or select-
ive corrosion. The processof measuring using reactivation from
the incomplete passivity region indicates local changes in che-
mical composition in relation with the phase transformation.

KEYWORDS

Electrochemical potentiodynamic reactivation method; stainless

steels; intercrystalline corrosion; intergranular stress cor-
rosion cracking; passivity; transpassivity.

INTRODUCTION

Following upon the initial potentiodynamic registering of stain-

less steels we followed the procedures aimed atthe detection
of the tendency to intercrystalline corrosion (Cihal et Prazäk,
1956, 1960) as wellas for the etching of various structural
phases or regions (Cihal et Prazäk, 1959).

The efforts to use this method for a quantitative evaluation of

the sensitivity of stainless steels to intercrystalline cor-
rosion continue to be of interest. Up till the present, as the
criteria of evaluation of the tendency to intercrystalline cor-
rosion, the measurements of the values of the critical passiva-
tion current density were being applied, later eventually also

557
558
the values of the current density on reactivation from the pas-
sive or the transpassive state (Cihal et al. , 1970)°. In some pa-
pers the sensitivity is related to changes in the passivation or
the activation potential. However, all these indicators appear
as not being entirely sufficient for a dependable quantitative
evaluation of the tendency of the steels toward intercrystalline
corrosion. In connexion with the complex of a wider study of
electrochemical and corrosion characteristics of the phases in
stainless steels particuraly of the microstructural dissolution
of TiC and Ti^S before 22 years in "Centre de Recherches d U n i -
eux de la CAFE", at present "Societe U N I R E C , Groupe USINOR-SACI-
LOR", suitable testing conditions were established to follow the
intercrystalline corrosion, on the principle of reactivation
from the passive or transpassive state (Cihal et al., (1969),
Fig.l. The most convenient criterion for the determination on
[A/0,5 ein]

Fig. 1. Potentiodynamic polarization curves for

reverse recording from the transpassive state of
low-carbon steel (0.025*sC, 12.4%Ni, 18.5%Cr -
-curves 1,2,3) and stabilized steel (0.06%C,
12.05%Ni, 18.0%Cr, 0.65%Ti-curves 3,' 4) in
Η950Δ (2.5 mol/1) at 70°C (N9), v = 9 V/h.
lz lI50°C/20min/water + 650°C/lh/water
2 1150°C/20min/water + 550°C/20h/water
3,3 'll50°C/20min/water + 550°C/200h/water
4 1300°C/20min/water + 550°C/200h/water

the degree of corrodibility appears to be the following of the

entire reactivation region, be it its area or, still better, its
electric charge (Fig. 2), which reflects the major effect of the
preferential dissolution of the grain boundaries impoverished in
chromium. The measurements carried out on low-carbon, unstabili-
zed or sxabilized austenitic chromium-nickel steels (Cihal et al
1976, 1977, 1980, Clarke,1976, 1980), also applied to imperfec-
tly stabilized steels and ferritic chromium steels, laid founda-
tions to a new potentiodynamic polarization method for following
up the tendency to intercrystalline corrosion and intergranular
 559

Fig. 2. Schematic polarization curves for the

single and double loop of potentiodynamic reac-
tivation method.

stress c orrosior
Dn cracking. The detailing a nd rendering this me-
thod mor e accurE
rate also became the object of efforts of other
institut ions (Be
3orello et al., 1981, Mignon e et al., 1982, Han-
ninen ejt al. , 1989); we as well are focusing our attention at it
in this paper .
A progra m was r ecently comp leted to d evelo p a quan titat lve m e-
thod for nondes tructiv ely m easur ing t he de gree of sensi tizat ion
in auste nitic ( Nazarov 198 4) an d fer ritic , martensitic or m ar-
tensite- austeni tic ste els ( Cihal et a 984, 198 5, 19 88).
Those ef fort in eluded the f abric ation and qualific ation of a
niaturiz ed elec trochem ical field cell and the desi gn of arra nge-
ments fo r fabri cation of po rtabl e pol ariza tion sys tern t o be used
with pot entiody namic r eacti vatio n eel 1. Th e techni que w as ex
tended t o chara cterize weld heat -affe cted zones an d to corre late
the degr ee of s ensitiz ation with inte rgran ular str ess c orros ion
cracking resist ance (C larke ,1980 ). Al 1 tests used by th e ind u-
stry to detect degree of se nsiti zatio n are conside red d ef icient,
and thes e defic iencies limi t the use of th ese test s in shop- fa-
bricated and fi eld-con struc ted ( welde d) co mponents . It was a nti-
cipated that th e resul ts of the poten tiody namic re activ ation
measurem ents co uld be compa red t o results of stres s corrosio n
cracking tests on mate rial with a sim ilar degree o f sensitiz a-
tion. Th us, a judgment coul d be made conce rning th e pos sibil ity
of inter granula r stress cor rosio n era eking occurin g in the c om-
ponent i n servi ce. The proc edure s and spec ificatio ns fo r con duct-
ing pote ntiodyn amic re activ ation meas ureme nts are prese nted in
the stan dard pr actice forma t.

The principle of the potentiodynamic reactivation method

560
Compared with the standard test in the solution of H«S0.+ CuS0.+
Cu, the described method is quicker and much more accurate. In
order to check it we followed chrom-nickel steels with graduated
carbon contents and cold deformation. Developing the method we
are bearing in mind the greatest possible unification respecting
at the mean time the postulate of optimum accuracy of measure-
ment .
In consideration of the said facts and on the basis of provisio-
nal measurements the conclusion was reached that if we are to
judge the extent of impoverishment in chromium and consequently
also the degree of tendency to intercrystalline corrosion and
stress corrosion cracking it is necessary to choose a comparative
measurement from which the retardation of the total activation
as a results of the formation of a passive layer would follow.On
the surface of the passivable steels, as a result of action by a
suitable electrolyte and by an extrinsic forced potential, a pas-
sive layer is formed, its character depending chiefly on the che-
mical composition of the basic solid solution and on the compo-
sition of the corrosive medium, and to a some extent on the
stresses developed around from loading and the precipitated pha-
ses.

EXPERIMENTAL CONDITIONS

The potentiodynamic test is accomplished by developing potentio-

dynamic curves of a polarized sample obtained by controlled po-
tential survey particularly from the passive to the active re-
gion (reactivation) in a specific electrolyte. Referring to the
polarization curves in Fig. 2, the potentiodynamic test is con-
cerned with the active portion of the curve. The passive film
may remain intact for a limited time also in the active poten-
tial region. Because this is a metastable state, any defect in
the film will cause the surrouding film to breakdown. A sensiti-
zed steel passivated almost normally, but when the potential is
changed from the passive to the active region, the current den-
sity will rise as a result of the passive film breakdown. If the
steel is not sensitized, the time to breakdown is much longer.
The criteria used to distinguish between sensitized annealed sam-
ples include the reactivation charge C (in Coulombs) or ratios
of reactivating and passivating current densities peaks and char-
ges C /C (in %)(given by the integrated area below the reactiva-
tion or The passivation peaks of the curves), and the potential,
at which the active curve breaks upward (Flade potential).
These measured values are all dependent on polarization rate,
composition, and temperature of the electrolyte, composition of
the steel tested, sample surface condition, and other factors.
The test parameters, therefore must be kept constant to study
the reactivation of steels and alloys that exhibit active-passive
behavior. To complete the measurement, the value C is normalized
by both specimen size and grain size; the data normalized in
this fashion are called P or Q, and represent the charge (in Cou-
lombs/cm ) of grain-boundary area (Clarke,1980) or grain bounda-
ry length (in Coulombs/m) (Hanninen, 1989), QL=0.0104.P . This
treatment of the data permits normalized direct comparisons of
different C values solely as a result of differences in grain
 561
size. Initial studies were conducted using I^SCK (2.5 mol/1) at
70°C. Greater sensitivity particularly by titanium stabilized
steels could be obtained by adding some activator, to sulphuric
acid (0.5-2 mol/1), e.g. potasium and ammonium thiocyanate or
other. This test face an added advantage because it is generally
performed at 30°C or ambient temperature (Fig. 3 ) . One must also

1Cr18NM0Ti 2M HtS04 CSN

IQjOKKCNS 03 8169
m l 20'c
Ca-Cpm

Fig. 3. Results of tests of the potentiodynamic

reactivation method in H2Sü\(2 mol/1) at 70 C and
with 0.01%KSCN at normal temperature, compared
with depth of penetration of intercrystalline cor-
rosion from test in H?S0.+CuS04+Cu(Standard 1967)
for austenitic lCrl8Nl9Ti steel, and sensibilized
on 650 C. Polarization curves were taken from test
in H 2 S0 4 (2 mol/1) + 0.01%KSCN at normal temperature.

balance the reactivation scan rate with the test temperature to

intensify adequately the,measured,response for sensitized speci-
mens. The scan rate 6Vh or 9Vh was related because of the
limitations of the instruments. There is about a twoorder-of-
magnitude increase in C for example, when scanning at the slo-
wer scan rates are preferred over the faster techniques.
562

°25ΠθΠ50°4θΟ

Fig. 4. Influence of tempering temperatures (4h)

on the critical passivation current density 3
and raportjC^/C of martensitic 15Crl7Ni2 stain-
less steel quenched from 1040°C/3min/oil. Mea-
sured in H 2 S0 4 (0.5 mol/l)+0.01%KSCN at normal
temperature (v=0.5 V/h).

The usual technique for potentiodynamik reactivation testing is

to expose a freshly polished sample to the electrolyte, it is
charged cathodically and than the passivation potential applied
using e.g. the following procedure -0 . 7<* + 0 . 5 «·- -0 . 7 V(SCE) for
the determination of sensitivity to intercristalline corrosion.
The sensitivity of the potentiodynamic reactivation test for
Crl8Nil2Mo2 steels can be increased by increasing the amout of
activator and/or by using slower reactivation scan rates. This
method can be used on nickel alloys or on ferritic steels (Cihal
1984, Borello et al., 1981). The advantage of this method is
speed and perception of the effect of more factors affecting the
properties of stainless materials; e.g. in addition to depletion
the effect of carbides or phases rich in molybdenum, the effect
of titanium carbides and sulphides in stabilized steels, etc.,
ca be involved (Fig.l).
Also martensitic and martensite-austenitic steels were measured
in the upper potential range with the purpose to evaluate the
effect of a molybdenum addition on the corrosion-electrochemical
properties of this type of steels (Cihal et al., 1984, Hubäckovä
et al. , 1986). Low carbon type of 03Crl3-16Ni4-6 steels, alloye
with molybdenum to relieve susceptibility to temperbrittleness,
may be prone to intergranular corrosion penetration along the
austenite grains after being heat-affected at around 450-600°C,
even if they are relatively low in carbon, and similar behaviour
may be observed in 15Crl7Ni2 martensitic steel (Cihal et al.,
1988) (Fig.4). With steel 03Crl3Ni6MoO.5, this procedure was sup
plemented with measurement based on reverse decreasing of the
potential before the full passivity, using the procedure -0.7-*
— -0.1 -~-0.7 V (SCE). The latter procedure is significant in
view of the splitting of the peak critical passivation current
 563

Er»«]'

Fig. 5. Potentiodynamic polarization curves of

steel 03Crl3Ni6Mo determinated on specimens after
quenching at 1050°C/2h/air (c), quenching and
tempering at 575°C/6h/air (b), quenching and tem-
pering at 625°C/6h/air (a) (v = 9V/h).

density, manifesting itself more distinctly at decreasing poten-

tial from -0.1 — - 0 . 7 V (Fig.5).
The reverse decrease of potential from incomplete passivity re-
gion leads to amplificat ion of the manifestations of phenomena
taking place even in the first stage -0.7 «—-0.1 V in the acti-
vity region.. The splitt ing of the current density peak in the
activity region and the intensification of this splitting during
the reverse process has only been observed with steels alloyed
additionally with molybd enum additions, after tempering in the
region of intercritical temperatures, while the level of the
peak corresponding to th e more positive potential was higher at
the higher content of th e transformed phase. This splitting is
not directly related to the splitting of polarization curves
typical for Fe-Cr alloys containing about 9% Cr(Cihal, 1984).
In this connection it sh ould be noted that according to the pre-
liminary results of elec tron microanalysis no redistribution of
chromium was observed in the base matrix, but present austenitic
regions were shown to be enriched with nickel. The results of
potentiostatic etching imply that the first peak obviously cor-
responds to dissolution of the martensitic matrix and the other,
situated at the more possitive potential, corresponds to disso-
lution of a phase richer in nickel, which may be either stable
austenite or the product of its reverse transformation to marten-
site (non tempered martensite). if he process of measuring using re-
activation from the incomplete passivity regions indicates local
changes in chemical comp osition in relation with the phase trans-
formation that is taking place.
564
REFERENCES

Borello, A., La Barbera A., Mignone., A. and Vittori, M.(1981).

Intergranular corrosion of alloys 800 by the electrochemical
potentiokinetic reactivation method. Werkstoffe und Korrosion
22, 332-7.
Cihal, V., Prazak, M. (1956,1960). A contribution to the expla-
nation of intergranular corrosion of chromium-nickel steels.
Hutnicke listy, 11, 225-230; Corrosion, 16, 530p - 32p.
Cihal, V., Prazäk, M.(1959). Corrosion and metalographic study of
stainless steels with potentiostat technique, 3. Iron Steel
v Inst.,193, 360-67.
Cihal, V., Desestret, A. et al. (1969). Rapports du Centre de
Recherches d'Unieux de la CAFL, Firminy,. N ü 943, 958.
Cihal, V., Desestret, A., Froment, H. and Wagner, G.H. (1970).
Influence des proprietes electrochimiques des carbures de chro-
me, de niobium et de titan sur la corrosion intergranulaire ou
incisive d#'aciers inoxydables. CITCE Praha,5ept.-Oct. , 287.
Cihal, V., Fürychovä 3., Kubelka, 3. (1976). Elektrochemische
Methode zur Untersuchung Anfaligkeit korrosions-bestandige
Stahle für interkrystalline Korrosion. Werkstoffe und Korros.
27., 782-87.
Cihal, V. (1977). Potentiodynamics methods of following up inter-
crystalline corrosion. Materials Chemistry, 2., 121-32.
Cihal, V. (1980). Potentiokinetic method for predicting the IGC
and IGSCC sensitivity of stainless steels and alloys.
Corrosion Science, 20, 737-44.
Cihal, V., Hubäckovä, 3., Kubelka, 3., Mazanec, K. (1984). The
potential polarisation method for the evaluation of martensite-
austenite stainless steels, Materials Chemistry and Physics,
n , 279-93.
Cihal, V., Hubäckovä, 3., Kubelka, 3., Mazanec, K. (1984).
Evaluation of martenzite austenitic stainless steels from the
full and incomplete passivity by potentiokinetic method.
Corrosion Science,24, 781-87.
Cihal, V. (1984). Intergranular Corrosion of Steels and Alloys.
SNTL-ELSEVIER, Praha-Amsterodam.
Cihal, V., Hubäckovä, 3., Kubelka, 3., Mazanec, K. (1985). A Study
of corrosion electrochemical properties of martensite-auste-
nite steel Crl5Ni6Mo. Corrosion, 41, 625-30.
Cihal, V., Kubelka, 3., Tupy, 3., Bouska, P. (1988). Comparison
of two measuring sets for potenciokinetic study. Koroze
a ochrana materiälu, No 3, 50-51.
Clarke, W.L., Cowan, R.L. (1976,1980). EPR method for detection
of sensitization. Seminars for BWR Safety, Palo Alto, 3an.
Hanninen, H.(1989). Intergranular stress corrosion cracking.Rep.
NKA Pro.jet MAT 530, VTT Finland, Sept.
Hubäckovä, 3. et al.,(1986). Intergranular failures in Crl3Ni6
steel. 9th Congr.Mater.Testing, Budapest, Sept. - Oct.
Majidi, A.P., Streicher, M.A. Cl984).Potentiodynamic Reactivat.
method for Detecting Sensitization. Corrosion,40, 393, 584.
Mignon, A., et al. (1982). Electrochemial Potentiokinetic Reacti-
vation Method. Corrosion, 38, 390-402.
Nazarov, A.A. (1984). 0b ispolzovanii metoda potenciokineticeskoj
reaktivacii. Vopr.Sudostrojenija,Metallurg!,ja, 41, 37-42.
Standard CSN 03 8169 (1967). Testing the resistance of stainless
steels to intercrystalline corrosion.
WS8a2

MONTE CARLO SIMULATION FOR ELECTROCHEMICAL NOISE

DUE TO LOCALIZED CORROSION

Toshio SHIBATA

Department of Materials Science and Processing,

Faculty of Engineering, Osaka University,
2-1 Yamadaoka, Suita, 565 JAPAN.

ABSTRACT

Electrochemical noise has been known to generate during corrosion

process, especially during localized corrosion such as pitting, crevice
corrosion and stress corrosion cracking. A characteristic power spectrum of
electrochemical noise showing a plateau in a lower frequency region and a
rapid decrease with frequency in a higher frequency region has been found.
The characteristic feature of the power spectrum was successfully simulated
by a Monte Carlo simulation based on the stochastic models which had been
proposed previously.

KEYWORDS

Localized corrosion; random noise; Monte Carlo simulation; stochastic model;

corrosion monitoring.

INTRODUCTION

Localized corrosion including pitting corrosion, crevice corrosion and

stress corrosion cracking had been known to generate various types of noise
in corrosion potential. Dawson(1983) had proposed a corrosion monitor
measuring a noise power in a specific frequency range. Loto and
Cottis(1987), and Yamakawa et al.(1988) had reported that changes in the
power spectrum density of corrosion potential noise could be an indication
of crack initiation. Other experimental evidences accumulated in recent
years(Okamoto et al, 1976, Tachibana, 1982) suggest that correlation would
be found between noise power and corrosion intensity including the number of
corrosion sites and their corresponding corrosion rate, but proper physical
models have not been presented.
We(Shibata,1976, 1981) had proposed various stochastic models for
explaining the probability distribution of pitting potential or induction
time for pit generation. Williams et al.(1985) had reported that noise
generation during pit generation and growth process of stainless steel could
be properly analyzed by assuming a stochastic model.
In this study, the birth and death stochastic model which had been
565
566
proposed previously(Shibata, 1981) was examined by using a Monte Carlo
method for simulating the noise spectrum for pit generation and
repassivation, because pit is the most representative form of localized
corrosion and an identical model could be applicable for the other form of
localized corrosion including SCC.

STOCHASTIC MODELS AND MONTE CARLO SIMULATION

A whole process of pit formation due to breakdown of the passive film

by chloride ions could be divided into generation of nucleus and its growth
to a macro pit. The growth process, however, is occasionally interrupted
by the film formation or repassivation. Both processes of generation and
repassivation are known to show a random fluctuation with time. Then
generation and repassivation are called a birth and death stochastic
process, respectively. If the growth process is not interrupted by
repassivation until the pit reaches to a critical size, the growth process
will continue and result in a macro pit. The time when the pit reaches the
critical size is conventionally defined as an induction time for a pit
formation.
Gabrielli et al.(1990) had emphasized the importance of a prepitting
stage, during which generation and repassivation are taking place at random
while any macro pit does not form, because the noise in this stage could
provide an information of the pitting resistance of the material without
macro pit formation.
In this study, the electrochemical noise during the prepitting stage
will be simulated based on the birth and death stochastic models. In the
following discussion, two models are assumed for generating the
electrochemical noise. The first is a constant probability(CP) model
proposed by Kendig and Hagen(1987). The second is an exponential
probability(EP) model which has been proposed by us(Shibata et al. 1981) for
the probability distribution of the induction time for the macro pit
generation. In either models, the initial state is the steady passive
state attained at a constant potential in a chloride free solution. Then a
constant amount of chloride ions is assumed to be added into the solution
with keeping the potential constant. After the introduction of chloride
ions, a pit generates followed by the growth, but repassivates. This
process repeats again and again, resulting in the current fluctuation.

The constant probability model

The constant probability(CP) model assumes that a random birth or
generation event occurs with a constant probability, Pb, which is
independent of time, and the pit generated increases its diameter with
time, resulting in current increase. The current increase, I(t), with time
after generation at the constant potential is assumed to obey the following
deterministic rate law

I(t)=kt (1)

where k is a constant depending on the applied potential. During the

growth, the pit happens to repassivate with a constant probability, Pd,
which is also independent of time. The program was written by N88-BASIC
and the space and time are expressed as a matrix, S(I,J) where time, I, is
changed up to N=1024 and space, J, is changed up to L=10 because limitation
of the dimension size of N88 BASiC.^ The parameters for this CP model are
Pb(s ) , Pd(s ) and k which are given as an appropriate number in the
program.
 567
The exponential probability model
The exponential probability(EP) model assumes that birth or generation
of a pit takes place by a Poisson process, because the birth event is rare
in a large number of possible sites. In case of the Poisson process, the
probability of finding k pits in an interval of length t is given by

p(k; Xt) = (Xt)kexp(-A t)/k! (2)

where λ is the pit generation rate. Then the probability of finding no

pit in an interval, t, is given by

p(0;Xt)=Pb=exp(-xt) (3)

which is equivalent to the probability of finding the first pit, or the

probability of the birth, Pb, after the time t. Experimental evidences
suggest that the parameters of λ depends on the applied potential, but a
constant value was assumed in this study, because the applied potential was
not altered. After generation, the current increase for the growth,
I(t), assumes to obey the same deterministic equation as eq.(l). The death
process is assumed to occur by the same Poisson process, so that the
probability of the death, Pd, is also given by the same exponential function
as eq.(3);

Pd=exp(-yt) (4)

where V is the repassivation rate (s ). Thus the parameters for the EP

model are λ, μ and k. The same matrix, S(I,J), for the space and time as
the CP model was used.

The fast Fourie transformation

The out put of the simulation is the current noise in the time domain ,
for which a fast Fourie transformation(FFT) was applied to analyze the
effect of the parameters of the model on the noise and its characteristics.
Total number of the sample is N=1024 and the sampling time is t=0.1 s, so
that the minimum frequency, f . , and the maximum frequency,
n f , which can
u n J · r iimm max
be analyzed are given as follows;
f . =1/N t=l/(1024)(0.1)=0.00976 Hz
f min =l/2 t=l/(2)(0.1)=5 Hz

RESULTS AND DISCUSSION

The constant probability model

Fig.1(a) is an example of the current noise generated by the simulation
for the CP model. In this simulation, the numerical value for Pb, Pd and k
is assumed to be 0.1 and L is changed to 10 as shown in the figure.
Increase in L means the increase in the specimen area, or in the number of
specimen, which, in turn, gives more chance for nucleation and
repassivation, so that more fluctuations in the current can be expected.
This situation was realized in a series of curves from the bottom to the
upper illustrated in Fig.1(a). The corresponding power spectrum
density(PSD) was shown in Fig.1(b) as a function of frequency and L in the
log-log scale. As can be seen in the figure, a characteristic shape of PSD
curves was obtained. A clear plateau, or white noise in the lower
frequency region below 200 mHz with a minus slope in the higher frequency
region was obtained. Thus the PSD curves can be properly described by the
following equation,
568
(a) (bU
Pb=.l S(1024,L) Pb=.l
Pd=.l Pd=.l
K=.l K=.l
10~-2
ARBITRARY POWER
UNIT DENSITY

SCALE FACTOR X 1

10A-2 10~-1 [ 10"0

FREQUENCY/Hz

Fig.l Noises generated by the Monte Carlo simulation based on the CP

model and corresponding power spectrums obtained by FFT.

G(f>G°(f)/(l+(f/f0)n) (5)
nO,
where G (f) is a constant equivalent to the plateau level at the lower
frequency region and n is the slope of the line in the high frequency
region. The cross point frequency of the line at a half level of the
plateau, that is, G (f)/2, is f n which is a measure dividing the lower and
higher frequency region.
The another example to demonstrate the effect of the death probability,
Pd, on the noise and the PSD curves with Pb=.l and E=10 are shown in
Fig.2(a) and (b). Again the random fluctuations were simulated and Pd was
found to cause a large effect on the noise level as can be seen in Fig.2(a).
This change in the noise level makes PSD higher, while the same shape is
still hold as shown in Fig.2(b). The effect of Pb was also examined and
found to have a relatively small effect compared to the other parameters.
(a)
<*>>,

ARBITRARY
UNIT POWER
DENSITY

SCALE FACTOR X .1

TIME/s FREQUENCY/Hz

Fig.2 Effect of the death probability on noise and power spectrum.

The results were summarized in Fig.3 , in which the white noise level,
G (f), is plotted as a function of parameters of Pb, Pd and k, and a
relation was expressed as follows;
0 43 3 2
G°(f). ^Pb - Pd- k (6)
0.83
Pd (7)

Consequently, it can be concluded that the most important parameter to

change the PSD is the repassivation probability, Pd.
 569
The exponential probability model
Fig.4(a) is the effect of the pit
generation rate, λ, on the noise generated by
the EP model. The specific feature of the
EP model is a high density of the generated
noise in the early stage of generation and
the decrease in the pit generation rate
contributes to disperse the concentrated
noise to the latter stage. The corresponding £-3\
<n
PSD as shown in Fig.4(b), however, showed a c
quite similar shape as for the CP model and L f. - R?
a very little effect of λ was found.
The effect of P on the noise was shown I
in Fig.5(a), in which the decrease in λ
increased the noise level. The -2 -1 0
corresponding PSD in Fig.5(b) showed a LogiPb.RO/s'1 Logk /As1
parallel shift to the higher level with Fig.3 Effect of parameters
decreasing the repassivation rate, μ , while on the white noise
the white level in the lower frequency region level.
still can be seen.
(a) (b)
MU=. 1
T0=0 RAMDA=.3 X 1

ARBITRARY
UNIT
f RAMDA=.l x 1

,/ RAMDA=.03 x 1

/ L. /I ,
A
/ 1
RAMDA=.01 x 1

M
, RAMDA=.003 x 1
,<L A
i it

1 RAMDA=.001 x 1

L L.-A- .A S. ■ /I
10*-2
FREQUENCY/HZ

Fig.4 Effect of the pit generation rate of the EP model on noises

and corresponding power spectrums.
(a)

itr-2
FREQUENCY/HZ

Fig.5 Effect of the repassivation rate of the Ep model on noises

and corresponding power spectrums.

The effect of the parameter for the EP model could be summarized as:
0.16 -2.2
G°(f)- (8)
and illustrated in Fig.6. Again, the repassivation rate is the most
570
important parameter to change PSD, while
causes a very slight shift.

Noise analysis for corrosion monitoring

The above simulation indicates that the -
PSD level in the low frequency region
strongly depends on the death probability or
repassivation rate for both models. Total
numbernof pit also increases thenlevel of the
PSD, G (f), so that if the G U (f) could be
monitored in situ, the occurrence of
localized corrosion could be detected.
Even for the general corrosion, a similar
model could be applied if generation and
repassivation process were replaced by
dissolution and inhibition at active sites.
In fact, the same shape of the PSD as eq.(5) -3 -2 -1
was observed for the noise of corrosion Log λ ,Log μ /s"\
Fig ,6 Effect of parameters
potential of Type 304 stainless steel
immersed in MgCL· solutions(Shibata et al, on the white noise
1989). The G (fj was found to decrease with level.
time, suggesting the decrease in corrosion rate with the film formation.
Thus the white noise level could be used as a measure for the corrosion rate
with repassivation or inhibition of active dissolution as suggested by
Dawson(1983).

CONCLUSION

The PSD obtained by FFT from the simulated noise for the constant
probability model and the exponential probability model can be described^ by
eq.(5). It was found that the most important parameter to change the G (f)
was the death probability in case of the CP model, and the repassivation
rate in case of the EP model. The white noise level at the low frequency
region, G (f), is a good measure for occurrence of the birth and death
stochastic process in corrosion.

LITERATURES
Dawson, J. L., K. Hladky, and D. A. Eden (1983). In: Proc. Corrosion
Conference, UKT83. p.99.
Gabrielli. C , F. Huet, M. Keddam, and R. Oltra (1990). Corrosion,
46, 266-278.
Kendig, M. W. and G. Hagen (1987).In: 172nd Meeting of The Electrochem.
S o c , Extended abstracts. Vol.87-2. No.238.
Loto, C. A. and R. A. Cottis (1987). Corrosion, 43, 499.
Okamoto, G., K. Tachibana, S. Nishiyama, and T. Sugita(1976). In: Passivity
and Its Breakdown on Iron and Iron Base Alloys, pp.106-109. NACE, USA.
Shibata, T. and T. Takeyama (1976). Nature, 260, 315.
Shibata, T. and T. Takeyama (1981). In: Proc. 8th ICMC, p.146, DECHEMA.
Shibata, T., J. Horikawa, and S. Fujimoto(1989). Boshoku Gijutsu,38,155-160.
Tachibana, K. and G. Okamoto (1982). Rev. J. Coatig & Corrosion, 4, 229-267.
Williams, D. E. AND C. Westcott, and M. Fleishmann (1985).
J. Electrochem. S o c , 132, 1796-1804, 1804-1811.
Yamakawa, K. and N. Kajita, M. Murakami, and R. Hirayama (1988).
J. Soc. Mater. Sei., Japan, 37, 43-49.
 WS8a3

IMPROVED ELECTROCHEMICAL METHOD FOR PITTING

CORROSION INVESTIGATION

Rolf Qvarfort, Elisabet Alfonsson.

Research and Development, Corrosion Dept.

Avesta AB, S-774 01 Avesta, Sweden.

ABSTRACT

Due to the statistical nature of the pitting potential, it must be

concluded that a more appropriate parameter to use when ranking the pitting
resistance of different stainless steels is the critical pitting
temperature (CPT). This parameter is very easily determined if crevice
corrosion is eliminated during the test. This can be done with a newly
developed improved electrochemical cell - the Avesta-cell. At the CPT a
very drastic transition from transpassive corrosion to pitting is observed.

INTRODUCTION.

Over the past 15 to 20 years, electrochemical test methods have been

increasingly used to study pitting corrosion. In particular, the
potentiodynamic method, e.g. as described in ASTM Standard Practice G-61,
has been used as a rapid method to determine breakdown potentials of
different alloys. Experience shows, however, that the breakdown potential
varies considerably, also between specimens from the same sample. The
reason for this variation is in part of an experimental nature. With the
test techniques used it has not been possible to avoid simultaneous crevice
corrosion at the specimen mount, particularly when testing at elevated
temperatures.

Experimental difficulties is not the only cause of variations in the

measured breakdown potential. More recently the random nature of pit
initiation has been discussed and stochastic models have been developed to
describe its statistical nature. The basic features in the model presented
by Williams et.al. (1,2) are; (a) The pit initiation events have a
probability of dying (repassivation), (b) each event has an induction time
during which the local current does not increase but during which the pit
nucleus may repassivate, and (c) nucleation events which survive beyond a
critical age do not repassivate but develop into a propagating pit.

This means that, even under favorable conditions, it may take some time
before a propagating pit develops, and this time may vary between different
specimens. When the potentiodynamic method is used for testing and there is
a linear relation between time and potential, the measured breakdown
potential may vary considerably, even between different specimens from the
same sample. The breakdown potential is therefore not an appropriate
measure of the pitting corrosion resistance of a material, even if
experimental difficulties, e.g. simultaneous crevice corrosion, can be
avoided.

571
572
mV
SCE
1500
17-12-2.5L

1000

500·

-H 1 1 1 =1 1 1 — T"»»u I ·—^
10 20 30 40 50 60 70 80 90 100°C

Fig 1 Typical plots of breakdown (filled symbols) and

repassivation potential (open symbols) vs temperature for two
stainless steels.

A better choice is to use the CPT as a measure of the pitting resistance of

a material. This CPT was first mentioned by Brigham and Tozer (3) who
presented empirical evidence of its existence. Their conclusion was that
for every wholly austenitic steel there exists a CPT below which the steel
will not pit regardless of potential and exposure time. Their data,
however, is said only to approximate this parameter, obviously because of
crevice corrosion. Since that time there have been many papers published
which emphasizes this observation on empirical grounds. More recently, Le
Guevel et. al. (4) have discussed this matter on a more theorethical
ground. In their concept the incubation time for pit development accounts
for the existence of a CPT.

THE AVESTA TEST METHOD

The method we use to determine the CPT is based on a special
electrochemical cell for pitting corrosion which has been developed at our
laboratory. With this cell it is possible to completely avoid crevice
corrosion between the specimen and the specimen mount. The reason is that
there is no corrosive solution in this crevice, but a small quantity of
distilled water which is pumped through the crevice and out into the test
solution. The water flow, which typically is 4 - 5 ml/h, is too small to
significantly dilute the solution during the test. The design and function
of this cell, the Avesta pitting cell, is described elsewhere (5,6).
Our work with the Avesta cell has shown that the CPT can be measured with
very high accuracy if crevice corrosion in the specimen mount is avoided.
The determination of this parameter is based on anodic polarization curves
obtained at a series of temperatures. The polarization is done with a scan
rate of 20 mV/min starting at -300 mV(SCE). The scan direction is reversed
when the corrosion current density reaches 5 mA/cm2 and interrupted when it
falls below 10 ^A/cm2. The breakdown potential is defined as the potential
where the current density continuously exceeds 100 /iA/cm2 on the forward
scan and the repassivation potential where it reaches 10 /iA/cm2 on the
reversed scan. The CPT is then determined from plots of breakdown potential
versus test temperature as shown in Fig 1.
 573
The CPT can be determined quite easily from the very distinct transition
between transpassive corrosion and pitting. At temperatures below the
critical, the breakdown potential will reach high values and only
transpassive corrosion will occur. At temperatures above the critical the
breakdown potential, on the other hand, will be much lower and pitting
corrosion will develop. Above the CPT, there is a decrease in breakdown
potential with increasing temperature, but the measured values are
scattered also when there is no disturbance from crevice corrosion. This
must be considered to be an experimental evidence of the statistical nature
of the pitting corrosion process discussed earlier and confirms that the
pitting potential is not a good measure of pitting resistance.

EXPERIMENTS AND RESULTS

With the method described above a study was done on the influence of
nitrogen on the pitting resistance of stainless steels of type 316 and
316L.
Cold rolled samples of stainless steels, grades 17-11-2L, 17-11-2LN,
17-12-2,5L and 17-12-2,5LN, were investigated in normal solution annealed
condition. A sheet of grade 17-11-2 was investigated before and after
bright annealing in an atmosphere of cracked ammonia. The chemical
composition of the materials is reported in table 1. The 17-11-2 samples
were tested in the original surface condition while the others were wet
ground to 360 mesh finish.
The CPT:s obtained are shown in Fig. 2. The dashed part of the bars
indicate the minimum and maximum values obtained.

DISCUSSION
The CPT in 1 M NaCl is considerably higher for the nitrogen alloyed grades
17-11-2LN and 17-12-2,5LN than for the corresponding grades without
nitrogen. Several authors have reported similar positive effects of

Table 1. Test material, chemical composition.

Steel C Si Mn S P Cr Ni Mo N

17- - 1 1 - -2L 0.014 0.45 1.44 0.001 0.026 17.5 10.9 2.15 0.069
" 0.024 0.45 1.51 0.001 0.025 17.4 10.5 2.05 0.062
" 0.023 0.47 1.48 0.001 0.025 16.8 11.2 2.16 0.063
" 0.017 0.43 1.46 0.002 0.028 16.8 11.2 2.09 0.047

17- - 1 1 - -2LN 0.018 0.48 1.20 0.001 0.025 17.2 11.0 2.41 0.174
" 0.018 0.47 1.48 0.001 0.030 17.2 10.6 2.06 0.136

17- - 1 2 - - 2 , 5 L 0.023 0.45 1.56 0.006 0.028 17.3 12.5 2.46 0.070
" 0.020 0.39 1.42 0.002 0.029 17.3 12.6 2.72 0.066
·· 0.019 0.41 1.72 0.001 0.028 17.2 12.6 2.56 0.054
·· 0.030 0.37 1.78 0.001 0.027 17.4 12.8 2.58 0.050
·· 0.017 0.43 1.60 0.001 0.031 17.2 12.6 2.60 0.058
" 0.015 0.45 1.69 0.001 0.028 17.0 12.7 2.62 0.054

17- - 1 2 - - 2 , 5 L N 0.020 0.39 1.50 0.001 0.022 17.6 12.3 2.61 0.142
" 0.016 0.43 1.45 0.001 0.029 17.2 12.2 2.55 0.187
" 0.022 0.22 1.51 0.002 0.024 17.6 12.3 2.61 0.144

17-- 1 1 - -2 0.041 0.38 1.51 0.003 0.026 17.1 10.7 2.02 0.025
574

CPT/°C

Fig 2 CPT-values obtained in IM NaCl solution.

nitrogen, e g Ito and Yoshi(7) who investigated steels containing 0,5% Mo,
8-11% Ni, 19% Cr and 1,5% Cu. Streicher(8) found 0,12 % nitrogen in 304L
and 316L to reduce the number of pit initiation sites produced during
anodic polarisation in 0,1 M NaCl. Several authors, e g Herbsleb(9),
suggest that the positive effect of the elements Cr, Mo and N on the
pitting resistance is additive and can be expressed as a "pitting
resistance equivalent", PRE. Herbsleb(9) suggests the expression "PRE = %Cr
+ 3,3 %Mo + 30 %N" for austenitic stainless steels. Results reported by
other authors (10) indicate the existance of a synergistic effect between
nitrogen and other alloying elements, principally molybdenum. The latter is
not contradictory to our results. We found the "mean" increase in pitting
resistance by nitrogen alloying to be slightly bigger for 17-11-2L with
«2,2%Mo than for 17-12-2,5L with «2,6% Mo. The difference is, however,
rather small and the number of assessments to small for us to make any
general conclusion. The very marked increase in pitting resistance with
only a small increase of the nitrogen content, which was found by Truman et
al (11), in a steel with high enough contents of chromium and molybdenum,
Fig 3, is however attributed to the test method used. The reason for the
marked increase in pitting potential found for an alloy with 20% Cr and 3%
Mo is in our opinion the fact that, due to the nitrogen addition, the CPT
of the material is raised above the test temperature. Then the breakdown of
passivity is no longer caused by pitting but transpassive corrosion. A
similar influence of nitrogen addition could be observed also for the lower
alloyed steels of Fig 3 if the test was performed at a lower temperature.
When the relative pitting resistance of different alloys is investigated by
assessment of the pitting potential, the test temperature must be carefully
chosen to be well above the CPT of all alloys tested. Otherwise
unreasonable differences between alloys may be found as the measured
breakdown potentials are attributed to different corrosion mechanisms. This
can be completely avoided if instead the CPT is used as a criterion of the
pitting resistance.
A very marked increase in pitting resistance was found for the 17-11-2
sheet after bright annealing. By electron microprobe analysis an increased
nitrogen content was found in the surface layer of the annealed sheet,
Fig 4. No evidence of nitride particles in the surface layer was found for
 575

0,6MNaCl * Ο,ΙΜ KQHC03

♦1000

;*«o β l7Cr
* 17Cr 1Mo
]ä*S00 O J7Cr 3M*
c •22Cr
*2ZCr Wo
c • 2 2Cr 3Mo
*
.§♦200

* 0

V °,2 0,3 0/
Weight *& Nitrogen

fig 3 Breakdown potential of 20Ni 4 Mn alloys with various

Cr and Mo levels as a function of N-content (12).

this material, Fig 5. The nitrogen must therefore be assumed to be in solid

solution. From this results appears that an improvement of the pitting
resistance of a stainless surface by nitrogen pick up during heat treatment
in a nitrogen containing atmosphere is quite possible. A probable requisite
is that most of the added nitrogen remains in solid solution.

Wt % N

0 10 20 30 40 50
distance from surface μιη

Fig 4 Nitrogen content as a function of distance from the

rolled surface. Bright annealed 17-11-2.
576

Fig 5 SEM micrograph of bright annealed surface. Etched in

"aqua regia"

REFERENCES
1. D.E. Williams, C. Westcott, M. Fleischmann.
J. Electrochem. Soc. 132;8 (1985) pp 1796 - 1804
2. D.E. Williams, C. Westcott, M. Fleischmann.
J. Electrochem. Soc. 132:8 (1985) pp 1804 - 1811
3. R.J. Brigham, E.W. Tozer.
Corrosion 29:1 (1973) pp 33 - 36.
4. P. Le Guevel, N. Jallerat, K. Vu Quang
Proc. Pacific Corrosion -87, Melbourne, Nov. 22-28 1987.
5. R. Qvarfort, E. Alfonsson
Proc. 11th Scandinavian Corrosion Congress, Paper No F-79,
Stavanger (1989).
6. R. Qvarfort
ACOM (Avesta Corrosion Management) No: 2-3 (1988) pp 2-5.
7. K. Ito, T. Yoshi.
Transactions ISIJ, Vol. 28, 1988
8. M.A. Streicher.
Journal of the Electrochemical Society 103:7 (1956) 375-390
9. G. Herbsleb.
Werkstoffe und Korrosion 33:6 (1982) 334-340
10. R.F.A. Jargelius, T. Wallin.
Proc. 10th Scandinavian Corrosion Congress, Stockholm (1986)
pp 161 - 164.
11. J.E. Truman, M.J. Coleman, K.R. Pirt.
Brittish Corrosion Journal 12:4 (1977) 236-238
12. R.F.A. Jargelius
Swedish Inst, for Metal Research, Report IM-1867, (1983).
WS8a4

CORROSION RESISTANCE OF AMORPHOUS Fe-Cr-X ALLOY FILMS

BY ELECTRODEPOSITION
Y.Aoyagi and M.Kowaka
Central Research Laboratory, C.Uyemura Co.fc Ltd.
1-5-1 Deguchi, Hirakata, Osaka, Japan.

ABSTRACT

Amorphous Fe-Cr-X alloy films were prepared by electrodeposition and their

corrosion properties were investigated by electrochemical measurements and
immersion test in 0.IN acidic solutions at room temperature. The results
showed that the corrosion resistance was much more improved by codeposition
of Cr with Fe-X alloys.

KEYWORDS

Amorphous, Fe-X alloy film, corrosion, electrodeposition, H 2 S0 4 ,HC1.

INTRODUCTION

It has long been desired to prepare the stainless steel films by electrodepo-
sition, because of its excellent corrosion resistance, though it is not yet
successful. Here,the corrosion resistant electrodeposited Fe-Cr-X Alloy films
have been studied. Cr is the corrosion resistant element and much interest
has been centered on the effects of other alloying elements,X,such as P and
Mo. In particular,the effects of phosphorus and molybdenum,with and without
Cr, on the promotion of the stability of passive film have been investigated.
The results of these experiments showed that the corrosion resistance was
much improved by codeposition of Cr. Electrodeposited metal-metalloid amorph-
ous alloy films cannot show the excellent corrosion resistance,and much
improvement of corrosion resistance are expected by codeposition of Cr in
Fe-X alloys,i.e., X is phosphrous and / or molybdenum.

EXPERIMENTAL
Electrodeposition:

The amorphous alloys were prepared by electrodeposition in the solutions show-

en in Table I and the deposition conditions were also indicated in the same
Table. The composition of the alloy films was determined by the x-ray Fluore-
scent method and ICP emission spectrometry. The film structures were measur-
ed by x-ray diffraction method of Cu-ka radiation.

577
578

Table 1. Composition(g/1) of Electrolytes and Electrodeposition Conditions

Fe-Cr Fe-P Fe-Cr-P Fe-Cr-Mo
FeCl2-4H20 10/35 120 10/35 5/30 (g/l)
FeS0 4 -7H 2 0 50
CrCl 3 -6H 2 0 100/160 160 160
NaMo04-2H20 — 50
(NH 4 ) 2 S0 4 25
NH2CH2C00H 150 150 150
NaH 2 P0 2 H 2 0 1/30 5/10 -
NH4CI 100 100 100
H3BO3 37.2 37.2- -
Bath temperature 30 55 30 30 ( ~C)
pH 1.8/3.8 0.8/1.4 1.0/3.0 0.5/2.5
Current Density 5/30 10/60 10/40 10/50 (A/dm2)

Electrochemical measurement:

Anodic polarization measurements were performed in the solutions of 0.1NH 2 S0 4

and HC1 at 30 °C. And the sweep rate was 1 mV/s. Measurements of polarizat-
ion were made using potentiostat interfaced with a microcomputer.

Corrosion resistance:

The electrodeposited alloy samples were covered by resin to prevent the effect
of Cu substrate. And the samples were kept in the solu- tions for proper time
and the corrosion losses were measured.

Analysis of the surface:

The electrodeposited alloy films were polarized and films formed were analysed
by AES or ESCA measurement.

RESULTS

Fe-Cr Alloy:

Amorphous Fe-Cr alloys were prepared by the solution showen in Table I.

And the amorphous structure was obtained by the deposition condition indicated
in Fig.l. The amorphous structures were observed on electrodeposited Fe-Cr
alloy films contained above 30wt% of Cr depending upon the current density.
 579
FeCIHHiO CrCl,-6H,0
(1) 10g/L 160 g/L ! ; 30 "C. 0. IN H,S0«
I (2) 15 160
70 j .
Γ (3) 35 200
1 I (4) 35 100 \ ios L
60
I 3 f 1

. 50Γ · · —
f
40

30
Amorphous 1
CO
c k A+~^_jy
/■■?"'
'λ
Ί
20 / / Crystalline

rs ., ,3 ,I
ω
10 L A/
LL
0 i l l
-1.0 - 0.5 0.0 +0.5
0 10 20 30 40 50 60
2
Current density / A/dm Potential / mV vs. Ag/AgCl

Fig. 1 Effect of current density Fig.2 Anodic polarization curves

on the content of Cr in of Fe-Cr alloys in 0.IN H 2 S0<
deposit at 30 °C , sweep rate = 1 mV/s.

Figure 2 shows the anodic polarization curves of several electrodeposited Fe-

Cr alloys in the solution of 0.IN H 2 S0 4 at 30 °C. Nos.i,2,---5,and 6 in Fig. 2
are 48.1 , 44.7, 42.6, 38.4, 32.9, and 24.1 wt% of Cr in deposits,respectively.
The amorphous structure was 1,2,3 and 4, and crystalline structure was 5 and
6. Amorphous alloy films are passivated in the acidic solutions. And crystal-
line structure was actively dissolved.

Fe-P Alloy:

Electrodeposited Fe-P alloy films were prepared by the solution shown in Table
I. The crystalline structure of the film was detected by the x-ray diffraction
patterns of several Fe-P alloys obtained by electrodeposition. The amorphous
structure was defined above 7.68wt% P. Figure 3 shows the relation between
the crystallite size and P content in deposit. The result shows that the gra-
in size decreases with increaseing in P content. Figure 4 shows the anodic
curves of amorphous Fe-P alloys in 0.1N HCl at 30°C. The increase in content
of phosphorus results in the decrease of passive current density in the solut-
580
10' m ; . .

i--^—. 736wiXP

■' Λ
10'

5 10 15 I
P content in deposit /wt% 14 12 10 8 6 4 2 0 -2 -4 x 100
Potential / mV vs. Ag/AgCl
Fig. 3 Relation between the crystallite Fig.4 Anodic curves of Fe-P
size and the content of P in Fe-P alloys in 0.IN HC1 at
30 e C, lmV/s.

Fe-Cr-P Alloy:

Electrodeposited Fe-Cr-P alloy films were obtained by the solution shown in

Table I. Figure 5 shows the anodic curves of amorphous Fe-Cr-P alloy films in
0.1 N H2SO4 solution at 25°C. The excellent effect of phosphorus on electro-
chemical properties was accelerated by codeposition of Cr. Figure 6 shows the
relation between the pitting potential and Cr content in deposit.The pitting
potential becomes noble by codeposition of phosphorus in Fe-Cr alloy.

Figure 7 shows the immersion test results in the solution of 0.1 N H2SO4 at 25
°C and the corrosion rate of Fe-Cr-P alloy films was less than that of Fe-
Cr alloy. The effect of P on corrosion resistance of Fe-X alloys becomes
clear.

Fe-Cr-Mo Alloy:

Figure 8 shows the anodic polarization curves of Fe-Cr-Mo alloy films.

Fe-28Cr-l.5Mo alloy has crystalline structure and others have all amorphous
ones. Electrodeposited Fe-Mo alloy film did not show the excellent corrosion
resistance (Yao and Kowaka,1988),but, the codeposited film with Cr shows good
corrosion resistance as depicted in this Figure. The increase in Cr content
results in a decrease of passive current density. The excellent corrosion resi-
stance can be expected for the electrodeposited Fe-Cr-Mo alloys. The change
 581

ιο3
0.1 N H2SO<f 25*C
o 600
o

r
l v-27Cr-4P

102 / x
/ : * i
i ~J / / / '
' {raj 36Cr-3.5P'' / /

/ /' r-45Cr-3.7P/ ,
// /
i
\lz.-i' Λ47Cr-4P
1 30 40 50
10' _i_ JL
-0.5 0.0 0.5 1.0 1.5 Cr content in deposit / wt%
P o t e n t i a l . / V vs.Ag/AgCl
Fig.6 Relation between potential and
Fig. 5 Anodic curves of Fe-Cr-P a l l o y s the content of Cr in deposit
in 0.IN H2SO4 a t 25 °C.

in anodic current density of Fe-Cr-Mo alloy films at 700mV in Fig.8 decreases

with increasing of Cr+Mo content in the deposit.

CONCLUSIONS

1) Amorphous structure of Fe-Cr-X alloy films were obtained by codeposition

of phosphous and /or molybdenumum and corrosion resistance was improved.
2) Addition of phosphrous and /or molybdenum to the electrodeposited Fe-Cr
alloys resulted in the increase of pitting potential.

REFERENCES

S.Yao and M. Kowaka(1988) . Investigation of the electrodeposition condition of

amorphous Fe-Mo alloy films and their corrosion behavior. J. of Surface Finishing
Soc. of Japan,39, 736 .
582

80
0.1 N H,S0, , 25 *C ,Ι" ,ϊ"Τ"Τ"ϊ"Ί""Γ"ΐ"Τ"Ί"Ί ,,,Τ"ΐ"ϊ ,"Γ" ,Γ1

f 70 0. IN H , S 0 « . 3 0 *C 1

^ Fe-Cr
60h-
Γ o
50 l··^ o
^ - R
*'
• >.
a 40 L Fe-Cr-P"o^^-^ 1-

30 ^ / * ·
o
p 20 hh

o 10
Λ O

1 j 1 1 1 1
30 35 40 45 50
Cr content in deposit / wt%
I—t.—1—t—t—f—f-..-f.i„t—1—t—■—■■■ -U-B-—t-—i—l—.
Fig.7 Effect of the content of Cr
in deposit on corrosion rate Potential / mV vs.Ag/AgCl

Fig.8 Anodic curves of Fe-Cr-Mo alloys

in 0. IN H 2 S0 4 at 30°C.
 WS8a5

CORROSION-INHIBITING PROPERTY OF POLYMER-MODIFIED

MORTARS WITH RUST-INHIBITORS

Y. OHAMA*, K. DEMURA*, M. MIYAKE*, T. ONO*

and H. IBE

Department of Architecture, College of Engineering,

Nihon University, Koriyama, Fukushima-ken, 963 Japan
Onoda Corporation, Tokyo, 110 Japan

ABSTRACT

The present paper deals with a basic investigation of the corrosion-

inhibiting property of polymer-modified mortars with rust-inhibitors as
repair mortars for reinforced concrete structures. Calcium nitrite and
lithium nitrite are employed as rust-inhibitors. Polymer-modified mortars
using styrene-butadiene rubber latex, ethylene-vinyl acetate and polyacrylic
ester emulsions are prepared with variation of polymer-cement ratio and
rust-inhibitor content as repair mortars. Two types of specimens in which
a rebar is embedded in each repair mortar or each half portion in the
longitudinal direction of the rebar is covered with each repair mortar and
cement mortar, are molded. The specimens are cured, pretreated by exposures
to CO2 gas pressurization for carbonation and 2.5%-NaCl-solution
impregnation, and heated in polyethylene bags at 80°C for 24 hours for
accelerated corrosion. After that, the rebars are taken from the specimens,
and their corroded area is measured. In conclusion, the corrosion-
inhibiting property of the polymer-modified mortars with low polymer-cement
ratio is considerably improved by the addition of the rust-inhibitors
without increasing polymer-cement ratio. However, much corrosion in the
cement mortar covered portions of the rebars is recognized when the each
half portion in longitudinal direction of each rebar is covered with each
repair mortar and the cement mortar.

KEYWORDS

Corrosion-inhibiting property; polymer-modified mortars; repair mortars;

rust-inhibitor; rebars; corrosion rate

INTRODUCTION

Polymer-modified mortars have been recently used as repair materials for

reinforced concrete structures because of their superior inhibiting
properties for carbonation and chloride ion penetration (Ohama et_al.,
1988). In addition, rust-inhibitors are added to concrete to inhibit the
corrosion of rebars (Lundquist et al., 1979)· In some cases, the rust-
583
584
inhibitors are also added to the polymer-modified mortars as repair
materials· However, the effectiveness of the polymer-modified mortars with
the rust-inhibitors in the repairing works for the reinforced concrete
structures has hardly been reported in detail till now. The present paper
deals with a basic investigation of the corrosion-inhibiting property of the
polymer-modified mortars with the typical rust-inhibitors as repair mortars.

In the present paper, polymer-modified mortars with variation of polymer-

cement ratio and rust-inhibitor content are prepared as repair mortars, and
two types of specimens in which a rebar is embedded in each repair mortar or
each half portion in the longitudinal direction of the rebar is covered with
each repair mortar and cement mortar, are molded. The specimens are tested
for corrosion-inhibiting property under accelerated corrosion conditions.
After that, the corroded area of the rebars taken from the specimens is
measured to discuss the corrosion-inhibiting property of the polymer-
modified mortars with the rust-inhibitors.

MATERIALS

Materials for Cement Mortar and Polymer-Modified Mortars

Ordinary portland cement and Toyoura standard sand were used for preparing
cement mortar and polymer-modified mortars. Three types of commercial cement
modifiers, i.e., a styrene-butadiene rubber (SBR) latex, ethylene-vinyl
acetate (EVA) and polyacrylic ester (PAE) emulsions were used for preparing
polymer-modified mortars. Basic properties of the cement modifiers are
listed in Table 1. Before mixing, silicone-emulsion-type antifoamer was
added to the cement modifiers in a ratio of 0.7% of the silicone solids of
the antifoamer to the total solids of the cement modifiers.

Table 1. Properties of polymer dispersions as cement modifiers.

Type of polymer Specific pH Viscosi ty Total

dispersion gravity (20°C) (20°C,cP) solids
(20°C)
(%)
SBR 1.022 9. 7 64 45.0
EVA 1.056 5. 7 1588 44.4
PAE 1.074 9. 9 80 44. 9

Rebars

Rebars 010x130mm having the quality specified in J I S A 6205 (Corrosion

Inhibitor for Reinforcing Steel in Concrete) were used.

Rust-Inhibitor
The rust-inhibitors employed were as follows:
(1) Calcium nitrite solution having a solid content of 35%.
(2) Lithium nitrite solution having a solid content of 25%.

TESTING PROCEDURES

Preparation of Base Specimens

According to JIS R 5201 (Physical Testing Methods for Cement), cement mortar
was mixed with a weight ratio of ordinary portland cement: Toyoura standard
 585
sand 1:2 and a water-cement ratio of 65%· As shown in Fig.1, the half
portions in longitudinal directions of rebars were covered with the cement
mortar to prepare base specimens for Type-B specimen. The base specimens
were subjected to a 7-day moist(20°C, 80%R.H.)plus 7-day dry(20°C,50%R.H.)
cure. The corrosion of the open surfaces of the rebars was not recognized
after the curing of the base specimens.
Rebar Repair mortar Spacer Rebar
\i 13
° Mold

15 MJ 5
160 sill
Repair mortar Cement mortar
13
\, ° ,/ Mold Rebar
Type-B ΏΒΡΤTT\— 'II

Ppg^i ' 11
specimen
1 80 1 80 40
160 1

Fig.l. Geometry of specimens.

Preparation of Specimens

In accordance with JIS A 1171 (Method of Making Test Sample of Polymer-

Modified Mortar in the Laboratory), SBR-, EVA-, and PAE-modified mortars as
repair mortars were mixed with the following mix proportions;ordinary
Portland cement:Toyoura standard sand = 1:3 (by weight), polymer-cement
ratio (P/C) of 0, 5, 10 and 20%, rust-inhibitor contents of 0, 0.3, 0.5,
1.0 and 2.0% of cement (by weight). The flow was adjusted to be constant at
170±5. After mixing, two types of specimens 4-0x4-0x160mm molded with
rebars of 010x130mm were prepared as follows:

(a)Type-A specimen : A rebar is embedded in a repair mortar in the specimen,

(b)Type-B specimen : Each half portion in longitudinal direction of a rebar
is covered with a cement mortar and a repair mortar in
the specimen.

The geometry of the specimens is shown in Fig.1. After molding, the

specimens were subjected to a 2-day moist (20°C, 80% R.H.) plus 5-day dry
(20°C, 50% R.H.) cure.

Accelerated Corrosion Tests

The cured Type-A and Type-B specimens were tested for accelerated corrosion
for the rebars embedded in the specimens. For carbonation, the specimens
were placed in sealed vessel, evacuated to ImmHg or less at ambient
temperature for 1 hour, and then exposed to pressurized COo gas under
a pressure of 10kgf/cm for 24. hours. The carbonated specimens were dried
at 30°C for 168 hours, evacuated to ImmHg or less for 1 hour, and then
impregnated with 2.5% NaCl solution under a pressure of 10kgf/cm for 24-
hours in the vessel for chloride ion penetration. After impregnation, the
heating of the specimens wrapped with polyethylene bags was performed at
80°C for 24. hours.

Measurement of Corroded Area of Rebars

After accelerated corrosion test, the specimens were split, and the embedded
586
rebars were taken from two types of specimens· The rebars were slightly
brushed in 10% (NH,^HC^HcCU solution for 1 minute, and cleaned by
acetone. The corroded area of the rebars was traced on tracing papers, and
then measured by using a planimeter in accordance with JIS A 6205. The range
of the corroded area measurement for the rebars in Type-A specimens was
the portion of totalized 90mm of both sides 4-5mm lengthwise from the
center of the rebars. For the rebars in Type-B specimens, the total corroded
area in each portion covered with a cement mortar or a repair mortar was
measured. The corrosion rate of the rebars embedded in two types of
specimens was calculated as follows:

Corroded area (mm2)

Corrosion rate (%) = x100
Corrosible area (mm )

where the corroded area is the total corroded area of the rebars covered
with the cement mortar or repair mortars, and the corrosible area of
rebars in Type-A specimens is the surface area of the portion of
totalized 90mm of both sides 4.5mm lengthwise from the center of the rebars,
and the corrosible area of rebars in Type-B specimens is the surface area of
the rebars covered with these mortars. The corrosion rates of rebars in
three specimens for each test condition were averaged.

TEST RESULTS AND DISCUSSION

Figs.2 and 3 show the corrosion rate of rebars embedded in Type-A specimens
vs. the calcium nitrite and lithium nitrite contents of polymer-modified
mortars with polymer-cement ratios of 0 and 10% as repair mortars. The
corrosion rate of the rebars embedded in unmodified mortar without rust-
inhibitors is about 35%. The corrosion rate of the rebars embedded in the
polymer-modified mortars without the rust-inhibitors is one half or one
third of that in the unmodified mortar. The corrosion-inhibiting properties
of tjie unmodified and polymer-modified mortars as the repair mortars are
considerably improved by the addition of calcium nitrite and lithium nitrite
as the rust-inhibitors. With an increase in the rust-inhibitor content, the
corrosion rate of the rebars embedded in the repair mortars is decreased,

40

£ 30

t 10
o

o1- 0 0.5 1.01.52.0 0 0.5 1.01.5 2.0 0 0.5 1.0 1.52.0 0 0.5 1.0 l."5"2To
Calcium nitrite content (wt% of cement)

Unmodified SBR-10* EVA-10 PAE-10

Type of repair mortar
Fig.2. Corrosion rate of rebars embedded in Type-A specimens
vs. calcium nitrite content of polymer-modified
mortars with polymer-cement ratios of 0 and 10 % as
repair mortars.
Note, *:Polymer-cement ratio (%)
 587
40 l·

30

20

V^o
10

0 0.5 1.0 1.5 2.0 0 0.5 1.0 1.5 2.0 0 0.51.01.52.0 0 0.5 1.01.52.0
Lithium nitrite content (wt% of cement)

Unmodified SBR-10* EVA-10 PAE-10

Type of repair mortar
F i g . 3 . Corrosion rate of rebars embedded in Type-A specimens
vs. lithium nitrite content of polymer-modified
mortars with polymer-cement ratios of 0 and 10 % as
repair mortars.
Note, *:Polymer-cement ratio (%)

and becomes lesser than 5% at a rust-inhibitor content of 0.5% or more

regardless of the polymer and rust-inhibitor types. A difference in
corrosion inhibiting property between the calcium nitrite and lithium
nitrite as the rust-inhibitors is hardly recognized.

Fig.4. represents the corrosion rate of the rebars embedded in Type-A

specimens vs. the polymer-cement ratio of polymer-modified mortars with or
without calcium nitrite as repair mortars. The corrosion rate of the
rebars embedded in the repair mortars without the calcium nitrite is
reduced with increasing polymer-cement ratio regardless of the polymer
type. The corrosion rates of the rebars embedded in the repair mortars
without the calcium nitrite are 5 to 10% at a polymer-cement ratio of 20%.
However, the corrosion rate of the rebars embedded in the repair mortars
with a calcium nitrite content of 0.5% is 5% or less irrespective of the
polymer type and polymer-cement ratio. It is evident from the test results
that the corrosion-inhibiting property of the polymer-modified mortars with
low polymer-cement ratio as the repair mortars is remarkably improved by the
addition of the calcium nitrite without increasing polymer-cement ratio.

— 401-

30

20 h

10

o1- 10 15 20 10 15 20 10 15 20
Polymer-cement ratio (%)

SBR EVA PAE

Type of repair mortar
Fig.4. Corrosion rate of rebars embedded in Type-A specimens
vs. polymer-cement ratio of polymer-modified mortars
with or without calcium nitrite as repair mortars.
588
Fig.5 illustrates the corrosion rate of the rebars embedded in Type-B
specimens using polymer-modified mortars with polymer-cement ratio of 0 and
10% and calcium nitrite contents of 0 to 2.0% as repair mortars. In the
case of Type-B specimens, the corrosion rate of the cement mortar covered
portions of the rebars is much larger than that of the repair mortar covered
portions of the rebars regardless of the polymer type. The corrosion rate of
the cement mortar covered portions of the rebars is increased with an
increase in the calcium nitrite content of the repair mortars, nevertheless
the corroded area in the repair mortar containing calcium nitrite is hardly
recognized. In the repairing works for reinforced concrete structures, the
consideration for the corrosion of rebars in the portions behind repaired
portions may be important.

40
□ Cement mortar covered portion (C)
HRepair mortar covered portion (R)
+? 30

20

10

M M. Ell P I El
CR CR C R C R CR CR CR CR CR C R C R CR CR CR CR CR
^TT* θΤ? "irö* 12Τθ UÖ""J 0 5 * *ΪΤθ 2.0 V 0.5 1.0 2.0 0 0.5 1.0 2.0
C a l c i u m n i t r i t e c o n t e n t (wt% o f c e m e n t )
Unmodified SBR-10 EVA-10 PAE-10
Type o f r e p a i r mortar

Fig.5. Corrosion rate of rebars embedded in Type-B specimens

using polymer-modified mortars with polymer-cement
ratios of 0 and 10 % and calcium nitrite contents of
0 to 2.0 % as repair mortars.
Note, *:Polymer-cement ratio {%)

CONCLUSIONS

(1) The corrosion-inhibiting property of polymer-modified mortars as

repair mortars for reinforced concrete structures is improved with raising
polymer-cement ratio and the addition of rust-inhibitors such as calcium
nitrite and lithium nitrite.
(2) The corrosion-inhibiting property of polymer-modified mortars with low
polymer-cement ratio is remarkably improved by the addition of rust-
inhibitors without increasing polymer-cement ratio.
(3) In the case of Type-B specimens, the corrosion rate of the cement mortar
covered portions of the rebars is much larger than that of the repair
mortar covered portions regardless of rust-inhibitor addition.

REFERENCES

Ohama, Y., K. Demura, T. Ogi and S.N. Pareek (1988). Corrosion-Inhibiting

Property of Polymer-Modified Mortars. Proceedings of the MRS International
Meeting on Advanced Materials, 13« 99-104-.
Lundquist, J.T., A.M. Rosenberg and J.M. Gaidis (1979). Calcium Nitrite
as an Inhibitor of Rebar Corrosion in Chloride Containing Concrete.
Materials Performance, 18, 36-40.
WS8b1

EFFECT OF CU ON THE CORROSION BEHAVIOR

OF 18-8 STAINLESS STEEL
Hann-Tuw Lin, Wen-Ta Tsai, Ju-Tung Lee
and Chi-Shang Huang*
Dept. of Materials Engineering
National Cheng Kung University
Tainan, Taiwan, R.O.C.
* Tang Eng Stainless Steel Plant
Tang Eng Iron Works Co., LTD.
Kaoshiung, Taiwan, R.O.C.

ABSTRACT
The influence of Cu addition (0.41 ^ 3.09 wt%) on the
electrochemical and corrosion behavior of 18-8 austenitic
stainless steel was investigated. Potentiodynamic
polarization and potential decay measurements were conducted
in 0.1 M H2SO4 solution. The effect of dissolved oxygen in
the acidic solution was also evaluated. Surface
characterization was examined by Auger electron spectroscopy
(AES) and X-ray photoelectron spectroscopy (XPS). Corrosion
rates of the Cu containing austenitic stainless steels were
determined in various solutions. The role of Cu on the
corrosion behavior of the austenitic stainless steel observed
in this investigation is presented.

KEYWORDS
Copper, austenitic stainless steel, corrosion, polarization,
potential decay, corrosion rate.

INTRODUCTION
The addition of Cu could cause an increase in the stacking
fault energy and subsequently improve the deep drawing
quality of the austenitic stainless steel (Shimizu et__al.,
1970, Kao et al., 1990). The optimum addition of Cu to
increase the deep drawing quality of the austenitic stainless
steel is about 2^3 wt% (Shimizu et al. , 1970). However,
whether this addition of Cu to the stainless steel would
affect its corrosion resistance is of great interest.

Only a few research has been found in the literature

concerning the effect of Cu on the corrosion resistance of
stainless steels. In ferritic stainless steel, the presence

589
590

Table 1 Chemical Composition of the Steels Used (wt%)

C Si Mn P S Co Mo Al Cr Ni Cu Fe

A 0.048 0.41 1.45 0.030 0.008 0.17 0.07 0.003 18.17 8.19 0.41 bal.

B 0.020 0.17 1.05 0.030 0.001 0.17 0.22 0.002 16.51 6.96 2.00 bal.

c 0.022 1.34 1.65 0.030 0.001 0.19 0.20 0.002 17.18 7.43 2.62 bal.

D 0.026 1.15 1.15 0.030 0.002 0.17 0.21 0.002 17.11 7.55 3.09 bal.

E 0.044 0.44 1.42 0.030 0.001 0.17 0.07 0.003 18.03 8.01 0.34 bal.

F 0.036 1.23 1.84 0.030 0.001 0.17 0.16 - 16.65 6.82 2.08 bal.

G 0.021 1.29 2.04 0.030 0.001 0.17 0.17 0.003 16.40 6.92 2.58 bal.

of 0.4 wt% Cu could lower its anodic dissolution rate in

sulfuric acid (Seo et al., 1986). The addition of 0.1 ^ 1.0
wt% of Cu to austenitic stainless steel could also cause a
decrease of its corrosion rate in 5N H 2 S0 4 /NaCl solutions
(Ogura et al., 1976). The addition of Cu (3.5 wt%) to 20Cr-
33Ni-2.5Mo greatly enhance the alloy's resistance to sulfuric
and phosphoric acid environments (Streicher, 1985). However,
on the other hand, the detrimental effect of Cu on the
passivation (Seo et al., 1986) and localized corrosion (Seo
et al., 1986, Ogura et al., 1976, Streicher, 1985), such as
pitting corrosion, crevice corrosion, or intergranular
corrosion, etc., resistance was also reported.

Since the commercialized Cu containing austenitic stainless

steel derived from 18-8 grade contains approximately 2^3 wt%
Cu. And from the corrosion point of view, the role of Cu in
stainless steel is not quite clear. Further evaluation of the
corrosion behavior of Cu containing stainless steel is
needed. Therefore, in this study, the influence of Cu
(0.41^3.09 wt%) on the corrosion and electrochemical behavior
of the austenitic stainless steel is investigated.

EXPERIMENTAL PROCEDURES

Specimen Preparation

The materials used in this study are listed in Table 1. The

Cu content of the austenitic stainless steel ranges from 0.41
to 3.09 wt%. Alloy A was hot rolled to 5.5 mm thick. Alloys
E,F and G were cold rolled to 2.5 mm thick, while alloys B,C
and D were further cold rolled to 0.5 mm thick.

Electrochemical Measurement

Potentiodynamic polarization tests and potential decay

measurements were conducted in 0.1 M H 2 S0 4 solution either
deaerated with nitrogen gas or purged with air. A saturated
calomel electrode (SCE) was used as the reference electrode.
 591
1200 100Q

800 K ui 680 — —
o //' 0.41wtZ Cu
5 400 Η > % 360 V &62wt3i Cu
ε ({ 3.09w*% Cu
ö \ 0.1M HtSD4
u ö 40 - \ aerated
c +>
ω
■p
o -400 K c
ω 280 "" "********·**+ :—■■ -~

~ TBW^ a
UL +► -
-800^ o
α -600
10 10' a 10"
Current Density < JIA/cm Current Density <//A/cm >
Fig. 1 Potentiodynamic Fig. 2 Potentiodynamic
P o l a r i z a t i o n Curves P o l a r i z a t i o n Curves
of Cu Containing of Cu Containing
S t a i n l e s s Steels i n S t a i n l e s s Steels i n
Deaerated 0.1 M Aerated 0.1 M H2SOlt
Η 2 3(\ Solution. Solution.
The p o t e n t i o d y n a m i c p o l a r i z a t i o n c u r v e of e a c h s p e c i m e n was
m e a s u r e d from - 6 0 0 mV a t a p o t e n t i a l s c a n r a t e of 1
mV/sec t o w a r d s t h e anodic direction after cathodic
treated at - 1 5 0 0 mV f o r 10 m i n . In p o t e n t i a l decay
measurement, e a c h s p e c i m e n was f i r s t c a t h o d i c a l l y polarized
at - 1 5 0 0 mV for 10 min and t h e n p a s s i v a t e d a t 400 mV
for 2 h b e f o r e m o n i t o r i n g t h e c h a n g e of t h e open circuit
p o t e n t i a l (OCP). Some of t h e s p e c i m e n s , a f t e r p o t e n t i a l d e c a y
measurement, w e r e e x a m i n e d by Auger e l e c t r o n spectroscopy
(AES) and X - r a y p h o t o e l e c t r o n s p e c t r o s c o p y (XPS). A comined
AES/XPS s y s t e m made by V.G. S c i e n t i f i c was u s e d . Surface
composition depth p r o f i l e s were performed by Ar ion
sputtering and Auger a n a l y z e r . XPS w i t h magnesium r a d i a t i o n
was u s e d f o r s u r f a c e c h e m i c a l s t a t e a n a l y s i s .

Weight L o s s M e a s u r e m e n t

Weight l o s s e s w e r e m e a s u r e d f o r a l l o y s E, F , and G i n
d i f f e r e n t s o l u t i o n s with v a r i o u s immersion t i m e . The t e s t i n g
s o l u t i o n s w e r e 10% F e C l 3 , 10% HC1, 65% HNCL 10% H 2 S0 4 , 5%
HN03 + 5% H 2 SC\ + 4% N a C l , 50% H2SC\ + 42g/l Fe 2 (S(\ ) 3 , and
23% H 2 S0 4 + 1 . 2 % HCl + 1% FeCl 3 + 1% - - CuCl
-■ - All solutions
were h e a t e d t o b o i l i n g t e m p e r a t u r e .

RESULTS AND DISCUSSION

Figs. 1 and 2 show the potentiodynamic polarization curves of

alloys A, B, C and D in 0.1 M H 2 S0 4 solutions, deaerated and
aerated, repsectively, In the absence of dissolved oxygen,
the passive current density increased with increasing amount
of Cu in the stainless steel (Fig. 1 ) , indicating the
detrimental effect of Cu on the stability of surface film.
But in aerated solution, on the other hand, the passive
current density remained almost the same for the four alloys
tested (Fig.2). More importantly, the presence of dissolved
592
OL>U ■Ί

400
jfc * 0.41 %Cu
1 ^ ^ o 2.00%Cu
300
^Ρ§ΓΧ o 2.62%Cu
200 - ' \ \ « 3.09%Cu
ÜJ
O 100 Passivation 2 hrs
CO in 0.1 M H 2 S0 4 sol.
w
>
0 -
E -100
LÜ
-200
0 100 200 300 400 500 600 700 800
-300
...s S p u t t e r i n g Tine ( s e c )
-400
II 1 1 1 1 1 II 1 1 1 1 1 II 1
2 4 6 8 10 12 14 16 18
Time (min)
Fig. 3 Effect of Cu on the Fig. 4 AES Depth Profile
Potential Decay of of Specimen D after
18-8 Stainless Being Treated at
Steel in Deaerated 400 mV/2h + 0CP/16h
0.1 M H2S04 in Areated 0.1 M
Solution. H^SOu Solution.

oxygen caused a significant Change in the anodic peak Current

density which decreased with an increasing of Cu Content from
0.41 wt% to 3.09 wt%. Moreover, the measured Corrosion
potential also increased as the Cu Content increased. The
different role of Cu, observed in this study, on the
passivation of stainless steel in deaerated and aerated
sulfuric acid solution is probably due to the affinity of Cu
to oxygen. It is speculated that Cu may assist the adsorption
of oxygen and Consequently enhances the passivation ability
of stainless steel in aerated sulfuric acid solution.

Fig. 3 shows the potential decay curve of the stainless

steels with various Cu Content, in deaerated 0.1 M H SO
solution. After the potentiostat being turned off, the open
Circuit potentials gradually decreased from 400 mV to about
250 mV. They were then dropped sharply and remained at stead/
values of -380 mV for alloy A and of -320 mV for alloys B, C
and D. The time required to reach this steady potential is
defined as the reactivation time ( γ ) for the passivated
stainless steel. Clearly, γ was decreased as the Cu content
was increased, indicating that the passive film formed on the
high Cu containing stainless steel was less stable than that
rromed on the low Cu content steel in deaerated 0.1 M H SO
solution. In aerated solution, however, the reactivation time
γ was generally increased (except alloy B) with Cu Content.
The results imply that the addition of Cu to the stainless
steel could promote the passivation of stainless steel in air
saturated sulfuric acid. The results shown are in good
agreement with those shown in Figs. 1 and 2

Surface characterization was performed for the specimens

 593

Π 10*/. FeCts
(lllhrs)
• 10*/. HCl
<1.45hrs)
■ 10*/. H2SD<
<2.5hrs)
A 5'/· HND3 +
5V. H2 SÜ4 +
4'/. NaCl
<0.5hrs)
926 928 930 932 934 936 938 940 942 944 946 948 950
Binding Energy / e V Δ 507. H2SD<
4 2 g / L Fe 2 (SD4) 3
(98.5hrs)
Fig. 5 XPS Analysis of O 23*/. H 2 SD +
Specimen C after 1.2*/. HCI +
1% F e C l 3 +
Beina Treated at I'/. CuCU
400 mV/2h + OCP/16h i 2 3 <23.4hrs^
in Areated 0.1 M Cu <wt7.)
HgSOt, Solution.
Fig. 6 Effect of Cu on the
Weight Loss of 18-8
Stainless Steel in
Various Solutions.

subjected to 400 mV/2h or 400 mV/2h + OCP/16h treatment in

aerated 0.1 M H 2 SCU solution by AES and XPS. Surface
enrichment of Cu, as revealed by the AES depth profile, was
only observed for the specimens treated at 400 mV/2h +
OCP/16h. Fig. 4 is an example showing the surface
composition profile of alloy D. XPS analysis did not reveal
the presence of Cu on the specimen surfaces if they were
subjected to passivation at 400 mV/2h in 0.1 M H SO .
However, for the specimens holding at OCP for 16 h after
being passivated at 400 mV/2h, the XPS spectrum did show the
existence of Copper 2p3/2 line, indicating the presence of Cu
on these specimen surfaces. Fig. 6 illustrates the XPS result
of alloy C. But since the binding energies of Cu 2p3/2 for Cu
metal and for Cu 2 0 are so close U932.5 eV) (Mclntyre et al. .
1975) that it is not possible to distinguish them.

According to the potential-pH diagram for Cu-H 2 0 system

(Pourbaix, 1974) at 400 mV(SCE) Cu is dissolved as C u + 2 ion
in acidic solution. Therefore, the incorporation of Cu into
the surface film seems difficult. As a consequence, there was
no Cu found on the specimen surfaces for those stainless
steels passivated at 400 mV/2h. But if the potential is
lowered to -320 mV(SCE), the reduction of C u + 2 to Cu+ or Cu
metal in aerated 0.1 M Η 2 3(\ solution is possoble:

2 Cu+ 2 + 1/2 0 2 + 4 e~ = Cu 2 0 (1)

or C u + 2 + 2 e" = Cu (2)

The presence and enrichment of Cu on the surfaces of the

stainless steels subjected to 400 mv/2h + OCP/16h treatment
were thus observed. Similar results have been seen for the Cu
containing ferritic stainless steels (Seo et al., 1986).
594

The results obtained from weight loss measurements are shown

in Fig. 6. Although the immersion time differed from one
another, the results manifested that Cu improves the
corrosion resistance of the austenitic stainless steel. A
significant reduction in the weight loss due to the addition
of Cu was observed in boiling 10% HCl (1.45 h) or in boiling
23% Η 2 30^ + 1.2% HCl + 1% FeCl 3 + 1% CuCl 2 (23.4 h) solution.
But the calculated corrosion rates reveal that the Cu
containing stainless steels are most resistant to corrosion
in boiling 65% HN0 3 or 50% Η 2 8 0 4 + 42g/l Fe 2 (SO I+ ) 3 solution.

CONCLUSIONS
1. The passive Current density of the Cu Containing
austenitic stainless steels increased with increasing Cu
content, in the range of 0.4 ^ 3.0 wt%, in deaerated 0.1 M
H 2 S 0 4 solution.
2. In aerated 0.1 M Η 2 8 0 4 solution, an enhanced passivation
was found with the addition of Cu to the austenitic stainless
steel.
3. Surface enrichment of Cu on the steel surface was found
if the specimen was held at active potential in sulfuriC acid
solution.
4. A significant improvement in the corrosion resistance of
the austenitic stainless steel, due to the addition of Cu,
was observed in 10% HCl or 23% H 2 SO^ + 1 . 2 % HCl + 1% FeCl 3 +
1% CuCl solution.

ACKN OWLE DGEMENTS

The authors would like to acknowledge Tang Eng Stainless

Steel Plant and National science Council of the Republic of
China for the support of this work.

REFERENCES
Shimizu, T., I. Takahashi, and M. Ogaya, (1970) J. Jpn.
Inst. Metals, 34, p. 428.
Kao, P. W. and C. S. Huang, (1990) Chinese J. Materials
Science, 22, 112-122.
Seo, M., G. Hultquist, C. Leygraf, and N. Sato, (1986).
Corrosion Science, 26, 949-960.
Ogura, S., K. Sugimoto, and Y. Sawada, (1976). Corrosion
Science, 16, 323-337.
Streicher, M. A. (1985). Metal Progress, October, 29-42.
MClntyre, N. S. and M. G. Cook, (1975). Analytic Chemistry,
47, 2208-2213.
Pourbaix, M. (1974).In: Atlas of Electrochemical Equilibria
in Aqueous Solutions, NACE, pp. 384-392.
Adachi, T. and T. Yoshii, (1989). Corrosion/89, NACE, New
Orleans, Louisiana, Paper NO. 575.
WS8b2

EFFECT OF LASER SURFACE MELTING

ON THE CORROSION RESISTANCE OF STAINLESS STEEL

Kuo-Chin Tao, Ping-Ho Lo, Ju-Tung Lee,

and Wen-Ta Tsai

Department of Materials Engineering

National Cheng Rung university
Tainan, Taiwan, R.O.C.

ABSTRACT
The effect of laser-surface melting (LSM) on the corrosion
behavior of Type 304 stainless steel was investigated. A
continuous C0 2 laser at 40CK700 watts and at a scan rate of
4.5M5 mm/sec was used for surface treatment. Electrochemical
polarization measurements and various corrosion tests were
performed to evaluate the corrosion resistance of the LSM
treated 304 stainless steel. The results showed that LSM
treatment could improve the localized corrosion resistance of
the stainless steel.

KEYWORDS
Laser surface melting, stainless steel, electrochemical
behavior, pitting corrosion, crevice corrosion.

INTRODUCTION
The application of laser surface treatment to improve the
corrosion resistance of metals has been of great interest to
many researchers. Laser surface melting (LSM) of 304
stainless steel could cause an increase in the pitting
potential by at least 200 mV in 0.1 M NaCl solution
(McCafferty, 1985, McCafferty et al., 1986). LSM has also
been used to produce corrosion resistant ferritic and
austenitic stainless steel surfaces on mild steel (Chiba et.
al. , 1986). More recent report recognized the promising
application of LSM to prevent the intergranular stress
corrosion cracking (IGSCC) of sensitized stainless steel
(Stewart et al., 1990). Since stainless steels may be used in
a variety of corrosive environments, a wide range of
investigation on the effect of LSM on their corrosion
resistances is certainley needed.

595
596

Fig. 1 Transverse cross sections of 304 SS after LSM

treatment at 400 W and at a scan rate of (a).4.5, (b)
8.4, and (c) 15 mm/sec.

In this study, the electrochemical properties and localized

corrosion resistances of the LSM treated austenitic stainless
steel are presented.

EXPERIMENTAL PROCEDURES
Type 304 stainless steel with a composition (wt%) of 0.046 C,
18.10 Cr, 8.01 Ni, 0.28 Cu, 0.54 Si, 1.39 Mn, 0.026 P, and
0.002 S was used. Laser melting was performed with a
continuous wave C0 2 laser at 400^700 watts and at a scan
rate of 4.5, 8.4 and 15 mm/sec, respectively. Potentiodynamic
polarization curves of the laser processed samples were
conducted in 0.1 M Η 2 8(\ and 3.5 wt% NaCl solutions.
Immersion tests were performed in 6 wt% FeCl 3 , boiling 65%
HN0 3 , and 3.5 wt% NaCl + 1 N HCl solutions, respectively.

RESULTS AND DISCUSSION

Figure 1 shows the microstructures of the cross-sections of
laser treated specimens. The results manifest that the depth
of the melt pools is strongly affected by the power and the
scan rate of the laser beam applied. Fig. 2 shows that the
depth of the melting zone increases with increasing laser
power but it decreases with increasing scan rate. As the
 597

o - As-reaeved in 0.1 M Hi 5 0.
Loser Power 400W
N UJ 1000 . o S Rote 4.5mm/s

Γ
CD
C o • S Rote 8.4mm/s

{
+> g 500
Δ S. Rote 1 5 m m / s

%
£ o
~ 0
c
O <υ
_c o o o o\i (to "«u*

-p Q.-500
a
ω 1 1 1 l—Of
c
Q 1
10~2 10"' 10° 10' 10 2 10 3 104 io5
2
0 2 4 6 8 10 12 14 16 Current Density (uA/cm )
Fig. 3 Effect of laser scan
Laser Scan. Rate (nn/s) rate (at 400 W) on
the potentiodynamic
Fig. 2 Depth of melting polarization curves
zone as functions of 304 SS in 0.1 M
of laser power and H2S(\ solution.
scan rate.

laser beam scan rate exceeds 8.4 mm/sec, however, the depth
of the melting zone remains almost the same. Dentriric
structure was observed in the laser melted region. The
dendrite arm spacing was found ranging from 0.3 to 1 Aim,
implying that the cooling rate was about 10 ; 106 K/s
(Elmer et al. 1989). The resolidified microstructure
consists about 20% of ferrite phase in the austenitic matrix.
The volume fraction of the ferrite phase, as indicated by
others (Elmer et al., 1989), increases with increasing
cooling rate.
Figure 3 shows the potentiodynamic polarization curves of 304
stainless steel, with or without LSM treatment (400 W at
different scan rate), in 0.1 M H2SO,, solution. In both cases,
the feature of the polarization curves is almost the same,
all exhibiting a wide passive region ( -200^900 mV). The
results suggest that LSM would not affect the passivation
behavior of the 304 stainless steel in sulfuric acid
solution. Similar results were observed for the specimens LSM
treated at 520 and 700 W, respectively.

In 3.5 wt% NaCl solution, the cyclic potentiodynamic

polarization curves indicate that the pitting nucleation
potential (Enp) was shifted to the noble direction for the
LSM treated specimen Fig. 4 gives the example for the
specimen treated at 400 W and at different scan rate. A
maximum increase in Enp of 180 mV was found for the specimen
treated at 400 W and at a scan rate of 8.4 mm/sec. Despite
the change of Enp, the pitting protection potential (Epp) was
not affected by LSM. These results indicate that LSM could
inhibit pitting initiation of the stainless steel tested in
the Cl~ containing solution. Surface morphologies of the
specimens after being polarized in 3.5 wt% NaCl solution at
598

In 3.5 wt% NoO

- As-recieved
Loser Power 400W

_ o 5. Rote 4.5mrn / s

o 5. Rote 8.4mm/s

Δ S. Rote 15mnV s
> 0 ^

-
£ -400 μ 11
D A

1 1 1 i^hfci
"~~Ίσ 2 10" ~W W To2 To5 To4
Current Density ( u A / c m 2 )

Fig. 4 Effect of laser scan rate (at 400 W) on the cyclic

potentiodynamic polarization curves of 304 SS in 3.5
wt% NaCl solution.

Fig. 5 Surface morphology of 304 SS immersed in 3.5 wt% NaCl

at 50 mV(SCE) for 5 h, (a) as-received, and (b) LSM
treated.

50 mV(SCE), above Enp, for 5 h are given in Fig. 5. Careful

examination of the specimen surfaces reveals that the pit
density on the as received stainless steel was about 1180/cm
they were LSM treated. The beneficial effect on the pitting
corrosion of stainless steel is believed to be due to the
increasing surface homogeneity and the decreasing surface
inclusion (such as MnS) density caused by LSM treatment
(McCafferty et al.,1986). Once pits or defects are formed
on the specimen surfaces, however, their repassivation
abilities are the same regardless of LSM treatment.
LSM could also improve the crevice corrosion resistance.
Fig. 6 is an example showing the surface morphology of 304
stainless steel, with or without LSM, after being immersed in
6 wt% FeCl 3 solution for 6 h.

In boiling 65% HNO 3 solution, intergranular corrosion of the

sensitized 304 stainless steel was observed. However, no
 599

LSM As-received

Fig. 6 Effect of LSM on the

crevice corrosion of
304 SS in 6 wt% FeCl
Laser Power 400W solution, (a) LSM
treated, and (b) as-
S. Rate 4 . 5 m m / s received.

Fig. 7 Cross-section micrographs of 304 SS in boiling 65%

HNO solution for 72 h, (a) sensitized at 700 C/1 h,
(b) sensitized at 700 C/1 h + LSM at 700 W, 15
mm/sec.

localized corrosion was found on the sensitized steel if it

was treated by LSM (Fig. 7 ) .

Further evaluation of the corrosion resistance of the LSM

treated stainless steel was performed in 3.5 wt% NaCl + 1 N
HC1 solution. Fig. 8 compares the cross-section micrographs
of the stainless steel with or without LSM. Pitting corrosion
was clearly identified for the as-received stainless steel
(Fig. 8a). But in such acidic Cl~ containing solution,
severe attack was found in the region where overlap of LSM
occurred (Fig. 8b). In the overlap region, the dendrites were
grown perpendicularly to the specimen surface. Whether the
change in the solidified microstructure or the segregation of
alloying elements in the remelted area causes the variation
in the corrosion resistance of the LSM treated stainless
steel needs further investigation.
600

Fig. 8 Cross-sectionmicrographs of 304 SS in 3.5 wt% NaCl +

1 N HCL solution, (a) as-received, (b) LSM at 700 W,
15 mm/sec.

CONCLUSIONS
Laser surface melting treatment could improve the pitting and
crevice corrosion resistances of type 304 stainless steel.
But the overlap region between the two passes of laser beam
was found to be less resistant in 3.5 wt% NaCl + 1 N HCl
solution.

ACKNOWLEDGEMENTS
The authors greatly acknowledge the support of this work by
National Science Council (NSC-79-0405-E006-19) of the
Republic of China.

REFERENCES
McCafferty, E. (1985). Surface Modification by Laser or Ion
Beams. In: Critical Issues in Reducing the Corrosion of
Steels (H. Leidheiser, Jr., and S. Haruyama, E d . ) , NACE,
pp. 224-235.
McCafferty, E., P. G. Moore (1986). Corrosion Behavior of
Laser-Surface Melted and Laser-Surface Alloyed Steels. J.
Electrochem. Soc., 133, 1090-1096.
Chiba, S., T. Sato, A. Kawashima, K. Asami and K. Hashimoto
(1986). Some corrosion characteristics of stainless surface
alloys laser processed on a mild steel. Corrosion Science,
26., 311-328.
Stewart, J., D. B. Wells, P. M. Scott and A. S. Bransden
(1990). The prevention of IGSCC in sensitized stainless
steel. Corrosion, 46, 618-620.
Elmer, J. W., S. M. Allen and T. W. Eagar (1989).
Microstructural Development during Solidification of
Stainless Steel Alloys. Met. Trans., 16A, 2117-2131.
 WS8b3

HYDROSTATIC PRESSURE EFFECT ON NICKEL CORROSION BEHAVIOUR IN NaCl

SOLUTIONS
A.M. BECCARIA*, G. CASTELLO**, M.ARFELLI***, P.L. TRAVERSO*

♦Istituto per la Corrosione Marina dei Metalli - Consiglio Nazionale delle Ricerche, Via
Scarsellini 10, 16149 Genova, Italy
** Istituto di Chimica Industriale - Universita di Genova, Corso Europa 30, 16132 Genova, Italy
*** Istituto Teoria e Struttura Elettronica - Consiglio Nazionale delle Ricerche, Monterotondo,
Roma, Italy

ABSTRACT
The effect of hydrostatic pressure on nickel corrosion in NaCl solutions at different
concentrations (5.8xl0- 2 M/L; 1.2X10"1 M/L; 5.8x10-! M/L; 1.2 M/L) was investigated. The
experiments were carried out at 20°C and at 8.2 pH. The pressure ranged from 1 to 300 atm. By
increasing the pressure, nickel corrodibility was observed to decrease in diluted solutions and to
increase in concentrated ones. This was attributed to the different composition of the passive
layers formed on the nickel surface under different conditions. XPS analysis shows that
corrosion products formed at high pressure have a lower hydration degree. Moreover, chemical
analysis shows that by increasing Cl· concentration in the corrosive solutions, Cl· amount in the
corrosion products increases. The presence of "dry" oxides with negligible amount of Cl ions
may increase nickel corrosion resistance, thus explaining its lower corrodibility in diluted
solutions at high pressure.The presence of "dry" oxides with a great amount of Cl ions increases
passive layer dishomogeneity, thus reducing its covering power. Nickel corrodibility increase in
concentrated NaCl solutions at high pressure is thus explained.
KEYWORDS
Nickel; hydrostatic pressure; NaCl solutions; corrosion products.
Previous works have shown that hydrostatic pressure increase affects the corrosion behaviour
of many metals (Mor and Beccaria, 1978, 1979a, b; Beccaria and Poggi, 1985) and alloys
(Beccaria and Poggi, 1985; Beccaria etal., 1987; Festy and Beccaria, 1989) in slightly alkaline
solutions. Hydrostatic pressure effect is strictly linked to metal nature and to corrosive solution
composition. By increasing the hydrostatic pressure in the same corrosion solution (e.g. sea
water) the average corrosion rate of some metallic materials (Cu - Ni alloys) (Beccaria et aL,
1987) decreases, whereas it increases for some others (pure Cu or Al) (Mor and Beccaria, 1978;
Beccaria and Poggi, 1985). Moreover, hydrostatic pressure effect on the corrosion behaviour of
the same metal may change by modifying corrosive solution composition. By increasing the
hydrostatic pressure, nickel corrosion rate as well as pitting susceptibility increase in 3.5% NaCl
solutions, whereas they decrease in sea water. This was attributed to the different nature of
corrosion layers formed in these solutions: nickel oxides and/or hydroxides are formed in NaCl,
whereas nickel oxides, hydroxides and Ni-Mg carbonates are formed in sea water (Beccaria et
al.y 1989). With hydrostatic pressure increase, nickel oxides may be converted into soluble nickel

601
602

oxychlorides, due to increased activity of Cl ions (Home, 1969), thus forming pit initiation sites.
Conversely, under hydrostatic pressure effect, the concentration of Mg-Ni carbonates or
oxycarbonates increases, thus enhancing passive film covering power.
Passive layer composition and covering power also depend on salt concentration of the corrosive
solution, as shown by some experiments conducted on Aluminium in NaCl (Beccaria and Poggi,
1986) and Na2SC>4 (Beccaria and Poggi, 1987) at different pressures.
In order to verify whether concentration changes may affect corrosion behaviour at different
pressures even in the case of nickel, the behaviour of this metal was investigated in NaCl
solutions at different concentration values.
This paper describes the results of a series of experiments carried out at different hydrostatic
pressures (1, 100, 300 atm) in NaCl (5.8x10-2; 1.2X10"1; 5.8x10"! M/L), at a pH value of 8.2
and at 20°C.
EXPERIMENTAL METHOD
The experiments were carried out in pressure vessels pressurized with a hydropneumatic pump
by using the corrosive solution as working fluid, so as to maintain dissolved gas concentration
unchanged during pressure increase.
Electrochemical tests were conducted on specimens previously kept for 4 hours in the corrosive
solutions at various pressure values (1, 100, 300 atm). Corrosion current density and
polarization resistance were measured with polarization potentiodynamic curves obtained with a
scanning speed of 250 mV h-1. Impedance was measured by perturbing specimen equilibrium
potential with 10mV a.c. at a decreasing 10 KHz to 10 mHz frequency range. Free corrosion
potential was measured over a time range from 30 min to 240 h.
Both passivation film breakdown (Ep) and pitting protection potential (Epp) were measured with
semistationary potentiostatic polarization. Starting from equilibrium potential, the working
electrode potential was increased by 2 mV steps every 10 min up to E p value which was indicated
by the sharp increase of i corr . Once Ep was established, the working electrode potential was
lowered in the same way (2mV/10min) until the backward curve crossed the forward one. Free
corrosion tests were carried out at 1 and 300 atm. passive films formed on free corroded
specimens were characterized with chemical methods, IR and XPS spectroscopy. SEM
examinations were also conducted on these specimens to observe corrosion morphology.

RESULTS AND DISCUSSION

Nickel Behaviour at Atmospheric Pressure
Polarization curves (Fig. 1) and free corrosion tests (Fig. 2) show that nickel average corrosion
rate increases by increasing chloride concentration. ICOrr values obtained from polarization curves
show a linear relationship with log[Cl-] (Table 1) thus suggesting an adsorption process of Cl
ions on nickel metallic surface or on nickel corrosion products adhering to the metallic surface.
Formation of nickel chlorides is ruled out by the equilibrium potential (E res t) or corrosion
potential (E cor r) ai*d Cl concentration (Table 2) according to the following electrochemical
reaction: Ni+Cl"= (NiCl)ads + e.

Conversely, Cl- adsorption on nickel oxides or hydroxides is possible, thus forming soluble
oxychlorides and delaying passive film formation, as confirmed by many authors (Galvele,
1976, MacDougall, 1988, 1979; MacDougall etal., 1983; Bengali and Ken Nobe, 1979). Anodic
polarization enhances pitting susceptibility of nickel specimens, as shown by film breakdown rate
 603

and film self-repairing potential plotted in Fig. 3 as a funcion of Cl· concentration. The linear
relationship between E p and log[Cl·] suggests Cl· adsorption on Ni(OH)+ under anodic
polarization. Due to Cl· adsorption, the passive film may undergo continuous breakdown and
repair of localized areas. When a sufficient amount of Cl· is concentrated in certain areas, oxide
layer repair is not possible, thus localized corrosion takes place.
Moreover, the chemical analysis shows (Fig. 4) that oxidation layer composition depends on
NaCl concentration of the corrosive solution. In Fig. 4, Ni2+ species, which in the corrosion
products are combined as hydroxides or hydroxychlorides and cannot be discriminated by
chemical analysis, are indicated as Ni hydroxides.

The amount of Cl· bonded to nickel compounds is stoichiometrically calculated as the difference
between total Cl· amount (analytically measured) and the amount of Cl· bonded to Na+.
Nihydrox/Niox and Cl/Ni ratio increases by increasing Cl· concentration.

Moreover, only at lowest Cl· concentration, IR analysis shows the presence of O-H groups with
chelation bonds (O-H stretching vibrations 3,200-1,700 cm·1) which can be easily attributed to
the presence of Ni(OH)2-
These results are consistent with a higher presence of hydroxychloride compounds in more
concentrated Cl· solutions.
By increasing the amount of chlorinated compounds in the passive film, the protective power
against generalized and localized corrosion decreases, as shown by electrochemical (Figs. 1, 3)
and free corrosion tests (Fig. 2).

Effect of Hydrostatic pressure

By increasing the pressure, corrosion layer composition changes as indicated by XPS analysis
(Table 3). A greater amount of nickel hydroxides Ni(OH)2 (35% at 1 atm, 30% at 300 atm) and a
lower amount of NiO (23% vs 25%) is formed in the corrosion products at atmospheric pressure.

At low Cl· concentration, the negligible amount of Cl· contained in the corrosion layer (Fig. 4)
and the greater amount of NiO enhance nickel corrosion resistance against localized (Fig. 3) and
generalized corrosion (Figs. 1, 2). This result is in agreement with literature data (Marcus and
Oudar, 1983; Bennedorf et al.t 1981) showing that the "dry" NiO layer is more protective than
the "wet" Ni(OH)2 layer. At high Cl· concentration, by increasing the pressure, nickel corrosion
resistance decreases (Figs. 1-3) due to lower hydration degree which is likely to offer a lower
steric hindrance to Cl· penetration, thus favouring their chemisorption on nickel oxides and
further conversion into soluble hydroxychlorides.

CONCLUSION
Passive layer composition formed on pure nickel in NaCl solutions depends on salt
ceoncentration and on corrosive solution pressure.
This is confirmed by the following:

1) by increasing Cl· concentration, the amount of Cl ions in the corrosion layer increases, thus
reducing resistance to localized and generalized corrosion.
604

2) by increasing the pressure, the percentage of "wet" nickel oxides decreases and for this reason
nickel corrosion resistance increases in diluted NaCl solutions with negligible chlorine
content. In concentrated NaCl solutions, with greater chlorine content in the corrosion
products, corrosion resistance decreases.

Table 1. Icorr values obtained from polarization curves and relationship between
icon- and Cl· concentration in NaCl solutions
at different pressures

NaCl icorr (μΑ. cm•2)

IWL 1 atm 300 atm
0.8x10-2 0.011 0.008
1.2X10-1 0.012 0.012
5.8x10-! 0.018 0.022
1.2 0.022 0.029

i l a t m = O.O15[Cl-]012

i300atm = O.O39[Cl-p«

Table 2. ECOrr, Erest values in NaCl solutions at different pressures'.

NaCl rLcorr';mV,Ag/AgCl) Erest(mV,Ag/AgCl)
WL latm 300atm latm 300 atm

5.8xl0-2 -160 -220 -170 -225

1
1.2X10- -180 -200 -188 -205
5.8x10-1 -190 -190 -180 -190
1.2 -180 -160 -178 -170
 605

Table 3. Binding energy (eV) and percentage values of the analysed

compounds in the corrosion products

Ols Ni 2p3/2 ΔΕ C12p

Corrosive p Ox (OH)- H20 Nimet NiO Ni(OH)2 198.0

solution (atm)
NaCl 1 530.4 531.9 532.7 852.7 855.0 856.4 +3.8 198.7
0.58 M a (15) (40) (47) (40) (23) (35) (8)
300 530.4 531.7 532.9 852.7 855.0 856.3 +3.7 198.3
b (15) (50) (37) (40) (25) (30) (9)

Ni metal 852.9
NiO 529.9 854.5
Ni(OH)2 531.7 856.6 +5.8
H20 532.4
533.1

Δ E represents the energy separation of the satellite line from the Ni2p3/2 peak of the Ni(OH)2·
The percentage of the species is shown in parentheses.

REFERENCES
Beccaria A.M. and G. Poggi (1985), Eurocorr '85 - Cefracor Nice, Paper No. 30
Beccaria A.M. and G. Poggi (inS),British Corros. Jr., 20, 183-186
Beccaria A.M. and G. Poggi (1986), Corrosion, 42, 470-475
Beccaria A.M. and G. Poggi (1987), Corrosion , 43, 153-158
Beccaria A.M., G. Fiordiponti and G. Mattogno (1989), Corrosion Sc, 29, 4, 403-416
Beccaria A.M., G. Poggi and G. Castello (1987) - Proc. 10th Intern. Congress on Metallic
Corrosion, Madras, Ed. Oxford, Vol. 4, 3327-3337
Bengali A. and Ken Nobe( 1979), J. Electrochem. Soc, 126, 1118-1123
Bennedorf C , C. Nobl, M. Rosemberg and F. Thiene (1981), Surf. Science, 111, 87-92
Festy D. and A.M. Beccaria (1989), Proc. of Corrosion NACE - Paper 292, New Orleans 17-21
April
Galvele J.R. (1976), /. Electrochem. Soc, 123, 464-474
Hörne H. (1969), Marine Chemistry, (Wiley Intersciences), New York, 73.
MacDougall B. (1979), //. Electrochem. Soc, 126, 919-925
MacDougall B. (1988), Corrosion Sei., 28, 211-220
MacDougall B., D.F. Mitchell, G.I. Sproule and M.J. Graham (1983), /. Electrochem Soc,
130, 543-547
Marcus P. and J. Oudar (1983), Passivity of Metals and Semiconductors (Froment Ed.)
Amsterdam, 119-124
Mor E.D. and A.M. Beccaria (1978), British Corros. Jr., 13, 142-146
Mor E.D. and A.M. Beccaria (1979), Proc. Symp. Intern. Corrosion Protection Offshore, paper
124
Mor E.D. and A.M. Beccaria (1979), Werkst undKorr, 30, 551-558
606
606

,Aq/AqCI) CD
100
f ^£
100
I SSg
iF ~~^
300

C
100
£ FIG.2- Polarization
FIG.l- Polarization curves of
curves of
100
*=^ nickel at -#-+-
nickel -4—#— 11 and
and at
at —0—0—
-0-0-
300 100 atm
300 atm in
in NaCl
NaCl solutions
solutions at
at
.11 different
different concentrations:
concentrations:

r
C
^-*~^^ CD
100
2 2 2
2
100 (T)5.8X10"
0)5. aX10- MI L;
M/L; 1.2X10~ MI
(?) 1.2Xl0- L
M/L
300
-300
(J)5.axl0-
1
(ζ)5.8Χ10~ΊΜ/1;MI L; 0(7) 1. 2 MIL
1.2 M/L
100 c*
100

300

10"' 10"'
Η μ Α α ι Γ 2)

CD
FIG. 22-- (7) Weight
Weight loss
loss of
of nicke
nickell:
specimens
specimens exposed at
exposed at -.-+-
—4—*— 11 and
at -0—0— ZOO
at ~ 300 atm in
in NaCl solutions
soLutions
WU30O
-0.e25fCli°·
CD
®.
2) Weight
Weight of
of nickel
nickel as solid
solid corro-
corro-
sion product adherent to the metaLlic
sion product adherent to the metallic
surfaces of
surfaces specimens exposed
of specimens exposed at —#—f-
at-~
1 and at -0—0— 300
at -0-0- ZOO atm.
atm.

0.1
[CI-) (MILl
[CI-] (M/L)

Elmy.Aq/AqCI)

'200~ Eo FIG. 3- Corrosion

FIG.3- Corrosion potential (Ecorr),
potential (Ecorr),
.100 • ~ beakdown
beakdown film
fiLm potential(Ep),
potentiaL(Ep), pro- pro-
tection
tection pitting
pitting potential (Epp)
potentiaL (Epp)
o~ values
values for
~
for specimens
* 4 11 and
specimens exposed
and atat -0-0-
exposed at
-0—0— 300
ZOO atm.
atm.
at

\~Ecorr
10
[CI-J(M/Ll

FIG.4-
FIG. hydroxlNi oxide
4- Ni hydrox/Ni oxide ratio
ratio
and Cl/Ni
and CLINi atomic
atomic ratio
ratio inin corro-
corro-
sion product
sion product adherent
adherent toto the
the me-
me-
005
taLLic surfaces
tallic surfaces ofof specimens
specimens ex-ex-
posed at
posed at -#-#-
-4 ■# "11 and
and at-()-()-
at
ZOO
300 atm.atm.

0.1 1.0
[CI-] (MILl
[CI"] (M/L)
W S 8 b 4 INTRAGRAIN SENSITIZATION OF FE-28CR-5NI
STAINLESS STEEL ASSOCIATED WITH 475t
EMBRITTLEMENT

Yuichi ISHIKAWA, Toshihiko YOSHIMURA

Mechanical Engineering Research Laboratory,
Hitachi, Ltd.
502 Kandatsu, Tsuchiura-shi, IBARAKI 300 JAPAN
and
Toshinori OZAKI
Metals Research Laboratory, Hitachi Cable Ltd.
3-1-1 Sukegawa-cho, Hitachi-shi, IBARAKI 317
JAPAN

ABSTRACT
Iron-28%chromium-5%nickel stainless steel was aged at 450t for
up to 5000h. Microstructural change upon ageing was examined
by atom probe-field ion microscopy (FIM). Change in corrosion
resistance of the steel upon ageing was evaluated by
electrochemical potentiokinetic reactivation (EPR) method.
Upon ageing the steel undergoes phase separation via spinodal
decomposition. This results in a closely knitted precipitation
of Cr-rich alpha prime phase of 2nm in size in the matrix of Cr-
depleted alpha phase of several nm in size upon ageing for
5000h. In the Cr-depleted alpha phase, the Cr concentration is
below 12at%. Simultaneously the steel becomes hardened and
shows the sensitization in the grain. Upon ageing for 100h,
two distinct reactivation peaks appear at -200 and -410mV (vs
Ag/AgCl). These peaks grow as the ageing proceeds. The peak
at -200mV is attributed to the Cr-depleted a phase where Cr
concentration is below 12at%.

KEYWORDS

Ferritic stainless steel; ageing; sensitization; atom-probe

INTRODUCTION

Ferritic stainless steel has been known for being embrittled by

ageing at intermediate temperatures. This is called 475Ϊ
embrittlement and can be considered as a result of
precipitation of Cr-rich a' (Williams and Paxton, 1957).
Identification of Cr-rich α' precipitates has been carried out
mostly by transmission electron microscope and its relation to
embrittlement has been discussed by several papers (Blackburn
and Nutting, 1964; Lagneborg, 1967; Plumtree and Gullberg,
1976). In Fe-Cr system difference in d-spacing between a and
a' and in atomic scattering factor between Fe and Cr is so
small that most studies failed to clarify the microstructural
607
608
evolution in the early period of phase separation. The recent
microstructural investigation (Yoshimura et al, 1990) of Fe-
28Cr-5Ni ferritic stainless steel by Mossbauer effect and atom-
probe-FIM has shown that the phase separation occurs via
spinodal decomposition and precipitation of Cr-rich a* is
accompanied with formation of Fe-rich (Cr depleted) a phase.
Some studies have shown the change in electrochemical behaviour
of ferritic stainless with ageing at 475t (Sugawara and
Konishi, 1976), however, they failed to correlate that change
with microstructural change.

In the present study, the change in electrochemical behaviour

and in microstructures of Fe-28Cr-5Ni ferritic stainless steel
upon long term ageing at 450t has been investigated by
electrochemical potentiokinetic reactivation (EPR) method and
atom-probe-FIM (AP-FIM). An attempt has been made to correlate
microstructural evolutions in the steel to the change in
electrochemical behaviour of the steel.

EXPERIMENTAL

A vacuum arc remelted 20kg ingot of Fe-28Cr-5Ni steel was cold

rolled to 6mm thick plates. Then the steel was solution
treated at 1250Έ for 30min and water quenched to attain a fully
ferritic phase. This was used as the unaged specimen and
ageing of the steel was carried out at 450Ϊ for 100, 1000 and
5000h in an electric furnace. The chemical composition of the
steel (wt%) is Fe-28. 4Cr-4. 99Ni-0. 28Si-0. 012C-0. 002N-0. 009P-
0.009S. The composition is expressed in wt% throughout the
paper unless otherwise stated.

We used the pulsed laser atom-probe for examination of

microstructural evolution in the steel upon ageing. Details of
the atom-probe were described elsewhere(Ishikawa et al, 1986).
Ions are removed from the specimen surface by field evaporation
by the application to the specimen of laser pulses (provided by
a N2 gas laser with a power of 200kW and a pulse width of
1.3ns), superimposed on the DC voltage (5~10kV). The field
evaporated ions are accelerated towards the FIM screen and
those ions that pass through the aperture hole of the screen
are elementally identified from their time of flight to the
particle detector with a single-ion sensitivity located at the
end of the TOF spectrometer. Successive application of laser
pulses to the specimen leads to progressive field evaporation
of atomic layer from the surface. The composition is
determined by simply counting the number of atoms of interest
compared to the total number of atoms collected from one atomic
layer. The bulk materials were mechanically cut into square
rods that are approximately 0. 2mm on a side by 15mm in length.
These blanks were fabricated into a sharp needle by
electropolishing in (HC1/HN03)=(1/3) solution with 3~4V AC.
This produces specimen with an end radius about lOOnm suitable
for FIM. At least 20000 ions were collected from each
specimen.

The EPR method has been used for detection of the presence of
Cr depleted zone along grain boundaries and for evaluation of
 609
the susceptibity to intergranular corrosion (Novak et al,
1975). In the present study the presence of Cr depleted region
in the grains was evaluated from potentiokinetic curves
obtained by a controlled potential sweep from the open circuit
to the passive region and then from the passive to the active
region. The criterion used to distinguish between sensitized
and sound samples has been the ratio of the reactivation peak
current density (ir) in the reactivated state (reverse scan) to
the activation peak current density (i,) in the activated state
(forward scan). The test electrolyte was 0. 1MH2SO«+0. 01MKSCN
held at 26Ϊ. The potential scan was 20mV/min. The specimens
were sectioned, mounted and polished to a 1/zm diamond finish.

RESULTS

AP-FIM

Figure 1 shows a random area atom-probe analysis model for a

spinodal decomposed alloy (Brenner et al, 1984). The spinodal
decomposition is believed to produce an isotropic network where
both a and a' phases are highly interconnected networks in the
tip. In the AP analysis, a cylinder of atoms is collected from
the specimen and the composition variations are measured as a
function of distance. As material is removed, a' phases
present in the specimen will eventually intersect the surface
and those that emerge in the sampling volume will be analyzed.
Upon development of spinodal decomposition, the Cr
concentration profile determined by dividing the ion-by-ion
data into blocks containing equal numbers of atoms (here 50)
would change as shown in the lower portion of Fig. 1.

/
Material
Removed

ΛΛΛ. m DIM
Progress
of early intermediate late
Ageing

Fig. 1 Ramdom area atom-probe analysis model for

spinodally decomposed microstructure

Figure 2 shows a portion of experimentally determined Cr

concentration profiles as a function of ageing time. Similar
to the model described, the amplitude of the Cr concentration
fluctuation develops upon ageing. The amplitude of Cr
concentration fluctuation becomes large and the frequency of Fe-
rich a phase where Cr concentration is less than 12at%
increases.

Autocorrelation analysis of Cr concentration profiles and FIM

610
observation (Yoshimura et al, 1990) have indicated that the
size of α' phase is in the range of l~3nm and the spacing is
2~5nm for the 5000h aged and that both phases are highly
interconnected networks.
\oj uitayeu

0 10 20 30 40 50
Number of blocks (distance) i nm

Fig. 2 Cr concentration profile as a function of

ageing time

EPR
Figures 3(a) through (d) are, respectively, the potentiokinetic
curves for the unaged and the aged at 450t for 100, 1000 and
5000h. In case of 300 series austenitic stainless steels, a
solution treated and unaged steel does not show any
reactivation peak, whereas the solution treated and unaged
ferritic stainless steel shows a reactivation peak as in
Fig.3(a). This results from the grain boundary sensitization
because of a lower solubility of carbon in ferrite.
Metallographic examination shows carbide precipitation along
the grain boundany in the solution treated and unaged specimen.

Fig.3 EPR curves as a function of ageing time

Ageing at 450Έ promotes the diffusion of Cr into the Cr

depleted grain boundary area and the grain boundary
sensitization disappears. This results in disappearance of the
 611
reactivation peak at -300mV, but two reactivation peaks appear,
one at -200mV and the other at -410mV in the steel aged for
100h, as shown in Fig. 3(b). Further ageing increases the two
reactivation peaks as shown in Fig. 3(c) for 1000h ageing and
consequently the peak at -200mV becomes so large that the peak
at -410mV appears to be contained in the peak at -200mV.
Moreover the passivation potential becomes more noble and the
passivation current density increases, indicating that the
steel becomes less readily to be passivated and the passive
film becomes less stable.

DISCUSSION

The reactivation ratio is determined for both peaks at -200mV

and -410mV and plotted as a function of ageing time in Fig. 4,
together with Vickers microhardness values (Hv) and the maximum
amplitude of Cr concentration fluctuation (ACr).

Ageing time (h)

Fig. 4 Dependence of microhardness, the maximum

amplitude of Cr concentration fluctuation
and the reativation ratio on ageing time

The reactivation ratio determined for the peak at -200mV

(ir!/ia) increases with ageing time, as do the hardness and
ACr, while the reactivation ratio for the peak at -410mV
(ir2/ia) peaks at the ageing time of 1000h. This suggests that
the development of phase separation via spinodal decomposition
is closely related to the reactivation ratio for the peak at -
200mV as well as to the hardness increase.

The reactivation ratio increases largely from 1000 to 5000h

ageing and the reactivation peak shifts to more noble
potential. This can be attributed to the decrease in the
minimum Cr concentration in the Fe-rich a phase, as shown in
Fig. 2. The fraction of the area where Cr concentration is less
than 12at% (FCr<12) is determined and plotted against the
reactivation ratio for the peak at -200mV (irt/ia). This
yields a straight line and leads us to identity that the
reactivation peak at -200mV results from the Cr depleted region
in the grain, that is, Fe-rich a phase formed with the
precipitation of Cr-rich α' phase. This intragrain sensitized
region appears to have Cr concentration about 10at% on the
average and to be several nm in width and highly interconnected.
612
The reactivation peak at -410raV (irÄ/ia) appears to result from
the Cr depleted region in which the minimum Cr concentration is
higher than 12at%. However it may be premature to attribute
this peak to the Fe-rich a phase with a certain Cr
concentration range.

CONCLUSION

Atom-probe-FIM analysis and EPR test were carried out for the
Fe-28Cr-5Ni ferritic stainless steel aged at 450*C for up to
5000h. The following are the important conclusion of this
study.
1) Ageing at 450Ϊ results in phase separation via spinodal
decomposition.
2) The phase separation results in interconnected networks of
Fe-rich a phase and Cr-rich α' phase, both of several nm in
width.
3) In the Fe-rich a phase, the minimum Cr concentration
decreases to less than 12at% and shows the intragrain
sensitization behaviour in EPR test.

REFERENCES

Blackburn, M. J. and J. Nutting (1964). Metallography of an iron-

21% chromium alloy subjected to 475Έ embrittlement.
J. Iron S Steel Inst. , 202, 610-613.
Brennner, S. S. , M.K.Miller and W. A. Sotta (1984). Atom probe
field-ion microscopy studies of modulated structures. NATO
ASI Ser. E, 83, 309-323.
Ishikawa, Y. , K. Takahashi and T. Yoshimura (1986). An atom probe
study of molybdenum-carbon reaction. J. de Physique, C2, 365-
370.
Lagneborg, R. (1967). Metallography of the 475t embrittlement in
an iron-30% chromium alloy. Trans. ASM. , |60f 67-78.
Novak, P. , R. Stef ec and F.Franz (1975). Testing the
susceptibility of stainless steel to intergranular corrosion
by a reactivation method. Corrosion, 31, 344-347.
Plumtree, A. and R. Gullberg (1976). Embrittlement of a
continuously cooled Fe-25Cr alloy. Metall. Trans. , 7A, 1451-
1458.
Sugawara, H. and K. Konishi (1976). The influence of 475t aging
on anodic polalrization and pitting corrosion of 13-52%Cr-Fe
alloys. J. Japan Inst. Metals. 40, 551-558.
Williams, R. 0. and H. W. Paxton (1957). The nature of ageing of
binary iron-chromium alloys around 500Έ. J. Iron & steel
Inst. , 185, 358-374.
Yoshimura, T. , Y. Ishikawa, H. Kuwano and Y. Hamaguchi (1990).
Submitted to J. Japan Inst. Metals.
 WS8b5

THE INVESTIGATION OF THE PITTING CORROSION OF

STAINLESS AND ALLOY BY THE RAPID SCRATCH TECHNIQUE

GUO JIAJU, CHEN HONGYU and ZHANG WENQI

Department of Surface Science and Corrosion Engineering,

University of Science and Technology Beijing, P.R.C.

ABSTRACT

The pitting corrosion of austenite stainless steel and Alloy 800 in sodium chloride solution has
been studied by rapid scratch technique. The mechanism of pitting corrosion on the bare metal
surface has been discussed and the physical sense of the critical pitting potential of the bare
metal surface (Ec) has been proposed. Ec changes linearly with the logarithm of chlorion
concentration: Ec=a'-b'logCcr. Ec and Eb change in the same law within a large PH range.
In order to explain it, the coefficients of repassivation, a1 and a2 are measured.

KEYWORDS

Localized corrosion; pitting; passivation; passive film; stainless steel; chloride solution.

INTRODUCTION

The pen recorder in the ordinary scratch method is at second grade, however, the bare metal
surface finishes repassivation within decades of seconds and the pitting begins in two hundred
milliseconds(Zhu Yingyang et al.. 1986a). The pittings have propagated at different time
before the scratch knife leaves the specimen. It is impossible for the pen recorder to get the
early information of pitting. The pitting current and critical potential are influenced by this
method. In order to solve the problem, the rapid scratch technique and the new recording
system are adopted to investigate the pitting in this paper.

EXPERIMENTAL

The experimental apparatus, as shown in Fig.l, is composed of the scratch apparatus and the
recording data system.

613
614

V
ICON.
Oil «}ll
λ-|
I«*..

Fig.l Experimental apparatus.

1. working electrode 8. spring

2. reference electrode 9. power pack
3. counter electrode 10. potentiostat
4. scratch knife 11. pen recorder
5. circle motor 12. oscilloscope
6. electrolyte 13. computer
7. support pot

The shape of the scratch knife is cylinder of which diameter is 2 mm, The time between the
knife reaching and leaving the specimen is within 10ms. The recording data system is
composed of two parts. The early current is recorded by the oscilloscope and computer. The
later current is taken by the pen recorder. The pitting on the specimen can be watched under
the micrograph. The specimens are Types 321 and 316L stainless steels and Incoloy 800.

RESULTS AND DISCUSSIONS

Measurement and Physical Sense of Ec

The later pitting current and micrograph are used to measure the critical pitting potential of
the bare metal surface (Ec). The results of pen recorder is shown in Fig.2.

Fig.2 Current vs time curves for 50mv Type 321 in 3.5%Nacl at different potentials
((l)-100mv;(2)50mv;(3)75mv;(4)100mv).
 615

The early current is recorded by the oscilloscope. The current of the bare metal decreases
quickly at E<Ec, as shown in Fig.3, and there is no pitting. The current decreases slowly at
E>Ec, as shown in Fig.4, and there is pitting.

f\

l\ Λ
i
- U - W * < V H «* :· ..* £ * *
1 i
1 1
Fig.3 Current vs time curves at begining without pitting(316L,5%Nacl,100mv).

1
ΓΝ^ 1
/1
* 1 {
I 1
1
!
i«
i ;
i
ΓΤ I

Fig.4 Current vs time curves at begining with pitting(316L,5%Nacl,200mv).

By means of calculating reliability of Ec which is measured by the above methods, Ec is very

accurate and has a good repeat. Ec can strictly determine whether repassivation or pitting.

According to the experimental results and references(Zhu Yingyang et al„ 1986a, Burstein el
al, 1983), the mechanism of pitting on the bare metal surface is proposed.

Me+H20=Me· H2Oads (1)

Me+Cl~=Me· C l ' a d s (2)
Me· Cl"ads+XH20=Me(OH)x· Cl"+xH++xe (3)
Me(OH)x· Cl"=Mex++xOH"+Cl* (4)
Me· H,Oads=MeOHads+H++e (5)
+
Me Cl"ads+H20==MeOHads+Cl~+H +e (6)
MeOHads =MeO+H++e (7)

The chlorion adsorbs primarily at the defect where there is a high surface energy. When the
adsorption of chlorion at the defect adds to a specified critical value-[Cl~]c, reaction (6) does
not occur and the adsorbed chlorion can not depart from the defect. Reaction (3) and Reaction
(4) occur, and the defect becomes soluble. There are active pits at the defect of the bare metal
surface. It is the site of pit nucleation. If the adsorption of chlorion at the defect does not add
to [Cl"]c, the adsorbed chlorion will depart from the bare surface by reaction (6). The
repassivation happens rapidly. [Cl~]c determines whether or not reaction (6) occurs. [Cl ]c
depends on Ec. Ec is called the critical pitting potential of the bare metal.
616
Besides chlorion solution, the physical sense of Ec can be widely defined. With the
temperature, medium and anion activity fixed, Ec is the lowest potential that makes the
adsorption of the anion on the bare metal surface where there is defect and the surface energy
is the biggest add to a specified critical value-[X~]c and the defect become soluble.

Effect of Chlorion Concentration of Ec

A relationship between Ec and chlorion concentration Ccl", as shown in Fig.5, is found,

•IncoloyßOO

Log(Naol wt#)
Fig.5 Relationship between Ec and chloring concentration.

Ec=a'-b'logCcl" (8)

The following relations are the calculating results.

Type 321 Ec=0.158-0.1771ogCcl" (9)

Type 316L Ec=0.242-0.1371ogCcl" (10)
Incoly 800 Ec=0.290-0.1411ogCcl* (ID

Effect of PH
The critical pitting potential of the bare metal surface (Ec) and breakdown potential (Eb) have
been measured in 3.5% Nacl solution with different PH values, as shown in Fig.6, Fig.7 and
Fig.8.

6. 7 8 9 10 11 12 13

Fig.6 Effect of PH on Ec and Eb of Type 321.

 617

2 3 Ί 5 & 1 a 9 10 11 12 13
Hi

Fig.7 Effect of PH on Ec and Eb of Type 316L.

5 6. 7 8 9 10 11 12 13

Fig.8 Effect of PH on Ec and Eb of Incoloy 800.

Figures show that Ec and Eb are almost constant at PH<11, but above 11, they increase
quickly. The effect of PH on Eb occurs through the effect of PH on Ec. In order to avoid the
influence of the passive film, the repassivation is investigated. The repassivation kinetics has
been described as:
I(t)-C 1 exp(-a 1 t)+C 2 exp(-a 2 t) (12)

Where ax describes the absorbed rate of the Me(OH), d^ describes the rate of oxide film (Zhu
Yingyang ejLaL, 1986b). The results of the effect of PH on coefficients are shown in Fig.9 and
Fig.10. The coefficients ax and 2^ are almost constant at PH<11, but they increase quickly at
PH>11. It corresponds to the effect of PH on Ec and Eb.

5· 6 ? 6 9 10 11 12 13

Fig.9 Effect of PH on coefficient a2 (3.5%Nacl,E=10mv).

618

017
oIncoloy 100
016 • 3l6L
«321
0)5
oiu

013

012

Oil
^jFZZ? ^. * =*=Ξ/
O10

009
3 ~k $ 6 T "Tf t~
,
10 ii ia~ 1 3 ^

Fig.10 Effect of PH on coefficient ^ (3.5%Nacl,E=10mv).

There are competitive adsorptions between the chlorion and oxygenium. At PH<11, the
adsorption of oxygenium is constant because ax is constant. The adsorption of chlorion is
constant. The potential Ec corresponding to [CF ]c is also constant. At PH>11, ax increases
quickly and the adsorption of chlorion is repelled seriously by the oxygenium. Ec increases
so rapidly as to make the adsorption of chlorion add to [CF]c and the pitting occur. With the
chlorion concentration fixed, Eb corresponds to Ec. It can explain the effect of PH on Eb.

CONCLUSION

The critical pitting potential of the bare metal surface (Ec) has been obtained by the rapid
scratch technique. The mechanism of pitting on the bare metal surface and the physical sense
of Ec has been proposed. Ec changes linearly with the logarithm of chlorion concentration.
At PH<11, the potentials Ec and Eb, coefficients aj and a2 are almost constant. They all
increase quickly at PH>11.

REFERENCES

Burstein,G.T. and G.W.Ashley(1983). Early steps in the anodic oxidation of iron in

aqueous solution. Corrosion,39,241 -247.
Zhu Yingyang, Wang Kuang, Zhu Rizhang and Zhang Wenqi(1986a). Pitting corrosion of
fresh stainless steel in chloride solution. Journal of Beijing University of Iron and Steel
Technology,29,91-99.
Zhu Yingyang, Zhu Rizhang, Wang Kuang and Zhang Wenqi (1986b). Kinetics of
passivation of stainless steel in chloride solution. Journal of Beijing University of Iron
and Steel Technology, 30,&5-9l.
 WS8C1

Localization in the Crevice Corrosion of Titanium

B.M. Ikeda, M.G. Bailey, M.J. Quinn, and D.W. Shoesmith

Whiteshell Laboratories, AECL Research

Pinawa, Manitoba, Canada ROE 1L0

ABSTRACT

The impact of chloride concentration, temperature and oxygen reduction on

the depth and localization of crevice corrosion οη. Grade-2 titanium has been
studied using a combination of electrochemical, metallographic and image
analysis techniques. Oxygen reduction was found to control the total amount
of corrosion over a wide range of conditions. Depending on the temperature,
the amount and depth of corrosion decreased with increasing chloride
concentration. A decrease in temperature resulted in deeper penetration at
fewer sites and a lower overall corrosion rate.

KEYWORDS

Crevice corrosion; Grade-2 titanium; aqueous chloride.

INTRODUCTION

In the Canadian Nuclear Fuel Waste Management Program, Grade-2 titanium has
been chosen as the primary candidate material for the construction of
nuclear fuel waste containers because of its excellent resistance to general
and localized corrosion in saline environments. However, the use of Grade-2
titanium in hot saline environments may be limited by its tendency to
crevice corrode (Schutz, 1986), and this process appears to be the most
likely failure mode under disposal vault conditions.

Most studies on the crevice corrosion of titanium alloys have concentrated

on the determination of susceptibility diagrams (Imperial Metal Industries,
1970; Iki and Tsujikawa, 1986), which outline the conditions of salinity,
temperature, redox potential and material properties under which the alloy
is immune to this form of corrosion. However, immunity is a difficult
concept to prove, especially in the absence of a significant catalogue of
corrosion data under the operating conditions of interest. Such proof by
observation is impossible under disposal vault conditions because of the
period of containment required (-500 to 1000 years). Furthermore,

619
620
statements of susceptibility do not enable us to predict container
lifetimes.

For these reasons, we have chosen an electrochemical experimental approach

that forces crevice corrosion to initiate (Ikeda et al., 1989), and have
attempted to obtain a detailed understanding of the mode and kinetics of the
crevice propagation reaction (Ikeda et al., 1990a).

Many factors will influence the mode and depth of penetration within an
active crevice (Schutz, 1988). We have shown that the most important of
these are temperature (Ikeda et al., 1990b), oxygen concentration (McKay,
1987; McKay and Mitton, 1985), chloride content of the groundwater (Bailey
et al., 1991a; Ikeda et al., 1990c), and the composition and microstructure
of the titanium alloy used (Ikeda et al., 1990a; 1990b). Many of these
parameters act together on crevice corrosion. In this paper, we concentrate
on describing the impact of temperature, chloride concentration, and oxygen
concentration on the rate of crevice propagation.

EXPERIMENTAL

Our experimental arrangement and procedure have been discussed elsewhere

(Ikeda et al., 1989) and only a minimum of detail is presented here.
Commercially available ASTM Grade-2 titanium plate with an iron content
<0.08 wt.% was used. The crevice corrosion specimens consisted of two
planar coupons sandwiching an untreated PTFE crevice former, and were
assembled under the solution to ensure that the creviced area was wet from
the start of the experiment. The artificially creviced working electrode
was coupled to a large-surface-area titanium-foil counter electrode through
a zero-resistance ammeter and the resulting coupled crevice current (Ic) was
measured. A silver/silver chloride (in 0.1 mol/kg KCl) internal reference
electrode was used to measure the crevice potential (E c ). This reference
electrode has a potential of +0.2 V vs. the standard hydrogen electrode
(SHE) at 150°C (King et al., 1989). Depths of corrosion penetration were
measured using a combination of metallographic and image analysis techniques
(Ikeda et al., 1990b; Quinn et al., 1991).

RESULTS AND DISCUSSION

The coupled-current (Ic) is not a true measure of the crevice corrosion

rate, since a major portion of the metal dissolution reaction is driven by
proton reduction within the crevice. The charge consumed (Q), which is the
integral of the current over the duration of the experiment, is a measure of
the extent of crevice corrosion driven by oxygen reduction on the coupled
cathode. The overall extent of crevice corrosion, i.e., the total supported
both externally by oxygen reduction and internally by proton reduction, can
be obtained from weight change measurements (W) once the experiment is
complete. This weight change can be converted to an equivalent charge (w)
using Faraday's law and assuming the corrosion product Ti02 is formed by a
four-electron oxidation of titanium. The ratio, Q/w, is a measure of the
fraction of crevice corrosion driven by external oxygen reduction.

Effect of Chloride Concentration and Temperature

We have studied the impact of chloride concentration on crevice corrosion at

150°C (Bailey et al., 1991b) and 105°C, as well as the impact of temperature
at a chloride concentration of 0.27 mol/L. In these experiments, crevice
 621

1 2 3 4
Chloride Concentration / mol/L
Fig. 1. The dependence of weight gain on chloride
concentration for crevice corrosion of Grade-2
titanium at (·) 150°C and (0) 105°C.

corrosion was allowed to continue until all the oxygen in the pressure
vessel was consumed. At 150°C, increasing chloride concentration resulted
in a decreased weight gain but this effect is not observed at 105°C, Fig. 1,
although the amount of charge consumed, Q, is the same (within 20%) for all
experiments. Consequently, the ratio Q/w increases with chloride
concentration at 150°C but remains constant at 105°C.

Previously, we attributed this increase in Q/w to an increased ability of

chloride to complex dissolved titanium at the higher chloride concentrations
(Bailey et al., 1991b). By inhibiting hydrolysis, this complex formation
would lead to less acidic conditions at active sites within the crevice, and
a corresponding decrease in the extent of crevice corrosion supported by
proton reduction inside the crevice. If this were the only impact of
increasing chloride concentration, we would be forced to conclude that
complex formation is not important at 105°C. Unfortunately, information on
titanium chloride complex ions is only available at ambient temperatures
(Nabivanets et al., 1967; Gardner 1967; Babko et al., 1969). It seems
likely that the kinetics of inititating active crevice sites within the
creviced area are altered by the combined effects of increased chloride
concentration and temperature. We have observed faster rates of crevice
activation at the higher chloride concentration and a difference in noise
patterns in the coupled currents, which supports this claim.

Figure 2 shows the maximum depth of penetration as a function of chloride

concentration (Fig. 2A) and weight change (Fig. 2B). At 150°C there is a
linear relationship between the maximum depth of penetration and the overall
extent of crevice corrosion (Fig. 2B), whereas at 105°C the penetration
depth increases with a decrease in chloride concentration (Fig. 2A) but is
unrelated to the total extent of crevice corrosion (Fig. 2B). Visual
examination of the specimens exposed to solutions of different chloride
concentrations at 105°C shows that at the higher concentrations the active
sites are randomly distributed throughout the creviced area, whereas at the
lower concentrations active sites are clustered around the periphery of the
creviced area.

There appear to be two effects contributing to this localization of active

corrosion at lower chloride concentrations: (i) the active sites are more
slowly and more locally initiated, which results in fewer but more distinct
622

1000

BOO

I 600
Pt
400

200

0 1 2 3 4 5 100 200 300 400 500 600

Concentration Chloride / mol/L Weight Gain / mg
Fig. 2. The relationship between the maximum penetration
depth and (A) chloride concentration, and (B)
weight gain, for crevice corrosion at (·) 150°C
and (0) 105°C.

active sites; and (ii) the IR drop increases with increasing distance into
the crevice, which confines propagation to the outer rim of the crevice.
The consequence of confining the same amount of corrosion to fewer sites is
an increased depth of penetration at these sites.

A similar clustering of the active sites is observed in 0.27 mol/L NaCl when
the temperature is decreased from 150 to 105°C. As shown previously (Ikeda
et al., 1990b), Ic decreases markedly over this temperature range. However,
there is no evidence that Q/w changes significantly, indicating that the
conditions (particularly pH) at active sites within the crevice do not vary
markedly with temperature. The clustering of active sites could lead to an
increase in local current density at these sites despite the overall
decrease in I c . Such an increase in local current density would account for
the deeper penetration observed at the lower temperatures.

Effect of Oxidant Concentration

McKay (1987) and McKay and Mit ton (1985) have clearly demonstrated that the
propagation of crevice corrosion is dependent upon the presence of oxygen.
This is further demonstrated in Fig. 3, which shows that Q, a measure of the
amount of oxygen consumed, is proportional to the weight gain, a measure of
the total amount of crevice corrosion, for a wide range of conditions. This
correlation holds over the temperature range from 100 to 150°C, the chloride
concentration range from 0.1 to 5.0 mol/L, and for oxygen contents varied by
a factor of three. The good linear correlation shows that the oxygen
reduction is the dominant parameter controlling the extent of crevice
corrosion. The reduction of protons within the crevice cannot sustain
crevice propagation in the absence of oxygen reduction on the surfaces
external to the crevice.

The amount of available oxygen was the same for most of the experiments and
hence the amount of charge passed for the completion of crevice corrosion
was relatively constant. During the period when Ic decreases with time,
crevice propagation is under cathodic control (McKay and Mitton, 1985).
This cathodic control suggests that the propagation reaction should
 623

2.0 1 1 1

bfl
1.5 O
>A
Ü 1.0 [ 0 1
sä

\jf.
£ 0.5 H

0.0
0 1000 2000 3000 4000
Charge / C

Fig. 3. The relationship between the total amount of

oxygen consumed by the external cathodic reaction
as measured by the electrochemical charge passed
(Q) and the total weight gain due to crevice
corrosion.

be sensitive to the total amount of oxygen available, and also to the oxygen
fugacity of the environment. In an experiment at 95°C in an open glass cell
with an air purge, we allowed Ic to reach a steady state representing an
approximately constant active area within the crevice. The oxygen content
of the purge gas was varied and the resulting Ic was found to depend on the
square root of the oxygen concentra tion of the purge gas. This suggests
that the oxygen reduction reaction proceeds through dissociation of oxygen
on the passive surface; the mechani sm may be complex because of the
semiconducting nature of the passiv e film.

The existence of active corrosion conditions within the crevice is

demonstrated by the decrease in Ic concomitant with a negative shift in Ec
when the oxygen concentration decreases. In the active region, the IR drop
into the crevice will shift the potential to more negative values and
eventually drive the it past the critical potential specified by McKay
(1987) and Iki and Tsujikawa (1986). The active areas within the crevice
that undergo such a potential shift will stop corroding and repassivate. We
have some evidence that the active areas within the crevice become inactive
at low oxygen concentrations, since Ic does not fully recover when the
oxygen concentration is returned to the initial value. This repassivation
is a consequence of the corrosion rate decreasing to a value below that
necessary to maintain the low local pH at that active site.

The potential of an actively corroding crevice is 200-500 mV more negative

than the potential (Ep) of a planar electrode immersed in the same
environment, indicating the oxidizing condition of the solution. On oxygen
depletion, E p shifts to more negative values and Ec to more positive values.
Eventually both show similar behavior. Figure 4 shows this behavior at
125°C. The coincident potentials suggest that the crevice has repassivated,
a suggestion supported by our inability to cause further crevice propagation
by adding more oxygen. The repassivation of the crevice at 125°C appears to
begin before Ic = 0, i.e. before all the oxygen is exhausted (Region R,
Fig. 4). This behavior suggests that the conditions within the crevice at
this point in our experiment are equivalent to those described by Iki and
Tsujikawa (1986); under such conditions the authors claim propagation cannot
continue. They are also equivalent to the potentiostatic conditions of a
624
M
o
ex

3»

I
u a
Ul

0 100 200 300 400 500 600 pa

Time / h
Fig. 4. Electrochemical parameters for crevice corrosion
of Grade-2 titanium at 125°C in 0.27 mol/L NaCl
showing the repassivation of crevice corrosion in
region R. Ec; and En

threshold potential established by McKay (1987). These experiments confirm

that oxygen is essential to drive crevice propagation, and that
repassivation will occur if the creviced area is deprived of the external
oxygen reduction reaction.

GENERAL CONCLUSIONS

1. The depth of penetration is greater at lower chloride concentration and

temperature for the same extent of overall crevice corrosion, despite
decreases in the rate of crevice corrosion. This is due to the
localization of corrosion at a smaller number of active sites.

2. The variation in groundwater chloride concentrations will not drastically

affect the crevice corrosion of titanium waste containers, which will be
at temperatures less than 100°C.

3. The presence of oxidant is essential for crevice propagation to continue.

Its exhaustion will lead to the repassivation of active crevices.

4. It is possible to model crevice corrosion of titanium in terms of the

redox conditions it will be exposed to. A realistic prediction of
container lifetimes is possible, but the redox conditions within the
disposal vault must be considered.

Acknowledgemen t

The Canadian Nuclear Fuel Waste Management Program is jointly funded by AECL
and Ontario Hydro under the auspices of the CANDU Owners Group.

REFERENCES

Babko, A.K., E.A. Mazurenko and B.I. Nabivanets (1969). Russ. J. Inorg.
Chem., 14(8), 1091.
 625
Bailey, M.G., B.M. Ikeda, M.J. Quinn and D.W. Shoesmith (1991a). Crevice
corrosion of titanium alloys under nuclear waste disposal conditions - the
effect of chloride concentration and temperature. In preparation.
Bailey, M.G., B.M. Ikeda, M.J. Quinn and D.W. Shoesmith (1991b). Crevice
corrosion behavior of titanium grades 2 and 12 in hot aqueous chloride
solution - the effect of chloride concentration. In preparation.
Gardner, H.J. (1967). Aust. J. Chem., 20, 2357.
Ikeda, B.M., M.G. Bailey, C.F. Clarke and D.W. Shoesmith (1989). Atomic
Energy of Canada Limited Report, AECL-9568
Ikeda, B.M., M.G. Bailey, C.F. Clarke and D.W. Shoesmith (1990a). In:
Proceedings of the Workshop on Corrosion of Nuclear Fuel Waste Containers.
Atomic Energy of Canada Limited Report, AECL 10121, pp. 45-61. (Held Feb
9-10, 1988, Winnipeg, Canada.)
Ikeda, B.M., M.G. Bailey, M.J. Quinn and D.W. Shoesmith (1990b). In: Proc.
11th Int. Corr. Cong., Vol. 5, pp.5.371-5.378. Associazione Italiana di
Metallurgia, Milan, Italy. (Held April 2-6, 1990, Florence, Italy.)
Ikeda, B.M., M.G. Bailey, C D . Cann and D.W. Shoesmith (1990c). In: Proc.
Int. Cong, on Advances in Localized Corrosion (H.S. Isaacs Ed.), NACE 9.
In Press. NACE, Houston, Texas. (Held June 1-5 1987, Orlando, Florida.)
Iki, F. and S. Tsujikawa (1986). Tetsu to Hagane, 72(2), 292-299.
Imperial Metal Industries (Kynoch) Ltd. (1970). Titanium heat exchangers
for service in sea water brine and other natural aqueous environments. In:
Titanium Information Bulletin, IMI 5020/220.
King, F., M.G. Bailey, C.F. Clarke, B.M. Ikeda, C D . Litke and S.R. Ryan
(1989). Atomic Energy of Canada Limited Report, AECL-9890.
McKay, P. (1987). In: Proc. Conf. Corrosion Chemistry within Pits, Crevices
and Cracks, (A. Turnbull Ed.), pp. 107-128. Her Majesty's Stationery
Office, London. (Held Oct. 1-3, 1984, Teddington, England.)
McKay, P. and D.B. Mitton (1985). Corr., 41(1), 52-62.
Nabivanets, B.I. and L.N. Kuolvitskaya (1967). Russ. J. Inorg. Chem.,
12(6), 789.
Quinn, M.J., B.M. Ikeda and D.W. Shoesmith (1991). Image analysis techniques
for studying penetration of metals by crevice corrosion. Atomic Energy of
Canada Limited Report, In preparation.
Schutz, R.W. (1986). In: Process Industry Corrosion - The Theory and
Practice (B.J. Moniz and W.I. Pollock Eds.), pp. 503-527. NACE, Houston,
Texas.
Schutz, R.W. (1988). In: Proc. 6th Int. Conf. on Titanium. In press. (Held
June 1988, Cannes, France.)
WS8c2

EFFECTS OF DISSOLVED OXYGEN CONTENT ON

THE PROPAGATION OF LOCALIZED CORROSION OF CARBON STEEL
IN SYNTHETIC SEA WATER

N.Sasaki*,H.Ishikawa,*,T.Teshima*
and K.Fujiwara**
*Power Reactor and Nuclear Fuel Development Corp.
Muramatsu,Tokai-mura,Nakagun,Ibaraki,Japan 319-11
xxKobe Steel,Ltd.
2-3,lchome,Wakinohama-cho,Chuo-ku,Kobe,Japan 651

ABSTRACT
Effects of dissolved oxygen content on the propagation of localized corr-
osion of carbon steel have been investigated both by immersion type corr-
oion tests and electrochemical tests in synthetic sea water, which simu-
lated the ground water environment in deep geological formations. Altho-
ugh the propagation rates of localized corrosion were reduced with the
decrease of dissolved oxygen content, slight localized corrosion was
recognized even in deaerated condition by blowing pure N 2 gas.

KEYWORDS

Carbon Steel Synthetic Sea Water Localized Corrosion Dissolved Oxygen

Buffer Material Corrosion Potential Polarization Surface Film
Pitting Factor

INTRODUCTION

Vitrified high level radioactive wastes are planned to be isolated fina-

lly in deep geological formations, after packed in metallic containers.
Life over several hundred years is expected to the materials for the
containers and carbon steels, such as forged steel and cast iron, are
considered as primary candidate materials. The main life limiting factor
is considered to be corrosion through contact with ground water. Ground
water in deep geological formations is essentially strongly reducing, but
it is considered in the initial stage of isolation fairly oxidizing,
because oxygen enters during backfilling and is dissolved in the water.
Since the environments change gradually from oxidizing to reducing with
the progress of corrosion, it is required to comprehend the corrosion
behavior in the conditions ranging from oxidizing state to reducing state
in order to estimate the corrosion life of container material.

From the background mentioned above, we investigated the effects of diss-

olved oxygen content on the propagation of localized corrosion of carbon
steel,using immersion type corrosion testing and electrochemical techniq-
ues in synthetic sea water, which simulates the ground water in deep
geological formations, and tried to estimate the corrosion life.

627
628

EXPERIMENTAL METHODS
Test Materials
Commercial hot rolled steel sheet SM41B(JIS G3106)of 9mm thickness was
used throughout the experiments. The chemical composition is C:0.10, Si*.
0.22, Nn:1.01, P:0.014, S:0.003 in weight percent, and tensile properties
are yield strength:32kgf/mm 2 , ultimate tensile strength:44k§rf/mm 2 , elon-
gation:31%.
Immersion Type Corrosion Tests
As the immersion type corrosion tests, both simple immersion tests and
mixture immersion tests were performed. The former is the method to
immerse the coupon test specimens machined from the test material menti-
oned above for a fixed period, and the latter is the method to mount the
test specimens into the mixture of synthetic sea water and buffer materi-
al(bentonite). Both tests were carried out in vacuum desiccators with
internalvolume of 301. The details of corrosion test conditions are
summarized in Table 1.
Table 1. Summary of immersion type corrosion
test conditions
Items Simple Immersion Test Mixture Immersion Test

Test Material Carbon Steel(SM41B) Carbon Steel(SM41B) 1

Test Specimen Coupon Specimen Coupon Specimen

(60X120X5mm) (60X120X5mm)

Number of 15 for each condition 15 for each condition

Test Specimen

Test Vessel Vacuum Desiccator Vacuum Desiccator

Test Solution Syn.Sea Water Syn.Sea Water

(ASTM D-1141-52)
(ASTM D-1141-52) +
Buffer Material
(Weight Ratio=l:l)

Buffer Material None Na Type Fine Bentonite

Dissolved •Pure N 2 Gas •Pure N 2 Gas

Oxygen Content
r S •(7%0 2 +N 2 )Mixed Gas •Air
Atmosphere of
Gas Phase of ♦Air
Test Vessel
^ j

Test Temperature 80°C 80 °C

Test Duration 0.5,1,2,3,6 Month 0.5,1,2,3,6 Month

Evaluation •External Appearance •External Appearance

•Weight Change •Weight Change
•Penetration Depth •Penetration Depth
•Analysis of Corrosion ♦Analysis of Corrosion
Products Products
 629

Electrochemical Tests
As the electrochemical tests, time variation of corrosion potential and
both anodic and cathodic polarization curves were measured using heat-
proof glass flasks. Test electrode of 2 0 X 4 0 X 5 m m was machined from the
test material and silicon regin was coated except the measuring area of
l O X l O m m . The measurements were performed both by simple immersion and
mixture immersion methods mentioned above. The ratio of syn. sea water
to buffer material was taken as 8:1 due to the limitation of electroche-
mical measurements.
EXPERIMENTAL RESULTS
Simple Immersion Tests
Effects of dissolved oxygen content on the time variation of weight loss
and maximum penetration depth in simple immersion tests, are shown in
Fig.l.
2340 I
SIMPLE IMMERSION TEST SIMPLE IMMERSION TEST
1000 —o- : Pure N2 Blowing 2000 h — 0 - : Pure N2 Blowing
- * - : 7%02*93%N2 Blowing — · - : 7%θ2+93β/.Ν2 Blowing
900 —x- : Air Blowing 1800 - —x—: Air Blowing

800 4.1600

~ 700 f 1400
E 2
"^600 S 1200

§500 |I000
_i
£400
1
£

1 600
800
L
* 300 2 400
/
-\LLr^ |
200 200
x
100 Ω Λ t \ ^ \
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Immersion Time (Month) Immersion Time (Month)

Fig. 1. Time variation of weight loss and

maximum penetration depth in simple
immersion tests.
Weight loss is the difference between the weight before immersion and the
weight after descaling by cathodic electrolysis. And maximum penetration
depth is the maximum depth of localized corrosion among the 12 points
measured by dial depth gauge from the surface before immersion. Average,
maximum and minimum values of 15 test specimens for each test condition
are indicated in Fig.l.
The results of simple immersion tests are summarized as follows together
with the results of X-ray diffraction of corrosion products.
(l)In the pure N 2 gas blowing conditions with little dissolved oxygen
content, the corrosion mode was basically uniform corrosion, and the
corrosion rate was very little sufficiently to endue the life over seve-
ral hundred years and decreased until 2 months' immersion. However, the
corrosion rate increased after 3 months' immersion. This increase of
corrosion rate is caused by the pitting-like localized corrosion, which
was different from the localized corrosion caused in oxygen containing
environments mentioned below. According to the X-ray diffraction of
corrosion products, M g 6 F e C 0 3 ( O H ) i 6 * 4 H 2 0 film at the initial stage of
immersion and F e 3 0 4 film was formed after that.
(2)In the (7%0 2 +93%N 2 ) mixed gas blowing condition corresponding to the
dissolved oxygen content of about 1 ppm, corrosion mode was initially
uniform corrosion, localized corrosion began to propagate after 1 month
immersion and propagated rapidly after 3 months' immersion. According to
the results of X-ray diffraction of corrosion products, M g 6 F e C 0 3 ( O H ) i 6 ·
4H 2 0 film at the initial stage of immersion and F e 3 0 4 film was formed
630
after that.
(3)In the air blowing condition corresponding to the dissolved oxygen
content of about 3 ppm, the corrosion mode was localized corrosion from
the initial stage of immersion. Since the corrosion rate is fairly large,
the lasting of the rate would make the life over several hundred years
impossible. Both weight loss and maximum penetration depth tended to
propagate rapidly 3 months' immersion. According to the X-ray diffrac-
tion of corrosion products, thick F e 3 0 4 film was formed from the initial
stage of immersion.

Mixture Immersion Tests

Effects of dissolved oxygen content on the time variation of weight loss
and max imum penetration depth in mixture immersion tests, are shown in
Fig. 2.
1 MIXTURE IMMERSION T E S T , MIXTURE IMMERSION TEST
—0—: Pure N2 Blowing
L—°— : Pure N2 Blowing —x—: Air Blowing
Γ—x— : Air Blowing
1600
i\\
/\ | 1400
1
1 \
\\ 1

E 200C+ \\ £ 1200 / /\\ \\

1 >
Γ /
\ 3 // \ \
\
//Λ\\
c 1000

// > \ \\
\\ \ I 800
/// \\\
\ \ \ \\
c
£ lOOOl· ^ & 600 - /// \\\
/ / ^ \N E y
// \\ \
E 400 - f // \\ \
A
// // \ ^ \\ \\
- / ]J -»
1 * ~ " " "^ ; / ^ \ \
σ
/// \ \Yv\ V
^ϊ
Έ
200
L*^^»^»—«i—~»—-■—a 1
1 2 3 4 5
Immersion Time (Month)
0
IzL·^^,
c) 1 2 3 4 5
Immer sion Time (Month )
6

Fig.2. Time variation of weight loss and

maximum penetration depth in mixture
immersion tests.

The results of mixture immersion tests are summarized as follows together

with the results of X-ray diffraction of corrosion products.
(l)In the pure N 2 gas blowing conditions, the corrosion mode was basical-
ly uniform corrosion, and the corrosion rate decreased with immersion
time until 3 months' immersion, but tended to increase after 6 months'
immersion. This is due to the initiation of pitting-like localized corr-
osion after 6 months'immersion. According to the X-ray diffraction of
corrosion products, F e C 0 3 film at the initial stage of immersion and
thick F e 3 0 4 film was formed after that.
(2)In the air blowing conditions, the corrosion mode was uniform corrosi-
on until 0.5 month immersion and changed to localized corrosion after 1
month immersion. The corrosion rates after 1 month immersion is larger
than those of simple immersion and this indicates that localized corrosi-
on in mixture immersion is severer than in simple immersion. The curious
phenomena that both weight loss and maximum penetration depth decreased
rapidly after 6 months' immersion is due to the fact that the corrosion
tests were conducted using different vessels for each test duration, and
it suggests the contact condition between the test specimen and the
mixture affects remarkable effects on corrosion. According to the X-ray
diffraction of corrosion products, F e C 0 3 film after 0.5 and 6 months'
immersion and F e 3 0 4 film in other test durations were formed.

Electrochemical Tests
The time variations of corrosion potential of carbon steel with various
0 2 content in blowing gas from 0 to 100%, were measured.
The corrosion potential during simple immersion with very low 0 2 content,
 631
failed at first, then began to rise after 3 days' immersion and s t a b i l i z -
ed finally at about -700mVvs SCE. Such behavior was not observed during
simple immersion with high 0 2 content and mixture immersion. The rela-
tionship between the corrosion potential after stabilized and the 0 2
content in blowing gas is illustrated as Fig.3.

: Simple Immersion Test

: Mixture Immersion Test

Ö -600
en
>
1
~ -700
υ
LÜ

-800

0 07 7 20 100
Oxygen Content in Blowing Gas(Vol.%)

Fig.3. Relationship between the corrosion

potential after stabilized and the
0 2 content in blowing gas
Effects of immersion time on anodic polarization curve in N 2 gas blowing
condition are summariezed briefly as follows. Anodic polarization curve
rose steeply from corrosion potential irrespective of existence of buffer
material, but coexistence of buffer material tended to lessen anodic
polarization. Although the corrosion potential shifted toward noble
direction and vibration of anodic current w a s observed after several
days'immersion in simple immersion, such behavior was not observed in
mixture immersion.
Effects of 0 2 content in blowing gas on cathodic polarization immediately
after immersion are summarized briefly as follows. When 0 2 is contained
in blowing gas,limiting current of 0 2 diffusion was observed both in
simple immersion and mixture immersion. In pure N 2 gas blowing condition,
on the other hand,Tafel line with gradient of about 140mV/Decade was
observed in simple immersion, and this indicates the corrosion process is
rate-controled by hydrogen discharge reaction.
DISCUSSION

In the case of container material for high level radioactive wastes,

corrosion life over several hundred years is required. The estimation of
corrosion life is relatively easy if the corrosion mode is uniform corro-
sion, but accurate evaluation for the propagation rate of localized
corrosion is important because the corrosion mode of carbon steel is
basically localized corrosion accompaning general corrosion as mentioned
above. In the following paragraphs pitting factor in the "oxidizing
period" (oxygen existing period in the e n v i r o n m e n t ) and pitting phenomena
in "non-oxidizing period" (oxygen free period in the e n v i r o n m e n t ) will
be discussed.

Pitting Factor in Oxidizing Period

The relationship between the weight loss and the maximum penetration
depth is plotted for each test specimen tested under oxygen containing
conditions as shown in F i g . 4 .
632

Average Penetration Depth (/im)

50 100 150 200
E Syn. Sea Water
80°C
2000 Simple Immersion &
Mixture Immersion

1000

500 1000 1500 2000

Weight Loss (g/m 2 )

Fig.4. Relationship between the average

penetration depth and the maximum
penetration depth under oxygen
containing conditions.

Although the data in Fig.4. contain some scattering, the maximum penetra-
tion depth of localized corrosion can be estimated at most 10 times of
average penetration depth calculated from the weight loss, irrespective
of amounts of dissolved oxygen content, test period, existence of buffer
material, etc. In other words,the maximum pitting factor is estimated as
about 10.

Since the oxygen dissolved in ground water reacts with iron according to
the following equation, the corrosion loss of iron due to the oxygen
brought into by buffer material during backfilling, can easily be calcu-
lated.
2Fe+02+2H20-*2Fe(0H)2

According to NAGRA report the corrosion loss of iron due to oxygen is 32

kg for each container under the appropriate assumptions of disposal
conditions and backfills, and it c o r r e s p o n d s to the average penetration
depth less than 0.7mm for the surface a r e a ( 6 m 2 ) of a container. Similar
results of calculation have been reported by Westinghouse corporation.
Therefore, the maximum penetration depth of localized corrosion during
oxidizing period could be estimated to be fairly small, considering the
pitting factor discussed above.

Pitting Phenomena in Non-oxidizing Period

It was confirmed from this study that the corrosion mode changed from
localized corrosion to uniform corrosion and the corrosion rate reduced
extremely with the decrease of dissolved oxygen content. However, slight
pitting-like localized corrosion was observed after immersion of a fixed
time even under pure N 2 gas blowing conditions.

The mechanism and propagation rate of the pitting-like localized corrosi-

on caused under non-oxidizing conditions will be studied more in detail
in near future. From the results of this study, however, it might be
caused by the localized destruction of protective surface film formed
under non-oxidizing condition.
 WS8c3

DEVELOPMENT OF OPS83-BASED DIAGNOSTIC

EXPERT SYSTEM FOR SCC IN STAINLESS STEEL

K. Komai*, K. Minoshima* and M. Koyama**

* Department of Mechanical Engineering, Kyoto University,

Yoshidahonmachi, Sakyoku, Kyoto 606, Japan
** Mechanical Engineering Laboratory, Hitachi Ltd., Kandatsu,
Ibaragi 300, Japan

ABSTRACT

The 0PS83 based diagnostic expert system dealing with SCC damage analysis
of stainless steels have been developed and the expert system was proved to
be a powerful and affective tool. Certainty factors were a good parameters
to express unreliability and contribution of environmental, material, and
stress condition factors to cause SCC damage.

KEYWORDS

Artificial intelligence; expert system; SCC; austenitic stainless steel

INTRODUCTION

Damage of machinery and structure is caused by various closely related fac-

tors, including materials, environments, and stress conditions. Con-
sequently expertise and heuristic knowledge have been required for diag-
nosis of damage in a given material/environment system as well as for
structure maintenance and its control management (Task Group Activity,
1978, 1987b; Kowaka, 1983). If the system which can evaluate the pos-
sibility of damage is developed with the aide of knowledge technology, non-
expert can even know the possibility of damage through replying to the in-
quiry of the system. Fukuda (1985b, 1987a) developed the expert system for
maintenance of corrosion in oil tanks. The expert system which handles
with failure analyses has been also reported (Fjelheim et al. , 1988),
though the detailed specifications including diagnostic accuracy has not
yet been made clear.

In this investigation, we have developed the expert system which diagnoses

the possibility if damage of stress corrosion cracking (SCC) of austenitic
stainless steels occurs or not, and we have discussed a potential of the
expert system in the domain of SCC failure analyses.

SYSTEM ENVIRONMENT
633
634

Select envitonment:
Chloride solution or
high temperature water

Enter conditions of environment,

loading, materials STEP 1

Inference

Judge the proposition that SCC occurs

Enter fracture surface morphologies

if none
Inference
STEP 2

Judge the proposition

Conclusion

Fig. 1. Flow of a diagnosis adopted in the developed

system.

We have developed the expert system on an engineering workstation, HP9000

series model 350C (Hewlett Packard Corp.) equipped with a main CPU memory
of 8 MB and a harddisk of 150 MB. An operating system was HP-UNIX sup-
porting the processing of Japanese language, and the expert system thereby
handled input/output in Japanese. The system was built on the 0PS83
programming language (Forgy, 1985a).

DIAGNOSTIC EXPERT SYSTEM FOR SCC

Diagnostic Issues and the System Architecture

The system was designed to diagnose damage possibility, or sensitivity of

SCC of austenitic stainless steels (AISI 304 series) in high- or low-
concentration chloride solution and/or high-temperature, high-pressurized
water environments. Figure 1 shows the flow of the diagnosis involving two
steps; in the first step, it made pre-diagnosis of the damage possibility
of SCC based upon facts acquired with a system interview about environ-
ments, materials and stress conditions. At the end of this step, the sys-
tem reported the result of the pre-diagnosis of the damage possibility in-
duced by SCC. The report included the individual affecting factors and
their contributions to SCC. In the second step, the system made a post-
diagnosis by using fracture surface morphology, and the final conclusion
was deduced from the first and the second step diagnoses.

The system involved six program modules listed in Table 1. These modules
were compiled and linked, and we got the execution module. The module,
 635
Table 1. Program modules in the developed system.

Module Contents
sus. ops Initial setting up and start routines
susdef.ops Declare data type and define external functions
susq.ops Question module
susrules.ops Knowledge base
shell.ops Inference engine and debbuger
ailib.c Interface library

Table 2. Outlines of rule-based knowledge.

Rule name Contents

commonl Common rules to all environments
Knowledge of heat treatment, microstructure, surface
commonl3 finishing and pH of solution
mgcll Rules of SCC sensitivity in high concentration magnesium
chloride solution
mgcl23 Knowledge of heat treatment, MgCl2 concentration, dissolved
oxygen, chemical compositions, loading conditions, etc.
hhwl Rules of SCC sensitivity in low concentration chloride
solution and high temperature water
hhw68 Knowledge of interaction between chloride ion and dissolved
oxygen, heat treatments, cold working, chemical compositions,
loading conditions, etc.
fsl Rules of fracture surface analyses
Knowledge of fracture surface moprhologies (intergranular and/or
fs8 transgranular failures), fan-shaped pattern, etc.
others Rules of inference control, etc.

"shell.ops", in the inference engine was implemented in the standard 0PS83,

which we have re-written as it gave precedence to rating expressions.

Knowledge Base

The rule-based domain knowledge is listed in Table 2. It was classified

into two classes; rules which were fired to control reasoning processes
deriving subsequent facts with presently available facts, which are
referred to "others in Table 2; the other rules were the domain knowledge,
which affirmed or denied the proposition that "damage induced by SCC occurs
in a given materials/environment system". The latter rules had certainty
factors representing reliability (or contribution) in deriving consequents.
The certainty factor ranged -1 to +1. The certainty factor of 1 was the
absolute affirmation. From a decrease in certainty factor from +1 to zero,
reliability became lower, representing an "ambiguous" rule. A negative
(minus) certainty factor meant "negative" certainty; the factor of -1 was
the perfect negation.

The rule-based knowledge involved not only qualitative rules but also quan-
titative ones. For example, as for an interaction of chloride ion and dis-
solved oxygen on SCC, the boundary between SCC and no-SCC regions was for-
636

Properties that SCC occurs

Fire rule *-
I
Renew the certainty factor
I
Search other fulfilled rules
X if none
End of inference

Fig. 2. Flow of inference in the system.

mulated. The rules judged whether a system fell into a SCC or a no-SCC
region through contents of chloride ion and dissolved oxygen.

Inference Method

Figure 2 shows the flow of inference processes adopted in this system. The
system first set up the proposition that "SCC occurs in a given
material/environment system". The inference engine fired fulfilled rules
in a manner of a chain reaction. The system evaluated the damage pos-
sibility of SCC with the value of the finally obtained certainty factor of
the proposition. One of the most important issue in inference was how to
renew the certainty factor. A production system which made the inference
based upon unreliable knowledge sometimes had a "coupling relation", i.e.,
some rules affirmed the proposition and some denied. The system, then, was
required to have some "coupling function" to calculate the certainty fac-
tor.

Up to date there are some available method for this purpose. In our system
we installed the "modified" MYCIN method (Buchanan and Shortliffe, 1984),
which was one of the simplest method, and has been installed on many
general purpose expert system tools (shells). The modified point in our
method was that the affirmative certainty factor (CFP > 0) and the negative
factor (CFN < 0) of the proposition were respectively calculated during
reasoning, thereby giving a simpler method. After the system fired a rule
having a certainly factor, CF, the affirmative certainty factors (CFP' > 0)
or the negative one (CFN* < 0) was respectively calculated by the following
equations:
CFPf = CFP + CF - CFP'CF if CF > 0
and
CFN' = CFN' + CF - CFN-CF if CF < 0,
where the CFP and the CFN were the affirmative and negative certainty fac-
tors of the proposition before the rule was fired.

The system respectively renewed the affirmative and the negative certainty
factors, until there was no rule to be fired left. The final certainty
factor of the proposition was available by the addition of the finally ob-
tained affirmative and negative certainty factors. Table 3 shows diagnostic
messages displayed on a CRT according to the degrees of the certainty fac-
 637
Table 3. Diagnostic results of SCC case histories.

Certainty Number
Diagnostic message
facator of cases
1.0-0.6 probability of SCC: very high 17
0.6-0.2 probability of SCC: high 14
0.2-0 2
probability of SCC: medium
0-0.2 2
-0.2—0.6 probability of SCC: low 0
-0.6—1.0 probability of SCC: very low 0

Table 4. Diagnostic results of case histories, where some

improvement measures were taken after SCC damage.
After improvement, no SCC damage is reported for
these cases.

Case Diagnosis of case Diagnosis after

no. histories Improvement method improvement
(Certainty factor) (Certainty factor)
20014 Probability of SCC: Periodic removal of dust Probability of SCC:
very high (0.640) adhered to the inside of pipes low (-0.400)
40001 Probability of SCC: Water proof treatment of the Probability of SCC:
very high (0. 708) outside of pipes low (-0.228)
50012 Probability of SCC: Stress relief annealing in Probability of SCC:
high (0.505) heat-affected zone very low (-0.646)
60008 Probability of SCC: Rise of water level to Probability of SCC:
high (0.481) submerge pipe edges medium (-0.109)
70010 Probability of SCC: Dilution with ion exhanged Probability of SCC:
high (0.550) water low (-0.400)
B08 Probability of SCC: Solution treatment in Probability of SCC:
high (0.446) work-hardenend zone medium (-0.900)

tor of the proposition.

Tunin%-Up of Certainty Factors

The ideally best method to determine an individual certainty factor of each

rule is to be based upon some statistic facts or experts' heuristic
knowledge. In our system, however, we tentatively adopted the following
method as it would work in a well-trained manner; we selected five typical
case histories of SCC, one of which was the case, where SCC damage never
occurred, and we thereby tuned the certainty factors with trial and error,
until these five cases were well diagnosed. In the process of tuning up,
we had to notice that we should not set certainly factor too high, which
gave a too conservatively operating system. In order to avoid this, it was
worth selecting a sound case within case histories, and thereby we could
get appropriate certainty factors.

Validation of the System

We applied this developed expert system to 35 SCC case histories. Table 3

638
lists the results of diagnoses. For 33 cases of 94%, the system diagnosed
that the SCC probability was high or very high. This indicated that the
system diagnoses accurately.

We next examined how conservatively the system tended to diagnose SCC

damage probability; we selected some cases out of above mentioned cases
where SCC damage would no more occur after some improvement measures
against SCC having been taken. Table 4 summarizes the results. Though the
system worked somewhat conservatively, the diagnostic results for the all
cases showed the SCC damage probability less than zero, i.e., negative con-
clusion.

Although the developed system had the relatively small knowledge base con-
sisting of about 100 rules, it worked in an accurate manner. This meant,
an expert system which had even small knowledge base could be a powerful
and effective tool in damage analyses in an SCC environment, if the system
was designed to deal with limited domain issues.

CONCLUSIONS

1. An expert system can be a powerful and effective tool in SCC damage

analyses.
2. The expert system which has a small knowledge base of about 100 rules
can even work well, provided that it is designed to deal with limited
domain issues, like our developed system.
3. Certainty factors are good parameters to express unreliability and con
tribution of individual environmental, material, and stress condition
factors of a given material/environment system to cause SCC damage; the
reasoning method, in which the certainty factor of the proposition is
successively renewed with certainty factor of a fired rule, is suitable
for SCC damage diagnoses.

REFERENCES

Buchanan, B.G. and E.H. Shortliffe (1984). Rule-Based Expert Systems-The

MYCIN Experiments of the Standard Heuristic Programming Project. Addison-
Wesley.
Fjelheim, R.A., G. Coll and B. Johanson (1988). Expert Systems in Eng.,
372, Springer-Verlag.
Forgy, C.L. (1985a). 0PS83 User's Manual, Dept. of Computer Sei., Carnegie
Mellon Univ.
Fukuda, S. and T. Motooka (1985b). Trans. Japan Soc. Mech. Engrs., 51A,
1499.
Fukuda, S. (1987a). Trans. Japan Soc. Mech. Engrs., 53Α, 309.
Kowaka, M. (1983). Corrosion Damage and Protection Techniques of Metals.
AGUNE.
Task Group Activity (1978). Failure Analyses of SCC Case Histories.
Division of Corrosion Engineering, Japan Soc. Mat. Sei.
Task Group Activity (1987b). Case Histories of Corrosion Damage and
Analytical Techniques. Division of Corrosion Engineering, Japan Soc.
Mat. Sei.
 WS8C4

STRESS CORROSION CRACKING OF FERRITIC STEELS IN WATER

R.M. PEDRAZZOLI and M.O. SPEIDEL

Institute of Metallurgy, Swiss Federal Institute of Technology
CH-8092 Zurich, Switzerland

ABSTRACT

Ferritic high strength steels are in general susceptible to stress corrosion cracking when exposed to
water. The crack growth rates are primarily affected by the yield strength and the sulfur content as
well as the testing temperature.

KEYWORDS

Stress corrosion cracking, fracture mechanics testing technique, ferritic high strength steels,
environmentally-induced crack growth.

INTRODUCTION

High strength steels are well known to be susceptible to stress corrosion cracking when exposed to
aequeous environments. Numerous major failures in ferritic steel structures can undoubtedly be
attributed to this process.

Stress corrosion cracking consists of crack initiation and crack growth. The best method to measure
quantitatively stress corrosion crack growth is to apply fracture mechanics testing techniques.
Double cantilever beam specimens containing a fatigue precrack are stressed to a well defined stress
intensity and then exposed to the testing environment. The crack growth rate is determined by
dividing the crack elongation due to stress corrosion by the time it takes for the crack to grow
(Magdowski and Speidel, 1988). Such observed crack growth rates are plotted as a function of the
applied stress intensity. These curves are the basis for any quantitative comparison of stress
corrosion properties of different materials.

This paper presents stress corrosion crack growth data of several ferritic steels exposed to pure
water. The effect of the yield strength and the sulfur concentration as well as other influential
parameters are presented and discussed.
639
640
CARBON AND LOW ALLOY STEELS FOR STRUCTURAL APPLICATIONS

The designation and chemical composition of a number of structural steels investigated are given in
Table I. An important point to note there is the sulfur content of steels ETG 88 and ETG 100. These
steels had been resulfurized, ending up with a sulfur concentration twenty to thirty times higher
than that of the other steels in Table I. This extremely high sulfur content gives rise to a very high
stress corrosion susceptibility. This is indicated in Fig. 1, where the crack growth curves of the steels
listed in Table I are shown. The crack growth rates of the high sulfur steels lie far above those of
the low sulfur steels with similar yield strength. Aside from this strong sulfur effect, Fig. 1 gives a
first indication of the important role of the yield strength: in general, the higher the yield
strength, the faster grow stress corrosion cracks.

Table I. Chemical composition of high strength carbon and

low alloy steels for structural applications.

designation compc>sition, weight-perce nt

C Si Mn Cr S
St 830/1030 0.66 0.98 1.70 - 0.015
St 110/135 0.29 0.98 0.64 2.4 0.011
C75 0.80 0.25 0.78 0.04 0.017
ETG 88 0.42 0.14 1.7 0.09 0.34
ETG 100 0.45 0.15 1.5 0.07 0.25

1 1 1 1 1
SCC of high strength carbon and low alloy steels
H 20, ambient temperature, aerated
n p 0 2[ M P a ]
R, Sulfur
• ETG 100 926 0.25
O ETG 88 733 0.34
D St110/135 1220 0.015
■ St830/1030 850 0.011
To Δ C75 940 0.017
<

*PJp~

10 20 30 40 50 60
stress intensity, K,, [MPaVm]

Fig. 1. Stress corrosion crack growth curves of high strength

carbon and low alloy steels for structural applications.
 641
CARBON AND LOW ALLOY STEELS FOR SPRINGS

Spring steels are in most cases high strength quench and temper carbon and low alloy steels. The
chemical composition of a number of typical steels of this group are listed in Table II. Stress
corrosion crack growth curves of these spring steels have been measured. Fig. 2 shows an example of
the experimental results: Steel DIN 55Si7 was heat treated to various yield strength levels and
then exposed to water. The obtained stress corrosion crack growth curves (Fig. 2) clearly indicate
that with increasing tempering temperature and thus decreasing yield strength the steel becomes
less susceptible to stress corrosion cracking. This is expressed by both lower crack growth rates and
higher threshold values K i s c c · This behavior is typical for the majority of all spring steels
investigated.

Table II. Chemical composition of spring steels.

DIN com position, weight-percent

C Si Mn Cr Ni 1 Mo S
55Si7 0.57 1.8 0.89 0.03 - - 0.025
65Si7 0.60 1.62 0.77 0.07 - - 0.032
51CrMoV4 0.53 0.23 1.0 1.1 0.16 0.23 0.009
52SiCrNi5 0.54 1.6 0.75 0.82 0.56 - 0.003

1 1 1 1 1
SCC of spring steel DIN 55Si7 (UNS G92550)
H 2 0, ambient temperature, aerated
annealing temp. Rp0.2 ' M P a]
▲ 400°C 1490
• 450°C 1370
■ 500°C 1160
< ▼ 560°C 1030
Φ

S
O

1<T

U
20 40 60 80 100 120

stress intensity, K,, [MPaVm]

Fig. 2. Stress corrosion crack growth curves for spring steel

DIN 55Si7, heat treated to various yield strength levels.
642
ULTRA-HIGH STRENGTH STEELS

The class of ultra-high strength steels includes several distinctly different groups of steels,
including quench and temper steels as well as maraging steels and high strength stainless steels.
This paper concentrates on the quench and temper steels. Table III gives the chemical composition of
a number of steels tested, Fig. 3 illustrates their stress corrosion cracking behavior in water. It is
interesting to note that steel 4340 and 4340M exhibit very similar crack growth rates, even though
they differ in yield strength. On the other hand, steel D6AC exhibits a crack growth rate which is
three orders of magnitude lower than 4340 with similar yield strength. This observation can
possibly be attributed to the different sulfur content due to modern melting processes for D6AC and
the slightly different microstructure. Obviously, there exist ways to positively influence the stress
corrosion behavior of high strength steels, however, only to a certain extent. The enormous
differences in crack growth rates of ultra-high strength steels 4340 and D6AC (Fig. 3) are also
observed at other testing temperatures than room temperature. This is amplified in Fig. 4, where
the steels 4340, 4340M, and H 11 exhibit at all testing temperatures very high crack growth rates,
whereas the crack growth rates of D6AC are always several orders of magnitude lower. In any case,
however, higher temperatures cause higher stress corrosion crack growth rates.

Table III. Chemical composition of ultra-high strength steels.

com position, weight-pe rcent

designation C Si Mn Cr Ni Mo S
D6AC 0.47 0.19 0.83 1.06 0.5 1.0 0.004
4340 0.36 0.22 0.60 0.88 1.8 0.28 0.002
4340 M 0.41 1.8 0.73 0.86 1.9 0.47 0.011
H-ll 0.37-0.43 0.80-1.00 0.20-0.40 4.75-5.25 - 1.20-1.40 n.d.

SCC of ultrahigh strength steels

H 2 0 , ambient temperature, aerated

I L l # 4 3 4 0 ( U N S G43400) R 2==1 1480MPa

Γ I♦I Ij Δ
Δ4433440
0ΜΜ RR pn0 2=- 117 0 0 M P a "
^ ■ D 6 A C ( U N S K24728)R =l425MPa

20 40 60 80 100 120

stress intensity, Kh [MPaVrn]

Fig. 3. Stress corrosion crack growth curves of ultra-high strength

steels.
 643
test temperature, T, [°C]

80 60 40 23 4
1—i—ι—ι 1 I
(0 SCC of ultrahigh strength steels in H 20
i D H-11
O 4340
(UNS T20811) R 0 2 = 1590MPa
(UNS G43400) Rp0'2 = 1340MPa
tj io" l·-
- · 4340 (UNS G43400) R 0 2 = 1480MPa-J
j ▲ 4340M (UNS K44220) R 0 2 = 1700MPa
■ D6AC (UNS K24728) Rp0 2 = 1425MPa |

£ io h
l·

l·

■
l·
\ i
w
-a
8
£ io

reciprocal temperature, 1/T, [ 1 / K ] - 1 0 3

Fig. 4. Effect of temperature on the growth rate of stress corrosion cracks.

EFFECT OF YIELD STRENGTH AND SULFUR CONCENTRATION

In general, the yield strength has an important influence on the stress corrosion crack growth rate of
ferritic steels. This is demonstrated in Fig. 1 to 4, and specifically in Fig. 5, where the plateau crack
growth rates of a number of different steels, including those discussed above, are plotted as a
function of the yield strength. The overall trend is clear: the higher the yield strength, the faster
grow stress corrosion cracks. There are, however, other influential parameters which affect the
crack growth rate aside from the yield strength. A possibly decisive role has been attributed to the
element sulfur in the steel. In Fig. 6 the stress corrosion crack growth rates of a number of low alloy
steels with different sulfur contents are plotted as a function of the sulfur concentration in the steel.
It is obvious from this figure as well as from Fig. 1 that the crack growth rate increases with
increasing sulfur content.

CONCLUDING REMARKS

An extensive experimental investigation on stress corrosion cracking of steels in water has been
performed, some results of which are presented here. These data are the basis for a quantitative
prediction of the stress corrosion behavior of specific ferritic steels in water. Moreover, a
comprehensive knowledge of influential parameters is necessary in order to develop and evaluate a
fundamental understanding of stress corrosion cracking.

REFERENCES

Magdowski R.M. and Speidel M.O. (1988). Clean steels for steam turbine rotors- their stress
corrosion cracking resistance. Metall. Trans.. 19A, 1583-1596.
644

stress corrosion cracking of steels in water

ambient temperature

• X2NiCoMo1895
*▲ X3NiMoTi1932
55Si7

• 62SiMnCr4
65Si7
■ 29CrSi104
♦
♦ 2NiSiCrMoV
T 21CrMoV511

»j X90CrMoV18
X210Cr12
Δ X38CrMoV51
Φ 23CrNiMo747
• X155CrMoV121
O X20CrMoV121
Δ 80MnSi31
V 47CrMoNiV410
D 26NiCrMoV127
0 66MnSi74

600 800 1000 1200 1400 1600 1800 2000 2200 2400 2600 2800 3000

yield strength, R p 0 2 , [MPa]

Fig. 5. Effect of yield strength on the stress corrosion crack growth

rates in ferritic steels.

stress corrosion cracking of ferritic steels

in water, ambient temperature

• R»o a- 1220 MPa

650*850 MPa

0.00 0.01 0.02 0.03 0.04 0.05 0.06

sulfur content, [weight/percent]

Fig. 6. Stress corrosion crack growth rates as a function of the

sulfur content.
 WS8d1

RECENT STUDIES ON STRESS CORROSION CRACKING IN JAPAN

K.Yamakawa and H.Inoue

Department of Metallurgical Engineering, College of Engineering,
University of Osaka Prefecture
4-804, Mozu-Umemachi, Sakai, Osaka, 591 Japan

ABSTRACT

Recently, there have been many reports on the behavior of stress corrosion
cracking (SCC) in Japan. In these studies, the failure time or the crack
growth rate were measured under a constant stress or strain using the smooth
or precracked specimen in different environments, especially in high
temperature water. This report does not treat the SCC behavior itself but
the static and dynamic characteristics of passive film related to SCC.

KEYWORDS

Stress corrosion cracking, passive film, double layer structure, scratching

method, rapid straining method, fluctuation of corrosion potential.

STATIC CHARACTERISTICS OF PASSIVE FILM

Double layer structure of passive film

The chemical composition of passive film which formed in various

environments was analyzed with EPMA, SIMS, ESCA and/or AES. The results are
summarized in Fig.l. Except for the films formed in hydrochloric acid and in
high temperature water, it is noticed that the passive film takes the double
layer structure in any other environments.

Si-0 Ni-S Ni-0

Fe-Ni-0 Cr-0 Cr-0 Cr-0 Cr-0
substrate substrate substrate substrate substrate

(a) (b) (c) (d) (e)

Fig.l Summary of chemical compositions of passive films

formed in various solutions, (a) hydrochlonic acid, (b)
dilute chloride solution and high temperature water, (c)
nitric acid, (d) sulfide solution and hydroxide solution

645
646

Hydrochloric acid and chloride environments

The film formed in hydrochloric acid solution contained only ferric and
nickel oxides and was non-protective. On the other hand, it was observed
that the film contained mainly chromic oxide in dilute chloride solution
(Masamura et al., 1988). Addition of molybdenum compound in the solution,
however, led to the decrease in the chromium content in the film (Tsuge e_t
al., 1985). This is in conflict with the enhancement of the resistance to
localized corrosion by the addition of molybdenum compound. The authors had
discussed it from the viewpoint of the crystallization of passive film
without molybdenum compound, although the experimental evidence has not yet
been done.

Concentrated nitric acid solution

The addition of a few percent silicon to stainless steel promoted the

formation of Si-0 film on the chromium oxide film, as shown in Fig.2, and
hence the corrosion resistance was significantly improved in a concentrated
nitric acid solution (Oukubo et al., 1986). This improvement of the
resistance must be caused by the control of not anodic but cathodic
reaction. However, the role of Si-0 film in corrosion is not clear yet.

wU=zl(l=SI.O.Cr.Nl.Fe.N)/rxlOO 33 O O/G
7.l = ( l \ l l . ( c p l ) / S e n s l t l v l t y ) « A t o i l c weight ' Corrosion-resistan
t region
S e n s i t i v i t y Ke: 1.15 S i : 0.52
Cr: 1.3 0: 0.6
Nl: 1.15 N: 0.4 • · 3 fo O/D D
777777 π/77Λ Ρ MarklTnicltnes
s Composition

General corrosion 40.06

Ni ω *Ά /Π • 0.06-v.o.5
>0.5
Cr oxide

a JO.06 Ni sulfide
o a 0.06% 0.5
u >0.S Cr oxide
Cr ^
SI I
0 S 10 «5 30 25 30 IS
N I
Etching time (Hin) Fig. 3 Effect of Ni and Cr contents
on the composition and thickness
Fig.2 ESCA analysis of the passive film of passive film formed on alloy
formed on HCr-18Ni-6Si stainless steel containing 3-3.5% Mo (20% NaCl,
in 98% nitric acid (60°C). lOatm H2S, 200°C, 8hr)

Sulfide solution (Murayama et al., 1984)

In order to secure against corrosion in sulfide solution, it is necessary to

be more than 25% Ni as well as more than 25% Cr in alloys, as depicted in
Fig.3. Figure 4 shows that nickel contributes to form Ni-S film on the
chromium oxide, although why the addition of molybdenum enhances the
corrosion resistance could not be explained from the analysis of the
composition of passive film. Molybdenum is not concentrated in the film
and/or the interface between the film and the substrate.
 647

Alloy A 75XN1-OXO 25XF>

oC
N1 m0

• Cr
■ m|

t » M tm

Sputtering time (s)

Alloy C : 75XNi-15XCr-10Xf
>

N1-(Cr)-0

1. i
Matrix \

Cr-(N1)-(Fe)-
0

400
Sputtering time/s Sputtering time (s)

Alloy : 60tNi-30XCr-lOTF
e

N1-(Cr)-0

rixx
Matri \

Sputtering time (s)

Fig.4 SIMS analysis of the passive film Fig.5 SIMS analysis of the passive
of 40%Ni-3.5%Mo based alloy. (20% NaCl, film formed on 75% Ni based alloy
lOatm H2S, 200°C, 48hr) at potential of Ε Ο Ο Γ Γ +100 mV.
(a) 15% Cr, (b) 20% Cr and (c) 25% Cr (4% NaOH, 280°C)

High temperature water and hydroxide solution

Also in hydroxide solution, the double layer structure of Ni-(Cr)-0 and Cr-
(Ni)-O was confirmed, as shown in Fig.5. Furthermore, Fig.6 shows that the
increase in the nickel content resulted in the enrichment of chromium in the
inner layer. That fact may be important, because the composition of the
inner layer which seems to decide the corrosion resistance is affected by
that of the outer layer (Yamanaka et al., 1989).

Alloy E : 60XNt-15!Cr-ZSXF
t Alloy C : 75XN1-15XCr-IOIF
e Alloy J : 84INI- ISICr-lXF«

kr*-^-^
i^Z^t?. ...7^**"
^
Sputurin? tlac ( i)
^.

Ni content In alloy ( B U S S *)

Fig.6 Effect of Ni content in 15% Cr based alloy on Cr

content in inner layer. (4% NaOH, 280°C, Ecorr- +100mV)
648

In the high temperature water environment, only one layer which consisted
mainly of chromium oxide was found. Its thickness, composition and crystal
structure were ascertained to be affected by the environmental conditions.
As the solution is more acidic and has lower DO, the thickness and the
chromium content in the layer become thinner and more enriched, respectively
(Sakai et al., 1989). The film structure depends upon the electrochemical
potential, as shown in Fig.7. In the transpassive potential range where
intergranular SCC occurs, the film contains the fine platelet oxide of
corundum structure (M203) in the platelet spinel (M 3 0 4 ), although only the
polyhydric oxide of spinel exists in the film in the passive potential range
(Hirayama etal., 1985).

10° ASUS304
OHT80
Δ'
□ SM50B / 03Hz

<
~E 10·'

__rc / '-) 0.3 Hz

|o 2
1 " ,; Fe
J , 50Hz
-„ Δ ΐ 0 Η ζ
0.3 Hz
I
o TOHz
^ V Cr \ 10Hz
io-3 ,a
s (so s | s«c 1 0 20 40 50 80 100
\pel,ht<ln ploliltt ploflit
Corrosion r a t e on s l i p plane (X)

Potential. E . V (SHE)
Fig.8 Relationship between accel-
eration ratio of crack growth
Fig.7 Electron diffraction measurement rate to that in air and corrosion
of passive film formed on sensitized rate on slip plane. (3%NaCl,25°C)
304 stainless steel in high purity Δ 304 stainless steel
water at 290°C. O low alloy steel (HT 80)
Π carbon steel

In the high temperature water containing impurities, the passive film

usually takes double layer structure. For example, when the reducible sulfur
compound like CaS 2 0 3 was added in pure water, the enriched S layer was
observed to form on the chromium oxide layer (Sakai et al., 1989).

Role of double layer structure of passive film

in localized corrosion and SCC

As described above, the passive film was found to take the double layers
structure. However, the role of each layer in localized corrosion and SCC is
not clear yet. The corrosion resistance is estimated to depend upon the
inner layer composed mainly of chromium oxide. In a next stage of the
research, the structure and the properties of chromium oxide (degree of
crystallization, type of crystal, grain size, chemical composition,
thickness, electrical conductivity, etc.) must be made clear in relation to
corrosion resistance.
Chromium oxide is stable only in the pH range of 4 to 15 and in the narrow
potential range near 1.2 volts. However, stainless steel can be used even
more acidic or alkaline or oxidized environment except for the above
conditions. Therefore, the outer layer may play a protective role in the
attack against the chromium oxide layer. In order to elucidate the
phenomenon, the ionic conductivity and selectivity of the outer layer must
be studied besides the different properties of the chromium oxide.
 649

DYNAMIC CHARACTERISTICS OF PASSIVE FILM

Scratching method

It was assumed that the anodic current at the slip plane produced around
crack tip during fatigue crack growth corresponds to the dissolution current
of bare surface appeared by scratching method. With the assumptions that the
formation rate of slip plane and the disappearance rate are constant by
loading and by unloading, respectively, the anodic electricity for one cycle
was estimated from the experimental evidence of exponential decay in anodic
current by scratching method (Masuda et al., 1985). Figure 8 shows the
relationship between the acceleration ratio of crack growth rate to that in
air and the corrosion rate of slip plane. There was found to be good
correlation between the crack growth rate and the corrosion rate of bare
surface, independent of the kinds of steels.

Rapid straining method

The repassivation behaviors of several metals and a stainless steel were

studied using the rapid straining method. As shown in Fig.9, the
repassivation current is not greatly affected by the content of alloy
elements. Also, the repassivation rate of precracked specimen was found to
have good relation with the crack growth rate of stainless steel in high
temperature water.

Time/ s

Fig.9 Decay of anodic current of Fe-Cr-Ni alloy by rapid

straining lethod in borate buffer solution.
(150°C, -0.05 V vs. SHE)

Measurement of fluctuation of corrosion potential (Inoue et al.)

The fluctuation of corrosion potential was found to reflect the initiation

and growth of crack, as shown in Fig.10. With the initiation of crack (stage
A), the potential fluctuation of triangle shape whose amplitude is about
1 mV is recognized and the small wave of high frequency which may relates to
the formation of coarse slip in the crack is overlapped. The shape of
potential fluctuation changed in the smooth triangle with the growth of
crack (stages C, D ) . Such fluctuation was not observed without loading.
650

"Time ( 1 h/dlv.)
-i 1 r~

Potential (mV)
-330.43

Time ( 1 4 h/dlv.)

Time ( 1 h/dlv.)

Fig.10 Corrosion potential fluctuation of sensitized 304

stainless steel immersed in 25°C, MgCl2. (80°C, 25kgf/mra2)

CONCLUSIONS

The recent studies on static and dynamic characteristics of passive film was
arranged to relate to SCC and localized corrosion. In the near future, it is
desirable to make clear the break down and repassivation behavior of passive
film in more details.

REFERENCES

Hirayama.H, Y.Yamashina, S.Nakamura, T.Kawakubo and M.Hishida (1985).

Boshoku Gijutsu (Corr. Eng.), 34, 86-91.
Inoue.H and K.Yamakawa, private communication.
Masamura.K, T.Nishimura (1988). Boshoku Gijutsu (Corr. Eng.), 37, 546-552.
Masuda.H, S.Matsuda, S.Nishijima and M.Shimodaira (1985). ibid, 33, 27-34.
Murayama.J, H.Miyuki, T.Kudo, N.Fujino and F.Terasaki (1984). TMS-AIME paper
selection, A84-45.
Oukubo.K (1986). 13t Corrosion Seminar, Hakone, Japan Soc.Corr.Eng., 71.
Sakai.T, S.Okabayashi, K.Aoki, K.Matsumoto, F.Nakayasu and Y.Kishi (1989).
4th Intern. Sympo. on Environmental Degradation of Materials in Nuclear
Power Systems-Water Reactors, NFK-ES-5122, Jekyll Island, GA.
Sakai.T, S.Okabayashi, K.Aoki, F.Nakayasu and Y.Kishi (1989). 4th Intern.
Sympo. on Environmental degradation of Materials in Nuclear Power Systems-
Water Reactors, NFK-ES-5123, Jekyll Island, GA.
Shibata.T and S.Fujimoto (1987). Trans. Japan Inst Metals, 28, 424-433.
Tsuge.H, N.Usuki, H.Nagano (1985). Boshoku Gijutsu (Corr Eng.), 34, 99-106.
Yamanaka.K J.Murayama (1989). J. Japan Inst. Metals, 53, 550-557.
 WS8d3

DETERMINATION OF INITIATION AND CRITERIA JTSCC OF

STRESS CORROSION CRACK OF LCW STRENGTH STEEL WELDED JOINT

Z.X. Chen, X.-D. Pan-, P.L. Fan, J.M Dong, G.Q. Zhou

Department of Mechanical Engineering, Xi'an Jiaotong University

Xi'an, China

ABSTRACT

The stress corrosion crack initiation of low strength steel welded joint
was measured by using the load point displacement on precracked cantilever
bend specimens. The criteria J of different regions of welded joint
ISCC
was determined by J . - t. curves. The results show that the moment at
which the load point displacement starts increasing is proved being the
crack initiation point. The maximum J is located in the weld metal
and the fine grain region. J of the base metal is higher than that
ISCC
of the bond, and that of the mixed grain region is lowest in comparison
with the former. Obviously, the resistance to stress corrosion cracking
in different regions of welded joint is quite inhomogeneous and the mixed
grain region is a most link in welded joint.

KEYWORDS
stress corrosion cracking(SCC); welded joint; crack initiation point;
incubation period of crack initiation; J .- t. curves; criterion J
Ii l ISCC
INTRODUCTION
The conception J-integral of elastic-plastic fracture mechanics is employed
extensively for investigating the ability of resistance to stress corrosion
cracking(sec) bring forward the critical value J to be use as a new
ISCC
criterion for assessing the resistance of low strength material to SCC
and leads the futher use of the cantilever bend technique. This technique
has a series of advantages that make it possible to exert a larger
displacement by the application of a small load, yet the use for measuring
J value of welded joint is not reported as known to us. We have
ISCC
measured the J value of low strength steel welded joint by means of
ISCC
the initial J-integral value J . versus the time to fracture t and achieved
a satisfactory first success.

The initiation of stress corrosion crack(SC-crack) is determined by

measuring the load point displacement at the cantilever beam, the critical
value J in different regions of welded joint obtaining by J . - t, curves
ISCC Ii l
is studied in this paper.
651
652
EXPERIMENTAL

The boiler steel with tensile strength 480 MPa was used as base metal (BM)
in the present work. The dimension of the precracked cantilever bend
sprcimens(CBS) for SCC test was L=200 mm, W=24 mm, B=20 mm according to
ASTM 813-81. The multipass welded joints were U-grooved and welded by
basic low hydrogen type covered electrode with ultimate tensile strength
no less than 500 MPa. All of specimens were as-welded. The crack plane
was in L-T orientation. The crack length was a o =12 mm including 2 mm
fatigue crack. The precrack located at different regions of welded joint
i.e., centre of the weld, the bond, the fine grain region and -the mixed
grain region of heat affected zone and the unaffected zone of BM.

60% Ca(NC) ) + 3% NH „NC> was used as the test solution at the temperature
o o3 2 4 3
105 C(±5 C ) , experimental period 150 hrs, which was changed every 24 hrs.
A load was applied to the specimen via cantiever beam when the desired
temperature was reached.

The initiation and extension of crack was monitored as follows through

the larger displacement of the load point on the cantilever beam. At first,
calibrated the specimens with different crack length a c on the cantilever
bend(CB) machine to set up the P- Λ curves, i.e., the load versus the load
point displacement. Established a series of a - A curves by the relation
between the given crack length (a) and the corresponding load P. on P - Δ
curve. After the load was applied in process of SCC test, plotted the
Δ -t curve by measuring and recording the load point displacement with
a dial indicator attached the end of beam. Assuming that the crack length
and the load point displacement were same in air and in corrodent solution,
the a-t curve might be obtained through the a-Δ and Δ-t curves and
hereform, the crack initiation and extension at a given crack length of
the specimen under a certain load would be extracted. For the onset of
SC-crack initiation under a certain load through the calibrated Ρ-Δ curve,
the initial J-integral value was given by

2
2 M ψ
j = (U-U + >
Ii o . 2
B(W-a) B E' E

where
U,UQ= strain energy of specimens with and without crack at the same load
P. respectively,
M = bending moment of applied to the crack plane, a
ψ - geometry-dependent factor is equal to 12.73C1—(1- ) ] for CBS,
W
2
E'= E/(l-t) ) , E is elastic modulus and Poisson's ratio l^=o.33.

By the method above-mentioned, the J .—t. curves indicating the relationship

Ii l
between initial J-integral value and time to initiation t. was established.

RESULTS
Determination of The Initiation Point
The measured Δ (a)-t curves tested in mixed nitrate solution(MNS) by using
the load point displacement on precracked CBS are shown in Fig.l. As can be
seen, the SCC process may be divided in two stages as the time increases,
i.e., the crack initiation stage and the crack extension stage. In the
first stage regime the load point displacement A keeps constant until the
precrack starts to extend. Therefore, that moment, at which the displacement
Δ. is turning increasing, it may be regarded as the SC-crack initiation
 653

Fig. 1. Δ ( a ) - t curves of CBS of BM in MNS

under P.= 201.5 N.

a) b) c)
Fig. 2. Appearance of SC-crack initiation on fractured
surface of CBS of BM tested in MNS;
Corresponding Points A, B, C, in Fig.l.

point and the duration before which as the time to initiation t. of the
SC-crack.

This was confirmed by the following experiment. Took down the specimen
at Point A as soon as the displacement vary at the very onset and broken
off it after cooled in liquied nitrogen for 5 minutes. A number of small
SC-spots in front of the fatigue precrack on the fractured surface of the
specimen was observed (Fig. 2, a ) . For the sake of contrast, the fractured
surface of the specimens at Point B on the left and at Point C on the right
near by Point A were examined. Any variation in front of the precrack
does not exist the specimen at Point B, the SC-crack initiation there
occured not yet at that time (Fig.2 b ) . But the SC-crack extension starts
to occured on the fractured surface of the specimen at Point c(Fig. 2 , c ) ,
which wae shown that SC-crack extension has came into existence. It follows
from the fractured surface that the Point A, where the displacement vary
starts up, is precisely the SC-crack initiation point.

The J-integral value J . versus time to initiation t. curves of different

regions of welded joint tested in MNS by the CBS are shown in Fig. 3.
Obviously, these curves are similar in shape or form to the J-integral value
J . versus time to fracture t curves that we have obtained under otherwise
identical conditions. The corresponding critical value J , which the
SC-crack initiation there will not be occured, are summarized in Table. As
will be readily seen, the susceptibility at different regions of welded
joint to SCC evaluated by the criteria J varies in similar regularity.
I SCC
Make a comparison between the two, only the former in J value is lower
than the latter. It shows that the maximum J is located in the weld
ISCC
654

• Weld metal
obond
Δ fir» grain region
»mixed grain region
A base metal

Fig 3. J . versus t. curves of different regions of

Ii l
welded joint tested in MNS by using CBS.

Table Critical value J _ of different regions of

ISCC
welded joint obtained by J .-t. and J .-t_ curves
Ii l Ii f
ISCC N/mm
Regions Weld metal Bond Fine grain Mixed grain Base metal

by curves J -t. 5.77 2.94 5.76 1.01 4.17

by curves J .-t 8.65 3.46 7.24 2.25 5.06

metal and the fine grain region. J of the base metal is higher than
that of bond, and that of the mixed grain region is lowest in comparison
with the former. Obviously, the resistance to SCC of different regions of
welded joint is quite inhomogeneous and the mixed grain region is a most
link in welded joint.

DISCUSSION
Comparison of Criteria, t. and t
The feasibility using the critical value of J-integral as criteria of the
resistance of elastic-plastic materials to cracking has been proved by
experiment. The crack initiation point is usually used as the critcal
point in measuring J and is determined by the technique such as acoustic
emission, metallographic, electric potential and resistance etc. However,
none of them may be quite satisfied in use due to the complexity of the
device, external interference or the data scatter etc. These shortcomings
are conspicuous especially in the case of corrosive solutions.

In view of that J , as characteristic parameter of the elastic-plastic

materials may be provided as a criterion of the resistance of a cracked
body to crack extension in corrosive environments and is usually determined
by fracture of specimen as critical point, it seems not have to seek for
the crack initiation point. Yet the test of SCC for low strength steels in
MNS and particularly in caustic solution is a very slow and time consuming
process. Though the accelerated test method by strengthening the
environmental condition or the method by inferring the long-term result
from data obtained in short duration test is significance to be investigated,
but some problem in this respect remain to be solved. A easy way
determining the SC-crack initiation in the process of J n „ n measurement
* ISCC
 655
as the critical point is therefore undoutedly worthful to accelerating
the SCC test.

It is believed that the effect of the time to initiation t. is decison

on SCC process rather than that of the time to fracture t . The measurement
of time to initiation t. using the load point displacement is not only
simple and accurate but test period may be significantly shortened.

Incubation Period Prior to The SC-crack Initiation

The incubation period prior the SC-crack initiation (Kaesche 1979) is
defined as the difference between the time to fracture and time to
propagation (t -t ) . This indicates that there will be some "crack soure"
to be formed during such period. The fatigue precrack on the specimen
of the material which is originally unsusceptible to SCC plays a pole
of crack source and makes the incubation period disappear, so that the
material seems to be susceptible and then an excessively severe estimation
may be often concluded. In other words, there exist fatigue precrack is
certain to eliminates the incubation of SCC.

The fact is that the incubation period of the SC-crack in CB test comes
from the blunting of the crack tip under stress is due to plastic
deformation. Meantime, the SC-crack is proved by SEM analysis on the
fracture surface extended along the grain boundary but not along the
cleavage plane in front of the fatigue precrack. Thus, it is certain that
the precracked is not to be extended soon after applied load, so that there
exist a incubation period prior to the precrack extension and the Δ value
appeared as constant at longer the time t..

The initiation of SC-crack is a process of blunting and the formation and

rupture of the oxide film at the crack tip so the incubation period must
be under the influence of the applied load. At high load or J . value,
the crack tip is severely blunting which hinder the initiation of the crack.
In the meanwhile, the high stress causes the rupture of oxide film and
promotes the crack initiation. At low load or J , value, the oxide film
will be not easily ruptured due to small deformation of the plastic zone,
though the crack tip is blunting slightly. The J .-t. curves in Fig. 3
shows that the incubation period increases with the decreases of J . value.
Therefore, it may be deemed that the effect of load on rupture of oxide
film is still stronger than that on the blunting of the crack tip.

As indicated in the result that the incubation period is also influenced

by the microstructure of the welded joint as well as corrosive corrodent
and the yield strength of the material. The higher the J value at
I SCC
a certain region of the welded joint, the longer its incubation period
possesses. Contrarily, the region with lower J value has shorter
ISCC
incubation period and will be cracked preferentially.

To sum up, the incubation period prior to the crack initiation relates
to the applied load and the nicrostructure of the welded joint. As results
show that we have obtained, the SC-crack growth rate da/dt in the stable
subcritical propagation stage of the different regions of welded joint
is basically identical and the reason why these regions differ to each
other time to fracture t is distinctly that the latter is controlled to
a great extent by the incubation period. This results in difference of
the resistance to SCC of the different regions of welded joint. The way
making the weak region strengthened is to increase its J value and
ISCC
so to have the incubation period elongated. This is one of the main ways
for increasing the life of low strength steel welded joint in corrosive
656
environment.

CONCLUSIONS
1. The point or moment at which the load point displacement starts
increasing is proved being the SC-crack initiation point, whose confirmed
by fractured surface of the CBS. The SCC process is mainly decided by
the time to initiation t., but not by the time to fracture t . The
determination of t. is undoubtedly a way worthly to be investigated for
the development of accelerated test method.

2. There is an incubation period prior to the SC-crack initiation which

depends on the applied load and the microstructure of welded joint. The
t is controlled by incubation period t., increasing which is a main way
for increasing the service life of welded joint in corrosive environment.

3. The J .- t. curves of different regions of welded joint obtained by

measuring the load point displacement are similar in shape or form to the
J ,- t curves obtained under otherwise identical conditions. The
corresponding critical value J for both curves J - t. and J - t
in different regions of welded joint varied in similar regularity. The
maximum J is located at the weld metal and the fine grain region.
J of the base metal is higher than that of the bond. The resistance
ISCC
of different regions of welded joint to SCC is quite inhomogeneous and
the mixed grain region is a most link in welded joint.

REFERENCES
BROWN B.F. (1965). A Study of the stress factor in corrosion cracking by use
of the precracked cantilever beam specimen.Corrosion Soc., 5, 745-750.
Chen,Z.X., G.Q.Zhou et al(1987a). Stress corrosion cracking of welded joint
in caustic and nitrate solutions. Proc. 10th Conf.on metallic Corrosion.
Chen,ZoXo, G.P.Zhou et al(1987b). Subcritical propagation of SC-crack of
welded joints in caustic and nitrate solutions. Proc. 10th ICMC.
Chen,Z.X, G.Q.Zhou(1987c). Studies on stress corrosion cracking of low
carbon steel welded joints. Neue Entwichlungen and Anwendungen in der
Schweisstechnik-Vortrag der 1. Deutsh-Chinesischen Konferenx in Beijing.
Greenfield,P.(1971). Method of assessment. In: Stress Corrosion Failure,
Mills S. Boon Limited, Lodon, pp. 13-20.
Karpenko,G.V. & I.I.Vasilenko(1977). InrStress Corrosion Cracking of Steels,
Switzerland, pp.78-95.
Kaesche,H.(1979). Stress corrosion cracking, In:Die Korrosion der Meatlle,
Chap. 15. Berlin.
 WS8d4

The Behavior of Single Crystal Ta and W and Polycrystalline Nb-xTa Alloys in

Liquid U During Tensile Testing at 1473 K.

J. S. Huang and G. F. Gallegos

Lawrence Livermore National Laboratory

P.O. Box 808, Livermore, CA 94550, USA

ABSTRACT

The effects of exposure to liquid uranium on the tensile behavior of single crystal refractory
metals Ta, W and polycrystalline Nb-xTa binary alloys are evaluated with tensile testing at 1473
K. The results show that single crystal Ta and W are not embrittled by liquid U, while it is
known that polycrystalline Ta and W are readily embrittled by liquid U. For the Nb-xTa binary
alloys, the embrittlement occurs in alloys which have more than 60 wt% Ta. Cross sectional
metallographic and SEM examination of the tested samples indicate that the embrittlement in
these Nb-xTa alloys is caused by the wetting of liquid U along grain boundaries. Based on the
present single crystal test results and the previously observed effect of strain-rate on the
embrittlement in polycrystalline Ta, it is suggested that the embrittlement in polycrystalline Ta
and W is not a classical LME which is attributed to adsoption-induced reduction of interatomic
bond strength.

KEYWORDS

Liquid metal embrittlement; intergranular embrittlement; liquid metal wetting; stress corrosion
cracking; classical LME.

INTRODUCTION

The effect of exposure to liquid U on the tensile behavior of group VB and VIB refractory
metals Ta, W, Nb and V have been studied previously by the authors (Huang et al., 1989 and
1990). These studies showed polycrystalline Ta and W are embrittled due to the wetting by
liquid U along grain boundaries, whereas polycrystalline Nb and V are not wetted by liquid U
along grain boundaries and are not embrittled. The susceptibility of Ta and W to liquid U
intergranular penetration and embrittlement are possibly related to a special phase diagram
behavior in which the mutual solubilities between the solid and liquid elements near the melting
point of uranium, 1408 K, are very small as shown by the example of the Ta-U phase diagram
in Fig.l. In contrast Nb and U atoms in the Nb-U system, and V and U atoms in the V-U
systems are much more mutually soluble near the melting point of uranium. (The Nb-U system
almost forms an ideal solution near 1408 K, and the V-U system has an eutectic reaction at about
4 wt% of V and at 1313 K.) It should be noted that the low solubility and type of phase
behavior for the Ta-U and W-U is most commonly associated with liquid metal embrittlement
(LME) in the literature (Rostoker, W, et al.), although it is not always a sufficient condition.
657
658
For example, the authors recently studied the tensile behavior of Nb and V in liquid Pu at 1273
K. Although the phase diagrams of Nb-Pu and V-Pu are similar and the mutual solubilities
between Nb and Pu and between V and Pu are the same, Nb is embrittled by Pu while V is not.
This discrepancy prompts us to further study the tensile behavior of Nb, Ta and W in liquid U.
An obvious question is whether the the different tensile behavior in liquid U between Nb and Ta
could be caused by the difference in grain boundary chemistry in the commercially available high
purity (greater than 99.9 wt%) Nb and Ta. A second question is whether single crystal Ta and
W are embrittled by liquid U, for which the mechanism is usually attributed to adsoption-
induced reduction of interatomic bond strength (Stoloff et ah, 1963, and Westwood et ai,
1963), usually called classical LME. The objectives of this work are: (1) to investigate the
tensile behavior of Nb-xTa binary alloys with x range from 20 wt% to 90 wt%. Using a same
procedure to prepare these alloys, the grain boundary chemistry should essentially be the same
and should not be a factor contributing to the difference in the susceptibility of liquid U
embrittlement; and (2) to investigate the possibility of single crystal Ta and W being embrittled
by liquid U.

3300

2900

2500

O
g 2100
2 (Ta)
5
a)
E 1700

1300

900
760 °C

500 J I I I I I I I L
0 10 20 30 40 50 60 70 80 90 100
Atomic Percent Uranium

Fig. 1 Phase diagram of Ta-U system.

EXPERIMENTAL DETAILS
The Ta and W single crystals studied were greater than 99.9 wt% pure and are oriented with the
[111] direction being along the longitudinal axis of the tensile samples. The Nb-xTa alloys (the
content of Ta ranges from 20 to 90 wt%) were prepared by arc melting followed with electron
beam remelting. The ingots were swaged to 10 mm diameter rods and then machined into
tensile bars with a round cross section. The tensile bars were annealed at 1573 K for one hour
in vacuum before tensile testing. Chemical analyses indicated that these alloys have typical
impurities as follows: O: 50 ppm, C: 40 ppm, N: 20 ppm. The U used in the testing was
greater than 98.5 wt% pure and mostly of 238 U isotope.
Tensile testing was conducted using an electromechanical Instron universal testing machine with
a specially designed Brew vacuum furnace attached to the testing machine. The load was
 659

monitored using a load cell and the cross-head movement was monitored with a linear variable-
differential transformer. The engineering stress reported was calculated as the load divided by
the original cross section of the samples; the engineering strain was calculated as the cross-head
travel divided by the original gauge length; and the reported strain rate was calculated as the
corss-head travel speed divided by the original gauge length of the samples. Although the
reported strain and strain rate are not accurate, it should be noted that for each test in liquid U, a
parallel test was also conducted in vacuum to determine the effect of liquid U. For most
materials studied, the cross-head travel speed used for the tensile testing was 8.5xl0"3 mm-s"1.
Additional cross-head speeds between 8.5xl0" 4 and 8.5xl0 _ 1 mm-s' 1 were also used to
examine the effect of strain rate on the tensile behavior of single crystal Ta and W. It should be
noted that the strain rates are only approximate since the strain rate actually varies with time with
testing at a constant cross-head travel speed.

In order to expose a tensile bar to liquid U, a cylindrical thick bottom Ta crucible was utilized.
The bottom of the crucible was threaded on both sides, with the outside being attached to a pull
rod which was attached to the load frame. The inside thread was to connect the tensile bar.
Prior to usage the Ta crucible was oxidized to prevent wetting of the liquid U on the crucible.
The vacuum in the chamber was -lxlO" 3 Pa at the test temperature (1473 K) and -lxlO" 5 Pa at
room temperature. After tensile testing, the longitudinal cross-section (parallel to the tensile
axis) of the test sample was prepared and examined using conventional optical metallography or
scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS) x-ray, and in some
cases wavelength-dispersive spectroscopy (WDS) microanalysis.

EXPERIMENTAL RESULTS

Behavior of Single Crystal Ta and W

The behavior of single crystal Ta and W in liquid U at different strain rates are shown in
Figures. 2a and 2b. All the samples have large total elongation to failure and fail with a mode of
necking to a sharp line. The necking indicates that only two slip systems are operative and that
the samples are ductile. This result is in contrast to the previous results (Huang et al., 1990) that
polycrystalline Ta and W are embrittled by liquid U with the total elongation to failure being
about 1 and 3%, respectively. Examination of the longitudinal cross sections of the tested
samples tested in liquid U indicates that small surface cracks have developed, as shown in Fig.
3. The formation of these cracks are assisted by the presence of liquid U and are seemingly
oriented along the direction of the slip bands.

Behavior of Nb-xTa alloys

The results of tensile testing of Nb-xTa alloys at 1473 K and at strain rate of 3.0 x 10-4 s_1 are
presented in Figs. 4a and 4b, in which the ultimate tensile strength (UTS) and the total
elongation to failure are plotted versus the content of Ta. The tensile data for pure Nb and Ta
from previous results (Huang et al, 1989) are also included here for comparison. The ultimate
tensile strength in vacuum reaches a maximum at about 50 ~ 60 wt%Ta due to the effect of solid
solution strengthening. The total elongation to failure and ultimate tensile strength are reduced
by the exposure of liquid U when the content of Ta is above 60 wt%. A larger content of Ta
corresponded to a greater reduction in UTS and less total elongation to failure due to liquid U.
All the samples which were tested in vacuum and absense of U fail with the cross section
necking to a sharp tip. For testing in liquid U, the samples with 0, 20, 40, and 60 wt%Ta fail
by necking to sharp tips, while the samples with 80, 90 and 100 wt%Ta fail with little necking.
It can be concluded that Ta-riched alloys are more susceptible to liquid U embrittlement than the
Nb-riched alloys. Fig. 5 shows a SEM micrograph of the longitudinal cross section of the
tested Nb-80wt%Ta sample. Note that liquid U penetrates along the grain boundaries of this
specimen and is responsible for the embrittlement and loss of ductility. This failure mechanism
660
is the same as the one observed in pure Ta previous studied (Huang et al., 1989). A similar
result was also obtained for a tensile specimen of the Nb-90wt%Ta.

DISCUSSION
The impurities and amounts of each in the Nb-xTa alloy are similar since they are prepared from
the same heats of unalloyed materials with the same procedure. The results shows a distinctive
transition from ductile behavior to brittle behavior when the content of Ta increases. The
transition occurs between 60 and 80 wt% Ta. These results suggest that the difference between
polycrystalline Nb and Ta in the susceptibility to liquid U grain boundary wetting and
embrittlement is not caused by the difference in grain boundary impurities, but rather by some
inherent difference between Nb and Ta in their interactions with U. This difference is also
reflected in the difference between Nb-U and Ta-U phase diagrams. However it should be
noted that phase diagram does not always provide a successful guideline to predict the
susceptibility of liquid metal embrittlement. As mentioned in the introduction, the different
tensile behavior in liquid Pu between Nb and V is an example. Therefore explaining the
embrittlement of Group VB metals by liquid U and Pu will require a more fundamental
approach.
The current results clearly indicate that single crystal Ta and W are not embrittled by the
exposure to liquid U. The adsoption of liquid U atoms onto Ta and W apparently is not enough
to embrittle the materials. Although cracks are initiated on the surface, the amount of decohesion
is not sufficient enough to allow the cracks to propagate. Therefore we believe the mechanism
of embrittlement in polycrystalline Ta and W is not be a classical LME. In the previous work
(Huang et al, 1990), we have seen evidence of grain boundary dissolution from the fracture
surfaces of Ta samples tested in liquid U. We also showed that increasing strain rate reduced
the severeness of embrittlement of Ta by liquid U. It follows that, when the strain rate of testing
is increased, there is less time available for dissolution of the grain boundary to occur. If the
embrittlement were indeed a classical LME, then we would not expect a strain-rate effect as long
as there is a sufficient supply of U atoms at the crack tip, which is the case for our study.
Therefore, based on the present results obtained for single crystals and the previous results of
strain-rate effect, we suggest that the mechanism of the embrittlement in the polycrystalline Ta
and W is a type of stress corrosion cracking and not a classical LME.
Although the adsorption-induced reduction in interatomic strength may not be the dominant
mechanism responsible for the embrittlement in polycrystalline Ta, the interatomic bond strength
in Ta is definitely reduced to some degree, since crack initiation is facilitated by liquid U as
shown in Fig. 3. These cracks are not propagating because the stress intensity at the crack tip is
not high enough. If one were to pre-crack a single crystal sample with sufficiently large crack
length, the sample may embrittle, i. e., the crack may propagate, since the stress at a crack tip is
intensified when the crack length is increased.

REFERENCES
Huang, J.S., G.F. Gallegos, M.P. Stratman, and E. Sedillo (1989). Deformation and Failure
Mechanisms of Niobium and Tantalum During Tensile Testing in Uranium at 1473 K.
Scripta Metallurgies Vol. 23, pp. 103-108.
Huang, J.S., and G.F, Gallegos. Embrittlement by Liquid U in Some Group VB and VIB
Metals and alloys during Tensile Loading at 1473 K. Metallurgical Transactions A, Vol
21A, July 1990, pp 1959-1967.
Stoloff, N.S., and T.L. Johnston (1963). Crack Propagation in a Liquid Metal Environment.
Acta. Metall, Vol. 11, pp 251-56.
Westwood, A.R.C., and M.H. Kamdar (1963). Concerning Liquid Metal Embrittlement,
particularly of Zinc Monocrystals by Mercury. Phil. Mag., Vol. 8, pp. 787-804.
Rostoker, W., J.M. McCaughey, and H. Markus. In Embrittlement by Liquid Metals, Reinhold
Publishing Corp., New York, NY, 1960, pp. 30-31.
 661

60 120

Engineering strain Engineering strain

Fig. 2 Engineering stress-strain behavior of single crystal Ta (a) and W

(b) in liquid U at 1473 K and at different strain rates

Fig. 3 Typical Back-scattered-electron SEM micrograph of the longitudinal cross

section of single crystal W tensile-tested in liquid U at 1473 K and at strain rate of
0.01 s_1. Note that small cracks developed along the slip bands. (This behavior is
also observed in the tested single crystal Ta specimens.)
662

100
Nb-Ta alloys

in vacuum

in uranium

0 20 40 60 80 100 120 0 20 40 60 80 100 120

Content of Ta, wt% Content of Ta, wt%

Fig. 4 Ultimate tensile strength (a) and total elongation to failure (b) for
the Nb-xTa alloys tensile-tested in vacuum and in liquid U at
1473 K at a strain rate of 3*10"4 /sec.

Fig. 5 SEM micrograph of the longitudinal cross section of the Nb-80

wt% Ta alloy tensile-tested in liquid U at 1473 K and at strain rate
of 3 x 10"4 per second. Note the penetration of U along the grain
boundaries of this specimen.
 WS8d5

ON THE BEHAVIOUR OF INTERGRANULAR STRESS-CORROSION-CRACKING

IN [110]-TILT COPPER BICRYSTALS

T.MIMAKIt, M.YAMASHITAtt, S.HASHIMOTO!tt and S.MIURAttt

t Department of Mechanical Engineering, Faculty of

Engineering, Doshisha University, Kyoto-602 JAPAN
tt Department of Mechanical Engineering, Faculty of
Engineering, Doshisha University, Kyoto-602 JAPAN :
Now at Iron and Steel Research Laboratories,
Research and Development Division,
Sumitomo Metal Industries, LTD., Amagasaki-660 JAPAN
ttt Department of Engineering Science, Faculty of Engineering,
Kyoto University, Kyoto-606 JAPAN

ABSTRACT

The behaviour of Stress-Corrosion-Cracking (SCC) in copper bicrystals with

symmetrical [110]-tilt boundaries in a solution of IN NaN0 2 at 303+2K is
investigated. It is suggested that the susceptibility of low-angle boundary to SCC
is lower than that of high-angle one, whereas no apparent difference in the
susceptibility is observed amongst high-angle boundaries. It is found that the
behaviour of crack propagation along the grain boundary is dependent upon its
advancing direction. This may be caused by the difference in the geometrical
correlation between the crack advancing direction and the active slip plane.

KEYWORDS

Stress-Corrosion-Cracking (SCC); Pure copper; Single crystal; Bicrystal;

Coincidence-Site Lattice (CSL); Symmetrical [110]-tilt boundary.

INTRODUCTION

In the previous decade, it has been accomplished to develop a useful understanding

of transgranular Stress-Corrosion-Cracking (SCC) in pure copper through a few
single-crystal studies. Sieradzki et ai. (1984) have pointed out that the cracking
proceeds by discontinuous cleavage. Meletis and Hochman (1984) have considered
that the transgranular cracks in single crystals with different orientations are
due to the reduction of surface energy followed by mechanical fracture along the
lowest surface energy plane. In addition, it has been observed by Uchida et ai.
(1989) that the cracks preferentially propagate along a {110} plane. However,
there has been few experimental evidence useful for discussing the intergranular
SCC in copper (Mimaki et ai., 1990). The purpose of the present investigation is
to obtain preliminary information available for understanding the intergranular SCC
in high-purity copper employing orientation-controlled bicrystals with symmetrical
[110]-tilt boundaries.

EXPERIMENTAL PROCEDURES

Material used is 99.999% purity copper. Bicrystals with symmetrical [110]-tilt

boundaries were grown from seed crystals using the Bridgman method in a vacuum of

663
664
lXlO"3 Pa. Crystallographic orientations of the grown bicrystals were determined
within the accuracy of better than 0.2° using an automated analysis system of
back-reflection X-ray Laue patterns with a microcomputer (Itoh et ai., 1985;
Hashimoto et ai., 1985). By taking account of Brandon's geometrical criterion
(Brandon, 1966) for deviation angles from the ideal Coincidence-Site Lattice (CSL)
orientation relations, Δ Θ, these boundaries were regarded as the CSL boundaries.
The crystal lographic characteristics of each specimen are shown in Table 1, where
misorientation is the rotation angle about the rotation axis nearest the ideal tilt
axis, disorientation is the minimum rotation angle and its axis pair (Grimmer,
1973) and Σ is the reciprocal density of the CSL points.

Table 1. Crystallographic characteristics of specimens tested.

Disorientation Deviation Grain

Misorientation Rotation Rotation Σ-value angle boundary
/ deg. angle/deg. axis Δ θ/deg. plane
0.0 0.00 1.000 1.000 1.000 1 0.00 {110}*
10.5 10.77 0.714 0.660 0.235 1 10.77 {110}
35.3 35.26 0.710 0.704 0.021 9 3.76 {221}
51.7 51.68 0. 709 0. 704 0. 033 11 2.04 {332}
70.2 59.69 0.582 0.576 0.575 3 0.43 {111}
95.6 60.31 0.661 0.655 0.367 17b 2.63 {223}
142.7 37.32 0.719 0.695 0.010 9 1.78 {114}
* Single crystal

The grain boundaries of specimens employed were oriented perpendicular to the

tensile axis. The cross-section and the gauge length of the specimens were
controlled to be 3.0X1.5 mm 2 and 8.0 mm, respectively. All of the specimen
surfaces (3.0X8.0 mm 2 ) were normal to the tilt axis. A penetrating slit 0.5mm in
diameter was designed normal to the specimen surface along the grain boundary at
the centre of the specimen, in order to observe the propagation process of the
crack initiated from the centre of the specimen. The specimens were cyclically
annealed under vacuum and then were mechanically polished. Finally, a deformed
layer of specimen surface was removed by electro-polishing. Stress corrosion
cracking tests were carried out in a IN NaN0 2 solution at 303±2K using the Slow
Strain-Rate Technique (SSRT). Extension rate of 8.33Xl0~8m-s_1 was applied using a
constant extension rate machine.

RESULTS AND DISCUSSION

The relations between the applied load and elongation of the specimens are shown in
Fig. 1. The rate of increase in the load with increasing the elongation of specimen
depends on the misorientation and the maximum rate is observed in the 70.2°
bicrystal. This difference may be caused by that in the crystal lographic
orientation of the tensile axis, as will be discussed later. Stress corrosion
cracks were preferentially initiated at the centred slits approximately between 150
and 200 N and propagated along the grain boundaries in all the bicrystals with
high-angle boundaries, as shown in Fig.2. Finally, all of the high-angle
bicrystals were fractured at the grain boundaries, as shown in Fig. 3. Both
intergranular and intragranular cracks were observed at approximately 150N in the
bicrystal with the low-angle 10.5° boundary. The low-angle bicrystal was fractured
both intragranularly and intergranularly at the centre of the specimen. On the one
hand, in the single crystal specimen, 0°/Σ1{110}, the cracks were not found under
stresses lower than approximately 220N. The single crystal was fractured as a
result of the propagation of a macroscopic crack normal to the stress axis, which
was initiated at slip steps created in the side surface of the specimen. These
facts qualitatively suggest that the susceptibility of low-angle boundary to SCC is
 665

o.o 10 5 353

I 1
1.0 mm

I 1
1.0 mm

Elongation , Λ I

Fig. 1. The relations between the applied load, P, and

elongation, Al, of the specimens tested.

Fig. 2. Scanning electron micrographs of an intergranular

crack advancing in the direction of [114] observed
in the bicrystal with 35.3° boundary at 280N(a),
310N(b) and 320N(c).
666

Fig. 3. Intergranular fracture of the bicrystal with 35.3°

boundary.

lower than that of high-angle one and that the high-angle boundaries are more
susceptible to SCC than the grain interior. The maximum load achieved in a slow
strain-rate test has been usually used for evaluating the susceptibility to SCC.
The maximum load measured in the present experiment is indicated against the
misorientation in Fig.4. It is to be noted that the 70.2° bicrystal shows the
highest value amongst the bicrystal specimens. The 70.2° bicrystal is deformed by
triple slip from the early stage of deformation. Accordingly, the motion of

E 400 k
Q.

Ό
(0
o
E 200
3
E
x
(0
S
60 120 180

Misorientation , 0/deg.

Fig. 4. The relation between the maximum load achieved, P ma x,

and misorientation, 0.
 667
dislocation is frequently suppressed by the interaction between dislocations moving
on different slip planes in the grain interiors. Thus, the rate of increase in the
load with increasing the elongation of the 70.2° bicrystal is higher than those of
other specimens, as was shown in Fig. 1. It is considered that the higher rate of
increase in the load mainly causes the highest value of the maximum load amongst
the bicrystal specimens.
It was found that the behaviour of crack propagation is dependent upon its
advancing direction; i.e., the rate of crack propagation toward an orientation
along the grain boundary is higher than that in the opposite direction. Vehoff
et al. (1987) have suggested in intergranular SCC in Fe-Si bicrystals that the
shear stresses on the active slip planes in the immediate vicinity of the crack tip
are related to the angle between the direction of crack propagation and the slip
planes. Therefore, the magnitude of local stress concentration at the crack tip
depends on the crystallographic orientation of the crack advancing direction. As a
result, the susceptibility to intergranular SCC varies with the direction of crack
growth. The difference in the rate of crack propagation observed in the present
study is also most likely due to that in the magnitude of local stress concentration
at the crack tip depending on the geometrical correlation between the direction of
crack propagation and the active slip planes. Especially, the difference in the
propagation rate is much larger in the bicrystals with relatively lower
misorientations in comparison with those with the higher misorientations. Some
examples of the relations between the advanced length of crack and the applied load

E 1500
\

2C
O
2 1000
o
o

500

5
2 200 300 400

Load , P/N

Fig. 5. The relations between the advanced length of crack, a,

and applied load, P, in the bicrystals with 35.3° and
142.7° boundaries. The open and solid circles
represent the advanced length toward [Ϊ14] and [114]
along the 35.3° boundary, respectively. The open and
solid triangles correspond to the advanced length in
the directions of [221] and [221] along the 142.7°
boundary, respectively.

are shown in Fig. 5. It is interesting to note that the primary slip plane alters
between the misorientations lower and higher than 70.5°. One slip plane
perpendicular to the specimen surface, alone, is activated at the beginnings of the
plastic deformation in the bicrystals with misorientations lower than 70.5°, while
the bicrystals whose misorientations are higher than 70.5° possess two other
668
primary slip planes; thus, the geometrical correlation between the direction of
crack growth and the primary slip plane changes much at 70.5°. For instance, the
angles between the opposite crack advancing directions and the primary slip plane
in the 35.3° bicrystal are approximately 53° and 127°, respectively, whereas the
primary slip planes in the 142.7° bicrystal are almost parallel to the crack
advancing directions. It is considered that the difference in magnitude between
the localized stress fields at the tips of cracks advancing in the opposite
directions, which may arise from the difference in the geometrical correlation
between the crack advancing direction and the primary slip plane, is larger in the
bicrystals with misorientations lower than 70.5°.

ACKNOWLEDGMENTS
The authors gratefully acknowledge the financial supports of the Light Metal
Educational Foundation of Japan and the Ministry of Education, Science and Culture
of Japan, as a Grant-in-Aid.

REFERENCES
Brandon,D.G. (1966). The structure of high-angle grain boundaries. Acta Metall.,
14, 1479-1484.
Grimmer,H. (1973). Coincidence rotations for cubic lattices. Scripta Metall., 7,
1295-1300.
Hashimoto,S., 0. Itoh, H.Mukawa and S. Miura (1985).A new graphic representation of
grain boundary disorientation. J. Japan Inst. Metals, 49, 1016-1017.
Itoh, 0., S.Hashimoto and S.Miura (1985).Automated orientation analysis of
back-refleetion X-ray Laue patterns. J. Soc. Mater. Sei. Japan, 34, 1105-1109.
Meletis,E.I. and R. F. Hochman (1984).The crystallography of stress corrosion
cracking in face centered cubic single crystals. Corrs. Sei., 24, 843-862.
Mimaki,T., Y.Nakazawa, S.Hashimoto and S.Miura (1990).Stress corrosion cracking of
copper bicrystals with <110>-tilt Σ 3 , Σ 9 , and Σ11 coincident site lattice
boundaries. Metall. Trans., 21A, 2355-2361.
Sieradzki,K., R.L.Sabatini and R.C.Newman (1984).Stress-corrosion cracking of
copper single crystals. Metall. Trans., 15A, 1941-1946.
Uchida, H., S. Inoue, M.Koyama and K. Koterazawa (1989). Stress corrosion cracking of
pure copper single crystals in NaN02 solution. J. Soc. Mater. Sei. Japan, 38,
552-556.
Vehoff, H., H. Stenzel and P.Neumann (1987).Experiments on bicrystals concerning the
influence of localized slip on the nucleation and growth of intergranular stress
corrosion cracks. Z. Metallkde., 78, 550-556.
 WS8d6

Effect of Water Chemistry on The Thin Oxide Film of Alloy 600

in High Temperature Water Containing Lead

T.Sakai, K.Aoki, T.Shigemitsu and Y.Kishi

Engineering Service Div.
Nuclear Fuel Industries, Ltd.
950, Ohaza-Noda, Kumatori-Cho, Sennan-Gun,
Osaka τ590-04, JAPAN

ABSTRACT

Since lead may be one of the potential contributing causes of IGA/SCC that is found
in Alloy 600 steam generator tubing in PWR secondary systems, the effect of lead on the
tubing's thin film was investigated in this study. It was demonstrated that the presence of
lead in the oxide thin film enhanced the selective dissolution of nickel from Alloy 600 base
metal.

KEYWORDS : PWR, Steam Generator, Lead, Oxide Film, Corrosion

INTRODUCTION

Lead is one of the impurities in the secondary side system of PWR nuclear power
plants (1)(2). Laboratory testing has shown that lead may be a corrosive meterial for Alloy
600 steam generator tubing (3)(4), however, there is a little known about the actual
mechanism for lead-induced stress corroison.
The objective of the current study is to investigate the effect of water chemistry
with lead contaminant on the oxide thin film of Alloy 600 formed at high temperature. Since
the thin oxide film is an interface between an alloy and its environment, it is postulated
that the characteristics of the thin oxide film could be affected by the environment and
related to the corrosion process of the alloy in that environment. Therefore, the
information obtained from thin film studies seems to be a useful tool to evaluate the effect
of lead on the corrosion processes of Alloy 600 (5)(6).
In this sutdy, high temperature autoclave tests and the following oxide film
analysis with AES/ESCA were performed to investigate the characteristics of the film formed
in lead contaminated water. Also the test solution was analyzed.
It was demonstrated that the presence of soluble lead enhanced the selective
dissolution of nickel and also iron from Alloy 600 base metal.

EXPERIMENTAL

Two kinds of Alloy 600 test samples were used in the experiment. One is the mill-
annealed (MA) Alloy 600 steam generator tubing of 22.23mm O.D.Xl.27mm in thickness X50.0mm
in length, and the other is the solution-treated (ST) Alloy 600 capsule of 45mm O.D.XllOmm
in height (5mm wall thickness), which was machined from 50mm O.D. bar material. The chemical
compositions and heat treatments of specimens are shown in Table 1, while the test matrix is
shown in Table 2.
As for Alloy 600MA tube specimen, the surface of the specimen was polished by No.600
grit paper to remove any pre-existing oxidation and to delete the variation in surface
roughness among specimens. After ultrasonically cleaning in acetone, the specimens were set
up in the capsule. Capsules containing an Alloy 600 specimen and test solution of 50ml were
made of stainless steel (SUS 304 (45mm O.D.XllOmm in height, 5mm wall thickness)). The
inner surface of the capsules was coated with Teflon (PTFE) in order to prevent galvanic
corrosion between the capsule and the specimen. The capsules were also ultrasonically
cleaned in acetone. High purity argon degassing (>99.999% Ar) was used to attain low
dissolved oxygen (DO2) of less than 5 ppb. After DO2 levels of less than 5ppb were confirmed
with a digital DO2 meter (TDA Electronics Ltd. model DO-30A), the capsules containing the
specimens were sealed by TIG welding in a hood with an argon atmosphere. These capsules were
placed in an autoclave for one week at 280°C. After the high temperature exposure, the
specimens were removed from the capsules, rinsed with pure water and kept in a vacuum
desiccator. Finally, thin film analysis with Auger Electron Spectroscopy and ESCA was
conducted.
On the other hand, Alloy 600 ST capsule was especially used for the solution
analysis to investigate the concentration of metal ion dissolved from Alloy 600 capsule
inner wall. The capsule containing only test solution without tube specimen was kept in the
autoclave for one week at 280°C following the same procedure as mentioned above.
The test solution in the capsule after the autoclave testing was analyzed by Atomic
Absorption Spectroscopy and Inductively Coupled Plasma to measure the concentration of metal
ions dissolved from Alloy 600 capsule inner wall. As a reference, the test solution in the
SUS304 capsule of the former experiment was also analyzed.

669
670
RESULTS AND DISCUSSION

Thin film characteristics

In order to compare each thin film characteristics based on the depth profile of the
thin film, two parameters were used : Ni/(Ni+Cr+Fe) At% ratio and Cr/(Ni+Cr+Fe) At% ratio.
Although somewhat arbitrary, the film region is defined to be the area where Ni At% is less
than 60%, which represents most of the film region of Alloy 600.
The depth profiles of Ni/(Ni+Cr+Fe) At% ratio and Cr/(Ni+Cr+Fe) At% ratio of the
thin films are plotted in Fig. 1. The zero on the abscissa of these figures indicates the
boundary between the film and the base metal. Compared to those for non-lead environment, a
different appearance is observed in the plots of Ni/(Ni+Cr+Fe) At% ratio and Cr/(Ni+Cr+Fe)
At% ratio for lead-containing environment. That is, the relative nickel content is depleted
in the outer region in oxide film, while the relative chromium content is encriched there.
Figure 2 shows the average value of each of the above parameters in the film region
of Alloy 600 in various solution pH conditions with and without lead contaminants. Firstly,
in the case of the non-lead environment, we can see a general tendency for the relationship
between solution pH and relative concentration of nickel and chromium. That is, nickel is
depleted more in more acidic solutions in the neutral-acidic pH range, resulting in chromium
enrichment. This preferential depletion seems consistent with the thermodynamic stability of
Ni and Cr oxides based on the Pourbaix diagram applicable to the equilibrium condition (7).
This tendency is even stronger in the lead-containing environment, it is apparently being
enhanced by the presence of the lead. The outermost region of thin film (0<Ni<30 At%) shows
this tendency the clearest.
As shown in Fig. 3, the film thickness formed in lead containing solutions is
thinner than for the non-lead solutions.

Dissolved metal ion

Table 3 summarizes the results of solution analysis after autoclave testing. The
test solutions were analyzed by Atomic Absorption Spectroscopy and Inductively Coupled
Plasma to measure the concentrations of dissolved metal ions (Ni, Cr, Fe). In addition to
these major elements, the soluble lead concentration was also measured.
The results of solution analysis are as follows:

(1) Chromium ion concentration is less than the detection limit in every case,
confirming the stability of chromium and chromium-oxide in the test environments.
(2) Compared to the non-lead environment, nickel dissolves more in the lead-
containing environment, especially in acidic pH. A supersaturated lead condition
enhances the nickel dissolution at least at pH 3.
(3) Although not so much as nickel, iron is also dissolved more in more acidic test
solutions with higher soluble lead concentrations, as seen in Test No.Ill, IV and
V with use of Alloy 600 capsule.This tendency was concealed by the larger
contribution from SUS-304 capsule inner wall rather than Alloy 600 specimen in
the Test No. I and 11(8).

The soluble nickel and iron ion concentrations dissolved from Alloy 600 capsule
inner wall in Test No.Ill, IV and V are shown in Fig. 4. These results of solution analysis
suggest the selective dissolution of nickel and iron is caused by an electrochemical
reaction between nickel / iron and soluble lead. The decrease of soluble lead concentration
after autoclave testing and also the slight lead peak, detected over the film region during
thin film analysis by Auger Electron Spectroscopy, supports such an electrochemical
reaction. The chemical form of lead in the thin film analyzed by Electron Spectroscopy for
Chemical Analysis (ESCA. SHIMADZU Model ASIX-1000II) was predominantly lead oxide (PbO) in
the outermost region, while the mixture of lead oxide (PbO) and metal lead (Pb) was detected
in the middle region of the thin film (position of 30AT% Ni content).

CONCLUSION

1. The characteristics of oxide thin film of Alloy 600 formed in high-temperature lead-
contaminated water in various pH (mild acidic / neutral) conditions have been
investigated quantitatively. The oxide thin film shows the characteristics specific to
both pH and lead concentration of the solution. Generally, nickel gets depleted and
chromium enriches in the oxide film in the pH region from neutral to acidic. Soluble
lead enhances this tendency, especially in more acidic condition with higher soluble
lead concentration. The thickness of the oxide film formed in lead-containing water was
thinner than that in the non-lead environment, due to the active dissolution at the
surface of the alloy.
2. The dissolved nickel and iron concentrations after autoclave testing are higher in more
acidic test solutions with higher soluble lead concentrations. This fact, as well as
those obtained by thin film study, demonstrates the selective dissolution of nickel
and iron from Alloy 600, suggesting that an active electrochemical reaction between
soluble lead and nickel / iron among Alloy 600 constituents enhances the possibility of
corrosion.

REFERENCES
(1) J.M.Sarver, "IGSCC on Nickel Alloys in Lead Contaminated High Purity Water", Presented
at the EPRI Intergranular Corrosion Mechanisms Meeting, Washington, D.C., April 27-May
1, 1987.
(2) G.O.Hayner, et al., "Examination of Tubes Removed From St.Lucie Unit 1." Paper
presented at the Third International Symposium on Environmental Degradation of
Materials in Nuclear Power Systems-Water Reactors, Traverse City, Michigan, August 30-
September 3, 1987.
 671

(3) H.R.Copson and S.W.Dean, "Effect of Contaminants on Resistance to Stress Corrosion

Cracking of Ni-Cr Alloy 600 in Pressurized Water.", Corrosion, Vol. 21, Jan. 1965.
(4) G.P.Airey, "The Effect of Carbon Content and Thermal Treatment on the SCC Behavior of
Inconel Alloy 600 Steam Generator Tubing, Corrosion, March 1979, P.129.
(5) T.Sakai, K.Aoki, K.Matsumoto and F.Nakayasu, "Study on Oxide Thin Film of Alloy
600",NACE Symposium Corrosion '89, No.490, April, 1989.
(6) T.Sakai, S.Okabayashi, K.Aoki, K.Matsumoto, F.Nakayasu and Y.Kishi, "Effect of Reduced
Sulfur on High Temperature Aqueous Corrosion for Alloy 600", The Fourth International
Symposium on Environmental Degradation of Materials in Nuclear Power Systems-Water
Reactors, Jekyll Island, GA, August 1986. (in press).
(7) T.Sakai, S.Okabayashi, K.Aoki, K.Matsumoto, F.Nakayasu and Y.Kishi, "A study of The
Oxide Thin Film on Alloy 600 in High Temperature Water", The Fourth International
Symposium on Environmental Degradation of Materials in Nuclear Power Systems-Water
Reactors, Jekyll Island, GA, August 1986. (in press).
(8) T.Sakai, S.Okabayashi, K.Aoki, K.Matsumoto and Y.Kishi, "A Study of Oxide Thin Film of
Alloy 600 in High Temperature Water Containing Lead", NACE Symposium Corrosion '90,
No.520, April, 1990.

Table 1. Chemical compositions (wt%) and heat treatments.

C Si Mn P S Cu Ni Cr Fe Heat Treatment

A l l o y 600 MA SG Tube 0.03 0 . 3 1 0.30 0.007 0.001 0 . 0 1 74.85 15.90 8.1 925°Cx3mins.

A l l o y 600 ST Bar 0.04 0.14 0 . 2 1 0.005 0.001 0.03 73.78 15.75 9.10 1000°CXl.5hrs-WQ

Table 2. Test matrix.

Test Test Solution *3

No. Specimen Capsule Objective*4 Note
Lead Chemicals pH*1 Pb(ppm)*2 Cl(ppm)*2

1
1 '" -2
3

4.5
6900

3800
2557

1428
Film PbCI 2 = Saturated in

PbCI2 SUS-304 each pH

600 M A Analysis
-3 7 300 140
SG Tube (Teflon coat)
-4 3 PbCI2:50g/i PbCI2 = Supersaturation
Solution
11-1 3
Non Pb condition for
2
I " Non Pb
4.5
Analysis
Test No. 1 - 1 ~ 1-3
-3 7

•ft -1 3 5806 2329

-2 4.5 3609 1446

PbCI2 Same as
-3 7 157 132 Test No. 1 - 1 - 1-4.
No Alloy 600 Solution
-4 3 PbCI2:50g/i
Specimen
(ST) Analysis
IV-1 3 3453 1417 PbCl 2 =
PbCI2 in the
-2 4.5 3453 1382 less than saturation
capsule
V-1 3 51
Non Pb Same as
-2 4.5 15 Test No. 11-1 ~ 11-3.
-3 7

• 1 . pH i s adjusted by HC1 at room temperature.

♦ 2 . Pb i s measured by Atomic Absorption Spectroscopy.
Cl i s measured by Ion Chromatography.
* 3 . Dissol ved oxygen is less than 5ppb.
* 4 . Autocl ave test condition =280°Cxlweek (168hrs).
 672

Table 3. Results of test solution analysis.

Results of lest Solution Analysis *^

Test Test Before Testing After Testing

NO. Condition Note
pH*1 Pb(ppm) Cl(ppm) Ni(ppm) Cr(ppm) Fe(ppm) Pb(ppm) Cl(ppm) pH*1

1-1 3 6900 2557 55 <1 290 5200 3.03

PbCl 2 : Saturation
PbCI 2
-2 4.5 3800 1428 26 <1 228 2400 3.08
+
-3 600 MA SG Tube 7 300 140 18 <1 89 100 3.40

-4 3 PbCI2:50g/f 220 <1 476 6496 3.71 PbCl2 : Supersaturation

11-1 3 6 <1 35 3.68

Non Pb
-2 + 4.5 4 <1 27 4.03 Non Lead
600 MA SG Tube
-3 7 4 <1 18 4.06

111-1 3 5806 2329 136 <1 24 5571 2365

-2 PbCI 2 in 600 4.5 3609 1446 103 <1 15 3139 1417 PbCI 2: Saturation
ST capsule 7 157 132 4
-3 30 <1 78 130

-4 3 PbCl2:50g/i 311 <1 51 4943 2492 PbCI 2 : Supersaturation

IV-1 3 3453 1417 112 <1 17 2982 1368 PbCI 2 : Less than saturation
PbCl2 in 600 ST capsule
-2 4.5 3453 1382 102 <1 17 2825 1353

V-1 3 51 11 <1 1 50
Non PbCl 2 in 600
-2 ST capsule 4.5 15 <1 <1 <1 13 Non Lead
-3 7 <1 <1 <1

*1. pH at room temperature.

*2. Metal ions (Ni, Cr, Fe, Pb) are measured by Atomic Absorption Spectroscopy
and Inductively Coupled Plasma. Cl is measured by Ion Chromatography.
(RATIO) (RATIO)
DO,<5ppb,Non PbCI,

Test No. Π - Ι
0.8

\ /V_ „^^"^ Test No. D - 2

0.6
A V ^ - ^ ^ Test No. II- 3

0.4- . V/
0.2

0 1 1 1 1 1_
-1500 -KX» -500 0 500
(SEC) (SEC)
SPUTTERING TIME FROM INTERFACE SPUTTERING TIME FROM INTERFACE

(RATIO)
D O s < 5 p p b , N o n PbCI 2

Test No. Π- I

Test Ν ο . Π - 2

Test No. D-3

-600 -400 -200 200 500

(SEC) (SEC)
SPUTTERING TIME FROM INTERFACE SPUTTERING TIME FROM INTERFACE

Figure 1 . Evaluation of Alloy 600 MA t h i n f i l m c h a r a c t e r i s t i c s

f o r various conditions with and without lead contamination.
673
674

0SNI:S60AT·/. 0 2»NI£30AT%
o.r J
/
i

~j
•
/P/ °
0.6 - / /
<f /

0.9
_ J
t
\ \ J
\ *—
<\
0.4

- \\ H

0.3
1 1 1
J
4.3 7

pH

Figure 2 . Average values of ( N i , Cr)/(Ni+Cr+Fe)At% r a t i o

in f i l m region (0<Ni<60At%, 3 0 A U ) of Alloy 600 MA.

(SEC)

(ppm) D : PbClx 50g// 1 (ppm)

(Super Sot)
O : PbCI (Sot.)
c3 0 0 . Γ\ Δ : PbCIt Pb 4g/r
I50
. c
f
σ • : Non PbClx σ
c
»200
o
" o
o
§30

;k
O
oc c
o o 20
__ 100 ■ \

z 10

\ A
\ Ό
A 1
4.3
pH pH

O i Pb (Sot.) O i Pb (Suptnot.) A i Non Pb

Figure 4. Dissolved metal ion
concentrations in various
test solutions with Alloy
Figure 3. Film thickness of
600 ST capsules.
Alloy 600 MA.
(Test No.HI, IV, V )
 WS8d7

STRESS CORROSION CRACKING BEHABIOR OF STAINLESS STEELS

UNDER AGING AT LOW TEMPERATURE

H. NAGANO AND H. TSUGE

Research and Development Division, Sumitomo Metal Indus-

trios Ltd., 1-8, Fusoh-cho, Amagasaki, 660, Japan

ABSTRACT

The low-temperature sensitization(LTS) behavior of weld heat-affected zones

(HAZ) of stainless steels is very important for predicting their susceptibi-
lity to intergranular stress corrosion cracking (IGSCC) in boiling water
reactor (BWR) environments during their service life. Studies of LTS were
carried out on regular stainless steels such as Types 304, 304L, 316 and
316L, and nuclear grade (NG) stainless steels such as Types 304NG, 316NG and
347NG. The weld HAZ of Type 304 stainless steel was sensitized by low-
temperature heat treatment, being susceptible to intergranular corrosion and
IGSCC. The LTS of the weld HAZ of Type 304 stainless steel was controlled by
chromium diffusion, the activation energy for which was 38.6 kcal/mol, lower
than the value for the base metal. The weld HAZ of Type 316 stainless steel
was less susceptible to LTS than 304 stainless steel owing to the effect of
molybdenum alloyed in the steel. Types 304NG, 316NG and 347NG stainless
steels were practically immune to LTS, because they contained no chromium
carbide from welding and subsequent low-temperature heat treatments.

KEYWORDS

LTS (low-temperature sensitization), weld HAZ (heat-affected zone), IGSCC

(intergranular stress corrosion cracking), BWR (boiling water reactor),
activation energy, intergranular corrosion

INTRODUCTION

Many studies on the prevention or retardation of IGSCC in the weld HAZ of

Type 304 stainless piping have succeeded in developing useful countermeasur-
es against IGSCC in BWR plants. IGSCC of the weld HAZ in recirculation pipes
of 304 stainless steel occurs under the co-existence of such conditions as
chromium-depleted grain boundaries on the weld HAZ, residual stress or
strain on welding, and dissolved oxygen in the primary cooling water of BWR
plants.
Therefore, a number of SCC countermeasures are based upon removing these
above-mentioned conditions:

675
676
(i) improving the welding procedure by heat sink welding(HSW) or corro-
sion-resistant cladding (CRC) on internal surface welds (Ando, 1978;
Akashi,1980);
(ii) improving the metallurgical conditions and stress levels by solution
heat treatment(SHT) or induction heating stress improvement(IHSI)
(Ando, 1978; Akashi,1980);
(iii) reducing the dissolved oxygen level on the primary cooling side
(Fejes,1980);
(iv) using the SCC-resistant stainless steels such as Types 304, 316 or
347 nuclear grade stainless steels (Nagano,1979; M.Kowaka et al.,19-
80).
The sensitization of stainless steels that is responsible for IGSCC is
incurred by the precipitation and growth of chromium carbides along grain
boundaries. The former phenomenon occurs in a high-temperature range
between 500 and 800°C, and the latter one proceeds at lower temperatures
below 500°C to the operating temperature of BWR plants (this is termed LTS).
It has been reported that the weld HAZ of Type 304 stainless piping was
sensitized by aging at low temperatures (Povich et al., 1978)
The resistance of alloys to LTS is very important for predicting their life
expectancy in a BWR environment. The purpose of this paper is to evaluate
the effect of LTS heat treatment on the susceptibility of IGSCC of various
kinds of stainless steel, including nuclear grade stainless steels.

EXPERIMENTAL PROCEDURE

Materials

The chemical composition of the stainless steels used is presented in

Table 1. Specimens for microstructural observation and corrosion tests were
prepared from 4B (8.6 wall thickness x 114mm outer diameter) stainless steel
piping of such commercial grades as Types 304, 304L, 316 and 316L, and
nuclear grades such as Types 316NG and 347NG stainless steels. The major
elements that affect sensitization are carbon and nitrogen, which combine
with chromium, resulting in chromium depletion along the grain boundaries.
The carbon content of such regular stainless steels as Types 304 and 316 is
about 0.05%, while Types 316NG and 347NG stainless steels have a very low
carbon content of 0.01% with the addition of some nitrogen.

Table 1. Chemical composition of stainless steels used

(wt%)

Steel C Si Mn P $ Ni Cr Mo Nb N
304 Ό.050 0.49 1.73 0.028 0.005 9.10 18.20 — — 0.025
304L 0.021 0.55 1.60 0.028 0.008 11.30 18.42 — — 0.023
304NG 0.016 0.51 1.44 0.020 0.002 10.17 19.49 — — 0.086
316 0.057 0.60 1.76 0.030 0.006 13.10 16.55 2.13 — 0.031
316L 0.017 0.43 1.60 0.030 0.008 14.60 17.40 2.50 — 0.042
316NG 0.010 0.44 1.46 0.023 0.006 12.55 17.15 2.88 — 0.089
347NG 0.009 0.39 1.45 0.012 0.001 9.90 18.35 — 0.32 0.085
 677

Heat Treatment

Fig. 1 shows the heat-treating conditions for the specimens. Since a prere-
quisite for LTS is the presence of nuclei of chromium carbides along the
grain boundaries, two methods were undertaken, one being TIG welding and the
other heat-treating at 750°C for 100 min. The aging temperatures were
500°C, 425°C and 350°C respectively, and the duration was up to maximum of
10000h. Analysis of sensitization of each stainless steel exposed to these
conditions made it possible to calculate an activation energy for chromium
diffusion and a life expectancy under the operating conditions of BWR
plants.

-H 500°C x 7, 24, 100, 300, 1,000 h |

[As received\- 750°C x H425°Cx24, 100, 300, 1,000, 3,000, 10,000 "h]
IQOmin, AC

Welding 350°C x 1,000, 3,000, 10,000 h

Fig. 1. Conditions for low-temperature sensitization.

Preparation of Welded Joints

The materials and welding conditions are given in Table 2. The welding
electrodes were 308 for 304 series, 316 for 316 series and 347L for 347
nuclear grade stainless steels. TIG welding was accomplished with 16
passes, the average heat input for each pass being about 8000-10000J/cm.

Table 2. Materials and welding conditions

Pipe material Welding material Welding condition

304 308
304L 308L • Welding speed

308L 10 cm/min
304NG
316 316 • 1 pass, 50 A
316L 316L 2 - 3 passes, 120 A
316NG 316L 4 - 1 6 passes, 140 A
347NG 347L

Corrosion Tests

Intergranular Corrosion.
The Strauss test (a boiling solution of sulfuric acid, copper sulfate and
copper tips with a 48-h immersion) was used for evaluating the LTS behavior
of stainless steels. The corrosion test specimen with or without the weld
was removed longitudinally from a portion 1 mm below the inner surface of
the tubing.

Stress Corrosion Cracking in High-Temperature Air-Saturated Water. The

678
double U-bend specimen with or without the welded joint was immersed in
recirculating water at 250°C with an oxygen content of 8ppm for 500h. The
crack lengths were microscopically observed in the specimen after the SCC
test.

RESULTS AND DISCUSSION

The Strauss test and SCC test results of the weld HAZ of Types 304, 304L,
316 and 316L stainless steels are shown in Fig. 2. Type 304L stainless steel
needed a longer heating time at low temperatures for the initiation of
intergranular corrosion and IGSCC because of its lower carbon content in
comparison with Type 304 stainless steel.

Referring to the effect of molybdenum, this retarded chromium diffusion in

the molybdenum-bearing stainless steels, and therefore Type 316 stainless
steel was more resistant to LTS than Type 304 stainless steel, as shown in
Fig. 2. In addition to this, molybdenum dissolved as Μοθ£ -ions from the
metal surface in high-temperature water, and then inhibited IGSCC even when
Type 316 stainless steel was considerably sensitized (Tsuge, 1984).

Temperature (°C) Temperature (°C) Temperature (°C) Temperature (°C)

500 425 350 300 500 425 350 300 500 425 350 300 500 425 350 300
1 r——i 1 i 1
304 and 304L (HAZ) 316 and 316L (HAZ) 304 and 304L (HAZ) 316 and 316L (HAZ)

1
° no crack o no crack
9
—
n
\
\
° no crack
o < 50μ o
o no crack
· <, 100μ °
< 50μ
· < 100μ o
10 _
J? jC \ x > 100μ x > 100μ \ x > 100μ
\XA o o o 9 O o o
E
Vx \ \ \ x\ \ o
" \r
£ +J 10 2 - \o o - o o 316
C c * 316
J
\ \ 304
xv x \ / • o x o / o o
316L
- Λ.Ν/.
«0
10 3 - x \ " \ . X \/o o o o o
+-> +j
\ \ \V \ \

.Y
*x \\ o •\ \\° o o

- λ\ \
c c
<D
oo 1 10- X\ 9 o o

304L ^ \ 304L \ \
10 5
10
(316L: no crack)
\ \
1 1 1 1 1 1 U-l 1 1 1 1 1 1 1 L_ _ l 1 1 ■ 1

103/ K 103/ K 10 3/ K 10 3 / K
a) Strauss test (48 h) b) Double U-bend SCC test (250°C, 8 ppm, D.O. 500h)

Fig. 2. Effect of temperature on the low-temperature

sensitization of austenitic stainless steels.

The major cause of LTS in stainless steels is the formation of chromium-

depleted zones accompanying the precipitation of chromium carbides along
grain boundaries. Equation (1) describes the reaction for chromium carbide
formation, which is controlled by choromium diffusion.

23Cr + 6C = Cr 23 C 6 (1)

Therefore, the rate of LTS primarily depends on chromium diffusion in stain-

less steels
When the average distance of chromium diffusion distance d is equal in all
LTS conditions in stainless steel, then the following equations can be
 679
applied to two points on the straight line defined as X(l/Ti,ti ) and Y(l/T2
,t 2 ):

D^CT^ti = D cr (T 2 )t 2 (2)

Dcr - D exp (- £ ) (3)

_ RT!T2 t2
Q T -T
ln
T~ (4)
1
1 J-2 tl

Q(T!-T2)
t 2 = tiexp (5)
RTiT2

where D cr = chromium diffusion constant at temperature T, R = gas constant,

Q = activation energy for chromium diffusion, Τχ and T 2 = absolute temperat-
ures, and ti and tz = heating times. The straight lines of LTS for the weld
HAZ of various kinds of stainless steel are drawn in Fig. 3. The activation
energy Q and time to LTS for the HAZ of each stainless steel are counted,the
time to LTS being estimated by extrapolating the straight line in Fig. 3 to
a service temperature of 300°C.

The activation energy for chromium diffusion in the weld HAZ of Type 304
stainless steel was 38.6 kcal/mol, while the value in the base metal was
about 70 kcal/mol. These values are significantly consistent with the data
reported by M.J. Povich and P. Rao (1978). They explain the difference of
activation energy for chromium diffusion between the weld (HAZ) and the base
metal by describing that chromium diffuses along the grain boundaries in the
weld HAZ, whereas it diffuses into the bulk in the base metal.

1 10 102
Sensitization time (year)
Fig. 3. Comparison between the low-temperature sensi-
tization in the weld HAZ of austenitic stain-
less steels. The LTS was evaluated by the
Strauss test.

The time required to sensitize the weld HAZ of Type 304 stainless steel was
about 7 years at 300°C. As for the weld HAZ of Type 316 stainless steel,
680
the activation energy for chromium diffusion and the time to LT3 at 300°C
were 42.7 kcal/mol and 850 years, respectively. This delayed LTS behavior
of Type 3io stainless steel presumably results from the effect of molybdenu-
m, as previously explained.

Both Types 316NG and 347NG stainless steels did not show any susceptibility
to LTS, because they had no chromium carbide in the weld HAZ. A conservative
calculation using the plot (500°C, 1000h) and an activation energy of 42.7
kcal/mol in the weld HAZ of Type 316 stainless steel gives more than 1750
years for the time to LTS in the weld HAZ of Types 316NG and 347NG stainless
steels.

CONCLUSIONS

The LTS behavior of regular stainless steels and nuclear grade stainless
steels was studied by applying the Strauss test and the SCC test in high-
temperature water.

The weld HAZ of Type 304 stainless steel was sensitized by low-temperature
heat treatment, being susceptible to intergranular corrosion and IGSCC. The
LTS in the weld HAZ of 304 stainless steel was controlled by chromium diffu-
sion, the activation energy for which is 38.6 kcal/mol, lower than the value
for the base metal.

The weld HAZ of Type 316 stainless steel was less susceptible to LTS than
Type 304 stainless steel owing to the effect of molybdenum alloyed in the
steel, which retarded chromium diffusion and also inhibited IGSCC in high-
temperature water.

Types 304NG, 316NG and 347NG stainless steels were practically immune to
LTS, because they contained no chromium carbide along the grain boundaries
from welding or from the subsequent low-temperature heat treatment.

REFERENSES

Akashi, M. (1980). Boshoku Gijutsu (Japan), 29^_ 142-151.

Ando, Y. (1987), Nuclear Eng. (Japan), 24, No.9, 9-16.
Fejes, P.P. (1980). EPRI Seminar on Countermeasures for BWR pipe Cracking,
USA.
Kowaka M., H.Nagano, K. Ohta and S. Nagata (1980), EPRI Seminar on Counter
measures for PWR pipe Cracking, USA.
Nagano,H., T.Kobayashi, H. Tsuge and N. Maruyama (1979), J. Iron & steel
Inst. (Japan), 6^, S1043.
Povich and P.Rao (1978), Corrosion 78, Houston, Texas, USA paper No.191.
Tsuge H. , N. Usuki, H.Maruyama and H. Nagano (1984), Proc. Int. Cong,
Metallic Corrosion, 4, 228-234.
WS8d8

Crystallographic Evaluation of Stress Corrosion Cracking

in Type 310S Steel Single Crystals

H. UCHIDA, S. INOUE and K. KOTERAZAWA

Department of Chemical Engineering, Himeji Institute of Technology,

Shosha, Himeji 671-22, Japan

ABSTRACT

The stress corrosion cracking (SCC) of type 310S steel single crystals
has been evaluated crystallographically. The susceptibility to SCC under
constant load conditions increased in the order of [111], [101] and [001]
tensile axis, although under slow strain rate conditions a less dependent
on their orientations was observed. Many cracks were preferentially
nucleated from the mechanically induced slip-steps, and then propagated
along the <110> direction on the {100} plane, regardless of test condi-
tions. Most of the fracture surfaces were characterized by the coalescent
steps, which composed of the other {100} planes. Furthermore, the SCC
growth was strongly controlled by the normal stress to the {100} crack
plane which made the smallest angle with respect to the tensile axis.

KEYWORDS

Austenitic stainless steel, stress corrosion cracking, single crystal,

tensile axis, crack orientation, fractography.

INTRODUCTION

The crystallography of SCC has been studied from the fractographic aspects
of transgranular fracture. For the austenitic stainless steels in hot
concentrated chloride solutions, there has been a variety of conclusions
in determining the crack orientation, as reviewed by Meletis and Hochman
(1986). This disagreement may be related the use of polycrystals of
several tens of microns in grain size, besides different conditions.

Following an earlier extensive study by Reed and Paxton (1962), a few

studies has been performed with 'as-grown' single crystals: Marek and
Hochman (1971), Ahlers and Riecke (1978), Silcock (1981), and others found
the definite indications in the crystallographic nature of SCC. Recently,
Uchida et al. (1986) also examined the crystallography of SCC in type 304
steel single crystals, and found that the cracking susceptibility was in-
fluenced by the tensile axis orientation (or Schmid factor). Therefore, an
attempt has been made in the present study to examine the determining fac-
tor of susceptibility in type 310S steel by employing the orientation-

681
682
controlled single crystals.

EXPERIMENTAL PROCEDURE

The single crystals of type 310S steel (C 0.02%, Si 0.25%, Mn 1.11%, P

0.029%, S 0.003%, Ni 19.28%, Cr 24.24%, Fe balance) were grown by the
Bridgman method in an argon gas atmosphere at 1773K, and then homogenized
at 1573K for 14.4ks. From a cylindrical single crystal 9mm in diameter
and 600mm in length, the regular prismatic specimens with a gauge dimen-
sion of 1.8xl.8x7mm were prepared by spark cutting, mechanically polishing
and electropolishing. The tensile axis orientations determined by the
back-reflection Laue method are illustrated on a stereographic projection,
as shown in Fig. 1. All specimens encapsulated in quartz in a vacuum were
annealed at 1373K for 3.6ks, and subsequently water quenched.

n
/Φ0 i \ x\
}
ΪΊΜ-
A^L
—sL z
/ \yo\
bqi t
TTp\
~OT!
Xa/ \ y
^Ήθ

Fig. 1. Stereographic projection of the test

specimens used. X: Normal to top surface. Y: Nor-
mal to side surface. Z: Tensile axis.

For SCC tests, the finally annealed specimens were mounted in a cantilever
beam type apparatus, and then exposed to a boiling 42% MgCl2 solution at
416K under constant load conditions. Some results were obtained from the
tensile tests under the slow strain rate conditions of 2.38xl0~ 7 s _1 to
2.38xl0"4s"1. For the crystallographic evaluation of SCC, the specimens
after testing were examined by a scanning electron microscope directly,
with no further preparation other than rinsing in acetone and drying.

EXPERIMENTAL RESULTS AND DISCUSSION

SCC Tests

The SCC tests under slow strain rate conditions were performed in a boil-
ing 42% MgCl2 solution at 416K, as compared the tensile tests in a non-
corrosive oil at the same temperature. The nominal stress-strain, ο-ε ,
curves at the strain rate of 2.38xl0~6s-1 are shown in Fig. 2. As might
be suspected, their curves in an oil are influenced by the tensile axis
orientation. The work-hardening rate in stage II is larger, for the
[001]- and [lll]-oriented specimen with multiple slip system. However,
the [101]-oriented specimen with single slip system shows a relatively
small work-hardening rate, following easy glide strain in stage I . On
the other hand, quite different stress-strain curves are found in a
boiling 42% MgCl2 solution. The tensile strength and elongation decrease
markedly due to the occurrence of SCC, as compared with the curves in an
 683
—r 1 ' 1 I | . | I | I

2600
/"S » A\
Σ
-
//
//
/
ΖΛ^
</f 400 -h 1/ Oil A
it / r$ Ή\ MgCl 2 I
if y' » ^-""%\2 1
i.
if
c' V S
1 >***'*
E
o
z
Γ \l 1 1 1 \l 1 1 I
0 20 40 60 80 100 120
Nominal strain, 6/7©
Fig. 2. Orientation dependence of nominal stress-
strain curves in a boiling 42% MgCl2 solution and
noncorrosive oil at 2.38xl0"6s_1.

oil. This decreasing tendency was observed at the strain rates lower than
2.38xl0_4s-1, where ductile fracture occurs only. The susceptibility to
SCC under slow strain rate conditions was evaluated by using the
susceptibility index (Okada et al., 1974). Thus, it was clarified that
the resulting susceptibility was less dependent on the tensile axis
orientations in comparison with the above-mentioned strain rate.

Fig. 3 shows the results obtained by the SCC tests under constant load
conditions, as plots of the logarithm of time to fracture tf against the
applied stress σ Α . There is an increasing tendency in the time to
fracture with a decreasing applied stress. The threshold stress to SCC
occurrence is lower in the order of [111], [101] and [001] tensile axis,
and the susceptibility to SCC increases correspondingly. The influence of
Schmid factor Sf on the susceptibility is disclosed by Fig. 4, which is
rearranged with the shear stress τ (=jA'Sf) on the (lTl) primary slip
plane. From the different threshold value in shear stress, it became
evident that the susceptibility to SCC in type 310S steel single crystals
was hardly influenced by the Schmid factor. The determining factor of the
susceptibility in this steel will be discussed later.

1 1 — r n —- p . . ■ i | - 1. 1 1

ΛH
a-
£200
s60
Λ ^
Σ
^160 A ^50

v^
LV4-
J120 - k ,-40 l·

80 A
^ - 1 ^ A 20
<
J...I 1 1 1 i 111 1
10 102 103 104 10 102 103
Time to fracture, tf / ks Time to fracture, t t / ks
Fig. 3. Orientation dependence of F i g . 4. R e l a t i o n s h i p between
applied s t r e s s vs. time to frac- shear s t r e s s on the (111) primary
t u r e c u r v e s in a b o i l i n g 42% s l i p plane and time to f r a c t u r e .
MgCl2 solution.
684
Frac tographic Observations
Fractographic results show that many cracks preferentially nucleate from
the mechanically induced slip-steps, but they do not follow the slip
planes. The crack orientation in all single crystals was determined by
the two-surface trace analysis, on the basis of (111) primary slip traces
and the assumption of no crystal rotation. Fig. 5 shows an example of
crack orientation for the [101]-oriented specimen, of which the SCC
propagates primarily along the (100) plane (or the equivalent (001)
plane). This is in agreement with the results obtained for the other
specimens, regardless of test conditions.

Fig. 5. Cracks and slip traces on (a) the top and

(b) side surface of [101]-oriented specimen
(120MPa applied).

The fracture surfaces are characterized by the coalescent steps which are
generally crystallographic, exhibiting a serrated appearance. It is well
known that these steps frequently form a fan-shaped and/or river-like
pattern. The fracture surfaces are also influenced by the tensile axis
orientation. Fig. 6(a) shows that for only the [001]-oriented specimen
the fracture surface is flat, due to the single crack growth along the
(001) plane. The other fracture surfaces, however, are relatively rough
and exhibit the crystallographic steps as shown in Fig. 6(b), where the
facets A to D are (100) cracks and the facet E is the equivalent (001)
crack. From the magnified views shown in Figs. 7(a) and 7(b), it is
apparent that the occurrence of coalescent steps is dependent on the
tensile axis orientation. They are observed on the (100) fracture surface
and composed of the other (010) and (001) planes (Fig. 7(b)). In
addition, it can be inferred that the SCC growth occurs along the <110>
direction by studying the flow direction of coalescent steps.

Crystallographic Evaluation of SCC

It became clear that the SCC in all single crystals of type 310S steel was
principally crystallographic, and propagated along the <110> direction on
the {100} plane. Previously, Ahlers and Riecke (1978) used the two-
surface trace analysis to identify the crack orientation, showed that the
crack plane in Fe-25Cr-20Ni steel single crystals lay near the {100}
plane, being in agreement with the results reported earlier by Reed and
Paxton (1962). Very similar results were also observed in type 310 steel
single crystals by Silcock (1981). None of the papers, however, has
 685

Fig. 7. Magnified views of the

rectangle in Fig. 6(a) and 6(b).
Fig. 6. Fracture surfaces of (a)
the [001]- and (b) [101]-oriented
specimen (60MPa and lOOMPa ap-
plied, respectively).

clarified the orientation dependence of the susceptibility to SCC by

employing the orientation-controlled single crystals. The intention of
the present study was focused on the determining factor of susceptibility,
i.e. the normal stress σ Ν to {100} crack plane which makes the smallest
angle Θ with respect of the tensile axis. The relationship between the
normal stress and time to fracture is shown in Fig. 8, where the normal
stress under slow strain rate conditions is derived on the basis of the
tensile stress σ τ . Almost all of the data under two different conditions
coincide well with the increase of time to fracture (or the decrease of
strain rate). In other words, it is concluded the SCC growth is strongly
controlled by the normal stress to the {100} crack plane which makes the
smallest angle with respect to the tensile axis.

CONCLUSIONS

The crystallography of transgranular SCC in type 310S steel was evaluated

by employing the orientation-controlled single crystals. The main results
obtained can be summarized as follows:
686
200 Γ-Π 1 1—m j 1—Γ-ΓΤ-
• Slow strain rate test a)
Σ160 • Constant load testb)

J20 -σΝ
A
% 80 ON
a) oN=aTcos29
b) SOACOS^O
40 2(9=45°
3(9=54.7°)
I I I I I i i i i I i
1 10 102
Time to fracture, tt / ks
Fig. 8. Relationship between normal stress to the
(001) crack plane and time to fracture under two
different conditions.

(1) The susceptibility to SCC under constant load conditions increased in

the order of [111], [101] and [001] tensile axis, although under slow
strain rate conditions a less dependent on their orientations was
observed.
(2) Many cracks were preferentially nucleated from the mechanically
induced slip-steps, and then propagated along the <110> direction on the
{100} plane.
(3) Most of the fracture surfaces were characterized by the coalescent
steps, which composed of the other {100} planes.
(4) The SCC growth was strongly controlled by the normal stress to the
{100} crack plane which made the smallest angle with respect to the
tensile axis.

ACKNOWLEDGMENTS

The authors are very grateful to Mr T. Oido, a graduate student, for his
contributions and assistance with the experimental work.

REFERENCES

Ahlers, M. and E. Riecke (1978). Stress corrosion cracking in single

crystals of Fe-25Cr-20Ni. Corros. Sei., 18, 21-38.
Marek, M. and R. F. Hochman (1971). Crystallography and kinetics of stress
corrosion cracking in type 316 stainless steel single crystals, Corrosion,
27, 361-370.
Meletis, E. I. and R. F. Hochman (1986). A review of the crystallography
of stress corrosion cracking. Corros. Sei., 26>, 63-90.
Okada, H., Y. Hosoi, S. Abe and S. Yamamoto (1974). A rapid testing method
of stress corrosion cracking of austenitic stainless steels. J. Japan
Inst. Metals, 38, 646-653.
Reed, R. E. and H. W. Paxton (1962). Stress-corrosion cracking of single
crystals of some austenitic stainless steels. First International Congress
on Metallic Corrosion, pp. 301-308. Butterworths, London.
Silcock, J. M. (1981). Orientations of transgranular stress corrosion
cracks in austenitic steels tested in MgCl2 solutions. Br. Corros. J., 16,
78-93.
Uchida, H., K. Koterazawa, K. Yoshida and I. Yamada (1986). Effect of
tensile orientation on stress corrosion cracking in SUS 304 steel single
crystals. J. Soc. Mater. Sei., Japan (Zairyo), 35., 7-12.
 WS8d9

RELATIONSHIP BETWEEN STRAINING ELECTRODE BEHAVIOR AND

CORROSION FILM OF NICKEL BASE ALLOYS IN A HIGH
TEMPERATURE CAUSTIC SOLUTION

Kazuo Yamanaka* and J u n i c h i r o Murayama**

* I r o n and S t e e l R e s e a r c h L a b o r a t o r i e s , R e s e a r c h and Development D i v i s i o n ,

Sumitomo M e t a l I n d u s t r i e s , L t d .
1-8, F u s o - c h o , Amagasaki, Hyogo, 660, J a p a n
** Technology D e p a r t m e n t , Sumikin Techno-Research C o . , L t d .
1-8, F u s o - c h o , Amagasaki, Hyogo, 6 6 0 , J a p a n

KEYWORDS

Straining electrode, aqueous solution of sodium hydroxide, high temperature

water, corrosion film, nickel base alloys, caustic stress corrosion
cracking.

ABSTRACT

SCC resistance may be influenced by the repassivation behavior at the crack

tip. In this time, the initial repassivation processes of anodic reaction
on newly created surfaces of nickel base alloys containing 0rv30wt% chromium
in a high temperature NaOH solution were investigated by a rapid straining
electrode technique. The corrosion films of these alloys were analyzed by
ion micro mass analyzer (IMMA). The following results were obtained:

(1) The repassivation rate of nickel base alloys increased with increasing
chromium content. And so the amounts of charge caused by the metal
dissolution were decreased with increasing chromium content.
(2) The corrosion film had a double layer structure, that is, nickel
hydroxide or oxide in the outer layer and chromium oxide in inner layer.
The chromium concentration in the inner layer increased with increasing
chromium content.
(3) The caustic SCC resistance seems to be influenced by the repassivation
rate and the inner chromium oxide layer, and to be important for the
existence of the outer nickel hydroxide and/or oxide layer.

INTRODUCTION

16 pressurized water reactors (PWRs) are currently in operation in Japan,

and Alloy 600 (15%Cr-75%Ni-9%Fe) is used for the steam generator (SG)
tubing.
Recent demand for higher quality and reliability has forced us to develop
more corrosion resistant alloy tubing. As a result^ we have developed
thermally treated (TT) Alloy 690 (30%Cr-60%Ni-9%Fe) ; ' ; .
It has been reported that Alloy 690, which contains a higher chromium
content than Alloy 600, has high corrosion resistance»an..the accelerated
primary water and off chemistry secondary water of PWRs ' '
687
688
However, the SCC resistance and corrosion resistance of Alloy 690 has not
yet been clarified, especially the relation between IGA* resistance and
surface oxide film formed in high temperature caustic solution. .
Thus, in the present work, a rapid straining electrode technique , which
can quantitatively analyze the transient anodic dissolution process on a
newly created surface, was used to investigate the repassivation behavior
of Ni base alloys containing 0^30wt%Cr in order to clarify the effect of
chromium content on the initial repassivation process of anodic reaction on
a newly created surface at the crack tip.

* Intergranular attack (IGA) is composed of intergranular corrosion (IGC)

and intergranular stress corrosion cracking (IGSCC) following IGC.

EXPERIMENTAL METHODS

Materials
The materials used in this study were vacuum-melted 75%Ni-0^23%Cr-bal. Fe
alloys and 60%Ni-15 ^30%Cr-bal. Fe alloys. The alloys were forged,
hot-rolled and drawn to thin wire 0.50mm in diameter. The wire specimens
were annealed in an argon atmosphere at 1373K for 0.5h (1.8ks) and then
water quenched. Then the wires were polished with up to No. 1000 Emery
paper and decreased with acetone.

Straining electrode equipment

A schematic drawing of rapid straining electrode equipment used in this
investigation is shown in Fig.l. The autoclave, the volume of which is
about 0.18m , is made of Alloy 690. The wire specimen is attached to the
chucks made of Hastelloy C, and zirconia coated zirconium plates are
inserted between the chuck and the specimen in order to electrically
isolate the specimen from the autoclave. One side (the upper part) of the
specimen holding chuck is connected to a pull rod made of Hastelloy C, and
the pull rod passes through the autoclave head plate fitted with a water
cooled pressure balanced fitting seal and is connected to a piston in a
cylinder. When high pressure argon gas is introduced into the cylinder,
the piston is pulled up rapidly and the pull rod is moved up, and then the
wire specimen is elongated. A constant amount of strain is given by a
stopper set in the cylinder, and the amount of strain is measured by a
transducer mounted on the top of the piston.

Irecorderl

. 2 channel
j |digilal memory |
i i i J I
Piston

counter electrode (Pt)

specimen electrode
reference electrode (Ag/AgCI)

Fig.l Schematic drawing of rapid strain electrode

equipment in high temperature caustic solution
 689
4%NaOH (pH=14 at a room temperature) solution was used as a testing
solution, and the test temperature was 553K. A reference electrode for
electrochemical measurement is used as an internal Ag/AgCl reference
electrode.

Analysis of corrosion film

The corrosion films of the alloys were mainly analyzed by ion micro mass
analyzer (IMMA, ARL made), and also by ESCÄ (VG made, ESCA3 Mark II) in
some alloys. The samples for film analysis were made in 4%NaOH solution at
598K for 2h (7.2ks) at a constant potential in a platinum container put
into the autoclave in order to avoid any contamination due to dissolution
of the autoclave container.

RESULTS

Alloy 690 has a higher IGA resistance than Alloy 600 . The reason why the
IGA/SCC resistance of thermally treated Alloy 690 is high is thought to be
attributable to both grain boundary carbides precipitation and the
corrosion resistant oxide film. In this paper, the corrosion films of Ni
base alloys formed in high temperature caustic solution were investigated.

Straining electrode behavior

Straining electrode tests were carried out by applying fixed potential
E +50mV [where E is around -0.97V (vs. Ag/AgCl)] corresponding to
the transition range of the active/passive state, ECOrr.+100mV and
E +250mV in the first passive stage, where IGA of Alloy 600 occurs.
Figure 2 shows the effect of chromium content on changes in transient
current densities for Ni base alloys at the fixed potentials E +100mV.
After elongation was stopped, distinct regions in the current decay over
time were observed. That is, the current decay consists of two stages.
Current density in a short period (within around 20ms) immediately after
rapid straining was stopped decays to the formula i α exp (-t )(i: current
density, t: time, n: constant)(named stagel), while densities of at least
up to 5000ms decay to the formula i^t (stage II). It can be seen from
Fig.2 that the effects of chromium content on the current decay curves were
small in concentration ranges of about 0^15wt%Cr, whereas they were large
in concentrations above about 20wt%Cr.
103

75%Ni-23%Cr- 1%Fe
■ 75%NI-15%Cr- 9%Fe
• 75%NI- 5%Cr-19%Fe
Straining stopped - 75%Ni- 0%Cr-24%Fe
• 60%Ni-15%Cr-24%Fe
60%NI-30%Cr- 9%Fe

10° \ > N 75%NI-5

\. ' V ie%Fe
N
N75%Ni-23%Cr- ™ % ■
\ 1%FeX
\ N.
\£0%Ni-30%Cr-s s
X 9%Fe s
\ (Alloy 690)
10 -1
1 10 100 1000 5000
Time (ms)
Fig.2 Effect of chromium content on current transient
curv esin 4%NaOH solution at 553K at the fixed
potential of ECorr.+100mV.
690
In particular, the repassivation rate of Alloy 690, which contains 30wt%Cr,
was considerably larger than that of Alloy 600, which contains 15wt%Cr.

The amount of charge passed in 5s following film rupture-repassivation

process can be obtained by integrating the current decay curves shown in
Fig.2. Figure 3 shows the effect of chromium content on amount of charge
of Ni base alloys in 4%NaOH solution at 553K. This figure shows that the
amounts of charge increased with increasing chromium content above about 15
wt%, and while the amount of charge of Alloy 690 containing 30wt%Cr was
lowered to 1/5^1/10 as compared with Alloy 600 containing 15wt%Cr. This
behavior seems to correspond to the effect of chromium content on the
caustic SCC resistance of Ni base alloys

O: £corr +50 mV
9 : Ecott + 100 mV
Ecorr +250 mV

(Alloy 600)
·:
£ c o r r. +100 mV I

Ecorr. +50 mV
o (Alloy 690)

CO

10°

75%Ni based
Cr content (wt%)
Fig. 3 Effects of Cr contents on amount of charge of
nickel base alloys in 4%NaOH solution at 553K

Fig.4 IMMA analysis of the corrosion film formed on 75%Ni-15%Cr-9%Fe

and 60%Ni-30%Cr-9%Fe alloys at the potentials E and
F . +100mV in 4%NaOH solution at 598K for 2h (7.2ks),corr·
r.orr.

Corrosion film
Figure 4 shows the depth profile of Ni, Cr, Fe and 0 elements by IMMA
the corrosion film formed on analysis of 75%Ni-15%Cr-9%Fe and
60%Ni-30%Cr-9%Fe alloys in 4%NaOH solution at 553K at the potentials E
and E +100mV. corr.
The cCo°rrrbsion film of 75%Ni-15%Cr-9%Fe alloy (Alloy 600) formed at the
 691
potential E (free potential) had a thin film of nickel hydroxide or
oxide as shown in Fig.4(a). On the other hand, the corrosion film of the
same alloy (Alloy 600) formed at the potential E +100mV had a double
layer structure of nickel hydroxide or oxide in outer layer and chromium
hydroxide or oxide in the inner layer, as shown in Fig.4(b). According to
ESCA analysis, it is thought that Ni and Cr were composed of mixtures of
nickel hydroxide [Ni(OH) ] + nickel oxide (NiO, Ni 0„) and chromium
hydroxide[Cr(OH)„] + chromium oxide (Cr«0 ) , respectively. Although the
corrosion film of 60%Ni-30%Cr-9%Fe alloy (Alloy 690) at the potential
E +100mV had a double layer structure, similar to that of Alloy 600,
trie chromium enrichment* in the inner layer was larger than that of Alloy
600, as can be seen in Fig.4(c). It has been confirmed that the chromium
enrichment of the inner layer increased with increasing chromium content,
and that this chromium enrichment in Alloy 690 was about twice as large as
that of Alloy 600.
Thus, it has experimentally been confirmed that the corrosion films of Ni
base alloys in the characterized potential region for IGA occurrence had a
double layer structure in which chromium hydroxide or oxide existed in the
inner layer.

* Chromium enrichment: product of chromium concentration (at %) and

thickness [i.e. sputtering time (sec)] of the inner chromium hydroxide or
oxide layer in the corrosion film obtained by IMMA depth profile of Cr
and 0 elements.

DISCUSSION

It was obtained that the current decay consisted of two stages: the current
density in a short period (within around 20ms) immediately after rapid
straining decayed to the formula iα exp (-t )(i:current density, t: time,
n: constant) (named stage I),_and then the density at least up to 5000ms
decayed to the formula i ^ t (stage II). The fact that current density
follows the formula i α t was already obtained by Shibata et al. in
high temperature Na«S0, and H«B0~ + Na«B,07 aqueous solutions.
It is thought that a monolayer of an oxide film may initially form in stage
I, followed by the growth of the oxide film thickness in stage II.

The value of n was about 0.5 in the low chromium content range of 0 ^
15wt%Cr, which means that the film growth followed the parabolic rate low.

NaOH solution NaOH solution

C n+r F e+ Ni-nyaroxiae
r , *r cFe*♦ C Ni-hvdroxida Cr-hydroxide
' .. Ni-hydroxidel
0 o r kji.oyido '
* 9 | | or Νί-oxide 0 " g £ o x i d e 7 0
P.9?.q? 9.9 99.99 9 9 . . ι—^ «^^wPw^vMiWffl?

(b)

Fig.5 Schematic figures of pH-potential diagram of Cr-H 0 system [(a)]

and the growth of the corrosion film of nickel Dase alloys in
high temperature NaOH solution [(b)]
692
The value of n was increased with increasing chromium content above about
15wt%. The value of n of 30%Cr-60%Ni-9%Fe alloy (Alloy 690) was about 1.0,
which means that the film growth was followed the inverse logarithmic rate
low.
Chromium hydroxide or oxide normally cannot exist stably in high
temperature caustic solutions, as can be clearly seen from the Pourbeix
pH-potential diagram of the Cr-H^O system shown in Fig.5(a).
Therefore, this suggests that the outer nickel hydroxide and/or oxide layer
may act as a protective film, such as a cation selective film. Figure 5(b)
shows schematic figures for the growth of the corrosion film of nickel base
alloys in high temperature NaOH solutions. By considering this, it is
thought that the inner chromium oxide layer can be formed by decreasing pH
beneath the cation selective outer nickel hydroxide or oxide film.
As discussed above, it is concluded that the IGA resistance of Ni base
alloys may be influenced by the repassivation rate and the corrosion film
at the crack tip, and became large the effect of chromium content above
about 15wt% on the repassivation processes in high temperature caustic
solution.

CONCLUSION

Repassivation behavior and the corrosion film of nickel base alloys

containing 0^30wt% chromium were investigated in high temperature NaOH
solution.

(1) The repassivation rate measured by rapid straining electrode

technique was found to increase with increasing chromium content above
about 15wt% chromium.
(2) The corrosion film, formed in the characterized potential region for
IGA(IGC + IGSCC) occurrence, had a double layer structure, that is,
nickel hydroxide or oxide in outer layer and chromium hydroxide or
oxide in inner layer. The chromium enrichment in the inner layer
increased with increasing chromium content.
(3) This behavior seems to correspond to the effect of chromium content on
IGA resistance of nickel base alloys in high temperature caustic
solution.

REFERENCES

1) H. Nagano, K. Yamanaka, K. Kobayashi and M. Inoue (1988):

Sumitomo Metals, 40, 371-382
2) T. Yonezawa, K. Onimura, N. Sasaguri, T. Kusakabe, H. Nagano,
K. Yamanaka, T. Minami and M. Inoue (1985): Proc. of 2nd Ins. Sym. on
Environmental Degradation of Materials in Nuclear Power Systems,
Monterey, California, 593-600
3) A.J. Sedriks, J.W. Schultz and A.M. Cordovi (1979): Boshoku Gijutsu,
28, 82-95
4) M.O. Speidel (1978): The First US-Japan Joint Symposium on Light Water
Reactors, Fuji, Japan, 45-60
5) T. Shibata and R.W. Staehle (1975): Proc. 5th Int. Congr. on Metallic
Corrosion, NACE, USA, 487-492
6) K. Yamanaka and T. Yonezawa (1989): "Optimum Time and Temperature of TT
Alloy 690", EPRI/Alloy 690 Workshop, New Orleans, USA.
7) H.E. Townsent (1970): Corrosion Science, 10, 343-350
8) T. Shibata and S. Fujimoto (1985): Boshoku Gijutsu, 34, 72-78
9) R.B. Diegle and D.A. Vermilyea (1975): J. Electro. Chem. S o c , 122,
180-189
10) F.P. Ford (1982): EPRI, NP-2589, Final Report
 WS8d10

Evaluation of SCC Susceptibility in Austenite

Stainless Steels with Film Rupture Testing Method
M. MURATA and Y.MUKAI
Department of Welding and Production Engineering,
Osaka University, Yamada-Oka 2-1, Suita City,
Osaka, JAPAN

ABSTRACT
Genarally, the susceptibility of stress corrosion cracking
(SCC) is connected with mechano-chemical film rupture process.
Especially, it seems to be the most important to get imformation
about the film repair rate for evaluating the susceptibility of
SCC in austenite stainless steels.
In this paper, the film repair rates of austenite stainless
steels in chloride solutions were measured with digital memory in
film rupture process by hitting the surface with crystal glass
needle. The results are as follows.
A current density was comfirmed to increase till up several
thausands times of a normal static exchanging current density by
breaking the film instantly. In case of film repairing fast, the
susceptibility of SCC increased of which phenomena was found in
type 316 steel.

KEY WORDS
SCC; Film rupture; Austenite stainless steel; Chloride solution

INTRODUCTION
Although the mechanism of APCSCC(Active Path Corrosion type SCC)
used to be explained by a correlationship between passive film
rupture and localized metal dissolution phenomena, it's rare
that the phenomena was measured with enough reliance. In the
paper, the correlationship between SCC susceptibility and
characteristics of electro-chemical and mechano-chemical reaction
was investigated by film rupture testing which was developed in
this study.

693
694

EXPERIMENTAL PROCEDURE

I n t h e s t u d y , s e v e r a l a u s t e n i t i c s t a i n l e s s s t e e l s w e r e u s e d . They
were performed solution treated ( 1373K, 3.6ks, W.Q). The
c h e m i c a l c o m p o s i t i o n s w e r e shown i n t a b l e 1. Film r u p t u r e tests
w e r e p e r f o r m e d w i t h a n e q u i p m e n t shown a s f i g u r e 1 .

Table 1 Chemical c o m p o s i t i o n s of m a t e r i a l s used

Chemical compositions (wt%)

Material
C Si Mn P S Cr Ni Mo Ti
Type304 0.06 0.58 0.86 0.02 0.011 18.33 9.18 —
Type316 0.07 0.73 1.64 0.029 0.010 17.04 11.84 2.24
Type310
[jype321
0.06
0.05
0.74 1.43 0.029 o.olo
ο.βδ 1.46 0.024 0.004
24.81
17.79
19.7
9.97
— —1
0.421

Stopper Working

Condenser

Specimen
Saturated
calomel electrode

20%NaCl+l%Na2Cr207-2H20

KC1 saturated
Heater — aq. solution

Pt.counter

Salt bridge

Fig.1 Schematic illustration of filn

ruputure test

The test specimens were fixed in the corrosion cell which was
filled with corrodents. A passive film was ruptured performed by
a brief striking of a needle made of crystal glass which had the
inartia force gained by springs. As the neutral location of
 695
needle tip was kept away from the specimen surface, the needle
came back to the neutral location immeadiatly after striking it.
The instantaneous electro-chemical reaction at film rupture
moments measured by potentio-stat. In this case, a transition
current at film rupture moment was detected with digital memory
equipment and memory scope under the potential of test specimen
being regulated to natural electrode potential (NEP) by potentio-
stat. As a repling speed of potentio-stat was more than 10kHz
and the transition current speed which was measured by memory
scope was the range from 500Hz to 1kHz, the measured transition
current value with potentio-stat was regarded as enough reliable.
An example of detected transition current with digital memory was
shown figure 2. In this study,42%MgCl2(416K),20%NaCl+Na?Cr?07.
2H20(375K),2.5kmol/mH2S04+0.5Kmol/mNaCl(298K)were used as test
environments.

RESULTS AND DISCUSSION

At first, characteristics of APCSCC was classified by the
correlation between threshold stress and 0.2% proof stress.
In _42%MgCl2 and 20%NaCl+l%Na2Crp07.2H20 solution, threshold
stress depended on yield strength. Namely, an active pass of
localized corrosion seemed to be prepared by film rupture
induced by plastic deformation. So, this type SCC would be
regarded as stress induced SCC (SISCC). On the other hand,
threshold stress was enough low and had no connection with yield
strength in 2.5kmol/mH2SO4+0.5NaCl solution. In this case, as
metal dissolution and selective corrosion were obserbed under
stress free condition, surface film was proved to be instability.
Consequently, the role of stress would be nothing but increasing
corrosion rate. We could classify this type of SCC as stress
assisted SCC (SASCC).

Striking 10: 1 1 r
Austenitic stainless . Λ
steel s ,

SISCC

Peak current
101 304 / U ° 3 1 0 ,
/
20%NaCl+ \ A 3 9v 4 7i6
Ll%Na2Cr207(376K)O^2'|
42%MgCl 2
(416K)
304 Trans
2.5kmol/m3H2S0t+ + ISASCCI
3
10l G0.5kmol/m NaC1 (298k)
k-llms-* 10 10 1
"TO5
/ MPa

F
' 9 · 2 Typical wave at F i g . 3 R e l a t i o n between t h r e s h o l d stress
an
film rupture d 0.2% p r o o f s t r e s s
696

Type304
ΊΟ4 ( 1 1 - ι 1 |i—i I 1 ' ■ ' ' l
3
Γ 42%MgCl Λ Ί f 2.5kmol/m3 H2S0it + 1 f20%NaCl+ol%Na,Cr907 \
416Κ j f 0.5kmol/m NaCl 376K
1 298K r v ^ b cr _J
f M
10Ξ Γ~ /Bare J
f \ fΒΛ Γ ΐ
Uare / Ί
/ 1
= 10 2 d \-
\
\
/
/ A
Γ
/I [ \ Γ\ f
/1 \ 1
ΊΟ1 h
-ρ L /J r
Γ
x
x
! "1
I H
// 1
J \ I
/ A k 1 \ I 1

1' 1
15
10°
X Bulk f A I Bulk \ J h

\ '
Ϊ j L j
!J
10 1 1J
-0.5 -0.4 -0.3 -0.5
i

Electrode potential vs SCE

I t

/
0
μ

1 ,1 , , , i 1 ,..!
1/ Bulk
1 1 1if L i. i. I
-0.5
II

Fig.4 Measurement of polarization curves in film rupture

tests in several environments

Then, we studied about the difference of characteristics of SCC

shown in figure 3 with mechano-chemical approach. As the
properties of passive films is sure to have a important role for
detamination of the type of APCSCC, we tried to apply the film
rupture testing to investigate the nature of passive films of
austenitic stainless steels in several environments.
Polarization curves gained by film rupture tests were shown in
figure 4. In these figures, dotted lines shows the normal anodic
and cathodic polarization curves which was measured under non
striking condition. Polarization curves at film rupture was
measured as follows. At first, a potential of test specimen was
fixed at natural electrode potential by potentio-stat. After the
current being confirmed to be zero, the specimen was striked by
the crystal glass needle. At the moment, remarkable increment of
current was recorded by digital memory. After the testing, the
striked trace on specimen surface was obserbed by optical
microscope with 400 magnifications and calculated the current
density from its mesured area. One dot in the figures was
detaminated by this procedure.
The potential of bared surface which was generated by needle
striking moved to less noble region and exchanging current
density came up to 3 or 4 orders high. This phenomena shows that
the remarkable metal dissolution was sure to be induced by
locally removal of passive film. Especially, concentration of
metal dossolution in nearly nertral solution with dense cholride
ion seemed to be much more than that in strong sulfate acid.
This could be caused by the stability of oxide or passive film in
such environments. In near neutral solutions, the oxide film
could exist comparable stabilizing, even if it contained Chloride
ion. But, once the film was ruptured, a localized metal
dissolution would occur. Because, the repair of ruputured film
 697
was prevented by the local galvanic cell which was formed between
bare surface (less noble part) and coated surface with film
(noble part). In SCC, the film rupture was sure to be originated
by appearance of new surface with plastic deformation. On the
other hand, in acid solution with ramarkably low ph, the oxide
and passive film became more instability. Especially, in case of
the solution containing aggresive anion such as chloride ion, the
surface film could be positively breaked by the film
instabilized. So, the increment of current density seemed to be
rather low compared with nearly neutral solution, because they
had a high background current which was origined to agressive
film rupture phenomena by chemical attack. As mentioned above, a
factor of concentration of metal dissolution at film rupture
moment and repair of film is sure to have a important role of
determinating a susceptibility of APCSCC. Then we aimed at the
ratio of exchanging current density i c o r r and that of bare
surface, it>are which was maeasured that under NEP condition, was
regulated by potentio-stat as a concentration factor of
corrosion. The relation between threshold stress and the ratio
was snown n
of i Q o r r to i-bare * figure 5.
The data of SISCC distributed in high value of the ratio compared
with those of SASCC, that was surely caused by the degree of
aconcetration of corrosion.

150
Γ"
SISCC I -"Π'
|(>310
I
304 I IO304
100 20% N a C U
1%Na2Cr207 j j
376K φΔ3Ί6
NEP I G321
ΕΊe c t r o d e potential I L 42%HgC
£ 50 U__SASCC
D I 416JC |-
2.5kmo"l/mTH7s0(,+
3
0.5kmol/m NaC1

304 + 298K | _L
10 2
10 3 10* Ί0 5 10 6 10 7
("»bare^NEP / ""corr

Fig.5 Relation between the ratio of dissolution current

density of bare surface under NEP condition to
exchanging current density and threshold stress
698

CONCLUSION
APC SCC could be roughly classified to two types, SASCC and
SISCC. In the former, threshold stresses depended on yield
strength. But, in the latter, their existence was not proved.
This defference in APC SCC type, was made clear to base on the
feature of film rupture. Namely, in SISCC, the region of metal
dissolution was localized to film repture point which was occured
by plastic deformation. So, in this case, the threshold stress
depended on plastic deformation in essential. On the other hand,
in SASCC, threshold stress didn't depend on macroscopic yield
stress, this would caused that the film rupture based on chemical
attack of a aggressive anion rather than mechanical effect, such
as slip or plastic deformation.

REFERENCES
P. Doig and P.E.J.Flewitt, " The electrode potential with in a
growing stress corrosion crack ", Proc. R. Soc. Lond. A357, 439-
452.
Y. Mukai and M. Murata: Preprint of The National Meeting of
J.W.S., Vol.34 (1984), 214-215.
Y. Mukai and M. Murata: ibid, Vol.35 (1984), 318-319
 WS8d11

STUDY ON BEHAVIOUR OF STRESS CORROSION CRACKING

OF WELDED JOINT

G.Q. Zhou, Z.X. Chen, J.G. Qi, J.M. Dong, P.L. Fan,

Department of Mechanical Engineering, Xi'an Jiaotong University

Xi'an, China

ABSTRACT

The SCC-susceptivity at the different regions on the welded joint of some

of the low-, medium- and high-strength steels in caustic, nitrate or/and H S
saturated solutions is reported briefly on the basis of some of the
experimental results studied in the past, by the test methods of constant--
load tension, implant or/and cantilever bend with the specimens prenotched
or precracked. The SCC behaviour of the welded joint is also studied by the
technique of electrochemical polarization and the fracture analysis as well.
The critical value <j σ . or/and J at the different regions of
sec t impscc ISCC
the welded joint are compared to each other. The weakness of the mixed
grained region on the heat-affected zone of the joint is noticed prior to
the bond in many cases. The SCC-resistance of the weld metal is closely
related to the welding material used and the problem for the latter to be
properly selected or anew developed is emphasized, though it matches the
the joint well in air.

KEYWORDS
HAZ; welding material; cautic; nitrate; H S; constant-load tension;
2
cantilever bend; implant.

INTRODUCTION
The distinct heterogeneity of microstructure inherent in the welded joint
leads to an inhomogeneity in mechanical and electrochemical properties and
then leads to a quite difference in its resistance to stress corrosion
cracking(SCC) as compared with that of the base metal. However, most of the
work in the past carried on in this field were confined to the base metals
themselves and gave no relevant consideration to their joints. Yet there
was an incorrect impression that the stydy on the welded joint might be
substituted by that on the base metal. The facts are just not in this way.
Even if the weld metal and its bond(fusion zone) were noticed as some
researchers did, the real situation of whole joint could not be fully
exposed.

The SCC-resistance of the welded joint made of various base metals in some
corrosive media was evaluated by us separately at their different regions,

699
700
such as the weld metal(WM), the bond(BD), the coarse grained region(CG),
the fine grained region(FG), the mixed grained region(MG) and the base
metal(BM). The experimental result showed that in the case of multi-pass
welding, the so-called coarse grained zone including the bond would not. be
inevitably the weakest link of the joint and the mixed grained region might
be sometimes the most susceptible for the low- and medium-strength steels.
On the contrary, the regularity of SCC-susceptivity at the different regions
of some high-strength steel joint presented just the opposite. Therefore, a
concrete analysis must be made for the joint in a given material-medium
system so that the SCC-resistance of the welded structure may be truly
estimated.

The study on the SCC-resistance of welded joint is intended on tree sides.

The first mission is to evaluate the behaviour of the base metal itself.
Some of the metals which are SCC-resi.stant in their supplied condition
may be quite susceptible at the heat-affected zone(HAZ) when welded to be
a joint and may evidently influence the susceptivity of the weld metal.
Actually, it is a problem of weldability in a broad sense. The information
obtained by the investigation on the welded joint may be fed back to the
metallurgical plant for the improvement of the metal.

Secondly, some of the welding material(e.g., covered electrodes, etc.)

usually matched well for the welded structure working in air may be
sometimes not suitable to that working in a given corrosion medium. Study
on the weld metal shows that it is more exact to believe its resistance to
SCC mainly affected by the microstructure and other metallurgical factors
than to consider any relation to its strength level. So it is indispensable
to develop some new type of welding material special for a given metal-envi-
ronment system.

The third focal point of study is to pursue an appropriate welding

technology including the preheating or/and the postweld heat-treatment in
some cases. The heart of the matter is to adjust the welding thermal cycle
so that an optimum microstructure transition may be achieved on the HAZ and
the weld metal to improve SCC-resistance.

The following are the essentials summarized from a part of the researches we
did in The Welding Division of Xi'an Jiaotong University on the welded joint
of some of steel.with low-, medium-and high-strength. The authors have to
express their regret for that all the figures are omitted in this paper due
to the limited space.

LOW-CARBON STEEL WELDED JOINT

The SCC-susceptivity was studied on both the plain low-carbon steel A3 and
the boiler, low-carbon steel 20 welded joints. The base metal was specially
grooved and was mutil-pass weeded with three kinds of covered electrodes
E4303, E4315 and E5015 respectively, and in another group of experiment was
single-pass submerged-arc welded. The flat notched specimens according to
ASTM E8-79 for the constant-load tension test and the rectangle precracked
ones according to ASTM 813-81 for the cantilever bend test were prepared
with their notch or precrack at different regions of the joint and were
checked metallographically. All the specimens were as-welded. Two liquid
media, the caustic 35%NaOH+0.125%PbO and nitrate 60%Ca(NO^) +3%NH NO„ were
3 2 o 4 3 o
used as the test solutions at their boiling temperature 120 C and 150 C
respectively. The experimental duration lasted 200 hrs for the caustic and
150 hrs for the nitrate.

The critical values a and J affirmed on the relation curves of

sec Iscc
 701
the initial applied stress ( 0".) or the initial J-integral (J .) versus the
time to failure of the specimen in both solutions are listed in Table 1.
It shows that the value σ is maximum at the fine grained region and
that at the mixed grained region is the lowest on the HAZ. It was shows
also that the maximum value of J is located at the fine grained region
ISCC
and the value of the base metal 20 in L-T orientation is higher than that
of both the bond and the weld metals with an exception of the E5015 weld
metal.
Table 1. Critical value a and J of low-carbon
sec ISCC
steel welded joint in boiling nitrate and
caustic solution.

Region ia_§iJtrate . in caus tic

a i N/mm J N/mm <T , N/mm1 J
sec iscC sec iscc' N / m m
WM E4303 265.3 0.98 407.6 6.50
WM E4315 269.5 1.20 442.3 9.41
WM E5015 — 8.65 — *
BD 324.8 3.46 -- *
FG 491.7 7.24 -- *
MG 300.2 2.25 450.9 *
BM 20g 231.2** 5.06*** 375.9** •

BM A3 -- 4.58*** -- *
* unfractured until 200 hrs; ** in T-s orientation; ***in L-t orientation.

To sum up, the bond of a multi-pass welded joint does not be the most SCC-
susceptible on the HAZ but the mixed grained region must be taken seriously
if the weld metal does not be taken into account. As to weld metal, the low
hydrogen type electrode E4315 is distinctly better than that of the lime
titania type E4303 of the same strength grade. The electrode E5015 of
higher strength grade seems to be the best choice which is proved owing to
relatively less developed proeutectoid ferrite crystallized from the molten
pool. The steel 20g is less SCC-susceptible than the steel A3 and the base
metal will be much susceptible if it is in T-S orientated. It is proved by
additional fracture analysis by SEM and the technique of potentiodynamic
polarization as well, the boiling mixed nitrate may be used as an accelera-
t i n g solution instead of the caustic.

LOW-ALLOY MANGANESE STEEL WELDED JOINT

The low-alloy manganese vessel steel 16MnR was used together with the steel
20 for comparison. The implant method which was proposed by Granjon,H. and
has been successfully used for the study of welding cold cracking, etc., was
used owing to its many advantages e.g., saving the metal and the time to
prepare specimens. The <f>Q cylindrical implant (specimen) is slightly altered
to suit to the test. The notch on the end of the implant is prepared
parallel( II) or perpendicular(i) to the rolling direction of the steel plate
and is located at the different regions of the joint by varying its height
to the top. A single bead is deposited on and across the outside of the
back plate and the top of the implant by the covered electrodes E4303, E4315
and E5015 respectively.

The test duration in boiling nitrate solution lasts 150 hrs, during which if
the implant does not be ruptured, the applied stress σ. will be regarded
imp . J. J
as the critical value or criterion and σ . termed. The CT. tested
impscc impscc
on steel 20 together with the values σ and J nnn at the different
g sec ISCC
regions of tne multi-pass metal-arc and the single-pass submerged-arc welded
702
Table 2. Comparison of <T with C and J of
. impscg . sec .ISCC
20g steel HAZ in boiling nitrate solution.

Test method Criterion BD FG MG BM

Implant(single-pass) σ . , N/mm 260 419 349 256( II )

imoscc 2
Submerged-arc (single-pass) σ / N/mm 274 420 359 288(11 )
S C
Metal-arc a ° » N/mra 324.8 491.7 300.2 231.2(11)
J N/mm 3'46 7#24 3*25 5 ·0 6 ( Π )
(multi-pass) TSCC'

butt joint are listed in Table 2. This comes to that for the single-pass
welded joint the critical value varies in the same regularity, i.e., in
sequence from high to low as FG-MG-BD, regardless of the test and welding
method. The values σ . and o are very close to each other and the
impscc sec
former is lower than the latter. The values σ. and J of the
impscc ISCC
weld metal made of different electrodes on 20 steel, joint in nitrate are
listed in Table 3. It displays the same regularity,too. The value G .
impscc
of steel 16MnR at different regions of the joint in boiling nitrate are
listed in Table 4. The sequence of the SCC-resistance varies identically
with those of steel 20 but the former is generally higher than the latter
in absolute value so that even the bond seems not too weak as compared
with the base metal.

Table 3. Comparison of σ. with J of 20 weld

impscc ISCC g
metal by different electrodes in nitrate solution.

Test method Criterion E4303 E4315 E5015

, 2
Implant(single-pass) O, , N/mm 100 148 328
impscc ,
Metal-arc(multi-pass) J N/mm 0.98 1.20 8.65
iscC

Table 4. Critical value σ. of steel 16MnR at

impscc
different regions in nitrate solution.
BM
Region BD FG MG „ 1
, 2
G. i N/mm 347 644 528 300 394
impscc

The experiment leads to a noticeable result, i.e., the bond of single-pass

welded joint either of the steel 16MnR or of the steel 20 or A3 is most
g
susceptible to SCC on the HAZ in nitrate. It shows once again that the
common covered electrode or the weld metal is too weak to match the joint.

PIPELLINE STEEL WELDED JOINT

The 500 MPa grade, 8mm thick pipeline steel X52 and T/S 52K as well were
submerged-arc welded by both side single-pass with the wire H08Mn2Si(WI) for
the inside and the wire H08MnA(WII) for the outside matched with the fused
flux S771. The flat notched specimen prepared from the outside was used for
the test in nitrate and the cylindrical notched specimen prepared from the
inside was used referring to NACE TM-01-77 for the test in H S solution. All
2
the specimens were in T-S orientated. The test duration in nitrate was
limited up to 150 hrs and that in H S was up to 400 hrs. The value
2
as well as its ratio to the yield strength of base metal in air tT / sec
<7
are lasted in Table 5 and Table 6. The SCC-resistance of X5"2 joint at
different regions in nitrate are arranged in sequence from high to low
 703
Table 5. σ and σ /σ of steel X52 welded joint and
sec sec s
the BM of T/S 52K in nitrate.

Steel X52 Γ/S 52K

Region WM(WI) WM(WII) BD FG MG BM WM BM

, 2
O , N/mm 299.9 172.7 272.4 337.1 291.1 307.7 147 .0 303.8
sec ,
σ /σ , % 83.8 48.3 76.0 94.2 81.4 86.0 41 .7 86.1
sec s

Table 6 σ and a /a of s teel X52 welded joint at

sec sec. s
different regions in H S at room temperatuire .

Steel X52 T/S 52K

Region WM BD CG FG MG BM BM
, 2
C , N/mm 225.4 143.1 178.9 232.5 214.6 153.8. 286.2
sec
e > % 63 40 50 65 60 43 80
sec s

as FG-BM-WM(WI)-CG-WM(II). All of them are high enough no less than o.76 σ

s
at the bond with an exception of the WM by wire II, which is too susceptible
to SCC to be accepted. It indicates that the wire H08MnA used for the out-
side of the pipe is quite not suitable, even though it matches well in air.
On the contrary, the wire H08Mn2Si may be give a WM much increased in its
resistance. As to the BM, both of them show a quite similar behaviour in
nitrate.

The SCC-resistance of the steel X52 joint at different regions in H S are in

sequence from high to low as FG-WM-MG-CG-BM-BD. All of them are much lower
as compared with those in nitrate. It is spectacular that the resistance of
steel X52 BM is so low as about similar to that at its bond and is nearly
half of the T/S 52K BM.

The experiment by the potentiodynamic fast-and—slow sweep technique in

nitrate shows that both the weld and BM of two steels are not susceptible to
o o
SCC up to 40 C. The susceptivity becomes more distinct at 55 C, especially
for the WM. The temperature at which the appearance of SCC initiates is
o
estimated about 50 C.

The fracture analysis shows that the welded joint in nitrate is ruptured
intergranularly due to anodic dissolution while there is a lot of distinct
feature of hydrogen embrittlement on the fracture in H S . As to the distinct
difference on the SCC-susceptivity of both steels in both solutions, the
cause may be found out from the metallurgical quality which influences: much
more in H S than in nitrate. Clearer banded structure and therefore more
2
secondary cracks along the rolling direction as well as more inclusions
observed on the fracture of steel X52 as -compared with steel T/S 52K may
be evidence for the conclusion.

HIGH-STRENGTH STEEL WELDED JOINT

The low-carbon low-alloy high-strength steel HG80 which was quenched and
tempered to strength grade of 80 MPa was used for the study of the effect of
microstructure on the SCC-susceptivity of its welded joint. The cylindrical
and the flat notched specimens for the constant-load tension in H S at room
temperature and in nitrate were welded with the covered electrode L80.Those
simulating the HAZ were individually obtained by synthetic HAZ. The values
704
Table 7. σ and σ /σ of steel HG80 welded joint at
sec sec s
different regions in H S and in nitrate.

Region in H S_ i n
T
ni trat e
0 , N/ 2 2 o / σ , % o
sec
, N/ 2 σ /
s
%
sec mm sec s mm sec
WM 88.1 10.4 750 87
CG 157.3 18.6 85 10
FG 175.8 20.8 75 9
MG 88.0 10.4 505 59
BM 131.3 15.5 251 29

σ and σ /σ as well in both solutions are listed in Table 7. The SCC-

sec scc s
susceptivity in H S is arranged from high to low in sequence as MG-WM-BM-
CG-FG and that in nitrate as FG-CG-BM-MG-WM. The fracture analysis by SEM
and TEM shows that the high-density dislocation of the martensite or the
tempered martensite and the intermittently distributed carbide along the
grain boundary may be the main reason causes the decrease of SCC-resistance.
It shows that the microstructure of MG on which a lot of martensite islands
especially at the triple-angle grain boundaries may be observed. The frac-
ture presents a distinct feature of hydrogen embrittlement in H S and
cracking propagates mainly along the boundary in nitrate. When tested in
the latter, the existance of a-lot fine globular martensite islands which may
stock up the passage of anodic dissolution, seems to be the reason why the
SCC-resistance of the MG is so much higher as compared with the other ones
on the joint.,

CONCLUSION

The SCC-resistance at the different regions of the welded joint is quite

different from that of the base metal so that an attention must be paid
particularly to the joint and the study on it cannot be substituted by
that on the base metal itself. The mixed grained region on HAZ of the
multi-layer or/and -pass welded joint of the researched low- and medium-
-strength steel presents most susceptible to SCC in the tested media and
only in the case of single-pass welding the bond may be the weakest link
of a joint. On the joint of a researched high-strength steel in a given
solution, the SCC-resistance at the mixed grained region may be increased
to the highest as compared with those at the other ones of HAZ. The SCC-
susceptivity of the base metal is related closely to the orientation of
the cracking propagation. The SCC-resistance of the weld metal may be
either the highest or the lowest on the joint according to its microstruc-
ture and the welding material used. Proper selection or development of
the welding material for a given metal-medium system is believed to be
a problem of great importance.

REFERENCES
Granjon, H. et a M l 9 7 3 ) . Implant method at the Institut de Soudure.
Construction and Br. Welding J., No.10.
Chen, Z.X. and G.Q. Zhou, et al(1987a). Stress corrosion cracking of welded
joints in caustic and nitrate solutions. Proc. 10th ICMC.
Chen, Z.X. abd G.Q. Zhou, et al(1987b). Subcritical propagation of SC-crack
of welded joints in caustic and nitrate solutions. Proc. 10th ICMC.
Zhou, G.Q. et al(1988). Study on stress corrosion cracking of welded joints
implant method. Paper IIW Asian Pacific Regional Welding Congress.
Zhou, .G.Q. et al(1990). Stress corrosion behaviour of pipeline steel welded
joint. Proc. Conf. Pipeline Technology, Ostend Belgium.
WS8d12

FAILURES OF THE ORTHOPAEDIC FIXATION DEVICES

J.K.PIRS

Department of Technology, Technical Faculty Rijeka

Narodnog Ustanka 58, 51000 Rijeka, Yugoslavia

ABSTRACT

Fractures of prosthetic hip joints were investigated to determine the cause

of failures. The fractures of cast Co-Cr base alloy showed that the
fracture resulted from the propagation of one crack from the surface on the
outher radius of the bend. Partly irregular fracture resulted in the final
stage being caused also by segregations. The failure of the subject T-28
prosthesis from 316 L stainless steel was caused by initiation and propa-
gation of a number of stress corrosion cracks which originated from the
inner surface of the bend in the stem where the residual tensile stresses
were introduced during the production process.

KEYWORDS

Cast Co-Cr base alloy; 316 L stainless steel: prosthetic hip joints;
stress corrosion cracking.

INTRODUCTION

For many centuries materials have been implanted in human body for surgi-
cal and dental purposes. With the developments in radiography and corro-
sion resistant alloys in recent years there has been an enormous increase
in the number of prosthetic devices. Comprehensive reviews of the deve-
lopment of metallic implants have been given (Bechtold et al., 1973;
Weisman, 1967). As the use of implanted devices hav increased there has
been a corresponding increase in the number of mechanical failures. Some
investigators (Cohen, 1966; Cahoon and Paxton, 1968; Colangelo and Greene,
1969; Dockal, 1972) have observed that general corrosion attack has
contributed significantly to the ultimate failure. In other instances
(Rose et al., 1972) corrosion pits have served as initiation sites for
subsequent fatigue cracks which lead to fracture. A number of cases where
material defects have resulted in fracture, have also been reported

705
706

(White and Le May, 1975). Stress corrosion cracking of the alloys commonly
used and under the conditions present i n v i v o is a rare occurrence
(Scully, 1967; Zitter and Schaschi - Outschar, 1981). Some authors
(Charosky et al., 1973) studied failures of fixation devices, where it was
clarly shown that mechanical failures can occur in cases where no metallur-
gical defects are present. These failures might result from the problems in
disign, but in most cases the high loads leading to failure result from
the patient activity before the bone completely heals. Other authors
(Grover, 1966; Pirs, 1985) showed that for the failure of endoprotheses
broken in fatigue, the number and distribution of microporosity was also
responsible. This paper presents additional examples of implants which have
failed i n v i v o where examinations of the prosthetic hip joints have
been conducted to determine causes of failure, with special attention to
stress corrosion cracks.

MATERIALS

A vast percentage of the surgical implants are made mainly from three
types of material: 316 L stainless steel, the cast Co-Cr-Mo-C alloy and
Ti - 6A1 - 4V alloy. During this investigation, the orthopaedic fixation
devices which were produced from stainless steel and cast Co - Cr - Mo
alloy, which failed during service life, were investigated. The chemical
composition of the investigated devices is shown in Table 1.

Table 1. The chemical composition of the

investigated fixation devices in wt.%

Element Stainless steel Cast alloy

c 0.01 0.25
Si 0.62 -
Mn 1.65 0.7
P 0.015 -
S 0.007 -
Cr 16.85 27.2
Ni 13.70 2.7
Mo 2.08 4.7
Co - base
Fe base 1.7

From the results in Table 1 can be concluded, that in accordance with ASTM
standard for surgical implants F 55 - 71, the investigated stainless steel
was 316 L quality. According to ASTM standard F 75 - 67 the investigated
cast alloy was standized Co Cr Mo casting alloy known under various trade
o
names. Material subjected to homogenization treatment at 1180 C
 707

exhibits an austenitic structure with interdendritically precipitated

chromium - molybdenum block carbides type M C . The hardness is between
200 and 300 HV.
The structure of the hip joint made from stainless steel was lightly cold
worked austenic steel, having a hardness of 23 HRc.
PROCEDURE AND RESULTS

Investigation of broken prosthetic hip joints, which failed i n vivo

were conducted to determine the causes of failures. Fractography was
done, using the SEM (Scanning Electron Microscope) together with metallo-
graphic laboratory techniques. This study indicates that two completely
different fracture modes were obtained. In the case of the fixation device
made from cast cobalt-chromium-molybdenum alloy, fracture occurred in the
stem, at a location approximately 4.3 centimeters from the tip Fig. 1.
No other cracks on the surface were observed and the fracture resulted
from the propagation of only one crack. As can be seen from the results
of investigations of the fractured surface on behalf of the scanning
electron microscope, Fig. 2, the origin region of the fracture was at the
outer surface of the stem, where first striations characteristic of
fatigue failure were observed, but later brittle fracture mode was
observed.

Fig. 1. Fracture of the fixation device made from

cast cobalt-chromium-molybdenum alloy
A different fracture mode of the hip joint made from stainless steel
was observed. The fracture resulted from the propagation of two separate
cracks, originating on opposing sides of the stem and which propagated
towards each other. The two cracks initiated on parallel planes that were
slightly displaced relative to each other, perpendicular to the stem axis.
Fracture occurred in the stem at a location approximately 8.2 centimetres
from the tip. The two cracks which propagated and joined together, formed
a step like fracture surface. A large portion of the fracture topography
708

Fig.2. Result of the fractographic investigation of the

fractured surface of fixation device from cast alloy

Fig. 3. Fractography of the fixation device made from

stainless steel

Fig.4* Details from Fig.3

a) surface crack
b) stress corrosion cracks
 709
has been destroyed during the rubbing of the two fracture surfaces,
obtained during the failure of the stem, a common occurrance in progre-
ssive failures. In addition to the fracture of the stem, there are several
parth-thru cracks which extend from the inner surface, i.e. the surface
on the inner radius of the bend. These secondary cracks are present both
above and below the plane of fracture Fig.3.
In Fig. 4 we see the results of fractographic examinations of the cracks
present on the surface of the bend produced from stainless steel and
also on the fractured surface of the bend. The cracks on the fractured
surface of the stem are typical stress corrosion cracks.

CONCLUSIONS

In the two implant failures examined, there was evidence of two completely
different fracture modes.
In the case of the fixation device made from cast cobalt-chromium-molydbe-
num alloy brittle fracture mode of the stem was observed. It appears that
the fixation device was subjected to high loads which resulted in stresses
above the fatigue endurance limit of the cast cobalt-chromium-molybdenum
alloy. This could occur that either the design was inadequate for the
expedted loads, or the loads imposed on the component were larger than
expected.
The failure of the subject prosthesis, made from stainless steel was
caused by initiation and propagation of two cracks one of them being a
fatigue crack, which initiated at the outside surface of the bend and
propagated across the section. On the inner surface of the bend in the
stem, there were also cracks present. These cracks reducted the load
carrying capability of the stem such that the stress levels in the
remaining section were increased above the endurance limit of the ma-
terial. The final failure occurred when the fatigue crack approached one
of these cracks and the remaining ligament could not support he applied
load.

REFERENCES

Bechtold,C.O., Ferguson, A.B. and P.E. Lang (1959). Metals and Enginering
in Bone and Joint Surgery The Williams and Wilkins Comp Baltimore
Charosky, C.B., Bullough, P.G. and P.D. Wilson (1973). Total hip
Replacement Failures. J.Bone and Joint Surg. 55-A, 49-58.
Cahoon, J.R.and H.V. Paxton (1968). Metallurgical analyses of failed
orthopedic implants J.Biomed. Mater. Res. 2_, 1-22.
Cohen, J. (1966). Performance and failure in Performance of Surgical
implants in orthopedic surgery. J.Materials I_, 354-365.
Colangelo, V.J. and N.D.Greene (1969). Corrosion and fracture of Type 316
5MO orthopedic implants. J.Biomed. Mater. Res. _3' 247-265.
Dockal, C. (1972). Corrosion behaviour of implantation materijal for arti-
fical joints, Sulzer Tech. Rev. 19-10.
710

Grover, H.J. (1966). Metal fatigue in some orthopaedic implants J. of

Materials, JL, 354-365.
Pirs, J.(1985). Untersuchungen zur Deutung des Danerschwingverhaltens von
CoCrMo-Gusslegierung dargestellt an Brüchen von Endoprothesen. J. Werk-
stoff tech. 26, 239-246.
Rose, R.M., Schiller, A.L.and E.L. Radin (1972). Corrosion accelerated
mechanical failure of a Vitallium Nail-Plate J.bone and Joint Surg.
54-4, 854-862.
Scully, S.C. (1967). Kinetic features of Stress - corrosion cracking,
Corrosion Science, 1_, 197-207*
Weisman, S. (1967). The Skeletal Structure of metal Implants.
In: Biomedical and Human Factors Symposium ASHE New York pp.87.
White, W.E.and I.Le May (1975). Optical and electron fractographic stu-
dies of fracture in orthopaedic implants. Microstructural Science Vol.3,
part 13, 911-930.
Zitter, D. and D.Schaschi - Outschar (1981). Schadensfälle an chirurgischen
Implantaten und deren Ursachen. Werkstoffe u. Korrosion, 32, 324-331.
WS8e1

CATASTROPHIC DAMAGE PHENOMENA: AN IN-SITU CRACK-TIP STUDY

Vinod S. Agarwala

Aerospace Materials Division

Naval Air Development Center
Warminster, PA 18974-5000
U.S.A.

ABSTRACT

The effects of naval environment on mechanical behavior of critical aircraft components of

high strength steels and aluminum alloys have been catastrophic in nature. The sudden loss of
strength under high stresses in the presence of moisture and saline atmosphere have been
attributed to only those processes which occur at cracks, crevice and defect sites. The
study involved in-situ experiments at the crack tip to determine the role of electrochemical
parameters: metal dissolution, hydrogen evolution and permeation. Methods were developed to
make transient potential and hydrogen measurements at the crack tip under dynamic test
conditions. The effects of hydrogen on the lattice parameters were studied by neutron
diffraction analysis. The results suggested hydrogen evolution reaction and diffusion
playing a prominent role in the embrittlement of the region ahead of the crack tip, and which
governed the fast fracture. The contributions of environmental effects on bulk surfaces were
insignificant in catastrophic failures.

KEYWORDS

In-situ experiments; high strength steels and aluminum alloys; naval environment; crack-tip
potential; hydrogen permeation; neutron diffraction; cathodic processes.

INTRODUCTION

Premature failures of critical load bearing structures of aircraft due to environmental

effects are major naval problems. These problems are even more intensified as higher
strength alloys are used. In large structures, as in aircraft, the existence of subcritical
flaws which go undetected by non-destructive 1βΰηηίςμβ8, is considered normal and acceptable.
However, these subcritical flaws or cracks have been found to grow in naval environments of
high humidity, salts and service stress, and ultimately, causing sudden failures under
dynamic (fatigue) and/or static stresses. The determination of the mechanisms by which this
subcritical cracks grow in high strength aircraft alloys is vital in the development of
better understanding for the materials and design criteria for structures. It also helps to
device methods of protection.

It is mostly believed that every crack that ultimately grows to cause catastrophic failure is
environmentally induced. The fresh cracks provide a sufficiently high surface energy for a
condensed phase of moisture to form, and impose chemical conditions and the reaction rates
that are very different from those occurring on an open surface or bulk solutions. Several
mechanistic questions related with the role of environment on the crack growth parameters
have been raised. Some of these have been explained based on the theoretical consideration
that sub-critical cracks ultimately grow to cause cracking damage (Brown, 1972). Most

711
712
theories, to date, address high crack growth rates based on the following mechanisms : (i)
the active path or anodic dissolution of metal; (ii) the hydrogen induced lattice decohesion
or embrittlement, and (Hi) the reduction of surface energy at the crack-tip by specific ion
absorption.

In an earlier study some theoretical concepts were developed to understand the mechanisms of
crack growth in high strength alloys (Agarwala, 1984). It was assumed that certain
electrochemical and mechanical factors dictated the crack tip processes, and if controlled,
could lead to inhibition of cracking. This approach was most successful, and a product
called DNBM was developed. It was a unique chemical formulation (system) producing several
fold increase in the fatigue life of the materials tested. However, this study was not
directed to any experimental verifications of theoretical concepts. It is highly possible
that the crack growth rate (CGR) controlling step may be one single mechanism which has not
be identified yet. A differentiation between the mechanisms considered should be made with
sufficient experimental evidence.

Most crack growth rate measurements have been made in quasi-transient state conditions, i.e.
over a time scale that extended well beyond the state where transient phenomena occur, and
after the initial stress has been applied (Troiano, 1960; Oriani, 1978; Pao and Wei, 1979;
Hirth, 1980). The literature model predictions were primarily based on defining the physico-
chemical processes occurring either after the cracking, or in quasi-steady state conditions
(Oriani et al., 19 ; Rice et al., 1978). Recently, few studies have been made which deal
with the measurements and characterization of crack tip processes occurring during the
transient crack growth (Chung et al., 1985; Pickering, 1986). The studies of Turnbull (1983)
and coworkers (Turnbull et al., 1987) were probably the first few which attempted to measure
the electrode potentials at the crack tip. However, these studies were made using the bulk
solution approach to measure the values. Under dynamic stresses the hydrodynamic forces
produced at the crack tip will alter in-situ chemistry if there is bulk solution. Wei et al.
(1986) have attempted some indirect approach to study the electrochemical processes in-situ.
In a recent paper by Turnbull et al. (1988) an experimental approach to determine electrode
potential in situ during corrosion fatigue was reported. It, however, dealt with the test
condition which was totally immersed. Hence, an experimental approach was required where
high humidity and saline environment is not represented by a bulk solution.

The study must involve measurements of potentials at the tip of an advancing crack in order
to determine the active/passive nature of the crack-tip surface and also the nature of the
electrochemical situation existed. If hydrogen is produced at the interface, it must be
measured in-situ to determine if the elastic and plastic zones ahead of the advancing crack
control the diffusion of hydrogen. The presence or effects of hydrogen in the metal lattice
must be determined in order to identify its resident sites. In this study, the role of
electrochemical parameters at the crack tip has been determined during transient crack growth
under environmentally enhanced cracking of high strength steel and aluminum alloy.
Experiments have been designed to make in-situ measurements of corrosion potential and [H].
The electrochemical permeation and the neutron scattering techniques have been used to
determine hydrogen [H] and its effect on metal lattice parameters.

EXPERIMENTAL PROCEDURE

Materials and Mechanical Tests

The materials used for in situ studies were AISI 300 M steel and AI 7075-T6 alloys of 280-300
ksi (1930-2070 MPa) and 76-82 ksi (520-560 MPa) ultimate tensile strength, respectively. A
number of fracture mechanics test specimens were designed, specifically to accommodate for
in-situ measurements of open-circuit potentials and pH at the crack tip, and for the
determination of hydrogen in the elastic-plastic zones ahead of the advancing crack. These
designs were as shown in Figures la and lb. A compliance relationship was established
between the fracture mechanics specimens with, and without (holes) modifications. Their
transient crack growth parameters in terms of crack growth rate and stress intensity factor
were determined and compared. The measurements under a static (constant) load were performed
on a cantilever beam creep test frame. The initial loads applied at the tip of the crack
were based on the starting stress intensities of 12 MPaVm and 35 MPa\/m for the aluminum
alloy and steel, respectively. For fatigue tests, a MTS Alpha System was used and, CT
 713
specimen were cycled at a frequency of 0.1 Hz and load ratio of 0.1. Transient
electrochemical potential and the crack length measurements were made as the crack
propagated.

The compact tension (CT) and double cantilever beam (DCB) specimens used for the measurement
of potential or pH contained four holes for insertion of reference micro-electrodes. These
holes were 2mm in diameter and 7mm apart from each other. The holes extended to
approximately 2mm beyond the plane of the tip of the notch. The first hole was made such
that tip of the pre-crack would be just above it, and would open up for exposure as soon as
the crack growth occurred under stress and environment. Fatigue tests were performed on
these specimens to determine their crack growth compliance with that of the conventional
specimens, i.e., without modifications (holes).

Crack Tip Potential Measurements

The reference electrodes used to measure potential or pH were silver/ silver chloride,
Ag/AgCl, micro-electrodes. They were specifically designed and prepared as follows. Half
the lengths of silver wires, approximately 1 mm in diameter and 40 mm long, were anodized in
2M HCl at about 20 mA/cm 2 current density to deposit a thick coherent film of AgCl on the
surface. The bare metal end was spot welded to a lead wire for contact and then encased in a
thin glass tube of 2 mm outer diameter with bare metal end sealed by epoxy. The AgCl
deposited end was about 0.5 mm recessed with the edge of the other end of the glass tube so
that when inserted into the holes of the compact tension specimen, the Ag/AgCl electrode does
not touch the specimen in the hole. Figure la illustrates the schematic of the electrode
assembly in the compact tension specimen. The electrodes and the specimen holes were kept
dry before the assembly was wax sealed. This was necessary in order to keep the Ag/AgCl
electrodes inactive before the test.

For the measurement of crack tip potential, the reference electrode and the specimen were
connected to a transient recorder, a Nicolet Digital Oscilloscope, through a Keithley
Electrometer. A cotton plug soaked with salt (NaCl) water was inserted into the notch of the
specimen for creating moist-chloride environment at the tip of the crack. As the specimen is
stressed or fatigued, the environment condenses at the crack tip and leads to accelerated
crack growth. When this crack tip reaches the first Ag/AgCl electrode, the condensed film
containing chloride ions activates the electrode and thus, enables the measurement of
potential at that location. Since it is a transient phenomenon, the lowest or most negative
potential recorded would represent the crack tip potential. Under the open circuit
condition, the potentials would be generally highly positive, signifying the high impedance
between the electrode and the specimen. Both the steel and aluminum alloy specimens were
tested for determining the crack tip potentials.

Hydrogen Permeation Experiments

In-situ measurements of hydrogen in the vicinity of the crack tip was made by electrochemical
permeation method reported elsewhere (Berman et al., 1988). In this particular case, the
source of hydrogen was reactions at the crack tip and not cathodic charging of the surface,
and the hydrogen oxidizing cell was fabricated within the compact tension specimen as shown
in Figure lb. The specifics of this experiment are as follows. The thickness side of the CT
specimen was drilled to create a hole of 9 mm diameter x 30 mm long in size. The bottom of
the hole was machined flat and polished , and was kept exactly 2 mm above the plane of the
notch-tip. The position (distance) of the hole relative to the tip of the notch was varied
so that all possible elastic and/or plastic zones can be studied for hydrogen permeability
and concentration. The bottom of the hole was potentiostated to about -0.500 V vs. SCE in
0.1 M NaOH solution to oxidize hydrogen. This potential was sufficiently negative to
minimize anodic currents arising from the dissolution of steel, and anodic enough for
oxidation of hydrogen. The side of the hole was either coated with epoxy or covered by a
teflon sleeve so that only the bottom surface area was involved in the current measurement.

The measurements of hydrogen were made at the crack tip with and without stresses and when
the notch was exposed to sodium chloride containing moist environment. Generally, it
required 6-8 hours to get a background steady state permeation current, which must be less
than 0.1 μ Α / c m . Due to the involvement of very low current measurements, it was desired
that the experiments be performed in a Faraday Cage to avoid low frequency interference in
714

ELECTROMETER

<-CRACK GROWTH PLANE

(a )
Fig 1 Modified CT specimen for in-situ electrochemical measurements at the crack-tip:
(a) set-up for potential with Ag/AgCl reference electrodes; (b) set-up for hydrogen
permeation measurements (0.040 in.) above the plane of the crack.

Δ OeAERA
DT E

-oee

-o.ee

-1Λ4 / /
-132

4 00 08 0 O
120 106 0 200 0

EXPOSURE TIME, HOURS <HUNDREDS)

LOO CURRENT DENSITY, A/Cm» 2

Fig. 2. Transient crack-tip potentials for Fig. 3. Cathodic polarization behavior for 300M steel
AI 7075-T6 alloy in 1% NaCl. showing hydrogen evolution potential range.

1.2 \~15 0 MPa/ffl 15 MPa / W 0 MPa/W

-
MPa/W

| i.o - 1 \ -
< _ / " ~ \ y^~~
a 0.8
-
-Z0.6 II 1 l
60 120 180 240 300
Time / Min

Fig. 4. Effects of stress on hydrogen permeation transients for

300M steel obtained from the zone ahead of the crack-tip.
 715
the current transient measurements. The proving rings were calibrated to about 1000 kg load
and a clip gage was used to determine the crack opening displacements. Since the CT specimen
is polarized in the hole, the loading fixture was insulated at the contact areas. The
experiments were performed to determine the effects of stress and environment at the crack
tip as they reflect upon the hydrogen permeation transients. Hydrogen permeation experiments
were not performed on Al alloy due to difficulty in keeping the surface free of oxide or
without causing anodic dissolution. The determination of hydrogen diffusion parameters for
stress relieved 300M steel was made independently using 0.8 mm thick plates and the
Devanathan and Stachurski permeation cell (Devanathan et al., 1960). The purpose of these
experiments was also to determine the effect of pH and also the levels of hydrogen required
to charge so that a measurable hydrogen permeation current can be obtained.

Neutron Diffraction Studies

The effects of hydrogen on lattice parameters near the crack tip, as it enters the metal
during processing and/or corrosion, were determined using an intense neutron pulse source
(IPNS). This was a unique approach in this research to determine and map out the location of
hydrogen during in-situ measurements. Neutrons can penetrate bulk iron and steel samples,
and neutron diffraction therefore affords an opportunity to monitor lattice dilation from the
incorporation of hydrogen. Since only low levels of hydrogen, less than 1 ppm, are involved
in the mechanical failures of high strength steel parts (landing gear etc.), only small
lattice dilations were expected. Thus, a high flux neutron scattering technique may offer
the needed resolution.

A General Purpose Powder Diffractometer (GPPD) at IPNS Laboratory (IPNS Report, 1983-85),
Argonne National Laboratory, IL, was used. The scientists of Argonne National Laboratory,
collaborated in this effort. The GPPD could provide a resolution of 0.0001 A. The compact
tension specimen was mounted in a proving ring fixture before it was placed in the neutron
beam chamber. The neutron beam from the IPNS pulses at 30 Hz and was of size, 2 mm X 2 mm X
25 mm. It was projected toward the notch of the CT specimen such that it positioned itself
in the elastic/plastic zone ahead oh the crack tip. The diffracted neutrons were counted on 3
sectors of 20 detectors split over 15 degree angle. Three separate experiments were
performed on 300 M steel CT specimens using IPNS neutrons, and each lasting for up to 6 hours
to make a statistical significance in the Bragg peak signals. The test conditions of the
specimen used for these experiments were: (i) specimen without load or minimal stress; (ii)
specimen stressed to provide 20 ksi\/in stress intensity at the crack tip; and (iii) specimen
was pre-charged with hydrogen electrochemically for 26 hours at a current density of 5mA/cm 2
and then immediately loaded to 20 ksiVin stress intensity. In the last experiment, the
specimen was installed within 15 minutes after loading in the neutron flux chamber and
exposed. This was necessary to observe the maximum possible dilation of the lattice at the
crack tip due to hydrogen before it diffuses out to either the environment or to the bulk of
the specimen. To lock up the free hydrogen in the lattice or elastic zones, loading the
specimen immediately after hydrogen charging was also essential. There was always some
relaxation of the crack tip with time. A system of FORTRAN programs (IPNS Report, 1983-85)
was used to develop Bragg reflection spectra. The Rietveld analysis of time-of-flight
diffraction data was carried out to determine Bragg peaks and full-width-half-height (FWHH)
values for d-spacings.

RESULTS

The design modifications made in CT and DCB specimens, to accommodate potential measurements,
showed no significant influence on the fracture mechanics compliance relationship. The
results reported elsewhere (Agarwala, 1990) confirm that specimens with and without holes
exhibited almost similar crack growth behavior when tested in either dry or (wet) moist-
chloride environment.

Crack Tip Potentials

The results of the potential measurements using the micro probes (Ag/AgCl reference
electrodes) on AI 7075-T6 alloy were plotted as shown in Figure 2. The potential transients
for Probe 1 through 3 show that the very first and lowest (most negative) readings of
potential recorded in all cases was near about -1.35 V. The very first reading has to be
716

most negative because by design the probe becomes active only on contact with chloride ions
(salt solution), and this comes as a consequence of crack propagation under load. After the
crack has passed through the probe, the potential starts rising and reaches a steady state
value at - 0.80 V. This potential is considered to be near the open circuit potential of the
alloy on an unrestricted surface. When calculated with respect to the Standard Normal
Hydrogen scale (Agarwala, 1990), the potentials of the test specimen were found to be - 0.95V
and - 0.40V for the crack tip and bulk surface, respectively. Which means, the crack tip is
cathodically polarized by a potential in excess of 400 mV and where anodic dissolution seems
almost impossible. Similar conclusions were also arrived through an indirect study performed
by Kendig et al. (1986). They used dc polarizing current superimposed over an ac, and
measured both the current components with respect to the polarizing potential, on a specimen
under going corrosion fatigue. They showed that the occurrences of an inflexion point
(minimum) in the ac current showed a major noble shift in the potential when the crack tip
was treated with a crack inhibiting compound DNBM (Agarwala, 1984)). The lowest potential
recorded in that study was only 200 mV more negative than the bulk potential.

The results of potential measurements on 300 M steel specimens showed a correspondingly

similar cathodic potential behavior. When measured on a CT specimen under fatigue, the
lowest (most negative) crack-tip potential recorded was about - 1.1 V with respect to Ag/AgCl
electrode. On a saturated calomel electrode, SCE scale, it is about - 0.94 V. On comparison
of this potential with the current density/potential diagram for the steel, as shown in
Figure 3, the value corresponded with the domain where hydrogen reduction reactions occur in
the de-oxygenated system. Because they are very active, it is reasonable to assume that the
pressure of oxygen at the crack tip and crevices must be insignificantly low. For, as the
crack opens up in dimension, the potentials recorded by the micro electrodes shift toward
noble direction indicating the oxygenation of the crack tip region.

Hydrogen Permeation

The results of electrochemical hydrogen permeation experiments for 300 M steel are reported
in Table I. It is shown that as the pH increase, the magnitude of hydrogen permeation
currents, Iu, decrease and the break-thru times, t^, increase. In acidic solutions (pH 2)
the break-thru times are very short. Ofcourse, the diffusion coefficient, D H , remains the
same. The results in the Table I also show that depending upon the crack tip pH, the
hydrogen in an unstressed lattice may take 2 to 30 min to diffuse a thickness of 0.8 mm or
diffuse at a rate in the range of 0.5 - 7 /im/sec. However, under stress this diffusion rate
could be significantly different. For a compact tension specimen (Figure lb) with a hole
nearly 2.5 mm away from the crack-tip, the shortest diffusion path for hydrogen, a break-thru
time of up to 2 hours could be expected in an unstrained lattice. This is based on the
diffusion parameters listed in Table 1 and at pH 6. Preliminary observations from the
permeation transient experiments on CT specimen under load and in the presence of a moist
chloride environment at the crack tip are as shown in Figure 4.

Table I. Hydrogen permeation parameters for 0.8 mm sheet of 300 M steel IIL
0.01 M N a 2 S 0 4 at an applied charging current density of 0.5 mA/cm 2 .

pH DJ_J, cm/s I , jiA/cm 2 t^, min.

-7
2 2 X 10 0.80 2.0
4 4 X 10"; 0.60 7.5
6 2 X 10-7 0.28 30

It showed a break-thru time of approximately 30-35 min. when the crack tip was strained. At
an applied stress intensity of 15 MPaVm at the crack tip, tiie magnitude of hydrogen
permeation current was measured to be approximately 0.2 μΑ/cm . At zero applied stress, the
current returns to almost background level.

Neutron Diffraction

The results of neutron scattering studies are summarized in Table II. It shows the changes
in the magnitude of d-spacings as the specimen was stressed and charged with hydrogen. For
tests under stress and H charged, the d-spacings were dilated most in the first 3 hours and
then relaxed back a little. Maximum dilation of 0.0065 A occurred in the 1.9951 A lattice
 717
dimension when the specimen was H charged and stressed. With time, it decreased a little but
not to the dimension of unstressed and uncharged lattice. This indicated that hydrogen
charging and stressing produced some irreversible effects on the lattice dimensions of the
specimen in the vicinity of the crack tip. The differences in the lattice changes were much
smaller under stress when the specimen was uncharged.

Table II. Results of in-situ neutron diffraction measurements on a CT

specimen at the crack tip under stress (20 ksiVm) and
charged with hydrogen using intense pulse neutron source.

Lattice Spacing, d, Angstroms

Neutron | Unstressed Stressed Lattice

Exposure | and Expansion
Time, hr | Uncharged Uncharged Charged Ad

2.5 | 1.99511 1.99572 2.00189 0.0060

3.0 | — 1.99593 2.00244 0.0065
4.5 | — — 2.00153
2.5 | 1.41132 1.41386 1.41522 0.0014
3.0 | -- 1.41204 1.41530 0.0033
4.5 | — — 1.41332
2.5 | 1.15211 1.15287 1.15449 0.0016
3.0 | — 1.15252 1.15544 0.0029
4.5 | — — 1.15511

DISCUSSIONS

The active path dissolution as the leading mechanism for cracking under the test conditions
has become very questionable, particularly for steel. The existence of highly active over
potential, -300 to -400 mV, for both the steel and aluminum alloy was a direct indication
that the electrochemical processes occurring at the crack tip must be predominantly cathodic.
If one compares this with the polarization behavior of these materials, the major cathodic
process has to be hydrogen reduction reaction. At -300 to -400 mV overvoltage, the hydrogen
reduction reaction could produce enormously (high fugacity) hydrogen at the interface. In
other words, it appears that the crack tip processes under stress are in fact equivalent to
cathodic charging with hydrogen. Based on the results of hydrogen permeation experiments at
the crack tip, it can be argued that the permeation current of 0.2 >iA/cm 2 could only be
measured if the crack tip was charged at cathodic applied current of nearly 0.5 mA/cm 2 (cf.
Table I). The magnitude of hydrogen permeation current changes with the stress and it is
greater at higher stresses. Base on the results on H break-thru times, one can also conclude
that the lower hydrogen break-thru time is a direct indication of either low pH and/or high
stresses at the crack tip. It has been theorized that high stress vectors can transport
hydrogen much faster than in an unstrained lattice (Bastien et al., 1951; Tien et al., 1976).
Similar observations were also recorded by Hagi et al. (1986) when working with deuterium,

The results of neutron diffraction analysis have shown a direct evidence of lattice expansion
when a hydrogen charged specimen is stressed ( Table II). Also as hydrogen enters toward a
region of high tri-axial stress, the dilation of lattice spacings change with time. In 3.0 h
neutron exposure the region which is approximately 2 m n r volume ahead of the tip, showed
greatest lattice dilation. But after 4 hours of exposure the d-spacings tend to return to
their original dimensions. However, at 20 ksi\/Tn stress intensity, a test parameter, there
will be always some region which will be permanently deformed or strained. This deformation
is usually the size of the plastic zone ahead of the crack tip. Since maximum widening of
the lattice has occurred near 1.995 A region, it was stipulated that the plane (220) was the
one most affected due to hydrogen and must be the site for hydrogen trapping. These could be
the centers of tetrahedra in the bcc structure of iron along the (220) plane.

CONCLUSIONS

A modification in the specimen design allowed an in-situ measurements of open-circuit

 718
potentials at the tip of an advancing crack. An existence of highly active over potential,
up to - 400 mV, was observed. The magnitude of hydrogen diffusing through the crack tip
could be measured in-situ by an electrochemical permeation technique under defined stress
conditions. New compact tension specimens were designed to enable these measurements.
Preliminary results indicated that hydrogen break-thru times were decreased by several
factors when the crack tip was under stress. The flux of hydrogen permeating through, ahead
of the crack tip, was approximately 0.2 jiA/cm 2 · The neutron diffraction studies indicated
that hydrogen causes most widening of the bcc lattice along the (220) plane, and most
probably the center of tetrahedra is the site for trapped hydrogen. Calculations based on
thermodynamic and Nernst relationships showed that the crack-tip processes produce enormously
high concentration (fugacity) of hydrogen. Hence, the active-path corrosion as the mechanism
of environment assisted cracking in high humidity-salt conditions may not be possible. Thus,
hydrogen embrittlement is considered the major factor for catastrophic failures in high
strength steels or even aluminum alloys. The methods which would compensate for the decrease
in potential, hydrogen reduction reaction and permeation, would, therefore, control the
susceptibility of the material to catastrophic failures. The use of multifunctional inhibitor
system such as DNBM developed earlier (Agarwala, 1984; Agarwala et al., 1987), at the crack-
tip has verified this conclusion.

REFERENCES

Brown, B.F. (1972). Stress Corrosion Cracking in High Strength Steels. Titanium and Aluminum
Alloys (Washington, D.C.: Naval Research Laboratory), Library of Congress, Cat.72-600053.
Agarwala, V.S. (1984). In: Embrittlement by the Localized Crack Environment (R.P. Gangloff,
Ed.). TMS Publication, 409-419.
Hirth, J.P. (1980). Metall. Trans.. 11A. 861.
. Troiano, A.R. (1960). Trans. ASM. 52. 54.
Oriani, R.A. (1978). Ann. Rev. Mater. Sei.. 8, 327.
Pao, P.S. and R.P. Wei (1979). In: Environment Sensitive Fracture of Engineering Materials
(Z.A. Foroulis, Ed.) The Metallurgical Society, 566-580.
Oriani, R.A. and P.H. Josephic (1979). Acta Metall.. 25. 979.
Rice, J.R. and M.A. Johnson (1978). In: Inelastic Behavior of Solids (M.F. Kanninen, Ed.)
McGraw Hill Publication.
Chung, H. and D.D. Macdonald (1985). Corrosion. 41. 150.
Pickering, H.W. (1986). Corrosion. 42. 125.
Turnbull, A. (1983). Corrosion Science. 23. 833.
Turnbull, A. and D.H. Ferriss (1986). Corrosion Science. 26. 601; TL 1323.
Alavi, A., C D . Miller and R.P. Wei (1986). Electrochemical Reactions with Bare Metal
Surfaces and Corrosion Fatigue Crack Growth, Lehigh U. Technical Rep. 19, IFSM 86-143.
Turnbull, A., A.S. Dolphin and F.A. Rackely (1988). Corrosion. 44. 55.
Agarwala, V.S. (1990). An In-Situ Experimental Study of the Mechanisms of Catastrophic
Damage Phenomena. In: Hydrogen Effects on Material Behavior (N.R. Moody & A.W. Thompson,
Eds.). TMS Publication, 1033-1045.
Berman, D.A. and V.S. Agarwala (1988). The Barnacle Electrode Method to Determine Diffusible
Hydrogen in Steels. In: Hydrogen Embrittlement: Prevention and Control (L. Raymond, Ed.)
(The ASTM), STP 962, 98-104.
Devanathan, M.A.V. and Z. Stachurski (1960). Proc. Rov. Soc. A270. 90.
IPNS Progress Report (1983-85). Argonne National Laboratory, Argonne, IL.
Kendig, M.W., F. Mansfeld and V.S. Agarwala (1986). Evaluation Electrochemical Kinetics of
the Fatigue Crack Tip of Aluminum Alloy. The ECS Abstracts, San Diego, CA.
Bastien, P. and P. Azou (1951). In: Proceedings of the First World Metallurgical Congress
(The ASM, Metals Park, OH) h 535.
Tien, J.K., A.W. Thompson, I.M. Bernstien and I.M. Richards (1976). Met. Trans.. 7A. 821.
Hagi, Hagi and Y. Hayashi ((1986). Lattice Strains due to Hydrogen and Deuterium in Iron.
In: Memoirs of Faculty of Engineering (Kyushu University, Japan), 46(1).
Agarwala, V.S. and J.B. Boodey (1987). Control of Stress Corrosion Cracking in High Strength
Aluminum Alloys. In: Proceedings of Third International Conference on Degradation of
Engineering Materials. (The Pennsylvania State University), 341-349.
WS8e2

Delayed Fracture Analysis in High Tension Bolts Induced by Hydrogen

Hagai SHIMOMURA *
Takeshi SHINODA **
Tadao HAZE ***

*) Department of Architecture, Gifu National College of

Technology, Shinsei-cho, Motosu-gun, Gifu, 501-04, JAPAN
**) Faculty of Engineering, Nagoya University,
Furo-cho, Chikusa-ku, Nagoya, Λ6Λ» JAPAN
***) S-S Engineering, Miyawaki-cho 1-95, Nakagawa-ku, Nagoya,
4.54-, JAPAN

ABSTRACT

The delayed failures of the high tension bolts have been reported since
they were introduced into steel structures and bridges. Most of these
failures have been thought to be induced by the diffusible hydrogen because
these failures often occurred under polluted circumstances like seaside or
industrial areas. There is the need to take into account not only the
density gradient of hydrogen but also the stress distribution in order to
solve the diffusional process of hydrogen in metals under stress.
Mathematical development including the contribution of the stress field was
done, results were applied into the finite element method (FEM), and a
numerical method was used to calculate the incubation time required for
diffusible hydrogen to accumulate around the root of a thread. Delayed
fracture tests with pre-charged specimens were also performed and compared
with analytical results.

KEYWORDS

Hydrogen induced crack; Delayed fracture; High tension bolt; Finite element
method (FEM); Fick's laws

NOMENCLATURE

D : hydrogen diffusivity J : hydrogen flux

Ö : hydrostatic component of stress tensor C : hydrogen concentration
r : activity R : gas constant
T : absolute temperature t : time
VH: specific molar volume of hydrogen atoms

INTRODUCTION

The present trend for taller buildings and greater spans has led to 590 MPa
tensile strength class or higher classes of high strength steels being
considered for use in building construction. Unlike in the case of mild
steel, a shortage of the ability of a stress re-distribution due to a

719
720
higher yield ratio won't show the sufficient deformability of frames after
reaching mechanism. This total deformability as a frame work depends much
on that of jointings such as beam to column connection which is jointed by
welding or bolt. In the case of bolted joints the sectional area of a base
metal has a loss due to bolt holes, where a stress concentration becomes
so higher that the yielding and deterioration generates earlier. The loss
of sectional area of base metal caused bolt holes must be smaller as far as
possible to prevent a premature stress re-distribution around bolt holes,
and it is necessary that the strength of a high tension bolt must be higher
to reduce the loss of section by bolt holes, and also to insure the
deformability of bolted joints.

MATHEMATICAL DEVELOPMENT and DISCRETIZATION

Diffusive Process and Discretization for Numeric FEM Analysis

Consider a cubic element dv in arbitrary location (x,y,z) and time t in

some body; hydrogen concentration can be defined as C(x,y,z,t). Volume of
hydrogen accumulated in its cubic element can be expressed by Fourier's
law and the variation of concentration with time t can be written as,

7
dt dx\ dx J ddy y\ \ d dy
y J d zdz \ \ d z dz
J I (1 )
2
= DP C
In the case of diffusion of hydrogen atoms in steel subjected to stress,
from Fick's first law, the flow vector J of the atoms diffusing through
unit area per unit time at any point in the material can be expressed as
follows
J
Vc r RT / (2)
Also, from Fick's second law

(3)
\r ' RT
Assuming the activity r is constant all over the object and the stress is a
single-valued and continuous function under analysis, V r andy 2 r in the
second and third terms of equation (3) respectively can be considered to be
zero so that the variation of hydrogen concentration with time can thus be
independent of the activity r and expressed as a function of the hydrogen
concentration and the stress gradient. Let us next consider the
application of numerical analysis to this result using the finite element
method (FEM). The object to be analyzed is divided into finite, triangular
elements, and, using the nodal concentration 0, the hydrogen concentration
C within an element at any time t is defined by,
(Λ)
C(x,y,z,t) = [N(x,y,z).0(t)]
Here, [N] is the interpolation function matrix. When [N] itself is taken as
the weighting function, the following equation is obtained using Galerkin's
method which is one of weighted residual methods:

Jve L J
I dt RT J (5)
 721
where Ve expresses the elemental volume.
Using Green's theorem and by some boundary conditions, considered as a
two-dimensional problem, equation (5) yields for a single triangular
element:

where,
W«H?l·*» (6)
[k]=[kd]+[ks]+[kc]
[kd] : hydrogen diffusion matrix of an element
[ks] : stress dependent hydrogen conductivity matrix
[kc] : concentration dependent hydrogen conductivity matrix
[m] : hydrogen capacity matrix
{f} : hydrogen flux vector
For the entire object under analysis,

[K]Wt)} + [ M ] { « ) = { F } (7)

U s i n g t h i s e q u a t i o n , t h e o b j e c t u n d e r a n a l y s i s can be s p a t i a l l y
discretized. Temporal d i s c r e t i z a t i o n a l s o becomes p o s s i b l e with t h i s
diffusion equation by employing Crank-Nicolson's f i n i t e difference method.
Therefore, using these two d i s c r e t e techniques, i t becomes possible to
solve the unsteady s t a t e problem involving hydrogen diffusion in s t e e l of a
given geometric shape.

EXPERIMENTS

Delayed Fracture Test Specimen

Delayed fracture tensile specimens was actual F13T high tension bolt (F13T
bolt) whose specified tensile strength is over 127Λ·9 MPa and diameter is
22 mm. This bolt was made from the same material of F10T bolt which is
lower class of strength, and is widely used in steel structures and
bridges. On the contrary, this F13T bolt is now prohibited by Japan
Industrial Standard because of the possibility of delayed fracture as it
had been reported. Features of this bolt are ; contained Boron to improve
hardenability, quenched and tempered, and rolled thread hot. The chemical
composition and mechanical properties are shown in table 1. The mechanical
saw notch, whose width and depth was 0.2 and 1 .2 mm respectively, was
inserted to promote the fracture at the imperfect root of the thread where
screw cutting starts and also a stress concentration is higher than the
axial part.

Pre-charging Condition

These specimens were pre-charged cathodically in 2 % i^SO, electrolyte for

1 or 2 hours with about 0.5 Amp./cm2 at room temperature. They were
shielded with a sealing material to be charged locally around the notch and
a part of threads. The charging system around the saw notch are
illustrated in Fig. 1 . While charging bubbles generated actively on both
surfaces of electrodes, but direct current was kept constant by a variable
voltage source.

Loading System

Pre-charged specimens were set up into the loading system as soon as

possible to prevent diffusible hydrogen from being dismissed into the
atmosphere. Specimens were tightened and stressed with each aimed
722
constant load.

Table 1 Chemical Composition and Mechanical

Properties of F13T Bolt
Chemical Composition (wt7e)

C Si Mn P S Cu Ni Cr B
0.34 0.22 1.27 0.024 0.018 0.01 0.02 0.03 0.0017

Mechanical Properties (MPa)

Yield strength Tensile Strength

F13T Bolt 1294.5 1363.1

Fig. 1 Charging System

Process util Failure and Test Results

The initiation and propagation of a crack was indirectly observed by events

of the acoustic emission (AE) over 90 deci Bel till the specimen was
fractured. When fractured earlier, AE signal occurred as soon as it was
tightened, and was intermittently counted in each cases. Fig. 2 shows
an example of series of time and events over 180 deci Bel until fracture.

Fig. 2 AE Events till Fracture

Test results were shown in Fig.3. In this figure, stress is normalized by

the specified stress 6s of F13T bolt. All specimens except for one case
were fractured even in the case of a 60 % stress level to the specified
one. It can be clearly seen from this figure that fracture time was
dependent on the charging time and applied stress. As for charging time,
it is considered to be equivalent to the quantity of a diffusionable
hydrogen which enters from the electrolyte into the bolt. Notched specimen
without hydrogen charge was also tried, but it didn't show any events of AE
regardless of its high crack sensitivity. This fact reveals that the
hydrogen charging by this system is effective and influential in assisting
the initiation and propagation of crack in this F13T bolt over 1300 MPa.

Fractography

SEM observation was done, and one of fractured surfaces ahead of notch is
shown in Fig. 4. This figure indicates that it was intergranular and
transgranular brittle fracture. Getting apart from the notch root, quasi-
cleavage fracture also could be observed accompanied with the plastic
deformation.

ANALYTICAL RESULT
 723
Numerical analysis of the unsteady state process of diffusible hydrogen in
metal was executed with the finite element method (FEM) based on the

1.0 •
o
0.8 o
O ·

0.6 o°
• Charged 1 hr.
O Charged 2 hrs.
:
·—
: 1 i i ■ ■ -■ *i α
_^^_^^α_^_,-α-^^
1 10 100 (hour)

Fracture Time after Loading

Fig. 3 Relation between Time and Stress till Fracture

development of Fick's laws and taking account of the stress field. In this
analysis a bolt could be treated as a two-dimensional problem that is a
plane plate with a unit thickness (1cm). The proportion of width to
thickness in the analytical section is almost the same so that the
analytical results solved by FEM as a plane strain problem would give
similar results as obtained in an actual bolt. Based on this assumption a
division of a part of bolt, considering a restraint of a nut, into
triangular elements is shown in Fig. 5· Assuming a specified tensile
stress and an initial permeation of hydrogen, Fig. 6 indicates the initial
state of hydrogen diffusional process.

Fig. U SEM Photograph Fig. 5 Division of a Bolt-

Nut into Elements

Values for computational analysis used here are ; specified stress level,
hydrogen diffusivity D=4.x1 0"8 ( cm 2 /sec ) , VH=2 ( c m 3 / m o l ) , absolute
temperature T=300 (K), gas constant R=1.98 (cal/mol K) and r is neglected.
The process of hydrogen diffusion from time t=0 onwards is shown in the
same figures. Shading represents hydrogen concentration which is
normalized by the maximum value of initial state in the case of charged 2
hours, and those figures, especially in 2 hours charged model, indicate
724
that these processes have a clear tendency for diffusive hydrogen to halt
around notch where the stress concentration is higher than other regions.

Fig. 6 Diffusional Process and Accumulation of Hydrogen

CONCLUSION

The hydrogen induced fracture in high tension bolts under stress was
investigated experimentally, and also analyzed by FEM. The results support
the following conclusions:
(a) Cathodically charged high tension bolts over 1300 MPa showed the
phenomenon of delayed fracture induced by hydrogen.
(b) Mathematical development based on Fick's laws taking account of stress
gradient and its discretization for numeric computational analysis were
done. Diffusible hydrogen was accumulated around notch where stress
intensity is higher, and its general behavior seems to agree with
experimental results.

REFERENCES

1) O.C.Zienkiewicz :" The Finite Element Method in Engineering Science ",

McGRAW-HILL,London (197TJ
2) H.J.Maier, W.Popp and H.Kaesche : "A Method to Evaluate the Critical
Hydrogen Concentration for Hydrogen-Induced Crack Propagation", Acta
Metal., Vol.33» No.Λ,(1987)
3) JSSC working group for delayed failure of high tension bolt :
"Atmospheric Weathering Test of High Strength Bolted Joints (Continued
Report 1,2,3,4)", JSSC journal, Vol.7 (1971), Vol.9 (1973), Vol.10
(1974), Vol.11 (1975) (in Japanese)
4.) H.Shimomura, T.Shinoda, K.Hoshino and R.Yamashita : "Analytical Study on
Hydrogen Induced Cracking in HT-Steel Welds ", Transaction of the Japan
Welding Society,Vol. 21, No.2, Oct. (1990)
5) H.Shimomura. T.Shinoda and T.Haze : " Study on the Hydrogen Induced
Fracture of High Tension Bolts ", 9th International Conference on Offshore
Mechanics and Polar Engineering, Vol.3-B, pp. 611-615,(1990)
 WS8e3

MECHANICAL BEHAVIOUR OF A VT20 TITANIUM ALLOY

AT DIFFERENT INITIAL STATES AND HYDROGEN CONTENTS

O.N. Senkov, I.O. Bashkin and E.G. Ponyatovsky

Institute of Solid State Physics, Acad. Sei. of the U.S.S.R.,

Chernogolovka, Moscow Distr., 142432, U.S.S.R.

ABSTRACT

Hydrogen-enhanced plasticity of a Ti-6Al-2Zr-l. 5V-lMo-xH alloys with x= 0 to

0.6wt.% has been found and studied at elevated temperatures. The nature of
considerable increase in ductility (up to 40 times) and decrease in strength
(down to 2.5 times) observed on hydrogen-charged alloys has been discussed.

KEYWORDS

Titanium alloys, hydrogen alloying, hydrogen-enhanced plasticity, stress -

strain rate-temperature relations, dynamic recrystallization.

INTRODUCTION

Titanium alloys charged with hydrogen display a considerable increase in

their ductility and decrease in strength at elevated temperatures
(Ponyatovsky, 1991), contrary to the well-known phenomenon of hydrogen
embrittlement. This paper deals with our results concerning effects of
temperature and strain rate on mechanical behavior of a VT20 titanium alloy
with different hydrogen contents and grain structure.

EXPERIMENTAL

This titanium alloy contains about 6Al-2Zr-l.5V-lMo (wt.%) and belongs to

the group of pseudo-a-alloys. Specimens for torsion tests were cut out of a
hot-rolled sheet annealed at 820 C for 1.5 h and had a cylindrical working
part of 5 mm in dia. and 5 mm in length. The procedure of gas-phase
hydrogenation of specimens was described by Ponyatovsky et al., 1989a.
Hydrogen content was measured by weighing to an accuracy of ± 0.02 wt%. All
these specimens had the same dispersed lamellar grain structure. Equiaxial
fine-grained structure was especially formed by hydrogen and deformation
treatment when necessary (see below).

725
726
RESULTS AND DISCUSSION

Figure 1 shows ductilities (ultimate torsional strain ε ) of specimens with

several hydrogen contents in dependence on temperature U T and strain rate ε.
Ductility of the hydrogen free alloy increases monotonously with increasing
T and decreasing ε. The temperature when ductility of the alloy begins
rapidly growing lowers as the strain rate decreases. Hydrogen alloying of
specimens leads to a considerable increase in their ductility and to a
change in dependence of ductility on temperature or strain rate which
becomes shaped as a curve with a maximum.

VT20 VT20 + 0,r/oH VT20 + 0,58%H

50

40
■ /V -V^ 3
30
■/A
20 ■ P\ \

10

0
V ^1
103 JO 2 1(ff 10°
Lsecj ijSec*

Fig. 1. The strain-rate dependencies of ductility

of alloys with various hydrogen contents.
T = 607(1), 660(2), 780°C(3).

High ductility values are closely connected with occurrence of a softening

stage in stress-strain curves followed by a steady-state flow at a lowered
stress. In other words, one can believe that the same relaxation processes
result in the above two stages and prevent from development of fracture. The
hydrogen-induced relaxation processes are so intense as to make the steady-
state stress much lower than the yield stress of the initial alloy.

Interrelations between the maximum stress, τ , temperature and strain rate,

τ (έ,Τ), measured for the initial stage whicR precedes the softening stage
are shown in Fig.2. These relations differ essentially from ones obtained
for steady-state flow (Fig.3). Figures 2 and 3 evidence that hydrogen
alloying decreases the maximum stress by a factor achieving 1.5 and the
steady-state flow stress by more than 2.0 times.

The following empirical equation is obtained in the first case both for
specimens with hydrogen and without it:

έ= έ exp[- U 1η(τ /τ )(1 - T/T )/kT] (1)

For the steady-state flow, i.e. for developed deformation, the relation has
the form:

e A(τ/G) (Gb/kT)expQ/kT) (2)

 727

ÜH 1Ö3 102 1Ö1 tO° P id5 is* a1 io° # * id3 io'2 io'1 io°
tr,sec
_1 Lsec'„-1 Lsec*
Fig. 2.The dependencies of maximum stress, τ , on strain
rate. T = 565(1), 607(2), 660(3), 720Ϊ4), 780°C(5).

ΐ>α|

W 10° Ψ 10Ί 101 )^ IO"3 10.2 10"1 10° ^'3 10"2 10"1 10°
£,sec"f
Fig. 3. The dependencies of steady-state flow stress on
strain rate. T= 607(1), 660(2), 720(3), 780°C(4).

Here k is the Boltzman constant, G is the shear modulus, b is the Burgers

vector, t = 2 5 sec , τ = 640 MPa, T = 1240 K, other parameters are
To, , . o o
given in Table 1.
The stated difference suggests that mechanisms which control the plastic
flow are essentially different at the initial stage and at the steady-state
(large strains) one. The type of relation (1) holds when thermally activated
cross slipping of screw dislocations is the governing process (Friedel,
1959, Wolf, 1960), and the expression 2 is typical for the mechanisms in
which recovery or recrystallization predominate (Poirier, 1976). The change
of the governing mechanisms appears to be due to qualitative modification of
the grain structure during deformation.
728
Table 1. Parameters of Eqs. (1) and (2) corresponding
to solid/dotted lines in Figs.2 and 3.

Alloy A, m /sec n Q,eV U , eV

o
VT20 4.7-102 6 2.3 3.2
VT20+0.4%H 1.9·104/7.8·10~3 6/4.3 2.4/1.9 2.5
4 5
VT20+0.58%H 1.9·10 /8.1·1θ" 6/4.3 2.4/1.6 2.5

Indeed, studies of microstructure suggest that dynamic recrystallization

proceeds from the beginning of softening stage. As a result, the initial
lamellar structure transforms to a fine-grained equiaxial one with grains of
1 to 5 μιιι in size (Fig.4). Hydrogen alloying decreases the lower limit of
the temperature range where dynamic recrystallization occurs. The study of
microstructure has shown that deformation in low-ductile specimens is
localized in very narrow zones, their total extension is usually less than
20% of the working part of the specimens. A strong strain-stimulated
fractionation of the lamellar structure and developed porosity is observed
in these zones. Fracture takes place by means of rapid growing of a crack
through the network of pores. As a result of increase in temperature,
decrease in strain rate and alloying with hydrogen, the zones of localized

a) b)
i 20μπι
Fig. 4. Initial structure (a) and that after deformation
ε = 5 at 720°C, t = 0.25 c X (b). VT20+0.4wt.% H.

deformation extend essentially and then merge, and the working part of
specimens is deformed still more uniformly. Cracks in the high-ductile
specimens develop slowly from the surface, have blunt tips and often branch.

It would be natural to put a question whether high ductility of a

hydrogenated alloy is due to formation at the beginning of deformation of
the equiaxial fine-grained structure possessing high dynamic activity (i.e.
such alloy gains superplastic properties, Likhachev et al.,1987) or due to
other particular hydrogen-induced relaxation processes. To elucidate this
question, we studied the behavior of specimens with the fine-grained
structure which was obtained by the preliminary deformation of hydrogenated
specimens at 820°C followed by removal of hydrogen.
 729
The studies showed that such preliminary grain refinement actually led to an
increase in ductility and decrease in stress of a VT20 alloy in the tempera-
ture range 700 to 800 C, however, these effects were small compared to those
induced by hydrogen (Figs.5,6). The contribution of structural_factor to the
effect of hydrogen-enhanced plasticity is maximal at έ £ 10 sec being
less than 10% at έ= 0.1 - 1.0 sec when the effect is largest. Therefore,
the enhancement of plasticity is mainly due to by the absorbed hydrogen.

660 720 7SÜ 840 600 660 m no a

Fig. 5.The dependencies of ductility (a) and maximum

stress (b) on temperature, έ = 0.09 sec
Alloys: VT20 (1,3), VT20+0.35wt.% H (2); grain
structure: lamellar (1,2), equiaxed (3).

10~2 1(T1 10°

Fig. 6. The dependencies of ductility (a) and maximum

stress (b) on strain rate. T = 780°C.
Curves are designated as in Fig. 5.

The nature of the effect of hydrogen-enhanced plasticity can be discussed on

the basis of available data.

Strong dependence of this effect on hydrogen content (Ponyatovsky et al. ,

1989a, 1991), temperature and strain rate (Bashkin et al. , 1990, Senkov et
al., 1989, 1990) indicates that both phase composition and especially kine-
730
tic factor can contribute to the effect. Due to high mobility, hydrogen can
accelerate dynamic recrystallization and phase transformation in overstress-
ed regions. E.g., Dutta and Birla, 1987, observed a multiple increase in
local hydrogen concentration in the region of deformation. Any stress gradi-
ents should induce local redistribution of hydrogen and initiation of phase
transformation, which would result in grain refinement, uniform deformation
and increase in ductility.

Hydrogen exerts a screening effect on the long-range internal stresses,

which shows up in a decrease of the yield strength by a magnitude which only
slightly depends on temperature (see Fig. 5). Hydrogen increases mobility of
screw dislocations and density of their sources (Matsumoto et al., 1981,
Tabata and Birnbaum, 1983). These phenomena would also contribute to stress
relaxation and hydrogen-enhanced plasticity.

REFERENCES

Bashkin,I.O., E.G. Ponyatovsky, O.N. Senkov and V.Yu. Malyshev (1990).

Strain rate sensitivity of the effect of hydrogen-enhanced plasticity of
a VT20 titanium alloy. Fizika Metallov i Metallovedeniye (USSR), No 2,
170-177.
Dutta, A. and N.C. Birla (1987) Stress induced hydrogen diffusion in a a + ß
titanium alloy during superplastic deformation. Scripta metallurgica, 21,
1051- 1054. ~~
Friedel, J. (1959). Prismatic slip with h.c.p. structure. In: Internal
stresses and fatigue in metals (G.M. Rassweiler and W.L. Grube Eds.),
p.238. New York.
Matsumoto, T., J. Eastman and H.K. Birnbaum (1981). Direct observation of
the enhanced dislocation mobility due to hydrogen. Scripta metallurgica,
15, No 9, 1033-1037.
Poirier, J.-P. (1976) Plasticite a haute temperature des solides cristallins.
Editions Eyrolles. Paris.
Ponyatovsky, E.G., 1.0. Bashkin, O.N. Senkov, Yu.A. Aksenov, V.L. Kolmogor-
ov, G.G. Taluts, V.K. Kataya, I.V. Levin, Yu.I. Potapenko and A.N. Trubin
(1989a). Hydrogen effect on ductility and flow stress of a VT20 titanium
alloy at temperatures to 740°C. Fizika Metallov i Metallovedeniye, 68,
—
1167-1172.
Ponyatovsky, E.G., 1.0. Bashkin, O.N. Senkov and V.Yu. Malyshev (1989 b ) .
Temperature, strain rate and hydrogen concentration influences on the
effect of hydrogen-enhanced plasticity of a VT20 titanium alloy (in
Russian). Doklady Acad. Nauk SSSR, 306, 613-616.
Ponyatovsky, E.G. (1991). Hydrogen plasticization of titanium alloys. This
conference.
Senkov, O.N., 1.0. Bashkin, E.G. Ponyatovsky and V.Yu. Malyshev (1989).
Structure and Mechanical properties of hydrogen-charged Ti-6Al-2Zr-lV-lMo
alloy. In: The Seventh Symposium on Metallography. Proceedings. Part 2,
pp. 424-428. CSVTS, Czechoslovakia.
Senkov, O.N., 1.0. Bashkin, V.Yu. Malyshev and E.G. Ponyatovsky (1990).
Study of plastic flow peculiarities of hydrogen-charged VT20 titanium
alloy in the temperature range from 823 to 1073 K. Fizika Metallov i
Metallovedeniye, No 7, 119-127.
Tabata, T. and H.K. Birnbaum (1983). Direct observation of the effect of
hydrogen on the behaviour of dislocations in iron. Scripta metallurgica,
17, 947-950.
Wolf H. (1961). Die Aktivirungsenergie für die Quergleitung aufgespaltener
Sehraubenversetzungen. Zs. Naturforshung, 15a, 180-193.
 WS8e4

EFFECT OF HYDRIDES
ON THE MECHANICAL PROPERTIES OF ZIRCALOY-4

J. B. BAI, C. PRIOUL and D. FRAN£OIS

Lab. MSS/MAT, CNRS URA 850, Ecole Centrale de Paris, 92295

Chätenay Malabry CEDEX, France

ABSTRACT

In order to better understand the embrittlement of Zircaloy-4 by hydrides and the ductile-brittle
transition on this alloy, Zircaloy-4 sheet tensile specimens in the stress-relieved, recrystallized
and ß treated states were hydrided (10 to 1500 ppm wt H) and then tested at two temperatures
(20°C, 350°C). Metallographic and fractographic analyses were carried out to determine the
fracture micro-mechanisms. The results showed that, at 20°C, Zircaloy-4 undergoes a
significant ductile to brittle transition for high hydrogen contents. Heat treatment shifts this
transition (to zero elongation) considerably, from 1050 ppm wt H for the stress-relieved state to
less than 250 ppm wt H for the ß treated state. However, at 350°C, Zircaloy-4 remains ductile
up to hydrogen content higher than 1100 ppm wt. At 20°C, the fracture surfaces are
characterized by voids and secondary cracks for low and medium hydrogen contents, and by
intergranular crack and decohesion through the continuous hydride network for high hydrogen
content. A model based on image analysis and hydride embrittlement micro-mechanism
observations is used to calculate the upper-limit hydrogen content which makes Zircaloy-4
totally brittle. The difference between the mechanical behaviors of stress-relieved and
recrystallized states is also explained.

KEYWORDS

Zircaloy-4, hydride embrittlement, ductile-brittle transition, cracked-hydride voids.

INTRODUCTION
Zircaloy-4 used as a cladding alloy absorbs hydrogen by the metal-water corrosion reaction.
Excess dissolved hydrogen precipitates as hydrides which embrittle the material. Numerous
papers (Coleman and Hardie, 1966; North wood and Kosasih 1983) have reported the results
about the effect of hydrides on the mechanical properties of Zircaloy-4. It is now well
established that for low and medium hydrogen contents the hydrides crack during tensile
loading and the cracked hydrides accelerate a ductile fracture process (Puls, 1988; Fan and
Koss, 1985; Simpson, 1981). However, for specimens containing high hydrogen contents
which become totally brittle (Lin et al.t 1979; Bai et ai, 1990), the mechanism is very different.
Furthermore, the micro-structure changes by heat treatment, can modify the fracture micro-
mechanism and consequently the influence of hydrides on the mechanical properties of
Zircaloy-4.
731
732

To identify the influence of heat treatments on the micro-mechanism of hydride cracking and on
the ductile-brittle transition, tensile tests at two temperatures (20°C, 350°C) have been carried
out on Zircaloy-4 sheet specimens. These specimens in three heat treatment states (stress-
relieved, recrystallized and ß treated) have been hydrided to different hydrogen contents up to
1400 ppm wt. Post-testing micro analysis consists of metallographic and fractographic
observations in order to study the evolution of the fracture micro-mechanisms as a function of
hydrogen content, temperature and heat treatment.
EXPERIMENTAL PROCEDURE

Material and Tensile Test

Tensile specimens used in this study were taken from 0.5 mm thick Zircaloy-4 sheets. The
composition of the material and the specimen size are shown in Table 1 and Fig. 1
respectively. Zircaloy-4 was cold-rolled 38% and then heat treated to obtain stress-relieved
(460°C, 24h), recrystallized (650°C, 3h) and ß treated (1030°C, 2 min followed by air
quenching) states. It may be noted that the crystallographic textures are characterized by a high
intensity of basal poles parallel to the sheet normal for the stress-relieved and recrystallized
states, and randomly distributed basal poles for the ß treated state.

The tensile tests were carried out at room temperature (20°C) and 350°C on a screwdriven
Instron machine. The specimens were loaded at an engineering strain rate of 4xl0"4/s.

Table 1. Chemical composition of Zircaloy-4 (wt%) | \J f 22 L/ IS2

Sn Fe Cr o H
1.50 0.22 0.10 0.13 ^ 5 ppm
Fig. 1. Tensile specimen geometry

Hydrogenation and Control

The material was gaseously hydrided at 400°C in an apparatus at a pressure of 0.12 MPa for
different durations. After charging, the specimens were controlled by optical observation of the
hydride distribution. For each specimen, after tensile test, offcut near the fracture surface was
taken for hydrogen content analysis at 850°C, using a vacuum desorption technique.

RESULTS
Hydride Morphology Study
The hydride morphology is a complex function of stress effects and micro-structure (texture,
grain size and shape) and has a significant influence on the mechanical behavior of Zircaloy-4.
In our study, the hydride morphology is very different in the three metallurgical states. For the
stress-relieved state, hydrides are aligned in the cold-rolled plan up to about 600 ppm wt H,
then begin to exhibit some random distribution, with platelets having an in-plane size of about
15-20 μπι; for the recrystallized sheet, there is a more random distribution of hydrides, having a
size determined by the grain boundary characteristics; in the case of the β treated state, the
hydrides are totally localized in the interfaces of the α-phase platelets in the large prior-ß grain.
Hydride thickness is very difficult to be determined experimentally, the values reported vary
between 0.1 and 2.5 μιη (Fan and Koss, 1985; Puls, 1988; Yuan and Tangri, 1982) for
different micro-structures, hydrogen contents and hydricüng procedures.

Tensile properties
At room temperature (20°C), for the three heat treated states, the effect on strength of increasing
hydrogen content is not significant and about 15% variation of yield strength and tensile
 733
strength was observed in all the range tested. The ductility (elongation and reduction of area) is
drastically reduced to zero (ductile-brittle transition), when a critical hydrogen content is
reached, as shown in Fig. 2. This critical value, which varies for the three states, is about 1050
ppm wt H for the stress-relieved state, 760 ppm wt H for the recrystallized state and less than
250 ppm wt H for the ß treated state. Of special note is that the transition is more spread out
(between 600 and 1050 ppm wt H) for the stress-relieved state.

recrystallized
40

20
1407pp|n
1248ppm,
I
-H20

200 400 600 800 1000 1200

hydrogen concentration (ppm)
2.9% - 5.6%
J L
8.3% i_
10.9% 13.4% 15.8
hydride volume fraction
Fig. 2. Influence of hydride on the ductility of Zircaloy-4 at 20°C

However, at 350°C, the specimens are ductile up to very important hydrogen contents (1000
ppm wt H). At this temperature, the ductility is only slightly reduced by hydrides, as shown in
Fig. 3.

Micro-mechanisms of Fracture

Metallography observations below the fracture surface reveal that for Zircaloy-4, in the stress-
relieved and recrystallized states containing low or medium hydrogen contents, a realignment of
the hydrides occurs during straining. Along these hydrides some fragmentation appears, with
fractures distributed more or less randomly along their length. Numerous spherical cavities
form in the necked region of the tensile specimens but these small and isolated cavities often
keep their initial size and have no influence on the tensile properties of Zircaloy-4. In fact, only
the voids originated in the cracked hydrides contribute to the fracture process.

For the specimens with high hydrogen contents (above the transition) the fracture path strictly
follows the continuous hydride network, which is intergranular in the stress-relieved and
recrystallized states and interfacial in the ß treated state.

Fractography observations show the presence of secondary cracks on the fracture surfaces, for
tests at 20°C, which are linked with the hydride precipitation sites. This phenomenon
disappears at 350°C under all tested conditions, the fracture surface having ductile appearance.
The hydrogen seems to exert no more influence on the fracture micro-mechanism.
734

60

stress-relieved

40

20

stress-relieved
~ J 20

ß treated 4

200 400 600 800 1000 1200

hydrogen concentration (ppm)
1 I
2.9% 5.6% 8.3% 10.9% 13.4% 15.8%
hydride volume fraction
Fig.3. Influence of hydride on the ductility of Zircaloy-4 at 350°C

DISCUSSION
Ductile Fracture

The ductile fracture of hydrided Zircaloy-4 occurs by the formation and subsequent growth and
coalescence of voids. The controlling stage appears to be the failure of the matrix connecting the
cracked hydrides (Simpson, 1981). Therefore, in Zircaloy-4 containing low or medium
hydrogen, the difference of mechanical properties between the stress-relieved and recrystallized
states can be explained by the different hydride morphology. In the former, the hydrides are
aligned in the stress direction and the small cavities which form at the hydride tips do not affect
the ductility. For the recrystallized state, the hydrides distribute randomly with some intrinsic
percentage of hydrides perpendicular to the stress direction. The number of cracked hydrides
increases continuously as a function of hydrogen content for all tests, thus inducing a
progressive ductility reduction.

Ductile-brittle Transition

For all the three states, the formation of a continuous hydride network makes the specimens
totally brittle because the tensile properties of the specimens are controlled by the brittle hydride
characteristics. The transition is more spread out for the stress-relieved state than for the
recrystallized state owing to the lower increase rate of the perpendicular hydrides percentage
demonstrated by the hydride morphology study.
 735

Figure 4 shows a fracture micro-mechanism map for hydrided Zircaloy-4 during tensile tests.
The fine micro-structure and favorable grain boundary orientation correspond to high hydrogen
content for the ductile-brittle transition for the stress-relieved and recrystallized states.

ductile fracture transition brittle fracture

- discontinuous hydride network 1 nucleation of cavities fy L * i
■ cracked-hydride voids coalescence at hydride tips i/A
. ... . ., 2 triple nodes or cracked Y/\
continuous
ductility reduces with perpendicularhydrides Pfl hydride network '
increasing void density Q hydride
U^L·*- Tl
low and medium CH fragmentation upper-limit calculation
1 - stress-relieved state, 2 - recrystallized state, 3 - ß treated state

Fig. 4. Fracture micro-mechanism map for hydrided Zircaloy-4 at 20°C.

Upper-limit Calculation

The basic idea is that totally brittle behavior corresponds to a continuous brittle hydride
network. Assuming that only the hydrides in the grain boundaries or interfaces of platelets
contribute to the brittle fracture and that the hydrides distribute homogeneously in the specimen
volume, the upper-limit is defined as the hydrogen content needed to build up a continuous
hydride network. The calculation thus becomes micro-structure controlled. Defining L*and S*
as:

L* : grain boundary or interface of platelets length by unit area (2D),

S* : grain boundary or interface of platelets surface by unit volume (3D).

Taking the hydride thickness h as the one for the grain boundaries or interfaces of platelets, the
upper-limit in terms of Vf (volume fraction of hydrides) is given by:

Vf=S*h = L * h -
π (1)

Using L* determined by the image analysis on the micro-structures of the three states, as
shown in Table 2, we can obtain the hydrogen content CH (ppm wt) in the specimen by:

H] _9100CH_ _

^ ™ 90C H 10 6 Vf=62
'4 (2)
+

assuming that the hydride consists of δ phase, having the composition corresponding to
ZrHi.66. From (1) and (2), the hydride thickness h can been calculated for the hydrogen
content at which the ductile-brittle transition occurs (labelled CJJT in table 2). The results
presented in table 2 are in good agreement with the usual hydride thickness reported and also
with our observations showing that h ranges from 0.1 to 0.5 μπι for different test conditions.
Some current TEM works will give a more complete knowledge of h for the Zircaloy-4.

Table 2. Upper-limit calculations and tensile tests results at 20°C

Zircaloy-4 L*/|jm CHT ppm (tensile test) h (calculated)

Stress-relieved 0.655 1050 0.17 μτη
Recrystallized 0.380 760 0.21 μπι
ßtreated 0.210 <255 0.14 um
736
From Table 2 we can see clearly the influence of hydride morphology, grain size and grain
shape. For the ß treated state, localized distribution and big platelets make this state more
sensitive to hydrides and less hydrogen is needed to form a continuous hydride network. Fine
micro-structures in stress-relieved and recrystallized states with high L* values (Fig. 4), shift
the transition to higher hydrogen contents. Especially for the stress-relieved state, elongated
micro-structure makes the hydrides less harmful and Zircaloy-4 undergo a less abrupt
transition.

CONCLUSION

The influence of hydrides on the mechanical properties of Zircaloy-4 in three heat treated states
have been evaluated by tensile tests at 20°C and 350°C. The most important results are as
follows:

1. For Zircaloy-4 sheet specimens at 20°C, the ductility reduces as a function of hydrogen
content, in a different way for each heat treated state. There is a ductile-brittle transition
when the hydrogen content is higher than a critical value. The heat treatment shifts this
transition (to zero elongation) considerably from 1050 ppm wt H for the stress-relieved
state, 760 ppm wt H for the recrystallized state to less 250 ppm wt H for the ß treated state.

2. At 350°C, the embrittlement by hydrides disappears for hydrogen contents up to 1000 ppm
wt H. Hydrides have no influence on the fracture micro-mechanism.

3. The micro-structural analyses show that it is the cracked hydride voids which contribute
essentially to the ductility reduction. The continuous hydride network makes the specimen
go through the ductile-brittle transition. The upper-limit model shows that L* is a very good
parameter to evaluate the influence of micro-structure on the ductile-brittle transition.

4. According to the model and the experimental results, the present authors suggest to use fine
micro-structures with elongated grains in the loading direction to delay the ductility
reduction of Zircaloy-4 at 20°C.

ACKNOWLEDGMENTS

The authors would like to thank the financial support of Commissariat ä l'Energie Atomique
(Saclay, France)(contract No. SA 9030/BJ). We are grateful to Dr. A. Alamo and Mrs. F.
Barcelo for allowing us to use their image analysis results.

REFERENCES
Bai J.B., Pelchat. J. and Prioul C. (1990). Mechanical properties of hydrided Zircaloy-4 (in
French). Revue de Metall., No. 9, 549.
Coleman C. E. and Hardie D. (1966). The hydrogen embrittlement of a-zirconium- a review.
J. Less-Common Metals, //, 168-185.
Fan Y. C. and Koss D. A. (1985). The influence of multiaxial states of stress on the hydrogen
embrittlement of zirconium alloy sheet. Metall. Trans., 16A, 675-681.
Lin S. C , Hamasaki M. and Chuang Y. D. (1979). The effect of dispersion and
spheroidization treatment of δ zirconium hydrides on the mechanical properties of Zircaloy.
Nucl. Sei. and Eng., 77, 251-266.
North wood D. O. and Kosasih U. (1983). Hydrides and delayed hydrogen cracking in
zirconium and its alloy. Int. Metals Reviews, 28, 92-121.
Puls M. P. (1988). The influence of hydride size and matrix strength on fracture initiation at
hydrides in zirconium alloys. Metall. Trans., 19A, 1507-1522.
Simpson L. A.(1981). Criteria for fracture initiation at hydrides in zirconium-2.5 pet niobium
alloy, Metall. Trans., 12A, 2113-2124.
Yuan X. Q. and Tangri K. (1982). Metallographic observations on the developing hydride
morphology at the crack tip during hydrogen induced delayed cracking in a Zr-2.5 Nb
alloy. J. Nuc. Mate., 105, 310-317.
WS8e5

ELECTROCHEMICAL MEASUREMENT OF HYDROGEN PERMEATED THROUGH STEEL

AT HIGH TEMPERATURE USING A CERAMIC SENSOR

S.Ando and K.Yamakawa

Department of Metallurgical Engineering, College of Engineering,
University of Osaka Prefecture
4-804, Mozu-Umemachi, Sakai 591, Japan

ABSTRACT

The possibility of the electrochemical measurements of the diffusivity and

the content of hydrogen permeated through a plain carbon steel at 823 K has
been studied using a proton conductive solid electrolyte (5mol%Yb203-
SrCe0 3 ). It was found possible to measure the hydrogen diffused through the
steel with high detectability using this ceramic sensor.

KEYWORDS

Hydrogen attack; electrochemical measurement of hydrogen: ceramic sensor;

proton conductive solid electrolyte.

BASIC CONCEPT TO MEASURE HYDROGEN CONTENT

The principle of the present electrochemical measurement using a proton

conductive solid electrolyte is shown in Fig.l. Hydrogen is introduced from

POTENTI05TAT
WE RE C
Alumina'
Tube
H2 V

H2
® H2 H*
Air
^ H 2 0
H2 \
Pt Past
Steel Glass Sealant
Filler Metal

Fig. 1. Principle of the present electrochemical method.

737
738
the entry side of steel, while the extraction side is held at an anodic
potential sufficient to ionize the hydrogen which diffused through the steel
and became molecule at the steel surface. The solid electrolyte was directly
joined to the steel with a filler metal in our previous experiments (Ando
et al., 1991) but in this study, we attempted to measure the hydrogen
without the direct joining of the electrolyte to the steel as shown in
Fig.l. From the detected ionization current, the permeation rate of hydrogen
can be evaluated. In this study, a proton conductive solid electrolyte
(5 mol% YbzOa-SrCeOa) was used as a ceramic sensor (Iwahara et al., 1981).
The following reaction occurs at the anode:

H 2 - * 2ΙΓ + 2e" (1)

while the following reaction takes place at the cathode:

2H* + l/202 + 2e" - ^ H 2 0 (2)

The hydrogen content in a specimen changes with time according to Fick's

second law. Theoretical permeation curves during build-up and decay
processes are calculated by applying the law under appropriate initial and
boundary conditions (Yoshizawa et al., 1975). The diffusion coefficient of
hydrogen in a specimen is obtained by comparing the theoretical curves with
the build-up and decay transient curves that are measured by changing the
hydrogen pressure as shown in Fig.2.

(F^ 2 ) 2 l·-

Extraction Side)

Time

Fig. 2. Schematic diagram of permeation transients

in the build-up and decay processes.

In the steady state (Yoshizawa et al., 1975), the hydrogen content CH(ppm)
can be calculated from

C„ (3)
F-D„-d
where A j e is the net ionization current density (Α·πΓ2), L the specimen
thickness(m), F the Faraday constant, D H the diffusion coefficient of
hydrogen in the specimen (m2.s_:L) and d the density of the specimen
(7.86 Mg-nr 3 ).
 739

EXPERIMENTAL PROCEDURES

The apparatus for the present experiment is schematically shown in Fig.3.

POTENTIOSTAT
WE RE CE
9 9 9

1 j ^ A n Wire
Thermocouple 111, Γ / Ν Ι Plate

^°HS
y c
Alumina Tube =^Ur ^Mica Plate
— Solid Electrolyte

Filler Metal
-II l
° !ITi G
jH Carbon Steel Cup
° 1111 111°
° 11 ΓΓ 1 °
Furnace
o 1 o
t '

U U
Lj J p
H2 gas Φ - Z J g O ^ J
> J V Φ» gas
Ar gas +Zf&^^

Fig. 3. Schematic diagram of the experimental apparatus.

The specimen had a hollow cylindrical shape and the thickness of its top was
about three times thinner than the side. The chemical composition of the
steel used is given in Table 1. The inner and outer top surfaces of the
specimen were mechanically polished with emery papers up to 500 grit. The
inner and outer radii of the specimen were 12 and 18 mm, respectively. The
top of the specimen, into which a steel pipe was bonded by electron beam
welding, separated the entry side and the extraction side of the hydrogen.

TABLE 1

Chemical composition of the specimen (mass%).

Specimen C Si Mn P S Al
Carbon Steel 0.19 0.22 1.00 0.018 0.012 0.015

On the entry side, argon gas was replaced to hydrogen gas (build-up) and
vice versa (decay) at a flow rate of 1.7 x 10" 6 nr'-s"1 and at a gas pressure
of 0.101 MPa. On the extraction side, the hydrogen which permeated through
the steel and became molecule at the steel surface was detected with the
solid electrolyte mounted to the top of the alumina tube as shown in Fig.3.
The solid electrolyte was 10 mm in diameter and 2 mm in thickness. It was
used as a reference electrode and a counter one; they were separated by a
coating porous platinum on the one side of the solid electrolyte as shown in
Fig.l. The platinum paste with which the ceramics was coated was dried for
1.8 ks at 623 K and then sintered for 0.9 ks at 1273 K. After the treatment,
joinings of the solid electrolyte to the alumina tube and the tube to the
740

steel were made with a glass sealant at 973 K and an amorphous copper filler
metal at 923 K, respectively.

The hydrogen diffused through the steel was extracted at an anodic potential
in the range of 0 to 180 mV vs. 02(SrCe03)/H20(air). The temperature was
maintained at 823 K within ±3 K by a controller with a thermocouple close to
the furnace. The permeated transient current during the built-up and the
decay processes was recorded as a function of time.

RESULTS AND DISCUSSION

A typical relationship between the extraction potential and the

permeation current density in the steady state (J») at a hydrogen pressure
of 0.101 MPa and at an argon pressure of 0.101 MPa are shown in Fig.4. Since
the electrolyte used has only p-type conduction (hole conduction) in an
atmosphere free from hydrogen or water vapor (Iwahara et al., 1981), the
permeation current in Ar gas is probably a residual anodic current by hole
conduction. From the difference between the two steady state permeation
current densities ( Δ ^ ) , or the net ionization current density, it can be
seen that the suitable potential range for detecting the permeated hydrogen
is from 0 to 180 mV vs. 02(SrCe03)/H20(air). We, therefore, selected 0 mV as
an anodic potential to ionize the hydrogen permeated through the steel.

0 40 80 120 160 200

Potential /mVvs. 02(5rCe03) H20(Air)

Fig. 4. Relationship between permeation current density

and extraction potential. J«, and AJ«, denote
the steady state permeation current density and
the difference between the two steady state
permeation current densities, respectively.

Figure 5 illustrates a comparison between the theoretical curves (solid

lines) and experimental data. The ordinate was normalized in units of
AJt/AJoj, and the plots were shifted on the abscissa to coincide with the
theoretical curves at AJ^/AJ«, =0.5. The experimental data agreed fairly well
with the theoretical curves.
 741

1.0

0.8

— .-Theoretical Curve
|" o :Build up
• :Decay

0.2

1 t (=Dt/l 2 )
(Build up)
(Decay)

Fig. 5. Comparison between the theoretical permeation

curves and experimental data in the build-up
and decay transients.

AJQQ.L (hydrogen permeability), D H (hydrogen diffusivity) and C H (hydrogen

content) obtained from the present experiments are given in Fig.6. From the
previous papers on the measurements of hydrogen diffusivity and
permeability (Sykes et al., 1947; Geller et al., 1950; Eichenauer et al.,
1958; Wagner et al., 1964), AJ^-L and D H for o<-iron at 823 K were 9.97xl0~3
-2.21xl0~2 A-rn"1 and 1.78xl0~e~ 3.74xl0"8 m2.s_:L, respectively. C H can be
calculated from Sievert's law (Tsubakino et al., 1985) to be 0.792 ppm. The
hydrogen diffusivity measured were small compared with the above values.

1 1 1 1 1 1

° o o o o ° o o o o _]
8
3
0 1 1 1 1 1 1
1 1 1 1 1
- Δ V
Δ V
Δ
v ν Ί
V Δ Δ H
Φ
8 s,
\- Δ : Build up v : Decay J
I 1 1
0.8
1 1 1

:o.4

Γ 1 1 1 1 1
2 4 6 8 10
Run Number

Fig. 6. Values of AJ^.L, D H and C H

measured using the ceramic sensor.

This may be due to a time-lag between the change in the hydrogen pressure
on the entry side and the detection of hydrogen on the extraction side.
AJoo-L was close to the value (2.21xl0~2 Α Ί Ι Γ 1 ) reported by Geller, so
that we took the D H value (3.74xl0~8 m2.s_:L) measured by Geller as hydrogen
diffusivity at 823 K and calculated C H . The CH's obtained were very close
to the value (0.792 ppm) estimated from Sievert's law as shown in Fig.6.
742
The variation of hydrogen permeability with time for 670 hr is shown in
Fig.7. From the figure, it was found possible to monitor the hydrogen
permeated through the steel with high detectability for such a long period
using the ceramic sensor.

300 400 500 700

Time /hr

Fig. 7. Variation of hydrogen permeability with time.

CONCLUSIONS

From these experiments, this method using the proton conductive electrolyte
has a possibility of application as an electrochemical technique for
prediction of hydrogen attack, although it has a problem on the measurement
of hydrogen diffusivity. It is being further improved to measure hydrogen
diffusivity with accuracy and to monitor the hydrogen content with high
detectability for a longer period.

REFERENCES

S.Ando, Y.Hisaoka, H.Hamada and K.Yamakawa (1991). A ceramic sensor for

prediction of hydrogen attack, ISIJ International, 31, in press.
H.Iwahara, T.Esaka, H.Uchida and N.Maeda (1981). Proton conduction in
sintered oxides and its application to steam electrolysis for hydrogen
production, Solid State Ionics, 3/4, 359-363.
S.Yoshizawa and K.Yamakawa (1975). Problems in measurement methods of
hydrogen permeability through steel, Boshoku Gijutsu, 24, 365-373.
W.Geller and T.H.Sun (1950). Einfluß von Legierungszusätzen auf die
Wasserstoffdiffusion im Eisen und Beitrag zum System Eisen-Wasserstoff,
Arch. Eisenhuttenw., 21, 423-430.
C.Sykes, H.H.Burton and C.C.Gegg (1947). Hydrogen in steel manufacture,
J. Iron Steel Inst. , 156, 155-180.
W.Eichenauer, H.Künzig and A.Pebler (1958). Diffusion und Löslichkeit von
Wasserstoff in o(-Eisen und Silber, Z. Metallk., 49, 220-225.
R.Wagner and R.Sizmann (1964). Die Diffusion und Permeation von Wasserstoff
in o(-Eisen, Z. angew. Phys., 18, 193-199.
H.Tsubakino and K.Yamakawa (1985). The relation between critical hydrogen
content of steels and temperature, evaluated from the Nelson chart,
Boshoku Gijutsu, 33, 159-161.
 WS8e6

Stress Corrosion Cracking of a Prestressing Strand

in a 3% NaCl Aqueous Solution

Yuki KOBAYASHI and Yoshihisa TANAKA

Ship Research Institute, Ministry of Transport

6-38-1, Shinkawa, Mitaka, Tokyo 181, Japan

ABSTRACT

Stress corrosion cracking (SCC) tests were performed under a constant load
and an anodic polarization. In a strand without mortar, a time to failure,
to, decreased linearly as an electrode potential was noble. When the ratio
or the applied load to the ultimate tensile load, Psc/Pu, exceeded 0.7,
short time to failure was observed for every electrode potential. But the
applied load did not affect t^ in Psc/Pu less than 0.6. The corrosion rate
was independent of the applied load. On the other hand, an improved
lifetime was observed in a strand covered with mortar, and consequently the
corrosion rate decreased markedly. When a localized corrosion occurred at
-450 to -400 mV vs. SCE, SCC of a type of active path corrosion was ob-
served on the surface of a side wire.

KEYWORDS

Stress corrosion cracking; Prestressing strand; Anodic polarization; Time

to failure; Corrosion rate; Active path corrosion; Localized corrosion.

INTRODUCTION

A large concrete offshore structure constructed by joining afloat struc-

tural sections is beyond repair in dock. The hulls of floating offshore
structures should be made light and thin, and so a corrosion of reinforcing
steels in seawater needs to be taken account of in the design of structure.
A prestressing strand is generally grouted within a sheath embedded in con-
crete. However, it is assumed that this prestressing strand also encounters
corrosive environments, that is, cracking, poor concrete cover, poor grout-
ing points, anchorage points, or jointed points of structural sections.
Stress corrosion characteristics are essential in order to predict the long
term operational life of the strand.

Previously, the authors experimentally investigated the prestressing

strand's susceptibility to stress corrosion cracking and corrosion fatigue
in a 3% NaCl aqueous solution (Kobayashi et al., 1990). In slow strain

743
744
rate tests, proof stress slightly decreased with a decrease in strain rate,
but contraction percentage of area did not decrease. A uniform elongation
decreased markedly. This trend indicated some susceptibility to SCC, but a
crack was not observed on a wire. In constant load tests, Psc/Pu=0.72 to
0.88, SCC also was not observed up to 9800 hours. But the breaking stress,
elongation and contraction percentage of area deteriorated in the tensile
tests after stress corrosion, and these deteriorations were dependent on
the applied load and corrosion time. The present paper now discusses the
SCC for the prestressing strand without and with mortar under the anodic
polarization.

EXPERIMENTAL PROCEDURE

Material and specimens

A seven-wire prestressing strand was based upon JIS G 3536 (type B,

SWPR7B) with one central wire and six side wires surrounding the central
wire. This strand was treated by hot stretching (strain tempering) under
tension for the improvement of the stress relaxation. The chemical com-
position and the mechanical properties of the steel are given in Tables 1
and 2 respectively. The nominal diameter of this strand subsequently
referred to as the prestressing strand was 12.7mm. The central wire had
Λ.39mm diameter and the side wires had 4.21mm diameter. The length of lay,
i.e. pitch was approximately 170mm. The proof stress, S Q 2> an(* stress at
the proportional limit, Sp, corresponded to a 0.2% and a 0.01% permanent
set respectively as given in Table 2. The ratio of the proof stress to the
ultimate tensile stress, Su, i.e. S Q p/^ u w a s 0.908, a n d the ratio Sp/Su
was 0.836. The uniform elongation, §J shown in Table 2 did not include the
breaking point in the tensile test.

Table 1 Chemical composition (%) Balance; Fe

C Si Mn P S Cu Ni Cr Al
0.82 0.26 0.73 0.019 0.006 0.01 0.01 0.02 0.037

Table 2 Mechanical properties

Load(kgf) Stress(kgf/mm ) Elastic modulus Elongation

Pu P0#2 Pp Su S0#2 Sp E (kgf/mm2) ό (%)

19500 17700 16300 197.6 179-3 165.1 19800 5·Λ

A coiled strand was cut into pieces of 1m length. Both a strand itself and
a strand covered with mortar were used as specimen for testing. The strand
with mortar was a strand embedded in a mortar of a 50mm diameter. The
cover was 18 to 19mm thick. The cover mortar had tensile cracks or a slit.
The tensile cracks were made by applying a testing load, and the crack
width, Wer, was less than 1mm. The slit was formed by a plate of 1 to 5mm
thick. It was regarded as a wide crack width. The mortar with the slit
also had the tensile cracks in applying the testing load.

Testing procedure

The SCC tests were performed through the anodic polarization under the con-
stant load; Psc/Pu=0.78, 0.7Λ and 0.6. A magnifying lever testing machines
 745
with a capacity 20tf were used. The length between grips was 720mm, and
the gage length was 500mm in a measurement of elongation. The specimen was
placed vertically in the corrosion tank as shown in Fig.1. It was electri-
cally insulated against the testing machine by plastic insulators at both
grips. A 250mm length of the specimen was in contact with the testing
solution, and held in a constant electrode potential during the test.

Salt was dissolved in distilled water to make the 3% NaCl aqueous solution.
The solution was slowly circulated through an 80 liter main tank to the 2
liter corrosion tank. The flow rate was controlled to lie between 1 to 2
liters per minute. The corrosion solution in the main tank was held at
constant temperature, 25±1°C, and saturated with dissolved oxygen by bub-
bling air through the solution. The pH range was 6.3 to 7.8 in the strand,
and 7.2 to 10.9 in the strand with mortar. The electrode potential, Φ, was
controlled by a potentiostat. Platinum was used for a counter electrode,
and a calomel half cell for a reference electrode.
>Load
Strand specimen
Potentiostat

In
37. NaCl

Fig.1 The testing method in the strand with mortar

RESULTS AND DISCUSSION

The time to failure in the SCC test

The time to failure was determined with the failure of one of the seven
wires. Sometimes several side wires failed simultaneously in a high ap-
plied load. A relationship between Φ and t f in the strand were shown in
Fig.2. The linear relationships were obtained in three cases of Psc/Pu.

-200
PSC
log t f = -1.51-0.00831 φ /PU
* o
—
σ
(/>- 3 0 0 - / ( P s c / P u =0.60) Δ 0.60
/ o 0.74
c > -400 / log tf=-1.31-0.00776φ α 0.78
φ >

&I -500 - B*i ( Psc/Pu =0.74 ) v 0.89

-D -600 ~ logtf=-1.06-0.006740/*^t^t^^
o E r r
- 7 0 0 - ( Psc / Pu =0.78 ) * w><D-> - ^ -
υ
' ' hiiil i l i 1 mil i i i 1 mil ι ι ι 1 im
101 102 103 10* 105
Time to failure, tf (hour)

Fig.2 Effect of the electrode potential on the time to failure

746

1I I I I I III
ImVvaSCEl
3 0.9 o -400
L_PP/PU ^ Δ-450
■ο'ο.β D -500
σ v-550
■2 0.7 T-580
-σ ♦ -620
£0.6 O Ecorr
Q.
<0.5 ■ i
i_L·
101 10 2 10 3 10A 10 5
Time to failure, tf ( h o u r )

Fig.3 Effect of the applied load on the time to failure

When Φ was nobler than the natural corrosion, Ecorr, the wires were dis-
solved in proportion to the electrode potential. But according to the
testing data under Ecorr, these data did not failed at the time which were
extrapolated from Φ-t^ linear lines. The effect of the applied load on the
time to failure was shown in Fig.3. In Psc/Pu more than 0.7, t|. decreased
markedly with an increase in the applied load. But t f is independent of
the applied load in Psc/Pu less than 0.6.

The relationships between Wer and t^ in the strand with mortar were shown
in Fig.4.. The Wer indicated the slit width or the crack width at failure
position. The strand without mortar were denoted by solid symbols and the
strand with mortar by open symbols. The t^ was improved on the strand with
mortar. In particular, a marked improvement was observed in narrow crack
width, 0.5 to 0.3mm. At the same time t^ was dependent on Psc/Pu and Φ in
the slit. As the reason of the improvement, it was considered that the
testing solution did not circulate through a narrow crack and dissolved
oxygen was not supplied sufficiently to an inside strand.

300 1—r—r-i 1 1—i i i ini| 1 1 1 1 1 III

1 H H
*mV Psc/Pu 1
vs.SCE 0.78 0.74 0.6
250 Without -400 • ▲ ■1
5
Pfc/Pu=078 J Ί I 1
mortar -500
With -400 O Δ D 1 +
5 _£=-400mV 1 '. 1 j mortar -500 ^ -ό-Ι
P»c/Pu=0.' '8
4 ~ Psc/Pu=o.6 JC\ I i/-"" * = - 5 0 0 m V Ί
#=-400mV \ \ 1 /\j.
3 P.c/Pu=0.6 1

ο\ ο\^τ -r>%
/ #= -500mV J
2

1
1 1 1 1Mill 1 1 1J 11 111 1 .Λ 1 1 1 11 I I III 1 l_±_LLLLll
w
10 1 10 2 10 3 10 4 10 5 10 6

Time to failure, U (hour)

Fig.4 Effect of crack width on the time to failure

Corrosion rate

A corrosion rate, Re, were shown in Fig.5. No treatment wire expressed the
side wire as being cut out from the strand and the polished wire expressed
the side wire which was polished by sand paper #J+00, These corrosion rates
were calculated from a current density in the anodic polarization. The Re
of no treatment wire was less than that of the polished wire, and such ten-
dency was remarkable in less noble electrode potential. The Ecorr of the
polished and no treatment wire reached -688 and -610mV vs. SCE respec-
tively. This difference seems to be influenced by a wire surface, that is,
 747
no treatment wire had oxide film and the polished wire had activated sur-
face. But in -450mV, there is little effect of the surface condition on
the corrosion rate.

A reaction weight obtained through an electric current during test agreed

with a weight loss obtained from the measurement of the wire diameter. So
the corrosion rate of the strand was calculated from the reaction weight.
Re was independent of the applied load in the strand without mortar. When
Φ was less than -600mV, Re ranged between the polished wire and no treat-
ment wire. But when Φ was more than -500 mV, Re was less than no treatment
wire. These values in Re were considered as imaginary values, because Re
of the strand was calculated from an assumption that a wire diameter was
dissolved uniformly. In practice, as localized corrosion was observed in
the noble electrode potential, the localized corrosion rate will give an
approximation to the corrosion rate in the polished wire.

o 1 1 ' 1 « '
P»c/Pu
-100 0.78 0.74 0.6
I I Without mortar o Δ D
-200 Γ I With mortar ▲
•
■
-300
L
/ / ^ Polished wire
-400 - ▲ · "9<j£
-500 Γ ■ ^ θ χ ^ ^ ^ No treatment wire
* -600 h
o
—' ^ $ ^ ^ ^ -
Z -700
t>
UJ
i 1 i I i 1 i 1 l l i 1
-800
10"2 10u 101 10' 103
Corrosion r a t e . Re ( g / m 2 / h )

Fig.5 Corrosion rate in the wires and strands

The corrosion rate of the strand with mortar was lower than that of the
strand itself as shown in Fig.5, and varied widely in same electrode poten-
tial. This was considered to be on account of the effect of the crack
width. Re depended on Wer as shown in Fig.6, but was independent of the
applied load. The corrosion rate gave approximately a constant value in
Wcr>2mm, and decreased markedly in Wcr<1mm. However Re also depended on Φ,
but this trend was not observed in Wcr<0.5mm.

~ 102 H—'—i—'—i—'—r ~ i — ■ — i — ·"

.c
-400mV

-500mV

*>mVvsSCE
Psc/Pu -4001-500
0.78 o ·
0.74 Δ
0.6 D 1■
J I I L_ J i L
2 3 4 5 6 7
Crack width , Wer (mm)
Fig.6 Effect of the crack width on the corrosion rate
748
Stress corrosion cracking under the anodic polarization

When the electrode potential was -450 to -4.00 mV, fine cracks were observed
on the surface of the wire at the position of failure as shown in Fig.7.
The same cracks also were observed at the portion of the slit. These
cracks contribute to the dissolution and fracture of the wire. The strand
in which cracks occurred showed t^ of less than 200 hours. In this case,
the small amount of the plastic strain was observed during test because of
the localized corrosion. On the other hand, the strand in which cracks did
not occurred showed t^ of more than 200 hours. In this case, the amount of
plastic strain increased with an increase of t^. because of the uniform cor-
rosion. As a consequence of above behavior, it is considered that SCC of a
type of active path corrosion occurs at -Λ50 to -4.00 mV vs. SCE under the
anodic polarization.

Fig.7 Stress corrosion cracks on the wire surface

CONCLUSIONS

SCC tests were performed on the seven-wire prestressing strand under the
anodic polarization. The results of this experiment are as follows.

(1) The time to failure, t^, decreased linearly as an electrode potential

was noble. The t^ decreased in the applied load, Psc/Pu, more than 0.7,
but was constant in Psc/Pu less than 0.6.

(2) The strand covered with mortar failed at the maximum crack width. The
t f improved markedly in the crack width 0.3 to 0.5mm.

(3) The localized corrosion occurred in a noble electrode potential, -4.50

to -400mV vs. SCE, and therefore SCC of a type of active path corrosion was
observed on the wire of the strand.

(4) The corrosion rate was independent of the applied load, but depended on
the electrode potential and crack width of mortar. The corrosion rate was
almost constant in the slit more than 2mm, and decreased markedly in the
crack width less than 0.5mm.

REFERENCE

Kobayashi,Y. and Tanaka,Y.(1990). Stress corrosion cracking and corrosion

fatigue of prestressing strand. The Ship Building Research Association of
Japan, Symposium on design and constructions of marine structures,pp.71-84-.
 WS8e7

HYDROGEN PLASTICIZATION OF TITANIUM ALLOYS

E.G. Ponyatovsky

Institute of Solid State Physics, Academy of

Sciences,Chernogolovka, Moscow distr., 142432 USSR

ABSTRACT

At some deformation conditions, hydrogen alloying results in an increase in

plasticity, a decrease in flow stress, and refined grain structure. These
phenomena are examplified here on several titanium alloys.

KEYWORDS

Hydrogen, plasticity, flow stress, titanium alloys.

High-pressure synthesis of hydrides of the main transition metals (Fe, Co,

Ni, Mn, Cr, Mo ets.) and their numerous alloys, study of their properties
have shown that hydrogen in trasition metals behaved as a donor of electrons
predominantly into the metal d-band. So, hydrogen could be considered as a
metallic interstitial alloying element with all ensuing consequences
(Ponyatovsky et al. , 1982, 1984). Numerous hydrogen effects on structural
and magnetic properties have been found in this field, such as changes in
Curie temperatures by several hundreds degrees, the F-AF, F-F, or AF-F phase
transitios, and so on.

Similarly, various hydrogen effects could be expected as concerns the

mechanical properties of alloys. The most customary of them was the
phenomenon of hydrogen embrittlement. A vast information on hydrogen
embrittlement at room and moderate temperatures was available at the
beginning of this study. We had an alternative question about the occurrence
of a specific hydrogen-induced mechanism of stress relaxation performed by
plastic flow which would result in an enhanced plasticity of metals. There
were some encouraging data by then (Kolachev et al., 1978, later reviewed by
Nosov and Kolachev, 1986; Kerr et al. , 1980) which reported an appreciably
enhanced workability of titanium alloys at hot- working temperatures of 800
to 1000 C and hydrogen contents n„ ^ 0.5wt.%.
Π

To set the plasticization mechanism to work, we intended to eliminate the

hydrogen embrittlement mechanism. So, a study was performed of the effect of
hydrostatic pressure to lGPa at T = 20 to 200 C on the mechanical properties
of hydrogen-free and hydrogen-alloyed Group IV and V metals (Ponyatovsky et
ai.,1985). It was found that stress-strain properties of hydrogen-alloyed

749
750
Zr,V, Nb, and Ti depended on pressure much stronger than those of initial
metals. Over P = 0.4 to 0.6GPa, the hydrogenated materials MeH became more
deformable than the hydrogen-free metals. Thus, hydrogen-induced
plasticization is realizable even below 200^C if deformation is performed
under conditions providing a sufficiently high hydrostatic component of the
stress tensor.

Further search of hydrogen effects was aimed at the study of stress-strain

properties of titanium and its alloys in a wide temperature range and
traditional patterns of stressed states which provide tensile,compressive,
and torsional tests. Variables were: hydrogen content, n = 0 to lwt.%,
o -4 -1
temperature, T = 20 to 900 C, strain rate, ε = 10 to Is , type of
deformation, and composition of alloying metals (Ti, Ti-6A1-4.5V, ets).
Studied were also crystal and grain structures as well as the influence of
hydrogenation and dehydrogenation cycles on structure and properties.
Experimental was detailed in (Aksenov et al., 1989; Bashkin et al., 1990a,b;
Ponyatovsky et al. , 1989a,b, 1990; Senkov et ai.,1990). An account of some
interesting results is given below.

Titanium. The Ti - H phase diagram is given in Fig.l, and Fig.2 shows the
temperature dependence of Ti - nH ductility, A , for several n„ values.

300 W0
nH,wt.% T,°C

Fig.l. Phase diagram of the Ti- Fig.2. Temperature dependense

ll system (San - Martin of ductility of Ti - nH
and Manchester, 1987). alloys.

-3 -1
Tensile tests were run at a rate ε 10 s . Ductility of the commercial
metal began appreciably growing over 550 C. At n u = 0.15 to 1.0 low A
n U.
values were observed in the range T = 20 to 250 C, but A sharply increased
near 300 C. A plateau-like region followed by the second rapid increase in
A were typical for higher test temperatures. E.g., ductility of the Ti -
0.16H alloy which was brittle at room temperature exceeded that of the
initial metal already at 250 C, remained constant in the range 300 to 600 C,
and displayed further sharp increase over 600 C. The sharpest increase in
 751
ductility at 280° to 400°C had the Ti - 0.5H alloy.

Other ductility behavior showed alloys with n u = 1.25 and 1.54 whose
Π
ductility Λ (T) jumped near 300 C, passed through a maximum at about 350 C,
and again decreased at higher test temperatures. Points in Fig.1 correspond
to temperatures of anomalous Λ (T) behavior for appropriate hydrogen
contents. A clear correlation is observed between the ductility anomalies
and special lines in the phase diagram, i.e., all points fall at the limits
of the two-phase regions or at the line equidistant from these limits.

The other interesting effect of hydrogen alloying concerned the changes in

flow stress. Concentrational curves <r(n„) in the range 300 to 750 C had a
Π
minimum that was more pronounced for developed plastic flow (see Fig.3).

u-0wt.%H li-6Al-2Zr-
-1.5V-1 Mo
Δ-0.58

500 S00 100 900 500 600 700 BOO

nu,wt-% TX τ°ο
Fig.3. Flow stress of Ti - Fig.4. Plasticity (ultimate angle
nH alloys at several strain) of the Ti-6Al-2Zr-
1.5V-nH alloy at torsional
temperatures and ac-
cumulated compres- strain rates c=0.25s - 1,
sive strain ε = 50%. 0.025s"1- 2, 0.0025s"1- 3.

Strain hardening of hydrogen-alloyed titanium was less than that of initial

metal over 350 - 400 C therefore compressive strain of 10 to 20% resulted in
lower values of σ for hydrogen-alloyed samples compared to hydrogen-free
ones. E.g.,at ε = 50% the cr values for samples with n = 0.35 to 0.60 made
bU H
only 30 to 60% of that for initial metal (Fig.3).

The third effect is connected with the strain-rate dependence of mechanical

properties. A more detailed study was carried out on a standard commercial
Ti-6Al-2Zr-1.5V-lMo(wt.%) alloy. Figures 4 and 5 show typical plasticity
patterns for alloys with several hydrogen contents in dependence on
temperature or torsional strain rate (Bashkin et al., 1990b, Senkov et al.,
1990). It is evident from Fig.5 that plasticity curves ε (c) of the
u
hydrogenated alloy have we11-pronounced maxima while plasticity of the
752

li-6AL-2Ir- ΠΗ = 0.58
-1.5V-1MO

e, s" e, s- e, sm
Fig.5. Plasticity (ultimate angle strain) of the Ti-6Al-2Zr-l.5V-
ΙΜο-ηΗ alloys at temperatures of torsion tests 607 C - 1,
660° - 2, 720°C 3, 780 C - 4.

-4
initial alloy decreases throughout the strain-rate range studied, ε = 5·10
-1 -1
to 5 -10 s . The effect of hydrogen-enhanced plasticity expressed as a
ratio α = ε (η )\ε (0) is represented in Fig.6. Function α(ε) is a curve

with a maximum and attains a value of about 27 at T = 607 C and ε = 10 s

li -6/11 -2Zr-1.5V-1Mo
nH = 0.40 nH = 0.5Swt.%H

e, s e, s-
Fig.6. Hydrogen-induced enhancement in plasticity of the Ti-
6A1 - 2Zr - 1.5V - IMo in torsion tests at temperatures
607°C - 2, 660°C 2, 720 C - 3, 780 C - 4.

and about 45 at T 660°C and ε = 10 s for n., = 0.58. I.e., at these

n
conditions of deformation plasticity of the hydrogenated alloy is 27 and 45
times that of the same alloy without hydrogen, respectively!
 753
Examination of the alloy grain structure after hydrogenation, different
steps of deformation, dehydrogenation displayed the following trend. Samples
with hydrogen-enhanced plasticity undergo a recrystallization process at the
initial flow steps which results in an equiaxial grain structure with a
grain size of 1 to 5mm. The grain refinement is concomitant with the lowered
flow stress. Both the main parameters of the formed fine-grained structure
and the low flow stress remain steady up to the sample fracture. A question
arose about the nature of the plasticization effect,i.e., is it due to
formation of the equiaxial fine-grained structure possessing a high dynamic
activity or due to some other particular relaxation processes induced by
hydrogen. To elucidate the question, we performed a special work
(Ponyatovsky et al., 1990) which evidenced that grain refinement itself
actually increased plasticity and decreased flow stress of the Ti-6Al-2Zr-
1.5V-lMo alloy. However, the contribution of the grain-size factor was
-1
negligible compared to hydrogen plasticization at optimum (ε ~ 0.1 - Is , T
« 700 C). Plasticity enhancement is caused primarily by the presence of
hydrogen itself, its specific effect on relaxation processes. Some
stress-relaxation mechanisms inherent in the hydrogen-containing alloys only
are conceivable from the extreemly high hydrogen mobility in titanium alloys
(Bashkin et al., 1989), e.g., by means of stimulated local phase
transformations, by variation of local hydrogen concentration due to stress
gradients (Dutta and Birla, 1987), by increased mobility of screw
dislocations and density of Frank - Read sources (Tabata and Birnbaum, 1983;
Thomson, 1987), and so on.

Hydrogen plasticization phenomena analogous to those described above were

also found in other alloys. For example, ductility maxima correlated with
broad flow-stress minima at n„ = 0.3 to 0.4 were observed in concentrational
Π
curves of the Ti-6A1-4.5V alloy heated over 630°C (Bashkin, et al., 1990).

A certain inherency was characteristic of each alloy studied. For example,

any hydrogen content embrittled the non-alloyed titanium at room
temperature. Other behavior was observed on the Ti-6A1-4.5V alloy at room
temperature and low strain rates. The ultimate compressive strain of this
-3 -1
alloy without hydrogen was about 8.5% at ε ~ 10 s while hydrogen alloying
to n = 0.27 increased this value to about 20%, other n - to 10 to 14%.

To conclude, an assumption can be made that hydrogen plasticization effects

are unlikely to be characteristic of only titanium alloys. It appears that
similar effects can be observed in other Group IV and V metals and their
alloys. Further detailed study of structures, phase diagrams and other
properties of these systems is necessary to elucidate the nature of this
interesting and promising phenomenon.

REFERENCES

Aksenov,Yu.A., I.0.Bashkin, V.L.Kolmogorov, E.G.Ponyatovsky, V.K.Kataya,

I.V.Levin, Yu.I.Potapenko and A.N.Trubin (1989). Hydrogen effect on
ductility and flow stress of commercial titanium at temperatures to 750 C.
Fiz. Metallov Metallovedeniye, 67^ 993-999.
Bashkin,I.0., A.I.Kolesnikov, V.Yu.Malyshev, E.G.Ponyatovsky, V.K.Fedotov,
J.Maier and I.Natkaniec (1989). Neutron vibrational spectroscopy on
ß-Ti_ „ X . ,H_ _ . Phonons 89. Proc. Ill Intern. Conf. on Phonon
U.»4 U.lb U.bl
754
Physics (S.Hunklinger, W.Ludwig and G.Weiss, eds.), Vol.1, pp.157-159.
World Scientific, London.
Bashkin,1.0., V.Yu.Malyshev, Yu.A.Aksenov, T.E.Antonova, E.G.Ponyatovsky,
V.L.Kolmogorov, V.K.Kataya, I.V.Levin, Yu.I.Potapenko, A.N.Trubin,
G.G.Taluts and S.V.Nikitin (1990a). Hydrogen effect on ductility and flow
stress of the Ti-6A1-4.5V alloy at temperatures to 930°C. Fiz. Metallov
Metallovedeniye, No.5, 168-174.
Bashkin,I.0., E.G.Ponyatovsky, O.N.Senkov and V.Yu.Malyshev (1990b). Strain
rate effect on hydrogen plasticization of the Ti-6Al-2Zr-l.5V-lMo. Fiz.
Metallov Metallovedeniye, No.2, 170-177.
Dutta,A. and N.C.Birla (1987). Stress induced hydrogen diffusion in a α+β
titanium alloy during superplastic deformation. Scripta Met. ,
21,1051-1054.
Kerr,W.R., P.R.Smith, M.E.Rosenblum, F.J.Gurney, Y.R.Mahajan and L.R.Bidwell
(1980). Hydrogen as an alloying element in titanium (hydrovac).
Titanium*80. Science and Technology, Proc. IV Intern. Conf. on Titanium
(H.Kimura and O.Izumi, eds.), Vol.4, pp.2477-2486, New York.
Kolachev.B.A., V.A.Livanov and V.K.Nosov, (1978). Hydrogen effect on
workability of titanium alloys with various phases. Titanium Science and
Technology. Proc. Ill Intern. Conf. on Titanium (A.F.Belov, ed.), Vol.3,
pp.61-68, VILS, Moscow.
Nosov.V.K. and B.A.Kolachev (1986). Hydrogen Plasticization at Hot Working
of Titanium Alloys. Metallurgiya, Moscow.
Ponyatovsky,E.G., V.E.Antonov and I.T.Belash (1982). Properties of
high-pressure phases in the metal - hydrogen systems. Soviet Phys.Usp.,
25, 596-619.
Ponyatovsky,E.G., V.E.Antonov and I.T.Belash (1984). High hydrogen
pressures. Synthesis and properties of new hydrides. In:Problems in Solid
State Physics (A.M.Prokhorov and A.S.Prokhorov, eds.), pp. 109-117. Mir
Publishers, Moscow.
Ponyatovsky.E.G., V.N. Larin, V.F. Shishmintsev, Yu.A.Aksenov and
I.O.Bashkin (1985). A production technique. Patent USSR No.1165525.
Ponyatovsky,E.G., I.O.Bashkin, O.N.Senkov, Yu.A.Aksenov, V.L.Kolmogorov,
G.G.Taluts, V.K.Kataya, I.V.Levin, Yu.I.Potapenko and A.N.Trubin (1989a).
Hydrogen effect on ductility and flow stress of the Ti-6Al-2Zr-l.5V-lMo
alloy at temperatures to 740 C. Fiz. Metallov Metallovedeniye, 68,
1167-1172. ~~
Ponyatovsky,E.G., I.O.Bashkin, O.N.Senkov and V.Yu.Malyshev (1989b). Effect
of temperature, strain rate and hydrogen content on hydrogen
plasticization of the Ti-6Al-2Zr-l,5V-lMo alloy. Doklady Acad. Sei. USSR,
306, 613-616.
Ponyatovsky,E.G., O.N.Senkov and I.O.Bashkin (1990). Effect of the initial
grain structure on hydrogen plasticization of the Ti-6Al-2Zr-l.5V-lMo
alloy. Metallofizika, 12^ 20-25.
San-Martin,A. and F.D.Manchester (1987). The H-Ti (hydrogen-titanium)
system. Bull. Alloy Phase Diagrams, 8, 30-42.
Senkov,0.N., I.O.Bashkin, V.Yu.Malyshev and E.G.Ponyatovsky (1990). Study of
plastic flow of the hydrogen-containing Ti- 6Al-2Zr-l.5V-lMo alloy in the
temperature range 823 to 1073K. Fiz. Metallov Metallovedeniye, No. 7,
119-127.
Tabata,T. and H.K.Birnbaum (1983). Derect observation of the effect of
hydrogen on the behaviour of dislocations in iron. Scripta Met., 17,
947-950.
Thomson,R.M. (1987). In: Physical Metallurgy (R.W.Cahn and P.Haasen, eds.),
Vol.3, Chap. 26, pp.324-391. Metallurgiya, Moscow.
 WS8e8

FRACTURE MECHANICS ASSESSMENT OF HYDROGEN INDUCED- AND

SULFID STRESS CORROSION CRACKING IN PIPELINES

M. BELLER 1 , C. MATTHECK 2

PREUSSAG Anlagenbau GmbH,

Pipeline-Service,
Breslauerstr.56b, 7500 Karlsruhe, Germany

Nuclear Research Center Karlsruhe GmbH,

Institute for Material and Solid State Research IV,
Postfach 3640, 7500 Karlsruhe, Germany

ABSTRACT

Advanced non destructive testing equipment (NDT) is being developed in order to assess the integrity
of oil- and gaspipelines. The flaws found have to be evaluated. Two major types of possible damage
found in pipelines are cracks and corrosion. These defects have to be assessed.
The paper presented will introduce a project concerned with the development of a lifetime-evaluation
technique for pipelines using data obtained through the application of intelligent pigs.
A short overview will be presented of the approach followed for the crack assessment. The fracture
mechanics assessment of hydrogen induced cracks (HIC) and sulfide stress corrosion (SSC) using the
concept of equivalent cracks will be introduced.

KEYWORDS

Pipelines, crack detection, hydrogen induced cracking, sulfide stress cracking

INTRODUCTION

It is well known that pipelines provide one of the safest, most reliable and most economic means for the
transportation of large quantities of liquids and gases, such as oil or natural gas. It is for these reasons
that large pipeline systems have been installed world wide, onshore and offshore. The amount of oil or
gas that can be transported through a pipeline is an important economic factor and there has been
therefore a trend over the years to construct pipelines with increased diameter operating with increased
pressure levels, requireing high strength steels such as X70 or X80. However some of the pipeline systems
in operation have reached an age of twenty to thirty years or more, which in Some cases is close to the

755
756
service life they had originally been designed for. It is therefore of increasing importance for the pipeline
operators to be able to assess the true state of their pipelines. Therefore advanced inspection tools have
been developed in recent years which allow the inline inspection of pipelines using non destructive testing
(NDT) techniques. These tools are generally called 'intelligent pigs' and the most recent pigs incorporate
sophisticated electronics, measuring and recording facilities to examine pipelines from within whilst being
propelled by the medium transported in the pipe. The data obtained is recorded on board and can then
be retrieved after the inspection run for a detailed evaluation. The flaws found by such inspections tools
will have to be assessed in order to determine the true condition of the examined pipe.

PIPELINE INSPECTION TOOLS

Pipelines have already been inspected for metal loss or cracks for a long time. This was and is still done
by proof testing of the pipes. In the case of pipelines hydrostatic testing is used. If the pipeline tested
survives the test, this indicates that any flaws present at the time of the test were below a specific critical
size. It is also reported in the literature (Dechant, 1972) that stress tests can increase the service life of a
pipeline. Optimum hydrotest strategies are currently being investigated (Leis and Brust, 1990). Using
NDT however should enable possible flaws to be detected (location and size) at a much earlier stage,
long before a certain, material specific critical size is reached. It is a further advantage that a line does
not have to be shut down, with the resulting production loss, for an inline inspection to be carried out.
Intelligent pigs are already in service which reliably detect flaws such as corrsosion, laminations or dents
(Beller and Schneider, 1990). An additional type of pig is required in order to detect another category
of serious flaws: cracks. Cracks are one of the major causes for possible service failures of pipelines
(Kiefner and Eiber, 1987). The development of crack detecting tools is still at an early stage. Appropriate
NDT-techniques are being investigated (Beller et at., 1990).

CRACKS IN PIPELINES

Cracks which are detected during inspection have to be assessed, in order to decide wether the pipe
section containing the flaw will have to be repaired immediately or wether it can remain in service for
some given time until repair and a consequent shut down of the line are more appropriate. Pipeline
integrity assessment is of great importance in order to ensure that failures resulting in possible loss of life,
environmental or economic damage are avoided! A project concerning the integrity assessment of pipe-
lines has therefore been initiated at the Karlsruhe Nuclear Research Center (KfK) in cooperation with
industry, concerning sub-critical crack growth in pipelines. The approach is basically a damage tolerance
analysis based on fracture mechanics. This paper will introduce this project with special respect to the
problem of hydrogen induced cracks (HIC) and sulfide stress corrosion (SSC).
The type of crack encountered in a pipeline will depend on any one of the following or their interaction:
the load collective the pipe experiences, the environment in which the pipe is placed, the characteristics
of the medium which is transported, possible malfunction of the active or passive corrosion protection
used and the actual fracture toughness of the material. Typical cracks are due to

• fatigue

• stress corrosion

• corrosion fatigue

• hydrogen embrittlement

• sulfide stress corrosion

USING FRACTURE MECHANICS APPROACH

Fracture mechanics provide the means to establish a procedure to assess the true state of pipelines
incorporating cracks. The basic problem consists of assessing a crack, once detected, and to determine
 757
the residual strength still provided by the pipe. In order to achieve this the following requirements must
be met:

• the crack detection tool (be it eddy current, ultrasonic or magnetic flux) must measure reliably and
accurately. Results must be reproducible.

• the dimension and location of a crack must be measured quantitatively

• the true loading and relevant material parameters must be known

Different concepts in order to assess the effect of cracks have been developed. In order to introduce the
procedure followed the validity of Linear Elastic Fracture Mechanics (LEFM) will be assumed here.
One such concept, well described in the literature (Broek, 1982, Knott, 1973) is the stress intensity factor,
K. The whole stress field at the crack tip is known when the stress intensity factor is known. The stress
intensity factor is defined as

K=aJ^Y (1)
where σ = applied stress, a = crack length, Y = geometry factor.
Whilst the stress intensity factor thus characterizes the loading side7 of a cracked structure, a toughness
value can also be determined experimentally for the 'material side7. This parameter is called fracture
toughness, usually denoted by K*. Depending on the loading mode, see Fig.l, of the crack tip and the
stress state at the tip one usually determines and tabulates the plane strain fracture toughness KIc.

j^n ^n ^ \

Fig.l: The three modes of cracking

A fracture criterion can thus be defined: Fracture or failure will occur if K for a given crack would equal
or surpass the fracture toughness for a given pipe material. For a mode I-situation this failure criterion
can be stated as
K,>KIC (2)
This simple equation clearly indicates the problems which have to be solved. A library of K-solutions
has to be established for typical pipeline cracks and relevant toughness values for pipeline steels will have
to be determined.

THE PROBLEM WITH SOUR GAS

Transmission pipelines have also been constructed for the transportation of sour gas. Two types of
hydrogen induced cracking can occur in such a wet hydrogen sulfide environment. One type is termed
758
hydrogen-induced cracking (HIC). This type can be observed in line pipe steels and can occur without
the presence of an external tensile stress (e.g. hoop stress). HIC's can either be observed as hydrogen
blistering close to the pipe surface or within the material, either as straight cracks or stepwise cracking
(see Fig.2a,b).

Hydrogen Induced Cracking

Sulfide Stress Cracking

Tl
Fig.2: Schematic drawing of HIC (a,b) and SSC (c,d)
The other type is termed sulfide stress corrosion cracking (SSC) and can occur under externally and
internally stressed or strained conditions and propagates at right angles to the tensile stress direction
(Kimura et.al.,19%9), as shown in Fig.2c,d. The mechanism of SSC in line pipe steel however is as yet
not fully understood.
Crack ensembles consisting of step-wise cracking or SSC detected by NDT-tools in pipeline-walls can
be arranged in any number of ways. A step by step fracture mechanics analysis needed in order to obtain
the K-solutions needed for an effective assessment would be very time consuming and thus costly. Due
to the variety and complexity of such ensembles it was therefore investigated wether a small number of
'equivalent cracks' of simpler geometry could be found for an easier and faster assessment. The equiv-
alent cracks found for circumferential crack ensembles (Beller and Mattheck, 1990) represent a 'worst
case' crack configuration found for each class of crack ensemble analysed. This paper will present these
equivalent cracks found for circumferential HIC-ensembles (step-wise cracking) and introduce an initial
approach for the fracture mechanics assessment of SSC.

Hydrogen Induced Cracking

Fig.3 shows a typical HIC-ensemble as found in the circumferential section of a pipe.

Fig.3: Typical HIC ensemble found in the section of a pipe (step-wise cracking)
The ensemble shown was analysed by Mattheck et.al (1989) using fracture mechanics and the Finite
Element Method (FEM). FEM and fracture mechanics are used throughout in order to determin
equivalent cracks. Extensive research has gone into the understanding of the initiation and propagation
of hydrogen induced cracks (Bruckhoff et.al., 1984, Craig, 1981, Herbsleb et.al., 1981, Kimura et.al.,
1989, Taira et.al.). This work is essential and of great importance in order to further improve line pipe
steel, however a simple method has to be devised in order to be able to assess the actual state of a
pipeline containing such a flaw.
 759
Two types of circumferential HIC ensembles can be observed. One type with circumferentially ending
crack tips (Fig.4a) and the other with radially ending crack tips (Fig.4b).

n surface T7

& surface Δ

Fig.4: a. circumferentially orientated crack tips

b. radially orientated crack tips

The latter can be arranged with crack tips equidistant (a = b) from the pipe surface (Fig. 5) or non
equidistant (a φ b), Fig.5. It is important to include the superimposed bending effect acting at the crack
tips due to the circumferential extension of the ensemble (Beller and Mattheck, 1990).

"-ι_τ

Fig.5: Distance of crack tip to free surface

a = b: equidistant
a^b: non-equidistant

Three equivalent cracks were defined for these configurations, as shown schematically in Fig.6a,b,c.
• a slanted crack which covers circumferentially ending ensembles (Fig.6a)
• a single step radial crack which covers radially ending ensembles with equidistant crack tips (Fig.6b)

• the angle crack which covers radially ending ensembles with non-equidistant crack tips (Fig.6c).

equivalent crack

Fig.6: Equivalent cracks:

a. circumferential
b. equidistant radial
c. non-equidistant radial
760
Sulfide Stress Cracking

FEM computations carried out sofar for different SSC configurations have indicated that an assessment
of such a crack ensemble is possible by using a single, radial equivalent edge crack, as shown in Fig.7.
The K-solutions obtained have been conservative for all geometries calculated sofar. However further
work ist still in progress.
equivalent crack

Fig.7: Sulfide stress crack

OUTLOOK

It is of great importance that operators are provided with the means to assess the true state of their
pipelines. For this reason advanced inline inspection tools using NDT-techniques are being developed
in order to detect possible cracks. These cracks must then be analysed in order to ensure an effective
integrity assessment. A project concerned with the development of such an integrity assessment proce-
dure has been introduced, with special regard to cracks caused by a sour gas environment. A small
number of equivalent cracks of simple geometry were introduced in order to characterize ensembles of
HIC's and SSC's. Further work on such ensembles is currently being carried. FE-calculations are being
performed investigating the effect of internal pressure at the crack tip as well as the stress distribution
around nonmetallic inclusions associated with HIC's.

REFERENCES

Beller, M. and C. Mattheck (1990). Assessment of unified ensembles of hydrogen induced cracks using
the concept of equivalent cracks. Proc.9th lnt.Conf.OMAE9l, No.l0296G, 27-33.
Beller, M. and U. Schneider (1990). Pipeline inspection with the intelligent ultrasonic pig. Oil Gas Europ.
Mag., 3, 24-26.
Beller, M., K. Germerdonk, C. Mattheck, D. Munz and U. Schneider (1990). On the problem of
detecting and assessing cracks in pipelines. To be presented at the ASME-OMAE 91 conference at
Stavangar, Norway.
Broek, D. (1989). Elementary Engineering Fracture Mechanics. Kluwer Academic Publishers, Dordrecht.
Bruckhoff, W., O. Geier and K. Hofbauer (1984). Erfahrungen und technische Erkenntnisse für den
sicheren Betrieb von Sauergasfeldleitungen. Erdöl-Erdgas, K), 339-346.
Craig, B. D. (1981). A fracture topographical feature characteristic of hydrogen embrittlement.
Corrosion, 9, 530-532.
Dechant, K. E. (1972). Stress Tests an Rohrleitungen zur Erhöhung der Sicherheit und Lebensdauer.
TU, 13(3], 83-85.
Herbsieb, G., R. K. Poepperling and W. Schwenk (1981). Occurence and prevention of hydrogen
induced stepwise cracking and stress corrosion of low alloy pipeline steels. Corrosion, 5, 247-256.
Kiefner, J. F. and R. J. Eiber (1987). Pipeline Failure Update-1. Oil&Gas J., Mar 30, 98-100.
Kimura, M., N. Totsuka, T. Kurisu, K. Amano, J. Matsuyama and Y. Nakai (1989). Sulfide stress
corrosion cracking of line pipe. Corrosion, 4, 340-345.
Knott, J. F. (1973). Fundamentals of Fracture Mechanics. Butterworths, London.
Leis, B. N. and F. W. Brust (1990). Ductile crack growth models and its implications with regard to
optimum hydrotest strategies. Proc. Pipeline Tech.Conf.Ostende, Vol. B, 13.11-13.17.
Mattheck, C, M. Beller and H. Moldenhauer (1989). Effective fracture mechanical assessment of unified
ensembles of hydrogen induced cracks. Proc. 8th Int.Conf.ASME-OMAE 89, Vol.V, 347-354.
Taira, T., K. Tsukada, Y. Kobayashi, H. Inagaki and T. Watanabe (1981). Sulfide corrosion cracking
of linepipe for sour gas service. Corrosion, j_, 5-16.
WS8e9

ELUCIDATION OF MICRO-KINETICS OF HYDROGEN ASSISTED CRACKING

OF LOW ALLOY STEEL BY ACOUSTIC EMISSION SOURCE INVERSION METHOD

Yasuhisa Hayashi, Tomonori Terasawa and Mikio Takemoto

College of Science and Engineering, Aoyama Gakuin University

6-16-1, Chitosedai, Setagaya-ku, Tokyo ,157 JAPAN

I. INTRODUCTION

Acoustic Emission(AE) has been widely used to monitor the progress of hydrogen assisted cracking.
However, the conventional AE was not successful in elucidating the microkinetics and kinematics of
isolated crack. On the contrary, a new signal processing ; "AE source wave analysis '" or "Source
mechanisms of AE '" is now making a remarkable progress, and making it possible to elucidate the mi-
crokinetics and kinematics. A macroscopic crack behavior is considered to be associated with the for-
mation and coalescence of microcracks. This phenomena is well formulated by the concept of "eigen-
strain '" in the field of micro-mechanics. A new AE monitoring system which could correctly measure
the surface displacement excited by stress waves has been developed . Inversion processing utilizing
theoretical Green's function was also developed, and applied to elucidate the microkinetics of hydrogen
assisted cracking. The source waves; the generated volume or released energy by crack formation are
obtained by this method. This paper introduces the microkinetics of hydrogen assisted cracking of QT-
treated chevron notched specimen under constant extension rate test(CERT).

Π. FORMULATION OF AE SOURCE WAVE INVERSION SYSTEM

According to the BEM and seismology, the displacement :Ui(x,t) at pointrx and time:t on the elastic
body:S due to the dipole source (microcrack generation) in the inner boundary:F at point:x' and time:t'
is given by Eq.(l) when the crack volumerAV^ (x* / ) is infinitesimal compared to the outer boundary. '

ui(x,t)=AVjk(x'/)*Tik(xtfS/) (i)
where the symbol * denotes the convolution integral in time. ΓΛ (*,/;*'/) is the second kind
Green's function, and given by Eq.(2)
T^XGijjni+vGikjnj+vGijtrij (2)
where the Gi^ is the spatial derivative of the Green's function in xj direction; dGij/dxk, and Λ, is the
unit vector normal to the crack surface: ΔΑ;·. The crack volume: AV is given by Eq.(3)
AV=bk-Mj (3)
where, bk is the discontinuity of displacement as shown in Fig.l, and corresponds to the " crack tip
opening displacement (CTOD)" in fracture mechanics. When the microcrack rapidly generates with the
rise time of ATr , the transient volume change could be approximated by a sinusoidal step function of
Eq. (4) under the condition of dV(t)/dt=0 for /<0

761
762

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ZHZ
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I

AD
8. 1
m
Time
(Source Wave)
Fig. 1 Schematic i l l u s t r a t i o n of new monitoring system
of surface displacement and source inversion
processing system

dV(t)/dt=V0sin\nt/ATr) , forO<t<ATr
=V0 for ATr<t (4)
By the way, Eq.(l) could be rearranged to Eq.(5) for the released energy: AD(x' /)
Uiix^ADjtix'/yGijtixrS/) (5)
The change of D(x\t') with time; dD(t)/dt, could also be expressed by a sinusoidal function. These
equations suggest that the kinetics of microcrack generation could be obtained by the inversion process-
ing of Eqs.(6) and (7)
Av^UiipctyPijbcjfj/yr1 (6)
AD^-OcO* [G^Ocr;*'/)]"1 (7)
where * [ ] _ 1 means the de-convolution integral. These equations also show that it is very important to
correctly measure the surface displacement: ί/,·(χ,ί) for inversion processing. Therefore, the authors
developed a new AE monitoring system which made it possible to monitor the surface displacement and
also to do the signal processing of above equations. Detected waves were digitized by the fast A/D
converter(digitizer) and processed by the AE Data Acquisition System(ADAS) developed by us. The
system was demonstrated to correctly measure the surface displacement up to 1.5MHz. The source
waves were obtained by the de-convolution integral in time domain utilizing the theoretical Green's
function . In order to examine whether the system correctly measures the surface displacement, a
computer simulation of displacement at sensor position was also done for an assumed kinetics of
Mode-I crack.

III. EXPERIMENTAL

The chevron notched QT treated low alloy steel (AISI 4135) with a geometry of Fig.2 was used. A
displacement sensor (DUNEGAN S9208) is mounted directly on the epicentral surface to the apex of
triangle ligament. This specimen-sensor configuration could minimize the wave distortion by reflected
waves from side wall, and also makes it easy to identify the front of macroscopic crack. Therefore, the
theoretical Green's function could be computed and used for inversion processing. The specimen was
cathodic hydrogen charged for 24 hours in the solution7) (IN H3B04 +0.033M KC1 +0.02M thiourea) at
current density: SmA/cm2 prior to the CERT. The crack opening displacement at load point and the
applied load were simultaneously monitored using a special clip gauge and load cell. The compliance
was experimentally determined.
 763

Displacement sensor Stress intensity factor: Kj of chevron

notched specimen under load: P and
ADAS System dimensionless crack length: a=alW is
given by Eqs.(8) and ( 9 Γ .
p
(8)

1 dCl cti-cto
with 7*= (9)
2 da α-αο

where Cl is dimensionless compliance.

B, W, a0 and al are shown in Fig.2.
Y*(a) was determined from compli-
ance change during the test, In this test
method, Y*(ct) usually changes as
Fig. 2 Chevron notched specinen shown in Fig.3, and reaches to the
with displacement AE minimum: Y*(a) at the dimensionless
sensor crack length of 0.60 where the load
reaches to the maximum. A relatively
200 good agreement was observed between
AE wave the experimental Y*(a) and that
1501 analysis zone estimated by "superpose method" after
D.Munz 8) . The coordinate of the
macroscopic crack front is then calcu-
100 lated by Eq.(9), and used for theoreti-
cal Green's function. AE source
inversion processing was done for the
50 detected waves in the test range as
Experimental Γ
shown in Fig.3.
0 J_ Fig.4 shows the change of load,
0.2 0.4 0.6 0.8 1.0 calculated Kj and crack length during
a,Dimensionless crack length the CERT at O.lmm/min. The black
Fig. 3 Relation between Y* and dimensionless arrows towarding the loading curve are
crack length for chevron notched the detected AE waves. It can be seen
specimen that subcritical cracks, or stable cracks
propagate through
Kj; Stress Intensity Factor, kgfmnr//:

the whole ligament

even under the
CERT. Fig.5 com-
Macroscopic crack length, mm

pares the computer

simulated surface
displacement (left)
& WAV^
i+_l 2,000 -
M
<T >^
>x
1
. / *i
and detected waves
(right) at crack
length of 4.04,
·* X /·
^ 12.10 and 17.27
3
• · ·
mm, respectively.
V)0U
Computer simula-
Load '^r
•3 tion was done for
H / ^ Crack the Mode-I cracks
length with a rise-time of
n — ^ : . . . _ i — _ , —__j i i . i_J 2 to 5 μ8βΰ.
TO 20 30
Test time, minute It could be seen
Fig. 4 Change of load, crack length and Kj of that the first few
hydrogen precharged Chevron notched low wave-forms of
alloy steel during CERT test. detected ones well
resemble with the
computer
764

χ ΐ θ •10 χΐθ simulated waves. This clearly

Sensor output, V
shows that (l)the developed
Displacement, m

system does measure the dis-

placement normal to the free
surface, and (2)the detected
waves are generated by pure
ΔΤΓ ; 2 Hsec|
Mode-I crack. Though the
wave-distortion by reflected
waves were observed at 8|isec.
10 20 30 10 20 30
later than the first arrival of P-
Time, p s e c Time, psec
wave. This wave distortion
Crack length : 4.04 mm a= 0.449 does not necessarily give the
source waves any serious prob-
xio xlO"' lems when the de-convolution

:V
Displacement, m

j 1 v 6 integral is done in time domain,

and the first behavior of source
tr t so /"Λ | wave is analyzed. As the
conversion factor; the ratio of
3
ΔΤΓ;2.3

I s- p /
sensors output voltage to the
unit surface displacement, was
determined to be 1.965x1ο8
10 20 30 0 10 20 30 volt/m by the "modified surface
impulse method" \ The sensor
Time, psec Time, p s e c
output was converted to the sur-
Crack length 1 2 , 1 0 mm a = 0.577 face displacement. Then, the
r 10 source waves were obtained by
xlO xlO '
Eqs,(6) and(7). Fig.6 shows
Displacement, m

- 4
some examples of source waves.
A Heaviside-type volume (or

l·r
^ k
energy) release shows that the
microcrack quickly generates
within a very short time. Fig.7
shows the change of the
8o released energy: AD with test
10 20 8-2 10 20 30 time.
Time, p s e c
en Time,psec
The released energy : AD is
S - 4 mm <*= 0.659
Crack length : 17.27 correlated with the "energy
Fig. 5 Conparison of computer constructed surface release rate: G" in the fracture
displacement(left) and detected waves(right) mechanics by Eqs.(10) and (11)
under plane strain condition.
AD=GAA (10)

(Π)
For the case of Eq.(6), the crack volume : AV can be converted to the crack area using the CTOD
which is calculated by Eq (12) under the assumption of small scale yielding at crack tip 9) .

bt^v-^
4£σ ν
(12)

where E and v are Young's modulus(207000 MN/m2) and Poisson's ratio(0.3) , and csy is the yield
strength (1210 MN/m2).
Therefore, the crack area : ΔΑ could be calculated by Eq.(13) and (14).

AA=AD^ ^ „ „ (13)

AA=AV ^~ (14)
πΚ\\-ν-)
 765
Crack volume, m

0.035 0.0361

°, 0.02

10 20
Time, psec
Ϊ 0.01
Released Energy,

Q
J- -L
25 30 35
I

Test time , min.

I

10 20 Fig. 7 Change of energy released

Time, usec
by Mode-I microcrack
Fig. 6 Source waves of hydrogen generation with test time
assisted cracking.
An equivalent crack length: Δ/ for square crack is given by Eq.(15).
Δ/=Λ/ΔΛ~ (15)

Fig.8, obtained by Eq.(13), shows that the micro-crack size is in the level of 50 to 200 μτη, and
corresponds to three to ten grains of previous austenitic grains. The crack size tends to increase with the
progress of macroscopic crack length.
As the rise-time : ΔΓΓ of source wave is considered to be the time for the microcrack to generate,
X10" therefore the crack velocity is given by Al/ATr. Fig.9
shows the crack velocity reaches to a maximum of 200
m/sec. A relatively good agreement between the data
from the released energy(white circles) and created
Δ1, Equivalent crack length, μπι

volume(black circles) suggests that the signal processing

ΔΑ, Crack opening area, mm2

and the concept of fracture mechanics used in this study

are appropriate.
Though, the exact source location of each AE signal
could not be identified in this experiment because only
one monitoring system is used, SEM observation of
fracture surface was carefully done to examine the
propriety of the source waves. It was found that there
are so many isolated cleavage transgranular fracture
with an equivalent diameter of 50 to 150 μτη as shown
in Fig. 10. The cleavage fracture is generally associated
with an elongated MnS and surrounded by dimple frac-
ture. The elongated MnS on fracture surface is due to
the specimen's configuration in C-R direction from
drawn rod. The authors have a opinion that the source
waves obtained by this signal processing corresponds to
25 30 35 the microkinetics of these cleavage TG-fracture associ-
Test time, min. ated by MnS, based on the following facts. (1) The
Fig. 8 Change of microcrack number of detected AE signals (43 waves) and cleavage
fracture spots well agrees and (2) the crack size
length :Δ1 and crack
estimated by source waves well agrees with the size of
area-.ΔΑ with test time
cleavage fracture on fracture surface.
766

ΤΓ IV. CONCLUSION
200 An advanced elastic wave monitoring and inversion
• ; Eq. 14 processing system (ADAS) was developed to elucidate
Equivalent crack length, pm

Ο ; Eq. 13 the micromechanics of hydrogen assisted cracking. The

system makes it possible to monitor the surface dis-
placement and to do the de-convolution integral of
detected waves by the theoretical Green's function. The
* source waves suggest that the Mode-I type cleavage
• O transgranular fracture associated with segregated MnS
O occurs at a maximum velocity of 200 m/sec.

OS Ό
ACKNOWLEDGMENT

Study was supported by undergraduate students;

Messrs. S. Tamazaki and T. Morikawa. Their earnest
cooperation is acknowledged.

LITERATURE CITED
< 50
,0 1.5 2.0
*-w Rise
ΧΛ-1-KJV- time.
i_-ui.^,f usec 1) Takanori Ohira and Teruo Kishi; JJap.Inst.Metals,
46-5, 518(1982).
Fig.9 Relation between crack
length and rise time 2) M.Ohtsu; J.Acoustic Emission, 1-2, 103(1982).
3) T.Mura; "Micro mechanics of Defects in Solids",
Martinus Nijhoff Published 1982).
4) Y.Hayashi and M.Takemoto;
JJap.Soc .Non-Destructive
Inspection, 39-11, 921(1990).
5) M.Ohtsu and K.Ono;
LAcoustic Emission, 3-1, 27
(1984).
6) L.RJohnson; Geophys. J. R.
astr. Soc., 37, 99 (1974).
7) K.Yamakawa, Y.Minamino,
K.Matsumoto, T.Yonezawa
and S.Yoshizawa; J. Soc.
Mat. Sei. Japan (ZAIRYO),
29, 1101(1980).
8) D.Munz, R.T.Bubsey and
LE.Srawley; IntJ.Fracture,
Fig. 10 SEM of fracture surface at crack 16-4, 359(1980).
front with miniraum Y(a). Note brittle
IG-microcrack with MnS in it. 9) Dovid Broek; "Elementary
Engineering Fracture
Mechanics", NOORDHOFF
INTERNATIONAL PUB-
LISHING, 215 (1974)
 WS8e10

Threshold Hydrogen Content for Hydrogen Embrittlement

of Low Alloy Steels and 13Cr Steels

Takahiro Kushida and Takeo Kudo

Iron and Steel Research Laboratories

Sumitomo Metal Industries,Ltd.
1-8 Fuso-cho, Amagasaki, Hyogo, 660, Japan

ABSTRACT
Hydrogen e m b r i t t l e m e n t (HE) of low a l l o y s t e e l s and 13Cr s t e e l s
was i n v e s t i g a t e d by t h e c o n s t a n t l o a d t e s t u n d e r cathodic
h y d r o g e n c h a r g i n g , and the electrochemical hydrogen permeation
t e s t was c o n d u c t e d t o measure t h e t h r e s h o l d h y d r o g e n p e r m e a t i o n
rate f o r HE ( J t h ) , t h e d i f f u s i o n c o e f f i c i e n t of h y d r o g e n (D)
a n d t h e t h r e s h o l d h y d r o g e n c o n t e n t ( C t h ) . The r e s u l t s w e r e a s
follows. The J t h was d e c r e a s e d w i t h t h e i n c r e a s e in t h e
s t r e n g t h and t h e a p p l i e d s t r e s s , and t h e J t h and t h e D of 13Cr
s t e e l s were a b o u t 1/10 of t h o s e of low a l l o y s t e e l s . On t h e
o t h e r h a n d , t h e Cth was a l m o s t c o n s t a n t r e g a r d l e s s of t h e
s t r e n g t h , a n d t h e C t h of 13Cr s t e e l s was a l m o s t t h e same a s
t h a t of low a l l o y s t e e l s . The C t h was d e c r e a s e d w i t h t h e
increase in the applied s t r e s s .

KEYWORDS

Hydrogen embrittlement, t h r e s h o l d h y d r o g e n c o n t e n t , low a l l o y

steel, 13Cr steel, hydrogen permeation rate, diffusion
coefficient of hydrogen , absorbed hydrogen content

INTRODUCTION
H y d r o g e n e m b r i t t l e m e n t (HE) s u c h a s h y d r o g e n i n d u c e d c r a c k i n g
(HIC) , s u l f i d e s t r e s s c r a c k i n g (SSC) a n d d e l a y e d f a i l u r e i s
o n e of s e r i o u s c o r r o s i o n p r o b l e m s f o r c a r b o n s t e e l s a n d low
alloy steels. 13Cr s t e e l h a s a l s o t h e h i g h s u s c e p t i b i l i t y t o
HE in s o u r (H 2 S) e n v i r o n m e n t s ( K u r a h a s h i e t a l . , 1985). HE i s
a common problem for f e r r i t i c s t e e l s .

HE s u s c e p t i b i l i t y h a s b e e n c o n s i d e r e d from two a s p e c t s : t h e
h y d r o g e n c o n t e n t in t h e s t e e l ( C Q ) a n d t h e t h r e s h o l d h y d r o g e n
c o n t e n t f o r c r a c k i n g ( C t h ) ( I k e d a e t a l . , 1977). It has been
a c c e p t e d t h a t HE o c c u r s when t h e CQ becomes h i g h e r t h a n t h e Cth
which i s d e c r e a s e d w i t h t h e h a r d n e s s of t h e s t e e l ( O k a d a e_t
al., 1973).
767
768
A n e w t e c h n i q u e " i n s i t u HIC M e a s u r e m e n t M e t h o d " h a s been
d e v e l o p e d , by which t h e Cth c a n be m e a s u r e d more exactly
( K u s h i d a 1990). I t w a s f o u n d b y t h i s n e w m e t h o d t h a t t h e C t h
f o r HIC in c e n t e r s e g r e g a t e d p o r t i o n s of l i n e p i p e s t e e l s was
constant regardless of the hardness and the content of
s e g r e g a t e d elements such as manganese, p h o s p h o r u s and c a r b o n
(Kushida e t a l . ) .

In t h i s p r e s e n t work, the effect of the hardness and the

a p p l i e d s t r e s s o n t h e HE s u s c e p t i b i l i t y o f l o w a l l o y s t e e l s and
13Cr s t e e l s was i n v e s t i g a t e d b y t h e c o n s t a n t l o a d t e s t under
the cathodic hydrogen charging, and the electrochemical
h y d r o g e n p e r m e a t i o n t e s t was a l s o c o n d u c t e d .

EXPERIMENTAL

Materials

Quenched and t e m p e r e d low a l l o y s t e e l s and 13Cr s t e e l s w h o s e

t e n s i l e s t r e n g t h r a n g e d f r o m 660Mpa t o 1410Mpa w e r e prepared.
C h e m i c a l c o m p o s i t i o n s a r e s h o w n i n T a b l e 1, a n d h e a t treatment
c o n d i t i o n s a n d t e n s i l e p r o p e r t i e s a r e shown in T a b l e 2.

Table 1. Chemical compo:sition of steels use d (mass %)

Steel C Si Mn P S Cr

Low alloy ί3te:el 0.17 0.26 1.29 0.015 0..005

13Cr steel 0.21 0.35 0.67 0.017 0..001 12.43

Table 2. Mechanical properties and heat tre atment

Stee 1 YS(MPa) TS(MPa)ι Quenching Tempering

Low 1120 1090 950° C X 30min WQ 350° C x 30min AC

alloy 930 1020 950° C X 30min WQ 450° C x 30min AC
steel 705 810 950" C X 30min WQ 550° C x 30min AC
520 660 950° C X 30min WQ 650° C x 30min AC
1090 1410 950° C X 30min WQ

13Cr 640 820 980° C x 30min 0Q 730° C x 30min AC

steel 820 970 980° C x 30min 0Q 620° C x 30min AC

WQ;Water q u e n c h i n g , 0 Q ; 0 i l q u e n c h i n g , AC;Air cooling

4mm b a r s p e c i m e n s w i t h a n o t c h (0.3mm d e p t h , 60° , 0.125R) w e r e
used for t h e c o n s t a n t l o a d t e s t u n d e r c a t h o d i c hydrogen
charging. Thin p l a t e specimens of 1mm t h i c k n e s s w e r e u s e d f o r
t h e e l e c t r o c h e m i c a l h y d r o g e n permeation t e s t (Yoshizawa e t a l . ,
1975).
Procedures

At f i r s t t h e HE s u s c e p t i b i l i t y was e v a l u a t e d a s t h e c r i t i c a l
c a t h o d i c c u r r e n t d e n s i t y o v e r which f a i l u r e o c c u r r e d by t h e
constant load test in 0.5% H 2 S 0 4 with 1.4g/l thiourea.
C h a r g i n g c u r r e n t d e n s i t y u s e d was 0 . 1 , 0 . 3 , 1, 3, 10> 30 a n d
 769

lOOmA/cm . The maximum t e s t duration was 200h.

Next h y d r o g e n p e r m e a t i o n r a t e (J) was measured a t e a c h c a t h o d i c
current density . D i f f u s i o n c o e f f i c i e n t of h y d r o g e n (D) was
given by f i t t i n g experimental permeation c u r v e s with t h e
t h e o r e t i c a l curve. The median of t h e minimum J a n d t h e maximum
o n e when HE o c c u r r e d a n d d i d n o t r e s p e c t i v e l y was d e f i n e d a s
t h e t h r e s h o l d hydrogen permeation r a t e (Jth).
A l t h o u g h t h e d i s t r i b u t i o n of t h e h y d r o g e n c o n t e n t in t h e s t e e l
in t h e c o n s t a n t l o a d t e s t b y r o u n d b a r s p e c i m e n s i s d i f f e r e n t
from t h a t in t h e h y d r o g e n p e r m e a t i o n t e s t , w h e r e h y d r o g e n
p e n e t r a t e s t h r o u g h t h e p l a t e from o n e s u r f a c e t o t h e o t h e r
s u r f a c e , t h e h y d r o g e n c o n t e n t (C 0 ) a t t h e c h a r g e d s u r f a c e i s
t h e same. So t h e Cth was given by t h e following formula .

Cth (ppm) = J t h (A/cm2) x l(cm) / D (cm 2 /s) (1)

( 1 ; thickness of p l a t e used for hydrogen permeation)
RESULTS
The c r i t i c a l c u r r e n t d e n s i t y f o r HE, t h a t i s , t h e t h r e s h o l d
h y d r o g e n p e r m e a t i o n r a t e ( J t h x 1), was d e c r e a s e d w i t h t h e
i n c r e a s e in t h e s t r e n g t h o f s t e e l s a s s h o w n i n F i g . l . I t was
confirmed that high strength steels had the high
s u s c e p t i b i l i t y t o HE. And t h e J t h x 1 of 13Cr s t e e l s was o n e
o r d e r in m a g n i t u d e l e s s t h a n t h a t of low a l l o y s t e e l s a t t h e
same s t r e n g t h l e v e l . I t w a s f o u n d t h a t 13Cr s t e e l s h a d t h e
higher s u s c e p t i b i l i t y t o HE than low a l l o y s t e e l s .

TOO
c 25°C oy(applied stress)
D
<u
en v = 650MPa
-σ to o
h
10h \ Low alloy steel
-a o ^ -
^ +-> o? D
W(1JA
Q) B - c N
S- £- 4-> \ J 3 C r steel
i— a . lh
1 I 1 L- 1
600 1000 1000 1400
Tensile strength (MPa)
Fig. 1 Effect of tensile strength on threshold hydrogen
permeation rate (Jth χ £)
And t h e t h r e s h o l d h y d r o g e n p e r m e a t i o n r a t e ( J t h x 1) was
d e c r e a s e d with t h e i n c r e a s e in t h e a p p l i e d s t r e s s as shown in
Fig.2. It was confirmed t h a t t h e a p p l i e d s t r e s s i n c r e a s e d t h e
HE susceptibility.
F i g u r e 3 shows t h a t t h e d i f f u s i o n c o e f f i c i e n t of h y d r o g e n (D)
was d e c r e a s e d with t h e i n c r e a s e in t h e t e n s i l e s t r e n g t h of
steels as p r e v i o u s l y r e p o r t e d (Yamakawa e t a l . , 1979). It
should be n o t e d t h a t 13Cr s t e e l s had t h e much s m a l l e r D t h a n
low alloy s t e e l s at the same s t r e n g t h l e v e l . It was s u g g e s t e d
770
from the r e s u l t s shown in F i g . l ,Fig.2 and Fig.3 t h a t t h e
s t e e l s with the small D had t h e small t h r e s h o l d h y d r o g e n
permeation r a t e (Jth x 1) and t h e r e f o r e t h e high s u s c e p t i b i l i t y
to HE.
100
810MPa) (Tensile strength)
25°C
c
ω
en
o ω^—
s- +J E
-O & O
>> * - > 10
-C <
7^.-^(800MPa)
c: 3.
fO
ΙΛ CU X
<U
o
S-
E -
+-> «=«*
S- 4->
13Cr steel
o- V
I— Q- --— J[970MPa)

400 600 800

Applied stress (MPa)
Fig. 2 Effect of applied stress on threshold hydrogen
permeation rate (Jth χ l)

10"
25°C

Low alloy steel

oo
o
O CM 10"
OJ E
c en o
o o—
•r- S-
tO Ό Q \ 13Cr steel

10"
6001000 1400
Tensile strength (MPa)
Fig. 3 Effect of tensile strength on diffusion coefficient
of hydrogen (D)

F i g u r e 4 shows t h e t h r e s h o l d h y d r o g e n c o n t e n t ( C t h ) w h i c h i s
o b t a i n e d from b o t h t h e t h r e s h o l d h y d r o g e n p e r m e a t i o n r a t e ( J t h
x 1) in F i g . l and t h e d i f f u s i o n c o e f f i c i e n t of h y d r o g e n (D) in
F i g . 3 by t h e f o r m u l a (1). The C t h was i n d e p e n d e n t of t h e
s t r e n g t h , and t h e C t h of 13Cr s t e e l s was a l m o s t t h e same a s
t h a t of low a l l o y s t e e l s , a l t h o u g h t h e J t h x 1 and t h e D w e r e
d e p e n d e n t on t h o s e f a c t o r s . On t h e o t h e r h a n d , t h e a p p l i e d
s t r e s s decreased the Cth as shown in Fig.5 .

DISCUSSION
It has been g e n e r a l l y a c c e p t e d t h a t t h e high s u s c e p t i b i l i t y t o
HE of h i g h s t r e n g t h s t e e l s i s d u e t o t h e d e c r e a s e in t h e
t h r e s h o l d h y d r o g e n c o n t e n t (Cth) (Okada e t a l . , 1 9 7 3 ) . However
i t h a s b e e n a l r e a d y o b s e r v e d t h a t t h e C t h f o r HIC w i t h o u t
 771

100 D low alloy steel

25°C o 13Cr steel

en ε 10hΓ
o CL o
S- Q. ja
O E □

1 i J .._.._! 1 1

600 1000 1400

Tensile strength (MPa)
Fig. 4 Effect of tensile strength on threshold hydrogen
content (Cth)
100
D Low alloy steel
25°C
o 13Cr steel

O Q. 10 L ° " "

-σο
'ο
C^r^^ *"*D

-o

LJ i 1 1_.....

400 600 800

Applied stress (MPa)
Fig. 5 Effect of applied stress on threshold hydrogen
contant (Cth)

e x t e r n a l s t r e s s measured by "in s i t u HIC Measurement Method"

was constant independent of the hardness in s e g r e g a t e d p o r t i o n s
(Kushida et al.). It has been a l s o shown t h a t t h e c r i t i c a l
s t r e s s i n t e n s i t y f a c t o r (K^JJ) of low a l l o y s t e e l s was n o t
affected by the s t r e n g t h , b u t by t h e h y d r o g e n c o n t e n t in t h e
s t e e l (CQ) (Kim et a l . , 1986). And in t h i s s t u d y , i t was
r e v e a l e d t h a t the Cth of 13Cr s t e e l s was a l s o c o n s t a n t
regardless of the strength , and that the 13Cr s t e e l s had the
almost same Cth as low a l l o y s t e e l s u n d e r t h e same a p p l i e d
stress. Therefore i t can be c o n c l u d e d t h a t t h e Cth of a l l
f e r r i t i c s t e e l s is c o n s t a n t r e g a r d l e s s of t h e s t r e n g t h and t h e
chemical compositions and is decreased by the applied stress.
As mentioned before, t h e d i f f u s i o n c o e f f i c i e n t of h y d r o g e n (D)
is decreased with t h e i n c r e a s e in t h e s t r e n g t h , while the
hydrogen permeation r a t e (J) in a c o r r o s i v e e n v i r o n m e n t is
independent of the s t r e n g t h b e c a u s e c o r r o s i o n r e a c t i o n is
affected only by the chemical c o m p o s i t i o n s of s t e e l s and the
environmental f a c t o r s such as pH and H2S c o n t e n t . So the
hydrogen c o n t e n t in t h e s t e e l (CQ), which is given by the
772
following formula, Cn = J / D, b e c o m e s h i g h e r when t h e s t e e l
becomes h a r d e r . T h e r e f o r e i t can be u n d e r s t o o d t h a t t h e r e a s o n
why h i g h e r s t r e n g t h s t e e l s h a v e t h e h i g h e r s u s c e p t i b i l i t y t o
HE i s b e c a u s e t h e CQ, w h i c h i s i n c r e a s e d w i t h t h e s t r e n g t h ,
more easily becomes over the constant Cth.

In t h e p r e s e n t work, i t was c o n f i r m e d t h a t t h e a p p l i e d s t r e s s
d e c r e a s e d t h e t h r e s h o l d h y d r o g e n c o n t e n t (Cth) as already
r e p o r t e d (Fukui e t a l . , 1 9 6 8 ) . When t h e s t r e s s i s a p p l i e d , H E
o c c u r s in the less hard s t e e l (Tanaka e t al.,1980). As t h e
l e s s h a r d s t e e l c o n t a i n s l e s s h y d r o g e n d u e t o t h e i n c r e a s e in
t h e d i f f u s i o n c o e f f i c i e n t of h y d r o g e n (D), t h e d e c r e a s e i n t h e
c r i t i c a l h a r d n e s s means t h a t t h e Cth is d e c r e a s e d by t h e
applied s t r e s s .

CONCLUSIONS

The HE s u s c e p t i b i l i t y of low a l l o y s t e e l s a n d 13Cr s t e e l s w i t h

v a r i o u s s t r e n g t h was i n v e s t i g a t e d from t h e v i e w p o i n t of
t h r e s h o l d h y d r o g e n permeation r a t e f o r HE ( J t h ) , t h e d i f f u s i o n
c o e f f i c i e n t of h y d r o g e n in t h e s t e e l (D) a n d t h e threshold
h y d r o g e n c o n t e n t of t h e s t e e l (Cth). The f o l l o w i n g r e s u l t s w e r e
obtained.

l)The J t h and t h e D w e r e d e c r e a s e d w i t h t h e i n c r e a s e i n t h e
s t r e n g t h and t h e a p p l i e d s t r e s s , a n d t h e s e v a l u e s of 13Cr
s t e e l s were much less than those of low alloy s t e e l s .
2)The Cth was a l m o s t c o n s t a n t r e g a r d l e s s of t h e s t r e n g t h , a n d
13Cr s t e e l s had the same Cth as low a l l o y s t e e l s .
3)The Cth was d e c r e a s e d w i t h t h e i n c r e a s e i n t h e applied
stress.
4)The Cth was c o n s i d e r e d t o b e c o n s t a n t r e g a r d l e s s of t h e
s t r e n g t h and t h e chemical composition.
5)The h i g h s u s c e p t i b i l i t y t o HE of h i g h s t r e n g t h s t e e l s c a n n o t
be e x p l a i n e d by t h e d e c r e a s e in t h e Cth b u t by t h e i n c r e a s e in
t h e hydrogen content (CQ), which is due t o t h e decrease in D.

REFERENCES
Fukui,S. and C.Asada(1968). Iron and Steel 54,1290
Ikeda,A., Y.Morita, F.Terasaki and M.Takeyama(1977).
Proc.2nd.Intern.Congr. Hydrogen in Metals, Paris 4A. 7
Kim,K., H.Mitsumata, H.Tsubakino and K.Yamakawa(1986).
Zairyo 35,1182-1188
Kurahashi.H., T.Kurisu, Y.Sone, K.Wada and Y.Nakai(1985).
Corrosion-NACE, 41,211-219
Kushida,T.(1990). In:The 83th Symposium of corrosion
engineering(JSCE.,Ed.), pp57-72
Kushida,T. and T.Kudo : To be published
0kada,H.(1973). R e p r i n t of I n t e r n a t i o n a l C o n f e r e n c e of SCC & HE
of Iron Base Alloys,A-4, Uniex-Firming, France
Tanaka,T., Y.Ito, M.Nakanishi, T.Kaneko and Y.Komizo(1980).
The Sumitomo Search, 23,27
Yamkawa,K.(1979). LP Gas Plant,16,12-20
Yoshizawa,S., T.Tsuruta and K.Yamakawa(1975).
Corrosion Engineering,24,511-515
 WS8f1
WEAR BEHAVIORS OF CARBON STEELS IN CORROSIVE ENVIRONMENTS

( Part 1, Mild and Severe Wear, and Transition )

Y. IWAI*, T. OKADA* and H. GOTO**

* Department of Mechanical Engineering,

Fukui University, Fukui, Japan

** Department of Mechanical Engineering

Fukuoka Institute of Technology, Fukuoka, Japan

ABSTRACT

S l i d i n g wear t e s t s of c a r b o n s t e e l s w e r e c o n d u c t e d i n c o r r o s i v e
environments. The t r a n s i t i o n from s e v e r e t o mild wear t a k e s p l a c e i n
ion-exchanged water and s a l i n e solution as well as in dry conditions. The
severe wear r a t e i s s l i g h t l y affected by environment. The mild wear r a t e s
in l i q u i d s a r e a l m o s t c o n s t a n t i n t h e range of low l o a d and i n c r e a s e
p r o p o r t i o n a l l y to load in t h e range of high l o a d . The former i s due t o
corrosion fatigue fracture, and t h e l a t t e r i s due t o t h e f r a c t u r e a t
adhered a s p e r i t i e s . Corrosion i n t e n s i t y of l i q u i d produces two o p p o s i t e
e f f e c t s : one i s t o promote mild wear l o s s and t h e o t h e r i s t o i n h i b i t t h e
occurrence of severe wear.

KEYWORDS

Corrosive Wear, Severe Wear, Mild Wear, Transition, Critical Load, Saline
Solution, Corrosion Intensity

INTRODUCTION

When metals are rubbed mutually in corrosive environments, wear occurs due
to the interaction of electrochemical corrosion and mechanical stress. The
study of corrosive wear has progressed little, and unfortunately, systematic
results on chemical factors as well as mechanical factors have not been
obtained (Endo et a l v 1971, 197Λ; Agarwala et al.t 1982; Rengstorff et_al.,
1982; Yahagi and Mizutani,1 986). Corrosive wear is strongly governed by
the breakdown and repair rates of surface films as in the case of corrosion
fatigue. In corrosion environments, the rubbed surface becomes so active
that a large amount of corrosion product may be formed and subsequently
removed by mechanical action. By contrast, the interfacial adhesion may be
decreased by the lubricating action of corrosion product. The effects of
corrosion are complex.

Generally, unlubricated wear occurs by transfer and removal of adhered

asperities in contact surfaces. Wear amount per unit sliding distance is
proportional to contact load, inverse-proportional to material hardness, and

773
774
independent of sliding velocity. In practice, however, these are not
likely to occur. In the ranges of low and high loads, wear rate is
approximately proportional to load, but it increases discontinously in the
intermediate load levels (ΊΥ and T 2 transition) (Welsh, 196$). The former
is called mild wear and the latter, severe wear. The difference in both
the wear rates is in several orders. In designs of machine components from
the viewpoint of anti-wear, it is very important to avoid severe wear and
produce mild wear.

In the present paper, sliding wear tests of carbon steels were carried out
in various kinds of environments. Severe wear, mild wear, and transition
behavior were studied. Such theme is significant to study the superimposed
effects of corrosion and mechanical stress as well as to obtain data for
practical use.

EXPERIMENTAL PROCEDURES AND MATERIALS

The two types of test rigs used are shown schematically in Fig.1. One was
a pin-on-disk type in which the pitch diameter of wear track was A3 mm; the
other was a cylinder-on-plate type in which a fixed plate test piece was
rubbed by an annular surface of a cylindrical test piece. The ratio of the
mating areas of large specimen to small was A3 and 2.6, respectively. The
sliding velocity for both tests was constant at 0.15 m/s.

A cylindrical water bath of acrylic resin was attached to a circular table

for mounting the disk or plate test piece. In the pin-on-disk tests, the
bath was filled with test liquid of about one liter and its surface was kept
at about 25 mm higher than the rubbing surfaces. The test liquid was

Plate test
Displacement piece
probe
2^. Z-Pin
V

■Φ-
E
Bath / l —
Test
tJJw D Liquid -=^
supply Drain
liquid
Weight

(a) Pin-on-disk type (b) C y l i n d e r - o n - p l a t e type

Fig. 1. S c h e m a t i c view of t h e t e s t apparatus

Table 1. Chemical compositions (wt.%), hardness of t h e

t e s t m a t e r i a l s , and d i m e n s i o n s of t e s t pieces

Chemical Composition (wtjK) Hardness Test Piece

c Si Mn _P_ s HV(0.5) Shape Size (mm)
S15C 0.16 0.27 0.49 0.023 0.025 140 Pin d=4, 1=52
0.14 0.26 0.37 0.012 0.005 152 Disk d=60, t=7
Cylinder inner d=16.0
S35C 0.37 0.24 0.77 0.019 0.023 182 outer d=19.6, 1=25
Plate 1=40, w=10, t=10
didiameter, K l e n g t h , wlwidth, tZthickness
 775
s t i r r e d during the t e s t since the bath r o t a t e d with the disk t e s t piece.
The l i q u i d t e m p e r a t u r e was m a i n t a i n e d a t 20°C by c i r c u l a t i n g c o o l i n g w a t e r
i n t o an a n n u l a r s t a i n l e s s s t e e l p i p e which was immersed i n t h e w a t e r b a t h .
I n t h e c y l i n d e r - o n - p l a t e t e s t s , l i q u i d was s u p p l i e d t o t h e t e s t s u r f a c e
t h r o u g h a p e n e t r a t i o n h o l e a t t h e c e n t e r of t h e p l a t e t e s t p i e c e from an
external reservoir. F l o w i n g r a t e was 50 ml p e r m i n u t e and t h e l i q u i d
s u r f a c e was a b o u t 3 mm h i g h e r t h a n t h e r u b b i n g s u r f a c e s . The l i q u i d
t e m p e r a t u r e was k e p t a t 25°C· The s u r f a c e s of t h e n o n - f r i c t i o n a l a r e a s of
t h e p i n and d i s k and t h e s i d e s u r f a c e s of t h e p l a t e were a l m o s t c o m p l e t e l y
c o a t e d w i t h c o a t i n g cement.

T e s t m a t e r i a l s were a n o r m a l i z e d m i l d s t e e l S15C and a medium carbon s t e e l

S35C i n t h e p i n - o n - d i s k and t h e c y l i n d e r - o n - p l a t e t e s t s , r e s p e c t i v e l y .
The c h e m i c a l c o m p o s i t i o n s and V i c k e r s h a r d n e s s numbers a r e l i s t e d i n Table
1. The m a t e r i a l s were machined t o t h e d i m e n s i o n s as d e s c r i b e d i n Table 1
and t h e n t h e s u r f a c e s were f i n i s h e d t o around 1 μπι Rmax w i t h emery p a p e r s .
The c y l i n d r i c a l and p l a t e t e s t p i e c e s were t h e n vacuum a n n e a l e d a t 600°C f o r
1 hour, but p i n and d i s k t e s t p i e c e s were used w i t h o u t h e a t t r e a t m e n t s .

The wear amounts were c o n t i n u o u s l y r e c o r d e d by d e t e c t i n g a d i s p l a c e m e n t of

t h e p i n specimen w i t h a s e n s o r i n t h e p i n - o n - d i s k t e s t s . The mass l o s s e s
were measured w i t h a p r e c i s i o n b a l a n c e i n t h e c y l i n d e r - o n - p l a t e t e s t s .
These measurement v a l u e s were c o n v e r t e d t o volume l o s s e s . The c o m p o s i t i o n
of wear p a r t i c l e s were a n a l y z e d by an X-ray d i f f r a c t i o n . The measurement
c o n d i t i o n i s a s f o l l o w s : t a r g e t i s Cu; t h e r a n g e of d i f f r a c t i o n a n g l e
(2Θ),10-100 d e g r e e ; c o u n t i n g t i m e , one second; s l i t c o n d i t i o n , i°_0.2mm-1°.

EXPERIMENTAL RESULTS AND DISCUSSION

Wear B e h a v i o r s i n Air

The w e a r c u r v e s of S1 5C p i n s i n w e t a i r and S35C p l a t e s i n room a i r are

shown i n F i g s . 2 a n d 3> r e s p e c t i v e l y . I n b o t h t y p e s of t e s t s , m i l d w e a r
o c c u r r e d w i t h s m a l l wear p a r t i c l e s from t h e b e g i n n i n g of t h e t e s t i n a r a n g e
of low l o a d s . As t h e l o a d was i n c r e a s e d , s e v e r e wear w i t h l a r g e m e t a l l i c
wear p a r t i c l e s g e n e r a t e d and was f o l l o w e d by s t e a d y s t a t e m i l d wear w i t h a
c h a n g e of f r i c t i o n a l s o u n d . F i n a l l y , s e v e r e w e a r c o n t i n u e d i n d e f i n i t e l y

in room air(RH=70%,20°C)
Cylinder-on-plate test

in wet air(RH=70%,24°C) 14.7 N

Pin-on-disk test
B A

4.9 N
—o—
0 0.5 1 1.5 2 1 2 3
Sliding distance L, km Sliding distance L, km

Fig.2. Wear curves of S15C pin Fig,3. Wear curves of S35C plate
in wet air in room air
776
and thus wear amount became large. In 10
the cylinder-on-plate test, the initial o S15C Pin in wet air
D S35C Plate in room air
knee points of the wear curves were
determined from a change of frictional
sound and wear losses were weighted at 10"
these points.

The relationships between wear rate and *10

load are shown on a log-log plot in Fig.4..
The severe wear rate (a group of points in
the upper part of the figure) is the
'10
initial wear loss divided by the initial
sliding distance. The mild wear rate (a
group of points in the lower part of the
figure) was determined from a slope of the |10'
wear curve in the steady state. The transition
range surrounded by two broken lines a and
A (S15C pin) or b and B (S35C plate) shows
the load range where initial severe wear 10
transfers to mild wear after a certain
sliding distance. Load a, b is called
the lower critical load Pc (M) , below which 10'
only mild wear appears, and load A, B is 10 100 1000
called the upper critical load Pc (s) , Load P, N
above which only severe wear appears. Fig.4. Relationship between wear
These critical loads will be studied rate and load in air
hereafter.

We have observed worn surfaces just when the severe wear transfers to mild
wear. The flat layers which are work-hardened up to more than HV=300 and a
little higher than the adhesively worn surface, were formed and oxidized.
The analysis of wear particles by X-ray diffraction indicated that there
were no oxides in the severe wear and Fe203 and FeO(OH) were generated in
the mild wear. This means that reaction under coexistence of oxygen and
water moisture has progressed in the mild wear.

Rabinowicz (1967) reported that an oxide layer of 0.01 μπι is needed to

provide effective lubrication without metallic contacts. Quinn (1983)
stated that oxide grows to a thickness of about 1 μπι on the rubbing surface
and above this thickness, oxide layer delaminates. Although the precise
measurement of the thickness of oxide layer has remained unclear, the most
significant factor in the transition to mild wear is an oxidation on the
contact surface. Wet corrosion due to adsorption of moisture is dominant
in ranges of low contact load and low sliding velocity (Miyakawa et al.t
1973)· In addition, the formation of a hardened layer is necessary to
prevent the breakdown and removal of an oxide film. Welsh (1965) mentioned
that the required hardness of a substrate for the transition is about
HV=350. The geometry of contact surface and the ratio of mating areas
affect the formation and maintenance of oxide films and hardened layers.
The transition to mild wear occurs at a shorter sliding distance and a
larger load for the wear test methods with large ratio of mating areas such
as a cylinder-on-plate test used here (Endo and Iwai, 1981). The addition
of Cr to steel is harmful in a given content because the range of initial
severe wear is enlarged by oxidation inhibition (Komai et al.t 1983; Farrel
and Eyre, 1970). By contrast, the Cr addition is beneficial because it pro-
motes surface hardening. When contact load or sliding velocity is greatly
increased, T 2 transition appears (it was not found in our experiment). This
is due to high temperature oxidation on the rubbing surfaces (Welsh, 1965)·
 777
Wear in Corrosive Liquid
As examples, wear curves of the S1 5C pin i n a i r - s a t u r a t e d ion-exchanged
water and those of the S35C p l a t e i n 0.5 wt% s a l i n e s o l u t i o n a r e shown in
Figs. 5 and 6, respectively. In l i q u i d , the t r a n s i t i o n phenomena were seen
as w e l l as in the dry c o n d i t i o n s , however, the s e i z u r e occurred w i t h o u t
continuation of severe wear at high load. The r e l a t i o n s h i p s between wear
r a t e and load a r e shown i n Fig.7: (a) i s the r e s u l t of S1 5C pin ; and (b) i s
S35C p l a t e . The region of mild wear i s enlarged to a higher load range
in l i q u i d s compared with that in a i r . In 3 wt% saline solutions, mild wear
continued even at the l a r g e s t load in the wear t e s t r i g used here.

lp=1040 N 880 N
in ion-ex. water P=392 N ,
20°C T. in 0.5% s a l i n e solu. / β

Pin-on-disk test Γ 25°C

Q
Cylinder-on / 706 N
plate t e s t s^
./*
s^ ^l/
524 N
^^^
*r s^ 3^^ 118 N

19.6 N

l ^ — i i 1
0.5 1 1.5 0 1 2 3
Sliding distance L, km Sliding distance L, km
Fig.5· Wear curves of S15C pin in air- F i g . 6 . Wear curves of S35C p l a t e in
saturated ion-exchanged water 0.5 wt.% saline solution

10'

.1(T

10

210'

10 o Wet a i r (ai,Ai) o Room a i r (tu.Bi)

Φ Ion-ex. water (a 2 ,A 2 ) <D Ion-ex. water ( b 2 , B2 )
o 0.5% s a l i n e (a 3 ) 3 0.5% s a l i n e ( b 3 f B 3 )
• 3 % saline • 3 % saline ■
10' _J I L_
1 10 100 1000 100 1000 5000
Load P, N Load P, N
a) S15C pin (b) S35C plate
Fig. 7 Relationship between wear rate and load in liquids
778
The lower and upper critical zuuu Seizure load S^
loads are shown in Fig. 8 as a
1000 - Severe _
function of the concentration wear ■
of saline solution. The 500
results in air and ion-ex- i. Seizure
load
changed water are also shown.
The critical loads in saline D^K^cP
M i l d wear
solution agree to those in
100
ion-exchanged water in the
vicinity of 0.01 to 0.05 wt% 50 ~ Pin-on Cyl.-on
concentration and increase disk plate
almost linearly on log-log O D P c(M)
plot with the concentration. ■ • ■ P c(s)
Especially, rubbing surfaces
10 ~o \\\^ / / / / / / S-M Trans.
reach seizure from mild wear / / / / / / region
without passing through the 5 - Qe-0
transition region at higher L< μ — ί ί — « — __l 1 1 I
3
concentration. The transition air Ion-ex. 0.05 0.1 0.5 1 5
region is norrower in pin-on- water Concentration of saline solu.,wt%
disk than cylinder-on-plate test.
Fig.8. Variations of critical loads as
In the saline solution used in a function of the concentration
this experiment, the dissolved of saline solution
oxygen concentration was
almost constant. The elect-
ric conductivity increased to about 1000 times in 0.01 wt.% saline solution
in comparison with that in ion-exchanged water and increased almost
linearly with concentration on a log-log plot (Okada and Hattori, 1985).
Therefore, it is considered that the critical loads of wear transition
become large corresponding to corrosion intensity of liquid.

Similar hardened flat surfaces were observed on the surface where the
transition to mild wear had occurred in liquid. Compositions of wear
particles were Fe2U3 , Fe3Ü4 and Fe0(0H). It is considered that the
mechanisms of transition in liquids are same as those in atmosphere. A
liquid film supports a part of contact load, and additionally, surface
adhesion is prevented by the lubricating action of both oxide layer and
corrosion products, so that the lower critical load shifts to a higher level
with an increase of corrosion intensity. Once severe wear occurs at the
high load, it may easily transfer to mild wear by subsequent rubbing be-
cause of high repair rates of an oxide film and of corrosion product layer.

Effect of Liquid Corrosion Intensity on Wear Rate

As seen in Fig.7, severe wear rates in liquid increase approximately in

proportion to load and lie on the prolongation of the line for those figures
obtained in air. The composition of severe wear particles was only Fe in
every liquid. It is considered that the severe wear process is slightly
affected by environment because the adhesion and fracture at the interface
proceed rapidly.
By contrast, the mild wear rate is almost constant at low load level but
increases in proportion to load above a given load. The relationship
between wear rate and load is described by the line with knee point. Mild
wear surfaces of S15C pin in 0.5 wt% saline solution are shown in Fig. 9·
At low load, although the worn surface is fairly similar to that of
lubricated wear in oil (Iwai and Endo, 1982), the removals caused by the
propagation of cracks which is considered to be by corrosion fatigue are
observed. The worn surface at high load shows an adhered surface. The
 779

(a) P = 49 N (b) P = 392 N

Fig.9. S1$C pin surface of mild wear in 0.5 wt.% saline solution

average roughness, Ra and hard- HV Ra

ness (10 points measurement) of <>
j Φ Ion-ex. water
the S1$C pin surface of mild wear ;300 J » 0.5% s a l i n e
are presented in Fig. 10. They
rapidly increase in the vicinity
of the load which corresponds to
a knee point in the curves as
shown in Fig.7(a). This indi- £200 5 o
cates that the rubbing surface is
subject to large mechanical frac-
ture in the range of high load.
The c o m p o s i t i o n of w e a r
particles were Fe203 and Fe0(0H)
in the range of low load. Fe 100
50 100 500 1000
and Fe30i+ were additionally de- Load P, N
tected in the range of high load.
Fig.10. Average roughness and hardness
Endo et al.(l971. 1974) reported of S1$C pin surface of mild wear
that the wear rate of steel at a
low load was almost one order of magnitude larger than the dissolution rate
due to corrosion calculated from corrosion current. It can be seen that
wear is not merely due to dissolution of the surface or removal of corrosion
products. We can deduce the following. The corrosion products act as
some sort of lubricant, but these lubricating films gradually fracture with
an increase in load. Thus principal wear mechanism transfers from
corrosion fatigue fracture under the repetition of stresses to fracture at
adhered asperities of metallic contacts.

The variations in the constant value of wear rate in a low load range and
the mean value of the specific wear rate, which is wear rate divided by
load in a high load range, are plotted against the concentration of saline
solution in Figs. 11 and 12, respectively. The constant values become
larger as the concentration is increased above 0.0$ wt%. By contrast, the
specific wear rates in the high load range increase a little with
concentration. This is because the decrease in corrosion fatigue strength
of materials with increase of corrosion intensity (Okada and Hattori, 198$)
markedly affects on the wear at low loads.

CONCLUSIONS

(1) The transition from severe to mild wear in atmosphere takes place due to
780

L—I J5 1 1 1 1 1 Φ 0 I 1 „ , 1 1 1 1
Ion-ex. 0.05 0.1 0.5 1 5 en -H I b n_ e x> 0.05 0.1 0.5 1 5
water C o n c e n t r a t i o n of s a l i n e s o l u . , wt.% water C o n c e n t r a t i o n of s a l i n e s o l u . , wt.%
F i g . 1 1 . V a r i a t i o n s of constant mild F i g . 1 2 . V a r i a t i o n s of s p e c i f i c wear
wear r a t e a t a low load range r a t e a t a high load range

the formation of an oxide film and work-hardened surface l a y e r .

(2) The t r a n s i t i o n phenomena a r e seen i n l i q u i d e n v i r o n m e n t as w e l l as i n
dry conditions. The region of mild wear extends t o a high load range
with an i n c r e a s e of corrosion i n t e n s i t y .
(3) The m i l d wear r a t e s i n l i q u i d s a r e a l m o s t c o n s t a n t i n t h e r a n g e of t h e
low l o a d s and i n c r e a s e p r o p o r t i o n a l l y t o l o a d i n t h e r a n g e of h i g h l o a d .
The f o r m e r , which i s due t o c o r r o s i o n f a t i g u e f a i l u r e , i n c r e a s e s w i t h an
i n c r e a s e o f t h e c o n c e n t r a t i o n o f s a l i n e s o l u t i o n a b o v e 0 . 0 5 wt%. The
l a t t e r , w h i c h i s d u e t o f r a c t u r e a t a d h e r e d a s p e r i t i e s on t h e m e t a l
c o n t a c t s , becomes a l i t t l e l a r g e r w i t h c o r r o s i o n i n t e n s i t y .
The s c a t t e r s i n t h e e x p e r i m e n t a l w e a r r e s u l t s seem t o be b e c a u s e of t h e
d i f f e r e n c e s i n t h e wear modes and t r a n s i t i o n c o n d i t i o n s . I t i s considered
t h a t more s t u d i e s on c o r r o s i v e wear a r e r e q u i r e d from t h e s e v i e w p o i n t s .

REFERENCES

Agarwala,V.S., K.Y.Kim and S.Bhattacharyya (1982). An e l e c t r o c h e m i c a l method f o r

i n v e s t i g a t i n g c o r r o s i o n i n r u b b i n g s u r f a c e s . ASTM STP. 780« 106-124.·
Endo,K., K.Komai and D.Fujita (1971). Wear of m e t a l s i n c o r r o s i v e e n v i r o n m e n t s .
B u l l , of JSME t 1 4 , 7Λ, 7 1 5 - 7 2 3 .
Endo,K., K.Komai and H.Shiomi (1974·)· E f f e c t s of d i s s o l v e d oxygen i n s a l i n e on
c o r r o s i v e wear of s t e e l . Wear, 3 0 , 285-297.
Endo.K and I . I w a i (1981). E f f e c t of t e s t method on wear of s t e e l . J . JSLE I n t .
E d i t i o n , No.2t A p r i l 1981, 11-16.
F a r r e l l , R.M. and T.S.Eyre (1970). The R e l a t i o n s h i p between load and s l i d i n g
d i s t a n c e i n t h e i n i t i a t i o n of mild wear i n s t e e l s . Wear, 1_5» 359-372
I w a i , I . and K.Endo (1982). T r a n s i t i o n of t h e l u b r i c a t e d wear of carbon s t e e l .
Wear, 25» 159-172.
Komai,K., E.Yagi and K.Endo(l983)· I n f l u e n c e of C r - c o n t e n t on t r a n s i t i o n of d r y wear
of s t e e l s . J . Soc. Mat. S e i . J p n , ^ 2 , 3 6 1 , 1 1 8 7 - 1 1 9 3 ( i n J a p a n e s e ) .
Miyakawa,Y., K.Seki-and M.Nishimura (1973). E f f e c t of m o i s t u r e and p i n h o l d e r
r i g i d i d i t y on w e a r . J . J p n . S o c . L u b r i . E n g . , 1_8, 4-» 323-334- ( i n J a p a n e s e ) .
0kada,T. and S.Hattori( 19851^ R e l a t i o n between c o n c e n t r a t i o n of s a l t w a t e r and
c o r r o s i o n f a t i g u e s t r e n g t h on 0.37% carbon s t r u c t u a l s t e e l . Trans. ASME.
J . o f Eng. M a t e r i . , 1 0 7 , 2 3 5 - 2 3 9 -
Quinn, T.F.J. (1983)· Review of o x i d a t i o n a l wear. Tribology I n t . 16, 5, 257-271.
Rabinowicz, E.O967). L u b r i c a t i o n of m e t a l s u r f a c e s by oxide f i l m s . ASLE Trans..
10, Λ00-Λ07.
Reng'storff, G.W.P, K.Miyoshi and D.H.Buckley (1982). F r i c t i o n and wear of i r o n i n
c o r r o s i v e media. NASA T e c h n i c a l Paper 1985.
W e l s h , N.C.O965). The d r y wear of s t e e l . P h i l . T r a n s . Roy. S o c , London, 2 5 7 , A-
1077, 31-79-
Yahagi,Y. and Y.Mizutani (1986). C o r r o s i v e wear of carbon and a u s t e n i t i c
s t a i n l e s s s t e e l s i n NaCl s o l u t i o n . Wear, 110, 4.01-408.
 WS8f2

CRACK INITIATION AND PROPAGATION IN FRETTING

R.B. Waterhouse

Department of Materials Engineering and Materials Design,

University of Nottingham, University Park,
Nottingham, NG7 2RD, UK

ABSTRACT

Fretting between two surfaces results in high alternating shear stresses in the surfaces,
their magnitude depending on the coefficient of friction and the oscillatory tangential
force producing the fretting. Local plastic deformation can occur and even local
welding in some instances. If one of the surfaces is experiencing a cyclic stress, i.e.
fatigue, or a static tensile stress, cracks may be initiated early in the process and
propagate under the influence of the additional stresses due to the fretting. One of the
features of the situation is the large number of cracks which are initiated and which
may be close enough together to influence their propagation. The environment has a
major role to play in these processes. Suggestions are made for the limitation of crack
initiation and propagation under fretting conditions.

KEY WORDS

Fretting; fretting fatigue; crack initiation; crack propagation; residual stress;

environment.

INTRODUCTION

In normal fatigue, cracks invariably develop and propagate from surface defects such
as scratches, inclusions, porosity, or corrosion pits. The process is therefore somewhat
haphazard depending on the number and distribution of these defects in relation to the
stress distribution in the specimen or component. In the case of fretting between two
surfaces the source of cracks is confined to the contact region, and, in experimental
studies of fretting fatigue, the repeatable location of initiation sites leads to
considerably less scatter than is usually experienced, except where notched specimens
are used.

781
782
In this paper some of the factors influencing the location and subsequent growth of
cracks initiated by fretting are considered. In practice three different situations can
be distinguished in which cracks may be initiated and these are considered in turn.

Cracks Initiated by Contact Stresses Alone

Under normal loads of no great magnitude, particularly if the surfaces are conforming
and flat, surface damage is apparent in the early stages and local welds may develop
at areas of real contact (Bethune and Waterhouse, 1965). This leads to initial
roughening of the surface, but as fretting proceeds, the surface becomes smoother and
wear particles are produced by a delamination process (Waterhouse and Taylor, 1974).
Although this proceeds by the propagation of sub-surface cracks parallel to the surface
as described by Suh (1973) such cracks remain in the surface region and do not
propagate into the body of the material because the alternating stresses in the contact
region fall off rapidly.

Under high normal loads, e.g. in a ball on flat configuration where the load is sufficient
to cause a Brinell impression, the slip annulus is very narrow and the local alternating
stresses are sufficiently great to cause limited propagation of the cracks outside the
contact region, Fig. 1 (Goto and Waterhouse, 1980). Similar cracking has been observed
by Kisu et al (1987) and also by Sato et al (1980) in brittle materials such as glass.

Cracks Initiated by Contact Stresses and Applied Tensile Stress

In experiments with a bearing ball on a bearing steel flat and with a moderate normal
load it was found possible to initiate and propagate fatigue cracks in the flat specimen
when it was subjected to a tensile stress. Cracks could be initiated both in the partial
and total slip condition, Fig. 2 (Kuno and Waterhouse, 1989). Subsequent analysis
applying the Ruiz criterion (Ruiz et al, 1984) showed that the cracks developed in the
slip region at positions of maximum alternating shear stress enhanced by the bulk stress
(Kuno et al, 1989).

Fig. 1. Fatigue crack spreading from slip Fig. 2. Symmetrical cracks in slip region
annulus - ball on flat. - ball on flat.
 783
In this particular experiment there was a residual compressive stress in the surface of
800 MPa. The applied tensile stress of 600 MPa did not neutralise this but brought the
change over from compressive stress to valancing tensile stress to within ΙΟμπι of the
surface, well within the field of the alternating stress arising from the fretting.

Cracks Initiated by Contact Stresses and Alternating Bulk Stresses

This is the situation which is normally termed fretting-fatigue. In rotating-bending

fatigue testing with mild steel specimens, to which bridge pieces of the same material
were attached to a parallel slide gauge length by a proving ring, cracks were found to
initiated at the boundary between a central non-slip area and the surrounding wear
damaged slip area (Waterhouse and Taylor, 1971). In more recent work in which the
fatigue specimen was a 5mm dia. 0.64C steel wire, to which was clamped a pair of
bridges made UD from short lengths of the same wire (i.e. a crossed cylinder
configuration), the contact area was circular and a pair of cracks were initiated in a
mirror image situation, Fig. 3 (Takeuchi and Waterhouse, 1987). By sectioning and
polishing specimens fatigues for different numbers of cycles without fracture, it was
possible to determine the crack profiles and hence the curves of crack length against
number of cycles. By taking tangents to these curves, da/dN growth curves could be
produced. Examples are shown in Fig. 4 for different values of the range of alternating
stress at a stress ratio R of 0.3, a clamping load of 100 N, and frequency of 5 Hz in
laboratory air (Takeuchi and Waterhouse, 1990). After an initial accelerated rate of
crack growth due to the additional shear stresses in the surface due to frictional forces,
and which are higher the greater the applied alternating stress, the growth rate passes
through a minimum and then propagates as a long crack out of the influence of the
fretting contact forces. These results very much confirm the observations of K. Sato
(1986)

Fig. 3. Fracture of steel wire in Fig. 4. Crack growth curves in air for

seawater - crossed cylinder. various alternating stress.

784

DISCUSSION

The preceding sections have shown that for fatigue cracks to propagate into the body
of the material away from the fretting zone there must be one of the three following
requirements:

(1) the normal load must be extremely high and hence a

correspondingly high tangential force to give the necessary
amplitude of movement, although in such circumstances the slip
annulus will be very narrow.

(2) there must be an applied tensile stress such that the material
influenced by the fretting action also experiences the tensile stress
(particularly where there is a residual compressive stress in the
surface).

(3) there must be an alternating stress in the surface with part or all
of the stress cycle in the tensile region.

In case (1) the cracks will rapidly cease to propagate when they reach a point at which
the alternating stress due to the fretting contact has diminished below a certain critical
value. In cases (2) and (3) the cracks are more likely to propagate to failure.

Since the alternating shear stresses arising from the fretting are a function of the
coefficient of friction, any change in the environment which causes a reduction in
friction will have a dramatic effect on the initiation of cracks, e.g. raising the
temperature so that an oxide film is formed on the surfaces has been shown to inhibit
crack initiation (Ruiz and Chen, 1986; Kuno and Waterhouse, 1989), also attempts to
initiate cracks in the presence of a lubricant have proved abortive (Miyagawa et al,
1989). On the other hand, a corrosive environment can not only increase the number
of cracks but also enhance their initial growth rate (Takeuchi and Waterhouse, 1990).
Where a number of cracks are generated close to each other, e.g. in seawater, their
growth rate can eventually become slower due to the interference of the stress fields
at the crack tip.

Another factor which can have an influence on the crack growth rate is the contact load
or clamping pressure. Where this is high the crack which grows obliquely below the
contact can be slowed or even stopped by the crack faces being forced together.
Removal of the fretting contact and allowing the crack to propagate under the
alternating stress causes it to speed up, Fig. 5, giving a reduced life to failure. Nowell
and Hills have analysed the situation of crack growth under a cylinder on flat fretting
contact and have indicated the increased contribution of Mode II crack growth and the
region where growth ceases (Nowell et al, 1987).

The clamping pressure can also influence the initiation site of the crack which
propagates to failure. In investigating the fretting-fatigue behaviour of a titanium alloy
with bridges of the same material making a flat on flat contact with the specimen, in
uniaxial loading, it was found that the minimum life was obtained at a pressure of 20
MPa and the crack initiated in the centre of the fretted area, whereas at clamping
 785
I I I II | 1—

^a=260MPa
L =180N
t ttttt 17.5 Hz

Fig. 5. Two stage tests - fretting

in air/plain fatigue.

NUMBER OF FRETTING CYCLES IN AIR

pressures greater than 35 MPa the life was longer and the crack initiated at the edge
of the contact area (Maruyama et al, 1990). At higher pressures of 200 MPa, Switek
(1985) found that failure occurred away from the fretting damage.

From the above considerations, it is apparent that the factor which is most effective
in initiating a crack in a fretting contact, is the coefficient of friction. This usually
rises to a high value in the first thousand or so cycles and it is at this stage that a crack
is formed. Its subsequent propagation to failure depends on the existence of a tensile
or alternating stress in the body. The recommended method for avoiding such failures
is to reduce the coefficient of friction by applying some suitable surface coating, e.g.
a bronze-filled polymer (Varley and Waterhouse, 1990). The other method is to prevent
the propagation of cracks by inducing a compressive stress in the surface by shot-
peening (Mutoh et al, 1987) or a diffusion treatment such as nitriding (Gregory, 1968).

CONCLUSION

Although fatigue cracks may be initiated in the wear process associated with fretting,
for cracks to initiated and propagate from the contact region a static tensile stress or
an alternating stress must also be present, except in certain exceptional circumstances
where the normal stress is abnormally high.

REFERENCES

Bethune, B. and Waterhouse, R.B. (1965). Adhesion between fretting steel surfaces.
Wear. 8, 22-29.
Goto, S. and Waterhouse, R.B. (1980). Fretting and fretting fatigue of titanium alloys
under conditions of high normal load. Titanium T80 Science and Technology. Proc. 4th
786
Int. Conf. on Titanium« 3, 1837-1844. Met. Soc. A1ME, New York.
Gregory, J.C. (1968). Improving the resistance of ferrous materials to scuffing, wear,
fretting and fatigue. Metal Forming, 35, 229-238.
Kuno, M. and Waterhouse, R.B. (1989). The effect of residual stress and temperature
on the fretting of bearing steel. Tribological Design of Machine Elements. Elsevier,
Amsterdam, pp. 245-252.
Kuno, M., Waterhouse, R.B., Nowell, D. and Hills, D.A. (1989). Initiation and growth of
fretting fatigue cracks in the partial slip regime. Fatigue Fract. Engng. Mater.
Struct. 12, 387-398.
Maruyama, M., Sumita, M. and Nakazawa, K. (1990). Fretting fatigue strength analysis
of Ti-6A1-4V in air. I. Iron and Steel Inst. Ton.. 76, 262-269.
Miyagawa, H., Takeuchi, M. and Waterhouse, R.B. (1989). Propagation of fatigue cracks
in high strength steel roping wire in oil and the influence of fretting. Proc. 5th Int.
Congr. on Tribology. 12-15 June 1989, 5, 267-271.
Mutoh, Y., Fair, G.H., Noble, B. and Waterhouse, R.B. (1987). The effect of residual
stresses induced by shot peening on fatigue crack propagation in two high strength
aluminium alloys. Fatigue Fract. Engng. Mater. Struct.« 10. 261-
Nowell, D., Hills, D.A. and O'Connor, J.J. (1987). An analysis of fretting fatigue.
Tribology - Friction, Lubrication and Wear Fifty Years On. 2, 965-973. I. Mech. E.,
London.
Ruiz, C , Boddington, P.H.B. and Chen, K.C. (1984). An investigation of fatigue and
fretting in a dove-tail joint. Exp. Mech.. 24, 208-217.
Ruiz, C. and Chen, K.C. (1986). Life assessment of dovetail joints between blades and
discs in aero-engines. Fatigue of Engineering Materials and Structures, i , 187-194.
I. Mech. E., London.
Sato, J., Ibarashi, J., Shima, M. and Waterhouse, R.B (1980). Fretting of glass. Wear.
65, 55-65.
Sato, K. and Fuji, H. (1986). Crack propagation behaviour in fretting fatigue. Wear.
107. 245-262.
Suh, N.P. (1973). The delamination theory of wear. Wear. 25, 111-124.
Switzek, W. (1985). Fretting fatigue strength of mechanical joints. Th. and Appl.
Fract. Mech.. 4, 59-63.
Takeuchi, M. and Waterhouse, R.B. (1987). An investigation into the fretting-corrosion-
fatigue of high strength steel wires. Proc. 10th Int. Congr. on Metallic Corrosion« 7-
11 Nov. 1987, Madras India, 3, 1959-1966. Oxford and IBH Publ. Co. Ltd.
Takeuchi, M. and Waterhouse, R.B. (1990). The initiation and propagation of fatigue
cracks under the influence of fretting in 0.64C roping steel wires in air and seawater.
Environment Assisted Fatigue. (P. Scott and R.A. Cottis, Eds.). M.E.P. Ltd., London,
367-379.
Varley, D.J. and Waterhouse, R.B. (1990). Fretting fatigue of bronze-filled PTFE
against mild steel. Proc. Int. Conf. on Tribology. 30 Oct. - 1 Nov. 1990, Nagoya,
Japan.
Waterhouse, R.B. and Taylor, D.E. (1971). The initiation of fatigue cracks in a 0.7C
steel by fretting. Wear. Π, 139-147.
Waterhouse, R.B. and Taylor, D.E. (1974). Fretting debris and the delamination theory
of wear. Wear. 29, 337-344.
 WS8f3

WEAR BEHAVIORS OF CARBON STEELS IN CORROSIVE ENVIRONMENTS

(Part 2, Effects of Cathodic Protection on Corrosive Wear)

H. GOTO*, Y. IWAI** and T. OKADA**

* Fukuoka Institute of Technology, Fukuoka,

811-02, JAPAN
** Faculty of Engineering, Fukui University,
Fukui, 910, JAPAN

ABSTRACT

Sliding wear tests of carbon steel in saline solution were conducted under
free corrosion at various applied potentials and loads to study the effects
of cathodic protection on the transition behavior between severe and mild
wear. The transition load at a potential level for complete corrosion pro-
tection is lower than that under free corrosion. With decreasing cathodic
potential from free corrosion, the mild wear rate at a high load is reduced
to a minimum at a specific potential, and then severe wear followed by sei-
zure appearing over the ranges of perfect protection and over-protection.

KEYWORDS

Corrosive Wear; Cathodic protection; Severe wear; Mild wear; Transition

INTRODUCTION

Sliding wear tests for steels in corrosive environments were conducted in

the previous paper(Iwai, Okada and Goto, 1991). As the corrosion intensity
of liquids was increased, the load range for the appearance of mild wear
shifted to high load levels although its mild wear rate was higher. The
transition mechanism between severe and mild wear in corrosive environments
was also clarified. Hence, a study on the wear behavior under electrochemi-
cal protection will be very important in order to find a countermeasure for
the reduction of corrosive wear. In the present study, sliding wear tests
of steel in saline solution were conducted up to high load levels under free
corrosion and at a cathodic potential of complete corrosion protection.
Wear tests were also conducted at various applied potentials to investigate
the effects of cathodic potential on the transition between severe and mild
wear. From the test results, the effectiveness of cathodic protection was
studied by comparing with that in such surface damages under dynamic
stresses as corrosion fatigue and fretting wear in corrosive environments.

EXPERIMENTAL DETAILS

The materials tested were 0.15 % C carbon steels and their chemical composi-
tions are shown in Tab. 1. The pin material was normalized and the disk

787
788
Table 1. Chemical Compositions of materials. ( % )
(a) Pin specimen

c Si Mn P S

0.16 0.27 0.49 0.023 0.025

(b) Disk specimen

c Si Mn P S Cu Ni Cr

0.14 0.26 0.37 0.012 0.005 0.15 0.04 0.15

material was used as received. Both the materials were machined to dimen-
sions of 4 mm in diameter, 52 mm in length for the pin and 60 mm in
diameter, 7 mm in thickness for the disk, and the test surfaces were then
finished with emery papers. RHmax of the surfaces was about 1 urn. Vickers
hardness numbers of the pin and disk were 140 and 152, respectively.

The wear test rig used was of pin-on-disk type and the outline has already
been described in the previous paper. The average wear track diameter on
the disk surface was 43 mm. Parts of the pin and disk other than the
rubbing surfaces were covered with coating cement to prevent unnecessary
corrosion of the specimens in liquids. Sliding velocity was constant at
0.15 m/s. The displacement of the upper surface of an arm for mounting the
pin was detected with a sensor and the change in the pin height was measured
continuously to determine the wear volume. The accuracy of the displacement
meter was+ 2 pi, which corresponded to a volume of 10.025 mm .

A cylindrical water bath made of acrylic resin was attached to a circular

table for mounting the disk. The bath was filled with test liquid of about
1 liter and its surface was kept at about 25 mm higher than the rubbing
surface. The test liquid was stirred during the test since the bath rotated
with the disk. The temperature of the liquid was kept at 20°C. An air-
saturated condition was maintained by blowing air into the liquid.

Cathodic protection under potentiostatic control was performed on the rubbi-

ng surfaces by using a potentiostat(response speed 10 ms/V under unloading
for external control) as shown in Fig. 1. Applied potential was varied on
the basis of an Ag/AgCl reference electrode located near the contact surfac-
öC1
of pin and disk in saline solution, and the wear test was then started.
The counter electrode was a platinum wire.
_A/D converter
isplacement n
probe ^[J
Potentiostat Personal
computer

A:Test electrode
B:Ag/AgCI electrode
^Counter electrode
- P t wire

-Weight

Fig. 1 Wear test rig and cathodic protection method.

 789
EXPERIMENTAL RESULTS AND DISCUSSION

Wear under cathodic protection

Wear curves obtained at various contact loads under free corrosion in 0.5
wt% saline solution are presented in Fig. 2. Mild wear continued throughout
a test at loads below 295 N. A sign of severe wear appeared in the early
stage of a test at a load of 590 N. After severe wear appeared at loads
above 640 N, the test rig soon stopped due to seizure.

Figure 3 shows wear curves under cathodic protection in 0.5 wt% saline solu-
tion. The applied potential of -0.95 V(SCE) used is more negative than the
cathodic protection potential of -0.78 V(SCE) under static corrosion. Wear
curves of mild wear, transition from severe to mild wear, and severe wear
followed by seizure are generally found with increasing load. However, the
load range for the appearance of each wear mode is quite different from that
under free corrosion.

The relationship between wear rate and load is presented on a log-log plot
in Fig. 4. The results in wet air and ion-exchanged water are also seen for
reference. As stated in the previous paper, the severe wear rate(a group of
points in the upper part of Fig. 4) is the value of total wear volume
divided by sliding distance in the initial wear period. The mild wear
rate(a group of points in the lower part) is the value determined from a
slope of wear curves in the steady-state period. In the load range between
two broken lines a and A, severe wear appears initially and then transfers
to mild wear after a certain sliding distance at a load. Load a_ is called
the critical load, below which only mild wear appears and load _A the
critical load, above which only severe wear appears.

Under cathodic protection in 0.5 wt% saline solution (Fig. 4) the lower
critical load is 195 N, which is lower than that of 635 N under free corro-
sion and that of 295 N in ion-exchanged water. At loads higher than the
upper critical load of 295 N, seizure often arises just after the appearance
of severe wear. When cathodic protection is performed to the rubbing sur-
faces, the corrosion rate becomes small, resulting in the reduction in
lubricating action of oxide films and corrosion product. Hence, the
critical load at which adhesive wear takes place is decreased. On the other
hand, the mild wear rate is lower than those under free corrosion and in
ion-exchanged water over the range below the lower critical load.

Sliding distance L, km Sliding distance L, km

Fig. 2 Wear curves of steel under Fig.3 Wear curves of steel under
free corrosion in 0.5wt% NaCl. cathodic protection in 0.5wt% NaCl.
790
Effect of cathodic potential

Wear tests at various applied potentials in 0.01, 0.5, and 3 wt% saline so-
lutions were conducted at a constant load 390 N. The wear curves in 0.5 wt%
saline solution are presented in Fig. 5 as an example. Mild wear continues
at potentials over the range -0.55 to -0.80 V(SCE). Initial wear with a
slightly lower rate than severe wear rate occurs over the range -0.80 to -
0.85 V(SCE), a transition to mild wear being subsequently evident. Severe
wear appears over the range -0.95 to -1.05 V(SCE). A marked difference in
the progress of wear is found with applied potential despite constant load.

Figure 6 shows the relationship between wear rate and applied potential in
saline solution of three concentrations. Mark S in the figure indicates the
occurrence of seizure. The transition region where severe wear moves to
mild wear during a test exists in a specific range of applied potential in
each saline solution. Only severe wear followed by sudden occurrence of
seizure appears at more negative potentials than the potential range of wear
transition. The critical applied potential for the wear transition shifts
to more cathodic range with higher concentration of saline solution. The
critical potential ranges are -0.75 to -0.85 V(SCE), -0.85 to -0.95 V(SCE),
and -0.90 to -1.00 V(SCE) in 0.01, 0.5, and 3 wt% saline solution, respec-
tively. The applied potential where two types of wear with a different
mechanism are observed depends on load and the pH value of solution(Abd~El-
Kader and El-Raghy, 1986).

The change of wear mode with applied potential will be discussed by using
the results in 0.5 wt% saline solution (Fig. 6 ) . Since corrosion protection
is insufficient over the range -0.55 to -0.75 V(SCE), a considerable amount
of corrosion product is generated. As a result, mild wear occurs and its
rate is reduced with decreasing applied potential. When it further falls to
the range -0.80 to -0.85 V(SCE), corrosion is so much inhibited that the
lubricating action of corrosion product becomes less effective. Hence adhe-
sive wear by metal-to-metal contact is ready to occur. Consequently, the
10
| _ o in w e t air
Φ in ion-exchanged
water
in 0.5wt% saline
10 o free c o r r o s i o n in0.5wt p/e saline
v=0.15m/s.20 e C.P=390N
D cathodic - 1 . 0 5 V(SCE)
E protection -0.95 V
£ -0.95V -0.85V
Γ (SCE)
εΐόί -0.825 V
E

no

10

1öe I I J L
10 100 1000 0.5 1.0 1.5
Load N Sliding distance L , km
Fig. 4 Relationship between wear Fig.5 Wear curves of steel at various
rate and load. applied potentials in 0.5 wt% NaCl.
 791
initial wear with a fairly higher rate appears just after the start of test.
However, by reconstruction of a surface coated film made of oxides and cor-
rosion products the wear moves to mild wear. When more cathodic potential
of -0.95 to -1.05 V(SCE) is impressed, the wear modes caused by mechanical
fracture of rubbing surfaces, i.e. severe wear and seizure, occur.

Figures 7 and 8 show a change in the hardness and roughness of the wear sur-
face as a function of applied potential. Both the values increase with de-
creasing applied potential. This demonstrates that the adhesion of the rub-
bing surfaces can not be prevented because lubricating action by corrosion
products is less effective with decreasing applied potential. Especially in
the severe wear range, the wear surface hardness increases considerably with
the wear rate, indicating that the extent of mechanical fracture at the
interfaces becomes larger at more cathodic potentials up to over-protection.

Such a change in wear mode with applied potential results in minimum wear
existing at a specific potential. For example a minimum rate of mild wear
is observed near -0.85 V(SCE) in 0.5 wt% saline solution (Fig. 6 ) . Endo et
al(1971) conducted wear tests for a carbon steel in 1 wt% saline solution at
various applied potentials and a light load of 9.8 N. The result is shown
in Fig. 9. As the applied potential becomes more negative than -0.45 V(SCE)
of free corrosion, the wear rate is reduced to a minimum value near -0.58
V(SCE). However, when a potential of -0.83 V(SCE) is impressed, which is
more negative than the cathodic protection potential under static corrosion,
the wear rate increases due to adhesive wear. Thus, an applied potential
level to minimize the wear rate exists even under a mild rubbing condition.
A level of about -0.95 V(SCE) was required to reach a minimum fretting wear
rate of high carbon roping steel in pH 8.2 seawater (Pearson et al, 1988).
A potential of -1.0 V(SCE) for minimum wear was observed in simulated fret-
ting wear of nickel in IM NaClO. solution(Naerheim and Kendig, 1985).

The potential at which the fatigue life in corrosive media recovers to the
fatigue life in air by cathodic protection is more negative than the cathod-
ic protection potential under static corrosion (Endo et al, 1970). The per-

10"
Cin 0.01wt% s a l i n e
• in 0.5 w t % saline
O in 3.0 wte/e saline
S: seizure o in 0.01wt7. saline
10 500
• in 0.5 wt*/· saline
O in 3.0 wt·/. saline

400 ,s ,
S 10 T v =0.15 m/s
J
A J■ i
P-390N
20 'C
' T„
t i
300 r 1 rf
i J £
2
200 i

10 J_ _L _L _L J_ 1 1 1 i i i
-1.2 -1.0 -0.8 -0.6 -0.4 -1.2 -1.0 -0.8 -0.6 -0.4
A p p l i e d p o t e n t i a l E , V(SCE)
Applied potential E, V(SCE)

Fig. 6 Wear rate as a function Fig. 7 Hardness of wear surface as a

of applied potential. function of applied potential.
792
20
S: s e i z u re Oin 0.0 wtV. saline
2.0
E
• in 0.5 w f / . saline O Fixed specimen
0 in 3.0 w f / . saline
a.
• Rotating specimen
:i5
" • 1.5
ΙΛ
s
in 1wt7. saline
o
-C o v =0.15 m/s
v=0.5m/s,P=9.8N
^10
- s
P.390N * 1.0
o
4)
• 20 *C

D 5
o
•° ° f 0.5
•
8 o ·

n__J
-1.2 -1.0
. -0.8
1
-0.6 -0.4
1
-0.9 -0.7 0.5
Applied potential E, V(SCE) Applied potential E, V(SCE)
Fig. 8 Roughness of wear surface Fig. 9 Wear r a t e a s a f u n c t i o n of
as a function of applied potential. applied p o t e n t i a l .

feet cathodic protection potential of the life recovery in corrosion fatigue

becomes more negative with decreasing pH of solution, which corresponds to
the decrease in wear transition potential with increasing concentrations of
saline solution(Fig. 6 ) . This is because repeated or frictional stress
moves the potential boundary between immunity and corrosion regions in nega-
tive directions. In corrosive wear, the occurrence of severe wear is en-
hanced by the perfect corrosion protection of the rubbing surfaces. Conse-
quently, special attention should be paid to the fact that corrosion protec-
tion leads to a reduction in.the wear resistance of materials at high loads.

CONCLUSIONS

Wear tests were conducted under free corrosion and at various potentials in
saline solution to study the effects of cathodic protection on the transi-
tion between severe and mild wear. The results obtained are as follows:
(1) When the cathodic potential exerting a complete corrosion protection
under static corrosion is impressed, the transition load is lower than that
under free corrosion. The load range for the appearance of mild wear shifts
to lower level, but its rate is lower than that under free corrosion.
(2) With decreasing applied potential at a constant load, the mild wear
moves to the transition from initial severe to steady mild wear and the mild
wear rate decreases to a minimum at a specific potential. Severe wear
followed by seizure occurs over the range of perfect protection and over-
protection. The applied potential where severe wear occurs shifts to more
cathodic levels with a higher concentration of saline solution.

REFERENCES
Abd-El-Kader, H. and El-Raghy, M.(1986). Wear-Corrosion Mechanism of
Stainless Steel in Chloride Media. Corrosion Sei., 26, 647-653.
Endo, K., Komai, K. and Fujita, D.(1971). Wear of Metals under Corrosive
Environments. Bull. Jpn. Soc. Mech. Eng., 14, 715.
Endo, K., Komai, K. and Oka, S.(1970). On the Potential-pH Diagram of Car-
bon Steel under Corrosion Fatigue. J. Soc. Mat. Sei. Jpn., 19, 36~42.
Iwai, Y., Okada T., and Goto H.(1991). Wear Behaviors of Carbon Steel in
Corrosive Environments Pt. 2. 6th Int. Conf. on Mech. Behavr. of Mat.
Naerheim, Y. and Kendig, N. W.(1985), The Influence of Electrochemical
Potential on Wear. Wear, 104, 139-150.
Pearson, P. A., Brook, P. A. and Waterhouse, R. B.(1988). Influence of Elec
trochemical Potential on The Wear of Metals, Particularly Nickel. Tribo-
logy Int., 11, 191-197.
 WS8f4

EFFECT OF CATHODIC PROTECTION ON CORROSION FATIGUE

OF NOTCHED HIGH-TENSION STEEL SPECIMENS

S. HATTORI and T. OKADA

Faculty of Engineering, Fukui University

3-9-1 Bunkyo, Fukui 910, Japan

ABSTRACT

The authors previously studied the notch effect on corrosion fatigue

strength of high tension steels under cathodic protection in synthetic
seawater, and found that the cathodic protection is more effective for a
notched specimen than for a smooth specimen. In this study, the effect of
cathodic protection on corrosion fatigue of notched specimens is discussed
in terms of microcrack initiation, its growth and the pioneer crack
propagation.

KEYWORDS

Corrosion fatigue; cathodic protection; high tension s t e e l ; corrosion;

microcracks; coalescence

INTRODUCTION

The e f f e c t of c a t h o d i c p r o t e c t i o n on c o r r o s i o n f a t i g u e of s t e e l s and a l l o y s
can vary w i d e l y , r a n g i n g from s t r o n g l y b e n e f i c i a l t o s t r o n g l y d e t r i m e n t a l
( B r o w n , 19-83). For e x a m p l e , H a r t t and Hooper ( 1 9 8 0 ) e m p h a s i z e d t h a t t h e
f o r m a t i o n of c a l c a r e o u s d e p o s i t p l a y s an i m p o r t a n t r o l e i n d e c r e a s i n g
f a t i g u e crack growth under c a t h o d i c p r o t e c t i o n in s y n t h e t i c s e a w a t e r .
C o n v e r s e l y , Boger and Crooker (1979) r e p o r t e d t h a t c a t h o d i c p r o t e c t i o n has
no b e n e f i c i a l e f f e c t s on c r a c k g r o w t h i n ASTM A516-60 s t e e l o v e r f r e e l y
c o r r o d i n g c o n d i t i o n s . The p r e s e n t a u t h o r s (Okada e t a l . , 1 9 9 0 ) found t h a t
t h e c a t h o d i c p r o t e c t i o n i s more e f f e c t i v e for notched specimens than f o r a
s m o o t h s p e c i m e n . H o w e v e r , t h e f i r s t t w o s t u d i e s c a n n o t be a p p l i e d t o o u r
p r e v i o u s r e s u l t , because a long s i n g l e crack growth behavior i s not
s u f f i c i e n t t o e v a l u a t e t h e c o r r o s i o n f a t i g u e of notched specimens i n c l u d i n g
a smooth specimen.

In t h i s s t u d y , t h e e f f e c t of c a t h o d i c p r o t e c t i o n on m i c r o c r a c k i n i t i a t i o n ,
i t s g r o w t h and t h e p i o n e e r c r a c k p r o p a g a t i o n i s d i s c u s s e d u s i n g a s l i g h t y
n o t c h e d s p e c i m e n ( s t r e s s c o n c e n t r a t i o n f a c t o r , K t = 1 . 0 8 ) and a s h a r p l y
notched specimen ( K t = 3 . 5 0 ) .
793
794
Table 1. Chemical compositions of the material (X) Table 2. Mechanical properties
of the material.
c Si Mn P S Cu Ni
S Hv
0.15 0.44 1.42 0.009 0.001 0.27 0.19 MPa MPa %

392 539 27 181

2-Φ8

-φ"^3Ε~·φ"
col ml
62 ol CN|
r , 1 , J
86 '
1
Φ

i °1
O/ ml
(b) Sharp notch (Kt=3.50)

(a) Slight notch (Kt=1.08)

Fig. 1. Test specimens.

TEST MATERIAL AND EXPERIMENTAL PROCEDURE

A high-tension structural steel (HT50) was used for the test. Chemical
analysis and mechanical properties are listed in Tables 1 and 2. The
material was machined into test specimens as shown in Fig.l. The specimens
are referred to as a slight notch one and as a sharp notch one. The stress
concentration factors, Kt, are 1.08 and 3.50, respectively. The surface was
polished with a 1200 grade emery paper, but the specimens were left unheat-
treated.

Push-pull fatigue tests were carried out with zero mean stress, using an
electric-hydraulic servo fatigue testing machine. Tests were performed at
30 Hz in 3 percent NaCl solution. Test specimens were fully immersed in the
test solution, which was circulated at 0.4 L/min between a test chamber and
a reservoir. The test solution was about 3 L and it was renewed for each
test. The temperature of the solution was kept at 25 degree C, but
dissolved oxygen was not controlled. A constant potential was applied by a
potentiostat with a caromel half-cell. Crack initiation and the growth were
observed by both scanning electron and optical microscopy.

EXPERIMENTAL RESULTS AND DISCUSSION

Cathodic Protection and Fatigue Strength

Previously, the authors (Okada et al.,1990) studied the notch effect on

rotating bending fatigue strength under cathodic protection (with
sacrificial anode of aluminum alloy, -1160mV vs. SCE) in synthetic seawater.
Figure 2 shows the relation between stress concetration factor, Kt, and the
fatigue strength at 10 cycles. In laboratory air, the smooth specimen (
Kt=1.03) reveals high fatigue strength of 290 MPa. The strength of a
notched specimen decreases remarkably with Kt and reaches a value of 95 MPa
 795
at Kt=4.6. Under free corrosion in synthetic seawater, the fatigue strength
is about 80 MPa for a smooth specimen (Kt=1.03) and is about 35 MPa at
Kt=2.4 or more. Cathodic protection restores the fatigue strength of a
smooth specimen to that in laboratory air. At Kt = 2 or more, the strength
remains at a constant value of twice as high as the fatigue strength at
Kt=4.6 in laboratory air or five times that under free corrosion. This
shows that cathodic protection is more effective for a notched specimen than
for a smooth specimen.

In this study, in order to clarify the effect of cathodic protection for

notched specimens, push-pull fatigue tests were carried out in 3% NaCl
solution using a slight notch specimen (Kt=1.08) and a sharp notch specimen
(Kt=3.50) at various potentials. The stress amplitudes were selected as the
specimen is to be fractured at about 10 cycles under free corrosion.
Figure 3 shows the relation between cathodic potential and the number of
cycles to fracture. For a slight notch specimen, the fatigue life increases
with decreased potential and, at -750 mV(SCE) or less, the specimen is not
fractured at 1 0 7 cycles. 0 * i n c i i c a t e s t n e result in synthetic seawater,
which is consistent with that in 3% NaCl solution. For a sharp notch
specimen, cathodic protection is more effective and the specimen is not
broken at -700 mV(SCE) or less. Under free corrosion, potential was -400
mV(SCE) at the beginning of the test and increased to approach about -700
mV(SCE) after 2x10 5 cycles. The saturated value was used for the potential
in Fig.3. The fatigue life of free corrosion is short, because corrosion
pits and microcracks initiate in early high potential stage.

Crack Initiation and Growth on a Slight Notch Specimen

Figure 4 shows the specimen surface after 1 0 5 cycles. A large localized

corrosion spot is observed at -500 mV(SCE). The size of corrosion spots

10 'br £

106 Ecorr{J

3*NaCI, 30Hz
ö Slight notch, a=150MPa
a Sharp notch, a=100MPa
1 2 3 A 5 10 ■H-
Stress concentration factor Kt 1000 800 -750 -700 -650 -600 -550 -500
Cathodic potential mV(SCE)
Fig. 2. Relation between the stress
concentration factor Kt and Fig. 3 Relation between the cathodic
the fatigue strength at 107 potential and the number of
cycles σ*. cycles to fracture.
796
d e c r e a s e s with p o t e n t i a l . Figure 5 shows the m i c r o c r a c k s observed in a
c o r r o s i o n spot a f t e r 3x10^ c y c l e s . At -500 mV(SCE), a long and wide
microcrack i n i t i a t e s . At -550 mV(SCE), a few long m i c r o c r a c k s and many
s h o r t m i c r o c r a c k s a r e observed. At -600 mV(SCE), many s h o r t m i c r o c r a c k s
only i n i t i a t e . Figure 6 shows the d e n s i t y and the average l e n g t h of
m i c r o c r a c k s a t SxlO^cycles, as a f u n c t i o n of c a t h o d i c p o t e n t i a l . The
d e n s i t y i s the number of m i c r o c r a c k s devided by t h e o b s e r v a t i o n area (590
micron x 440 micron). Microcracks increase in number and decrease in length
with decreased p o t e n t i a l . At -650 mV(SCE) or l e s s , only a few microcracks
a r e observed a t 3x10 5 c y c l e s because of t h e e f f e c t i v e n e s s of c a t h o d i c
protection.

Figure 7 shows the growth behavior of a pioneer crack l e a d i n g to a f i n a l

f r a c t u r e . After m i c r o c r a c k s grow up to 200 micron, some of them j o i n
together to form a pioneer crack. The pioneer crack propagates s i m i l a r l y
i r r e s p e c t i v e of the c a t h o d i c p o t e n t i a l . E v e n t u a l l y , c a t h o d i c p o t e n t i a l
plays an important r o l e to delay the microcrack growth to 200 micron.

Crack I n i t i a t i o n and Growth on a Sharp Notch Specimen

The s i z e of c o r r o s i o n s p o t s on a sharp notch specimen d e c r e a s e s with

decreased potential as observed on a s l i g h t notch specimen. Figure 8 shows
the microcracks in the notch root of the specimen, which was fatigued u n t i l l

Fig. 4. Corrosion on a slight notch Fig. 5. Microcracks in a corrosion spot

specimen after 105 cycles. after 3xl05 cycles.
 797

i8
x=3
"ff 'r r β -500mV
« -550mV ~11 1
• Ecorr
C
Ü? 1
>
1
/
φ -650mV
J
9

< i 1
jfr
o -700mV
1
</
σ
·:Fracture

M
«- 1

h .** J
1
Q£L
"
1
2
1
3
Number of cycles N
xio
Fig. 7. Pioneer crack growth,
(siight notch specimen)

-750 -700 -650 -600 -550 -500 -450

Cathodic potential mV(SCE)
Fig. 6. Cathodic potential vs. density and
average length of microcracks.
(slight notch specimen)

(a)-550mV

(b)-600mV
-750 -700 -650 -600 -550 -500 -450
Cathodic potential mV(SCE)

Fig. 9. Cathodic potential vs. density

, 100/im ,
and average length of microcracks.
(sharp notch specimen)
Fig. 8. Microcracks on a sharp notch
specimen after 3xl05 cycles.

3 x \05 cycles. Microcracks are shortened and increase in number at a

decreased potential. Figure 9 shows the density and the average length of
microcracks at 3x10 , as a function of cathodic potential. The density on a
sharp notch specimen is almost the same as observed on a slight notch
specimen. The average length of microcracks is higher on a sharp notch
specimen, because the notch root has a high stress concentration. Cathodic
protection reduces the microcrack length and raises the density.

Figure 10 shows a pioneer crack growth leading to a final fracture. A

pioneer crack initiates in early stage on a sharp notch specimen
irrespective of cathodic potential and the crack growth rate decreases with
decreased potential. At -700 mV(SCE), the crack is arrested to be a
nonpropagating crack after 2 x 106cycles. Thus, a large difference in
pioneer crack growth is observed between a slight notch specimen and a sharp
notch specimen.
798

Number of cycles N
Fig.10. Pioneer crack growth
(sharp notch specimen) Fig.11. An example of pioneer crack
formation.

Figure 11 shows an example of a pioneer crack formation. On a slight notch

specimen, a pioneer crack is formed by the coalescence of many microcracks
distributing over a wide region. On the other hand, on a sharp notch
specimen, a pioneer crack is formed by the joining of a few microcracks
initiating in a narrow area of notch root, and grows without coalescence of
adjacent microcracks. Therefore, cathodic protection is more effective for
a sharp notch specimen than for a slight notch specimen.

CONCLUSION

In order to clarify the effect of cathodic protection for notched specimens,

the microcrack initiation, its growth and the pioneer crack propagation were
discussed. For a slight notch specimen, cathodic protection is effective on
a microcrack growth, but not on a pioneer crack growth, because the pioneer
crack propagates by the coalescence of many microcracks distributing over a
wide region. On the other hand, for a sharp notch specimen, cathodic
protection is effective rather on a pineer crack growth, since the crack
grows by the joining of a few microcracks initiating in a narrow area of
notch root. Thus, cathodic protection is more effective for a sharp notch
specimen than for a slight notch specimen.

REFERENCES

Boger, F.D. and Crooker, T.W. (1979). The infuluence of Bulk-Solution-

Chemistry Conditions on Marine Corrosion Fatigue Crack Growth Rate. J.
Test & Eval., 7, 155-160.
Brown, E.F. (1983). Effects of Cathodic Protection on Corrosion Fatigue.
ASTM STP801, 508-515.
Hartt, W.H. and Hooper, W.C. (1980). Endurance Limit Enhancement of Notched
1018 Steel in Sea Water-Specimen Size and Frequency Effect.NACE, 36, 107-
112.
Okada, T., Hattori, S. and Asai, Y.(1990). Corrosion-Fatigue Strength of
Notched High-Tension Steel Specimens Under Cathodic Protection in
Synthetic Seawater, JSME Int. Jour., 33, 375-381.
 WS8g1

CORROSION FATIGUE CRACK INITIATION AND PROPAGATION

BEHAVIOR OF 12 Cr STAINLESS STEEL

Ryuichiro Ebara, Tamotsu Yamada and Tatsumasa Kobayashi

Hiroshima R & D Center, Mitsubishi Heavy Industries, Ltd.
* 4-6-22, Kan-on-shin machi, Hiroshima, 733, Japan

Haj ime Kawano

Nagasaki R & D Center, Mitsubishi Heavy Industries, Ltd.
** 1-1, Akunoura machi, Nagasaki, 850-91, Japan

ABSTRACT

This paper describes the microscopic features of the corrosion fatigue

process, specifically the initiation and growth of corrosion pits in
corrosion fatigue crack initiation process of 12 Cr stainless steel.
Quantitative analyzed examples of the size of corrosion pit by use of
recently developed image analyzing technology are also described.

KEYWORDS

Corrosion fatigue, crack initiation, corrosion pit, image analyzing

technology, 12 Cr stainless steel.

Introduction

It is demonstrated that corrosion fatigue crack initiation process of 12 Cr

stainless steel is governed by corrosion pit (Ebara et al, 1978). However,
not only the mechanism of pit formation, but also the critical size of pit
dominating corrosion fatigue crack initiation and propagation has not been
clarified in detail. In this paper it is reported on the sequential observa-
tion results of the initiation and growth of corrosion pit, crack initiation
and propagation from corrosion pit. Finally a quantitative analyzed example
of corrosion pit by use of recent developed image analyzing technology is

799
800
touched in brief.

Initiation and Growth of Corrosion Pits in Corrosion

Fatigue Process

Experimental Procedure
The material used in this investigation was martensitic stainless steel,
austenitized at 1243K for l/2h, oil quenched, tempered at 993K for 1/2 h
and air cooled. Chemical compositions and mechanical properties of the
tested steel are shown in Table 1. Corrosion fatigue tests were conducted
by use of a plane bending fatigue testing machine (4.9 kN).
The testing speed was 13.3 Hz and the stress ratio was 0.05.
The prepared environment was 3% NaCl aqueous solution (318 K) and was
circulated at a flow rate of 40 CC per minute. The defined area of the
specimen was exposed to 3% NaCl aqueous solution.
Before the test all specimens were polished with #1000 emery paper.

Table 1 Chemical compositions and mechanical properties of tested

material

Chemical compositions (wt %) Mechanical properties

c
Material C Si Mr. P S Cr Mo (TO. 2 OB E.L R.A ^ a r py HB
(MPa) (MPa) 1%) (2mm)
(%' (N-m/cm 2 )
|JOJ, O.IO 0.26 0.46 0.021 0.006 12.40 0.51 650.4 765.2 25.6 68.2 262.6 229

Note: heat treatmentiQuenching (1243K x l/2hr O.C), Tempering (993Kxl/2hr A.C )

The surface observations were sequentially conducted on a defined area

(15mm2) of a plane bending specimen as shown in Fig. 1 at intermittent number
of cycles by use of scanning electron microscope (JCM-840).

Masking

4Z
^
22 5 13

40

Fig. 1 Corrosion fatigue test specimen

 801

Results and Discussion

The S-N curves obtained in air and 3% NaCl aqueous solution are shown in
Fig. 2. 500r

400h

300

200 Plane bending

• - Air, R.T
100 O - 3%NaCI, 318K

I04 I0 5 I0 6 I0 7 I08
Number of cycles
Fig. 2 S-N curves of 12 Cr stainless steel in 3% NaCl
aqueous solution

The stage of crack initiation from the corrosion pit and the appearances o
the crack propagation from the corrosion pit were clearly seen in Fig. 5.

Fig. 3 Crack initiation and propagation from corrosion

pit, plane bending stress: 228 MPa, 3% NaCl
aqueous solution (318K)
802
The maximum depth, diameter and fraction of area of corrosion pit increases
with increasing number of cycles. The maximum depth of corrosion pit at
crack initiation stage is 23. 5 # m in plane bending stress of 228 MPa(N/N f =
0.968) and 17.8 ^ m in plane bending stress of 280 MPa(N/N f =0. 645) (Fig. 4).

xl0~2
30
Plane bending s t r e s s
O 2 8 0NlPa
• 2 28MPa
77777 Crack initiation

3% NaCl , 318K

20h-

10H

0.2 0.4 0.6 0.8

N/Nf

Fig. 4 Maximum depth of corrosion pit

The above observations revealed that crack initiation occurred at the bottom
of the corrosion pit where the stress concentration is large and is pre-
sumably electrochemically active.
It is apparent that the corrosion fatigue life of 12 Cr stainless steel is
governed by the crack initiation process. And most of the crack initiation
depends on initiation and growth of corrosion pit.
The da/dN calculated by use of the Newman-Raju' s (1979) equation from the
maximum depth of the corrosion pit as a function of Δ Κ is shown in Fig. 5.
The smaller the Δ Κ at crack initiation stage as smaller the plane bending
stress is. The Δ Κ when crack initiates is 2.3 MPa f~m in plane bending
stress of 228 MPa and 3.1 MPa J~m in plane bending stress of 280 MPa.
 803
1 I 1 ~ ~ "1—1
Ι(Γ 5 -
0 Crack 7
• Sub crack A
3#NaCl,3i8K ß

j
I0"6

lO"7 -
1 ]
A
i Jo
! tf Crack i n i t i a t i o n

I0~ 8

lO- 9 A

l(f10
0.5
_j 1
2 5
1 J
10
ΔΚ (MPa-m1/*)

Fig. 5 da/dN vs. Δ Κ (tfa =338 MPa)

An Application of Image Analyzing Technology for Measuring

the Size of Corrosion Pit

For accurate corrosion fatigue life estimation, it is necessary to measure

the size of corrosion pit exactly. By use of a recently developed image
analyzing technology, the figure of corrosion pit can be almost exactly
measured.
Fig. 6 shows an example of an analyzed image of a bird's eye view (three-
dimensional profile)(b) and a cross section (two-dimensional profile)(c) of
a corrosion pit (a) by use of sequential similarity detection algorithm
(SSDA). It is apparent that the figure of corrosion pit (Fig. 6(a)) is
almost semicircular.
The measured depth of corrosion pit was 5.5 ^ m and was relatively well
coincident with 6. 1 # m measured by stereofractography.
Even if some corrosion products were in the corrosion pit, it is possible to
measure the figure of corrosion pit by use of corrected sequential similari-
ty detection algorithm (SSDA) and the mutual correlation coefficient
technique (MCCT) together.
804

Fig. 6 Image analyzed corrosion pit (SSDA)(Ebara et al 1989)

CONCLUDING REMARKS

From the sequential observation results of the corrosion pit it was

clarified that corrosion fatigue life of 12 Cr stainless steel is governed
by initiation and growth of corrosion pit. However, information is still
limited on electrochemical and metallurgical aspects of corrosion pit
initiation. The development of an interdisciplinary approath is expected
to solve this subject.

REFERENCES

Ebara R., Kai T. and Inoue K. (1978): Corrosion Fatigue Technology, ASTM Spec.
Tech. Publ. No. 642, 155-168.
Ebara R., Kai T., Inoue K. and Masumoto 1.(1978): J. Soc. Mater. Sei., Jpn.,
27, 64~68.
Ebara R. and Yamada T. (1989): Recent Development of Image Analyzing
Technology for Microstructure of Metal, ISIJ, 96-102.
Newman J.C and Raju I. S (1979): NASA Technical paper 1578
WS8g2

EFFECTS OF COATING THICKNESS DISTRIBUTION

ON CORROSION FATIGUE STRENGTH OF STEEL

M. ARITA, S. NAITO, T. SHIBATA AND K. TAMURA

Ship Research Institute, Ministry of Transport of Japan

6-38-1 Shinkawa, Mitaka-shi Tokyo, Japan

ABSTRACT

Corrosion fatigue strength of paint coated fillet weld joint test specimen
was experimentally investigated from a view point of evaluating the effects
of coating thickness distribution on the corrosion preventing
characteristics of coating film.

Conclusions obtained are as following.

1) Fatigue strength of fillet weld specimens without coating film depends

largely on their configuration at higher stress level, but not depends on
it at lower stress level.
2) Corrosion fatigue strength of specimens with coating film is almost the
same as that of joint specimens in air, if the coating thickness
distribution level is good enough.
3) Bad coating thickness distribution results in the reduction of corrosion
fatigue strength at higher stress level, because of the fact that the
coating breaks at early stage of fatigue loading.
4) Coating thickness distribution can be evaluated by the fatigue strength
diagram proposed in this paper.

KEYWORDS

Corrosion fatigue; coating thickness distribution; fillet weld joint.

INTRODUCTION

Ocean is a severe corrosive environment for steel structures, and many

countermeasures have been investigated to prevent the corrosion. As one
of these countermeasures, anticorrosive paint coating has been widely
used. And the development of heavy duty paint made the effectiveness of
paint coating film much higher than before [1]. The endurance limit of
coating film made from heavy duty paint is usually assumed to be more than
ten years. In reality, however, this endurance limit is largely affected
by many factors relating to coating practice.

805
806

SPECIMEN TYPE A
(AS WELD)
6lx50_

Φ © ( 2 ) © © WELD
BEAD

Im
ft Le-J
SPECIMEN TYPE B SPECIMEN TYPE C
(STRAIGHT CUT) (F12 DRESSED)

Fig. 1. Test specimen.

Coating film thickness distribution, which is considered to be mainly

determined by the detailed configuration of structure to be coated, is the
most important factor to be discussed in relation to the effect of coating
practice on the anticorrosive properties of coating film.

BACKGROUND

Edges and corners of structural members are the places where the effect of
coating film thickness distributions on the corrosion preventing properties
of coating film is to be considered carefully, because of the difficulty to
get uniform thickness of coating film. Especially, corners in structural
member like fillet weld joints are usually the places where stress
concentration is apt to be found. Therefore corners are more important
places than edges from the view point of safety against corrosion and
fracture.

Authors have made data bases concerning coating film long-term properties
[2] in order to improve the reliability of anticorrosive properties of
coating film. Data base of coating film distribution was included in
these. It is necessary, however, to combine the coating film thickness
distribution and its effect on the strength of structural member on which
the coating film was applied. Therefore, as an attempt to get one of such
data to combine the two, we have made experimental works to get the
relation among weld configurations of fillet weld joints, coating film
distribution on them and corrosion fatigue strength of these joints.

EXPERIMENT

Figure 1 shows fillet weld joint test specimen used. There are three
configurations of fillet weld, as "as weld" (specimen type A ) , "straight
cut" (specimen type B) and "Φ12 dressed" (specimen type C) . Argon gas
shield welding was adopted. Table 1 shows chemical compositions and
mechanical properties of steel used for test specimens.
 807
Table 1. Chemical compositions and mechanical properties
of steel used.
Chemical Composition (%) Mechanical Properties
Thickness
V V
(mm) c Si Mn P S Cu Ni Cr AI V Mo (MPa)
El.
(MPa) L=50mm

6 0.14 0.20 0.57 0.021 0.023 0.11 0.076 0.14 0.002 0.001 0.013 682 729 18.2

Table 2. Specification of coating film applied.

Surface 1st 2nd 3rd
Preparation layer layer layer
Shot Blast inorganic zinc pure epoxy pure epoxy
SIS-Sa 2 1/2 primer paint ΙΟΟμΓΠ paint 100μίΠ

Fig. 2. Corrosion fatigue testing apparatus.

Table 2 shows the surface preparation and the specification of coating film
applied to test specimens. The film consists of three layers and has a
designed thickness of 2 00μπι. And specimens were coated carefully by the
maker of paints used. Edges of specimens were slightly cut off in order
not to get defects at these edges.

Three types of specimens with coating film were cut to slices and carefully
polished in order to measure coating film thickness distribution on the
cross section of them around fillet weld parts. Fifty coating thickness
data were obtained for each specimen along coating film on fillet weld,
starting from the point 1mm apart from weld toe boundary till the point 1mm
apart from the other toe boundary of the same weld.

Fatigue tests were conducted in air and in ASTM SOW (substitute ocean
water). Figure 2 shows the fatigue testing apparatus used. Test
specimens were fixed to the bed of the apparatus, SOW was fulfilled to the
water tank and the constant amplitude bending load was applied to the upper
part of specimens (maximum number of specimens to be tested simultaneously
was three).

Fatigue test in air were conducted for test specimens A, B, C without

808

Fig. 3. Coating film thickness along fillet weld.

Fig. 4. Coating film appearance at weld toe.

5a Test specimen A, 5b Test specimen B,
5c Test specimen C.

coating film, at room temperature, by loading rate of 0.5 Hz and at stress

ratio R=-l. Number of cycles to failure was obtained. Corrosion
fatigue tests in a water tank filled with SOW (temperature 2 5±1°C, air
being sufficiently supplied) were conducted for test specimens A, B, C with
and without coating film, by loading rate of 0.17 Hz and R = -1. SOW was
always circulating during fatigue test, at a rate of one replacement of
water in tank per every three minutes. Generation of defects in coating
film, growing up of rust and number of loading cycles to failure were
observed during fatigue tests.

DATA OBTAINED AND DISCUSSION ON THEM

Coating Film Thickness Distribution

Figure 3 shows coating thickness at measured position along fillet weld.

Figures 4 a, b, c show the appearances of fillet weld and coating film
cross section at the places corresponding to weld toe. It is observed
 809

Test'"·"- Paint ί Not Coated

AS WELD ! | P

STRAIGHT CUT j ^

Φ12 DRESSED j ^

R=-1
F=0.17Hz (in SOW)

I I I I I II ll I I I I I II ll I I I I II II
10 10

NUMBER OF CYCLES

Fig. 5. Fatigue strength diagram

(not coated specimens in SOW).

that coating thickness sharply changes at weld toe for test specimen B,
because of abrupt change of curvature at the place. Relatively smooth
coating thickness is observed for test specimen C, because of constant
curvature along whole fillet weld. For test specimen A (as weld), coating
thickness distribution has the intermediate appearance of test specimen A
and C, because of rather smooth change of curvature with cyclic hump and
hollow due to weld bead lines.

Mean coating film thickness tra, standard variation of coating thickness σ

and coefficient of variation o/tm obtained are as following.

specimen A (as weld) tm=0.32mm σ=0.037mm o/tm=0.12

specimen B (straight cut) ^=0.38πΰη σ=0.052mm ö/tm=0.14
specimen C (Φ12 dressed) t =0.31mm σ=0.030mm σ/t =0.097

We assume that the degree of coating film thickness distribution can be

expressed by the coefficient of variation o/tm. The coefficient of
variation o/tm of coating film of almost same specification, as used here,
and painted on flat surface is around a value of 1.0 [3]. This means that
almost same degree of coating film distribution as that on flat surface can
be obtained for film on fillet weld of specimen C. It should be noted
that the dressing of specimen C fillet weld of this dimension is so made
that the stress concentration coefficient at weld toe for bending moment
(as in this paper) becomes minimum.

Fatigue Strength

Figure 5 shows the relation between stress amplitude Δσ and corrosion

fatigue life of specimens without coating. At higher stress amplitude,
there exist effects of fillet weld shape on fatigue lives. But at lower
stress amplitude, there are little effects of the shape.

Nominal stress concentration factors a obtained for specimen A, B, C [4]

are as following.
810

Specimen ' · . · in Air ;

ASWELD · Q ■ φ

STRAIGHT CUT; ^ ; ^

Φ12 DRESSED
□ il
Jk # 0 DI

R=-1
F=0.17Hz (in SOW)
F=0.50Hz (in Air)

i i i i 111 il i i i i 111 il i ι ι ι im
10 10
NUMBER OF CYCLES

Fig. 6. Fatigue strength diagram (coated specimens

in SOW and not coated specimens in air).

specimen A (radius of curvature at weld toe measured is 4.40 mm)

a s less than, but not far from 2.1
specimen B (radius of curvature at weld toe measured is 3.25 mm)
a = 2.1
specimen C (measured constant radius of curvature of weld is 6.30 mm)
a = 1.13

It is considered that at higher stress amplitude, these stress

concentration factors have direct influence on the fatigue lives of
specimens. But at lower stress amplitude, corrosion proceeds at weld toe
before initiation of fatigue crack, and initial differences of stress
concentration factors among specimen types are going to vanish.

Figure 6 shows the relation of stress amplitude Δσ against fatigue lives

of specimens without coating film in air and that of corrosion fatigue of
specimens with coating film. It is shown in this figure that corrosion
fatigue strength of specimens with coating film is fairly affected by the
coating thickness distribution. For specimen B, which has the worst
coating thickness distribution (marks Δ and ▲ in Fig. 6 ) , corrosion
fatigue lives of coated specimens are always shorter than those of uncoated
specimens in air for wide range of stress amplitude. On the other hand,
for specimen C, which has the best coating thickness distribution among
specimens tested (marks □ and I in Fig. 6 ) , corrosion fatigue lives of
coated specimens are longer than those of uncoated specimens tested in air
for whole range of stress amplitude. For specimen A, which has the coating
film thickness distribution of an intermediate property between those of
specimens B and C, corrosion fatigue lives of coated specimens are longer
than those of uncoated specimens tested in air for higher stress range, but
they become shorter for lower stress range. These data can be understood
that, in case of specimens with poor coating thickness distribution,
thicker film parts are exposed to higher stress than they ought to be, and
thinner film parts are apt to be more easily invaded by particles like
chloride or oxygen which stimulate corrosion fatigue than the parts with
appropriate coating thickness. Figure 7 shows a pinhole of coating film
in case of specimen B, observed during experiment. The position of this
 811

Fig. 7. Pinhole of coating film at fillet weld toe

(test specimen B ) .

Fig. 8. Conceptional illustration of corrosion fatigue

strength of coated specimen.

pinhole corresponds to the place of film on the weld toe where coating
thickness show enormously large value.

Figure 8 shows the overall view of the property of corrosion fatigue.

Data obtained in this experiment and others [5] are taken into
consideration. Corrosion fatigue strength of uncoated specimens are
illustrated by bold solid line as is previously explained. The uppermost
dotted line just above a normal solid line which corresponds to corrosion
fatigue strength of specimen C shows idealized relation of stress amplitude
and fatigue life, assuming that coating film is perfectly made with
adequately uniform coating thickness distribution. At loading cycles of 3
x 106, the dotted line goes down crossing the solid line. The point (not
necessarily to be 3 x 106) corresponds to the time when the deterioration
of coating film proceeds. The indication that the dotted line is somewhat
higher than the solid line, corresponds to the increase of fatigue strength
812
of coated specimens due to surface preparation before coating (shot blast,
sand blast or others).

The lowermost dotted line, just below the solid line corresponding to
corrosion fatigue strength of specimen B, shows the relation between stress
amplitude and loading cycles to failure, assuming that the film thickness
distribution is bad. Defects in coating film initiates before the
initiation of fatigue crack in bulk metal.

The middle dotted line corresponds to the case of specimen A. The dotted
line crosses the solid line at number of loading cycles of 106. This
indicates that coating has not good enough thickness distribution and that
defects in coating film occur in the way of fatigue loading at lower stress
amplitude.

When the degree of coating film thickness distribution is determined based

on a figure strength diagram equivalent to Fig. 9, detailed configurations
of structures can be designed so as to much the degree.

CONCLUSION

Fatigue tests of fillet weld joints with and without coating film were
conducted in air and in SOW. Effects of coating film thickness on fatigue
strength were discussed. Conclusions obtained were as following.

1) Coating film thickness distributions were affected by configurations of

fillet weld. The best distribution could be obtained for fillet welds with
constant radius of curvature equivalent to the leg length of them.
2) Corrosion fatigue strength of not coated fillet weld joint specimens
were affected by configurations of fillet weld at higher stress amplitude,
but the affection decreased to zero at lower stress amplitude.
3) Corrosion fatigue strength of coated specimens were affected by coating
film thickness distribution. If coating film thickness distributions were
equivalent to those for flat parts, and if the deterioration of film did
not occur, it is possible to get equal or rather higher fatigue strength
for coated specimens in SOW than that for not coated specimens in air.
4) An illustration diagram which showed the effect of coating film
thickness distribution on fatigue strength is proposed. Detail
configurations of fillet weld can be designed, according to an anticipated
prolongation of corrosion fatigue life due to coating film based on the
diagram.

REFERENCE

1) Arita, M. (1985). Heavy Duty Painting, Bulletin of the Society of Naval

Architects of Japan, 667, 41.
2) Arita, M., K. Matsuoka, K. Ohnaga and T. Shibata (1985). Corrosion
Preventing System of Offshore Structures by Paint Coating, Proceeding of
Techno-Ocean 88, 2, 43-49
3) Report of Ship Research Association of Japan (1985). Researches on Heavy
Duty Painting for Offshore Structure, 376, pp.79-95.
4) Nishida (1988). Morikita Publishing Co. Ltd. In: Stress Concentration,
pp.637-639, pp.725-730.
5) Proceeding of 3rd symposium (1987). Ocean Environment Data and Analyses
of Cooperative Experiments on Steel Strength at Research group of
Environmental Strength of Steel. Japan institute of steel.
 WS8g3

PROBLEMS WITH LOCALIZED CORROSION AND FATIGUE IN STEAM

TURBINE AND WATER TURBINE ROTORS

L. Hagn

Allianz-Center for Technology GmbH

Ismaning

Federal Republic of Germany

ABSTRACT
Cracks caused by corrosion fatigue in low pressure steam
turbine and water turbine rotors have led to an investigation
of the course of the damage, which includes the diffusion and
concentration of the corrosive medium before pitting and crack
initiation occurs. Conclusions are also drawn on life assess-
ment and the avoidance of damage.

KEYWORDS
Turbine rotor; organic coating; water permeability; electrolyte
concentration; pitting corrosion; notch effect; crack forma-
tion; life; internal stresses.

DAMAGE
Steam turbines and water turbines are normally designed for
some 20 to 25 years of operation. In the case of steam turbi-
nes, high demands are made on the purity of the energy carrier
in order to reduce corrosion, including corrosion of the rotor.
These requirements specify the oxygen content, conductivity, pH
value, etc. In the case of hydro-electric power stations on the
other hand, the corrosion protection of the turbine and pump
rotors subject to the flow of water is effected by means of
organic coatings. Nevertheless, cases do occasionally occur in
which - usually after fairly long periods of operation - crack
damage appears necessitating remedial action. Two representa-
tive cases of damage are described.

The cyclic fatigue fracture on a low pressure turbine rotor

(1 % Cr, 0.2 % Co, 0.6 % Mn) with approximately 74,000 hours of
operation started from six pitting locations distributed around
the periphery of a rotor step (3 m m ) .

The crack had penetrated into the rotor to the point where
there was only 14 % residual area (560 mm j2J) when the turbine

813
814

was closed down. The crack followed a turning groove of maximum

depth 0.045 mm, Fig. 1, in which occasional pitting of up to

Fig. 1 Fatigue crack starting A at pitting in a turning grove

T in a rotor surface step N
Fig. 2 Corrosion pit P initiating the fatigue crack £c
0.06 mm depth was present. It was initiated by electrolyte with
a chloride content which was gradually concentrated from the
steam condensate in the approximately 1 mm wide gap between the
turbine disc and the shaft central collar, Fig. 2.
In the 2,400 kW Kaplan turbine with an oblique rotor subject to
the flow of water peripheral cracks up to 25 mm long were
found, shown as an example in Fig. 3, - two years after the
application of the tar/epoxy resin coating - in the unalloyed
Ck 35 steel rotor flange, especially near the flange nuts.
Using a surface sample, it was possible to show that the
fatigue cracks (up to 4.5 mm deep) originated at corrosion
pitting, Fig. 4, of up to 2.5 mm diameter and 0.4 mm deep.

Fig. 3 Fatigue crack R in the rotor flange surface near a

bolt nut.
Fig. 4 Corrosion cavity at fatigue crack initiation.
 815

The crack initiation in the low pressure steam turbine and

water turbine rotors is therefore caused by both corrosion
processes and the stress level.

CORROSION PROCESS
The occurrence of a local film of water (deionized water) on
the rotor surface takes place by condensation of the steam or
by permeation of water through the surface coating. At the same
time, long-term concentration of the deionized water to form
aggressive electrolytes containing chlorides or sulphates takes
place because of the precipitation of steam impurities
(Effertz, Hagn, 1982) or because of impurities dissolving from
the coating materials at the layers forming the boundary of the
coating.
The damage process when both fatigue loading and corrosion are
present - corrosion fatigue - is usually described as being
subdivided into the stages of incubation, crack initiation and
crack propagation. In the cases mentioned, however, the course
- of the incubation phase in particular - is substantially
unknown. Under operating conditions, the shafts described are
subjected to fatigue stress amplitudes of less than 50 MPa in
their unnotched regions. This is far below the infinite life
fatigue strength in air of the steels used (more than 250 MPa).
It is therefore certain that dislocation structures will only
form very slowly, if at all; persistent slip bands - extrusions
and intrusions - and hence highly reactive fresh surfaces are
practically more. This corrosive attack is therefore only
slightly affected by the fatigue load and starts at structural
inhomogeneities and inclusions where local elements of corro-
sion form. Pitting occurs even in NaCl solutions of low con-
centration (Effertz, Forchhammer, 1976) and after relatively
short times.

The S-N-curve from fatigue crack corrosion tests, Fig. 5, on

uncoated test pieces in the rotor steel Ck 45 in water conati-
ning NaCl (1,000 uS/cm PHZ 20 °C) shows a steady drop to well
below the infinite life strength in air (± 280 MPa) and down to
the operating stress level. The values for the depths of the
largest corrosion pits determined at the beginning of fracture,
also plotted on the diagram, make it possible to recognize the
known pit growth corresponding to the residence time - which is
presumably accelerated by the top layers breacking off cycli-
cally. With decreasing fatigue stress amplitude, the corrosion
notch initiating the crack must become greater and tend asymp-
totically towards its limiting value.
The intention is that the corrosion protection of rotors
subject to polluted river water with a high conductivity and
NaCl content should be ensured by the organic coating system.
Its effectiveness is determined by its permeability to gaseous
and liquid materials and its water absorption and swelling
behaviour. In practice, water absorption starts as soon as the
coating comes in contact with the water. The permeability to
water depends on the temperature and the thickness of the
coating. Initial measurements from a current research programme
816

give a water vapour diffusion density

2
of 0.7 to 26 g/m2D for
Polyurethane, 0.05 to 0.06 g/m D for epoxy resin and 0.18 to
0.78 g/m2D for unsaturated polyester. This indicates a certain
graduation but there is practically no operational proof.
i i 1—i i—r—ΓΤT TT 1— i — i 1 1 1 I I I 1
_ L 5 0 Oppm NaCI-Sol., Air ■aturati»d, pH 7, 20-Cat 50 Hz, R-0.1 J β

li I
\
III ^V* KIC uryel

V
^+
Pit dap h-T m·
I 3
100 III ^ * \
III λ. sU 1 iJJ I -
■sÜI I
VI

Cycles to Failure x10 ~ 6 / Time to Pit depth

Fig. 5 S-N-curve of steel Ck 45 in

NaCl-soln and pit growth trend

Fig. 6 Stess range diagramm for steel 25 Mo 4 for air and

sodium chloride soln.
It seems therefore impossible to avoid rapid access of the
water to the metal surface even in the case of an intact and
correctly applied coating. If the above assumptions are cor-
rect, the corrosion protection effect of the coatings is based
on preventing the access of the corrosive materials contained
in the water, such as chloride and sulphate. If there are no
ionic constituents in the coatings or on the boundary surfaces,
only deionized water gets to the steel and a higher fatigue
strength is to be expected than would be obtained in a salt
solution. The time necessary for any possible corrosive attack
is therefore substantially determined by the phase during which
the conncentration increases in the local water film to the
extent necessary to produce a corrosive electrolyte on the
surface. This has to be investigated in the future.
STRESS RELATIONSHIPS
A mean tensile stress induced by surface contraction or cen-
trifugal force is superimposed on the cyclic bending fatigue
loads, which are increased by stress concentrations in regions
with notches or changes in section. The fact that the stresses
are superimposed can raise the rotor stress locally into the
pulsating tension range - with positive stress ratios, R - the
mean stress also varying as a function of rotational speed.
Particullarly important locations are the transitions to shrink
fit seatings, the transitions to integrated rotor disks and
flanges and in the zones near rotor screw threads. In the case
of screwed connections, the contact pressure of the bolt heads
or the nuts will elastically compress the rotor surface under
them but the surface is being pulled elastically in the imme-
diate vicinity and is therefore subject to tensile stresses in
restricted regions. In the case described, peripheral cracks
 817

occurred at this location under conditions of threshold tensile

stress.
Stress Range * σ [MPa]

Fig. 7 Crack growth data for steel 25 Mo 4 in air

Fig. 8 Limiting threshold stress range for fatigue crack

growth of forged steels 2 - 4 % NiCrMoV in air and
NaCl-soln

LIFE ASSESSMENT
As is shown by the fatigue diagram for the forging steel
25 CrMo 4, Fig. 6, a 22 % NaCl solution reduces the tolerable
fatigue stress amplitude almost uniformly by a factor of 2.4
throughout the R range tested. In every case, the starting
point for the test piece fracture was pitting. This of course
means that the notch growth and-effect rather than the dislo-
cation mechanism determines the life. The question therefore
arises of how to deal with and calculate the effects on life of
pit growth and the consequent increase in stress. A form factor
calculation using the elementary equations of strength and
notch stress theory, taking account of the stress gradient
(Heywood, 1947) or the theory of the equivalent notch
(Petersen, 1977), becomes too inaccurate because of the small
dimensions - particularly since, in practical cases, notches
within notches have to be evaluated. The relationsships of
fracture mechanics, based on crack growth measurements over the
threshold stress intensity factor range Κ φ of the material
used, become useful in this case (Lindley at. al. 1982). Test
results on the forging steel 25 CrMo 4, Fig. 7, show a decrease
of the K T H value from 7 MPa m to 4 MPA m as the R value
increases from 0.1 to 0.8 (ESD 8023, 1982). This may be attri-
buted, very largely, to the decreasing influence of the crack-
closing effect. Using the known fracture mechanics relations-
ships, Fig. 8, a corrosion pit can be evaluated as the critical
defect size for initiating a crack which can grow (Kawai,
Kasai, 1985). The threshold stress intensity factor in air can
be used, at least at high R values, because the influence of
818

corrosion will not be large in this case. To assess the life of

rotating shafts under conditions which may be corrosive, the
elapsed time before fracture occurs can be considered as being
made up as follows:
water penetration through the covering layer (I) + concentra-
tion of the corrosive medium (II) + pitting growth to the point
of crack initiation (III) + crack propagation to the point of
unstable fracture (IV), or
H *2 *3 *c
(P )dt + (C )dt + pG dt+
'tot = J I J II J ( Hl» J < CG iv )dt
o t- to t~ with [t = time]
Only the last two terms of the equation are fixed by the
limiting characteristic values K T H and KI C of fracture
mechanics. No unambiguous way of recognizing the chemical and
physical/chemical course of the first three phases has been
found up to now and there are no laws which describe exactly
these phases. Life estimation is therefore mainly empirical in
nature.
There appear to be three ways of dealing with the problem
delaying or excluding Phases 1 to 3, i. e. the corrosion
processes, and/or reducing the dynamic loads by design measures
and/or use of corrosion resistent steels.
REFERENCES
Effertz, P.-H. and Forchhammer, P. (1977), The sensitivity to
localized corrosion of the quenched and tempered steel
X 20 CrMo 13 in solutions of sodium hydroxide. Der Maschinen-
schaden 50, 136 - 143
Effertz, P.-H. and Hagn, L. (1982), Investigation of the corro-
sion fatigue behaviour of turbine blade steels in the region of
initial steam condensation. Der Maschinenschaden 55, 67 - 80
Engineering Siencies Data No. 81012 (1981). Threschold stress
intensity factors ... Inst. Mech. Engineers.
Hagn, L. (1986), Critical surface areas in highly loaded shaft
regions. VGB-Konferenz Kraftwerkskomponenten 1986, p. 148 - 157
Haywood, R.-B. (1947). Aircraft NG Engineering 19, 81 - 86
Kawai, S. und Kasai, K. (1985), Considerations of allowable
stress of corrosion fatigue (focused on the influence of
pitting). Fatigue Fract. Engng. Mater. Struct. 8, 115 - 127
Lindley, T. C., Mclntyre, P., Trant, P. J. (1982): Fatigue-
crack initiation at corrosion pits. Metalls Technology 9,
135 - 142.
Petersen, C. (1952), Processes occurring in a grain structure
subject to tension and alternating loads. Zeitschrift Metall-
kunde 43, 429 - 433
 WS8g4

THE SMALL CORROSION FATIGUE CRACK GROWTH BEHAVIOR OF HIGH-

TENSILE STRENGTH STEEL HT50 UNDER CONDITIONS OF OXYGEN DIF-
FUSION-TYPE CORROSION AND HYDROGEN EVOLUTION-TYPE CORROSION

S. ISHIHARA, K. SHIOZAWA, K. MIYAO and H. FUKUCHI

Faculty of Engineering, Toyama University, Toyama 930, Japan

ABSTRACT

Small corrosion fatigue crack growth behavior was investigated using smooth
high-tensile strength steel HT50 plate specimens in sodium chloride aqueous
solution(oxygen diffusion-type corrosion) and acid solution(hydrogen evolu-
tion-type corrosion). At a constant effective stress intensity factor range
, crack growth rates of the surface cracks increase with increase of stress
amplitude range. That is, crack growth rates of the small-size surface
cracks are higher than those of the comparatively large-size surface cracks.
This experimental result was observed in both types of corrosion conditions:
oxygen diffusion-type corrosion and hydrogen evolution-type corrosion, and
this peculiar crack growth behavior became marked in the latter environment
whose corrosive capability is stronger than that of the former.

KEYWORDS

Corrosion Fatigue; Crack Growth; Small Crack; Oxygen Diffusion-type Corro-

sion; Hydrogen Evolution-type Corrosion.

INTRODUCTION

In corrosion fatigue, it has been pointed out that the small surface crack
growth behaviors observed on the smooth specimen surface are different from
those of the long through-thickness cracks. Many studies on the small cor-
rosion fatigue crack growth behaviors have been performed. But most of them
are concerned with high strength steels(Gangloff,1985; Nakai et al.,1989;
Nakajima et al.,1988). In the present study, small corrosion fatigue crack
growth behaviors were investigated using smooth high tensile strength steel
HT50 plate specimens in sodium chloride aqueous solution and acid solution
made by adding sulfuric acid to the salt water. Their behaviors were com-
pared with those in laboratory air and those of through-thickness cracks.
It was clarified that there were peculiar crack growth behaviors in the
small corrosion fatigue crack growth.

819
820
SPECIMENS AND EXPERIMENTAL PROCEDURES

The material tested was high strength steel HT50 and its chemical composi-
tions and mechanical properties are listed in Table.1 and Table.2 respec-
tively. Specimens were cut out into the figure shown in Fig.l from as-
received materials and electro-polished preceding fatigue tests. For inves-
tigating the through-thickness fatigue crack growth behaviors, specimens
with a circular notch in the center were used. Plane bending fatigue ma-
chine was used in the present tests and its cyclic speed was 10Hz. Three
types of corrosive environments were used. They are aerated and deaerated
sodium chloride aqueous solution kept at 298K and acid solution(pH=l.l).
Crack lengths were measured successively during the corrosion fatigue proc-
ess using an optical microscope. Crack depths were investigated by elimi-
nating the specimen surface with electro-polishing. The crack opening
points were determined by investigating the variation of the distance be-
tween two micro-Vickerse marks introduced near the crack tip during a stress
cycling.

EXPERIMENTAL RESULTS

Crack Aspect Ratio

Fig.2 shows the relationship between crack aspect ratio As(As=b/2a,2a:crack

length, b:crack depth) and crack length 2a. As seen from these figures, in
the region of short crack lengths, the values of As_ are above 0.5, while in
the region of long crack lengths, ks_ decrease with increase of crack lengths
and take a constant value. In the relation, stress amplitude dependence is
not seen.

Crack Growth Behaviors

Through-thickness Crack Fig.3 shows the relationship between crack growth

rates and stress intensity factor range for the three different environment.
These relations are concerned with through-thickness cracks. The measured
crack lengths was 0.8mm to 6mm. The values of stress intensity factor were
calculated using the results of Roberts and Rich(1967). From these figures,
crack growth rates of the through-thickness cracks are prescribed well by
the stress intensity factor range. In the low stress intensity factor range
, the acceleration of the crack growth rates due to corrosive environment is
observed, but the degree is not remarkable.

Small Crack The relationships between crack growth rates and stress in-
tensity factor range for small fatigue cracks in laboratory air, sodium
chloride aqueous solution and acid solution are shown in Fig.4. The range
of crack lengths measured was 0.1mm to 4mm. The stress intensity factors
were calculated using Raju-Newmann results(1979). From the results for
laboratory air, no stress amplitude dependence is observed in the relation.
This tendency is the same as that observed in the through-thickness crack
growth behavior, but the threshold stress intensity factor range for the
small fatigue cracks is lower than that of the through-thickness cracks.

While, in sodium chloride aqueous solution and acid solution, obvious stress
amplitude dependence is observed in the relations. At a constant stress
intensity factor range, the higher stress amplitude becomes, the faster
crack growth rates becomes. The same tendency was also observed in the
 821
small corrosion fatigue crack growth behaviors of an aluminum alloy(Ishihara
et al.,1988). In the low stress amplitude region of about lOOMPa, the
differences of the crack growth rates between sodium chloride aqueous solu-
tion and acid solution are not observed, while in the high stress amplitude
region of about 315MPa, crack growth rates in the acid solution are faster
than those in sodium chloride aqueous solution.

CONSIDERATIONS

The Small Crack Growth Behaviors under Conditions of Oxygen

Diffusion-type Corrosion

Fig.5 shows the relationships between crack growth rates da/dN and crack
length 2a at a constant effective stress intensity factor range for small
fatigue cracks. As seen from these figures, the values of da/dN in labora-
tory air are independent on crack lengths at the fixed effective stress
intensity factor range. While for fatigue in sodium chloride aqueous solu-
tion, the values of da/dN show the crack length dependence at a constant
effective stress intensity factor range. The values da/dN increase with
decrease of crack length 2a. Accordingly, it was clarified that there is a
peculiar stress amplitude dependence and crack length dependence in the
small corrosion fatigue crack growth behaviors which are not observed in
fatigue in laboratory air and the through-thickness fatigue crack growth
behaviors. It should be necessary to consider this phenomenon mentioned
above from the electro-chemical viewpoint because the difference in situa-
tion between small fatigue cracks in laboratory air and those in sodium
chloride aqueous solution is only environment under which they propagate.

The oxygen-diffusion type corrosion works in neutral salt water. Therefore,

if enough quantity of oxygen was supplied to the corrosion fatigue crack tip
region, the corrosive reaction in the neighborhood of the crack tip region
are considered to be promoted and sustained and increasing corrosion fatigue
crack growth rate. In opposition, if the oxygen supply was not enough, the
corrosive reaction should decrease and stop and the degree of the accelera-
tion of crack growth rates due to corrosive environment should decrease.

The small crack growth behaviors were investigated in deaerated salt water
made by putting the nitrogen gas in the salt water. The stress amplitude
dependence observed in the aerated salt water was apt to disappear in the
deaerated salt water. This fact means that the acceleration of the crack
growth rates due to corrosive environment in the high stress amplitude
region are lowered by decreasing the amount of oxygen in the solution, while
the crack growth rates in the low stress amplitude region are not affected
by the amount of oxygen in the solution.

From the experimental results mentioned above, we can speculate the follow-
ing matters. When the crack size is small, the oxygen in a bulk solution
outside of the crack is transferred easily into the crack tip region during
a stress cycling and the crack growth rate increases with increase of the
amount of oxygen due to corrosive reaction near the crack tip. While, when
the crack size is large, it is not always easy for the oxygen in a bulk so-
lution to enter in the crack tip region, accordingly the amount of oxygen do
not affect the crack growth rate.

The Small Crack Growth Behaviors under Condition of Hydrogen

822
Evolution-type Corrosion

Fig.6 shows the relationship between crack growth rates da/dN and crack
length 2a at a constant effective stress intensity factor range for small
cracks in the acid solution. As seen from this figure, the small crack
growth rate shows a clear crack length dependence at a constant effective
stress intensity factor range. The crack growth rate in the short crack
size region is about 10 times larger than that in the long crack size
region. This acceleration is considered as follows. The chemical species
in bulk solution outside of the crack are transferred into the crack tip
region during a stress cycling by diffusion and convection caused by the
oscillation of the crack wall. Chemical species needed for the anodic dis-
solution at the crack tip are easily transferred in the short crack size
region compared to the long crack size region.

The Effect of the Severeness of Corrosive Environment on the Small

Crack Growth Behaviors

Fig.7 shows the relationship between (da/dN)cf / (da/dN)f and crack length
2a, where (da/dN)cf means the corrosion fatigue crack growth rate and
(da/dN)f means the fatigue crack growth rate in laboratory air. From this
figure, the acceleration of crack growth rate due to corrosive environment
increases with increase of the severeness of the corrosive environment, that
is, in the order of deaerated salt water, aerated salt water and acid solu-
tion. Furthermore, the crack size dependence observed in the small crack
growth behaviors become notable with increase of the severeness of the
environment.

CONCLUSIONS

The results obtained in the present study are summarized as follows.

(l)In laboratory air, crack growth rates for through-thickness cracks and
small surface cracks are prescribed well by the stress intensity factor
range. On the other hand, in sodium chloride aqueous solution and acid so-
lution, the crack growth behaviors for through-thickness cracks are basical-
ly the same as those in laboratory air, while for small surface cracks, the
crack growth rates increase with increase of stress amplitude at a constant
stress intensity factor range.
(2)The acceleration of crack growth rates due to corrosive environment at
high stress amplitude region observed in small surface crack growth behav-
iors become remarkable with increase of the severeness of the environments.
(3)The transport process of the chemical species between the bulk solution
outside of the crack and the solution near the crack tip region and the
electro-chemical reactions at the crack tip are considered to be concerned
with the peculiar crack growth behaviors of the small corrosion fatigue
cracks.

REFERENCES

Gangloff, R.P.(1985). Metall.Trans.,A, _16, 953.

Nakai, Y., et al.,(1989). Trans.Japan Soc.Mech.Engrs.Ser.A,55,No.516,1724.
Nakajima, M. and Y.Kato(1988). Trans.Japan Soc.Mech.Engrs.Ser.A, 54,No.
500, 656.
Roberts,R. and T.Rich(1967). Trans.ASME,Ser.E,34,No.3,777.
Raju,I.S. and J.C.Newmann(1979). Eng.Fract.Mech.,11,817.
 823
Ishihara,S. and K.Miyao(1988).Trans.Japan Soc.Mech.Engrs.Ser.A,54,No.508,
2075.

Table 1. Chemical compositions of the

material.
wt(e/0)
c Si Mn P 5
0.09 0.41 0.32 0.087 0.006
Fig.l Shape and dimension of the
specimen.
Table 2. Mechanical properties of the
specimen.
.,1*1
Yield Tensile (a) In airjhrough crock
strength strength Elongation
o 318MRi
327 M R i 527.7 M P Q 17.7 ·/. Δ 280MPa

•8

|i<f|
0.8i
(a) In air
0.6| ο:σ=315ΜΡα
3
·:σ=260ΜΡα| 1ö10 20 30 40 50
"§04
Stress intensities *K MFbmf2
S ,
»Q2| (b) in sdt water, ρΗ=β8
u
<t _L_ I Through crack
0
0.8i (b) In salt water
Er o315MFb
PH = 6. 8
irfl
in A238MRI
<
Q6 ο:σ=315ΜΡα
•:a=220MPd
■ *

ΐ i

0
0.8i
J_
_!_
(c) In salt water pH=1.1
<
o.e\ o:Q=315MPa
• :a=260MFb Ml'10 20 30 40 50
2OA|
Stress intensities ΔΚ MF&rrl/2

ta21 fid 1(c) lh salt water.pH=1.1

Through crock
0.5 1.0 15 20 25 o 315MFb
A20CMFb /
r^
2Q r
^ίί
►

Fig.2 Relations between crack aspect

ratio _As_ and crack length 2a.
v; 5 6 7Θ9Κ)
u
tr 20 30 40 50
Stress intensities^ MFbmP2

Fig.3 Crack growth behaviors for the

through-thickness cracks.
824

In air. Surface crack 10%

o a=315MRi.NQl E ( a ) In a i r . Surface crack
• ,No2
-:aKeff = 5 M F W / i
*>O=220MRi.No.1
a O=100MRi. No.1
y^ E
-: AKeff = 7 ···

ilöV
§ itf

(a)
2 3 4 5 6 7 8910 20 30 4050
Stress intensities ΔΚ MRanrl'2 ICH,, ■ ■ ' I "..I, ■

E(b) In sail waler, Surface crack

t pH=&8
*Keff=3MrW>
*Keff = 5 »
*Keff = 7 »

2 3 4 5 6 7 8910 20 30 40 50
Stress intensities *K MRarrl72
6
ιό | In saltwater pH=1.1. Surface crack

lol
Fig.5 Effect of crack length on crack
o g=315MFb.No.1
.■if _ · growth rates of the small

ilfft
,No.2 .
© - ,No3
~ Δ a=250MFb.No.1
surface cracks in laboratory
A .. .No. 2 air and sodium chloride aqueous
5 1Ö3 US- -■
□ a=200MFa, No.1
·· ,No.2 solution.
_ D ·· ,No.3
v C£100MRi,'No.1

2 3 4 5 6 7 8910 20 30 40 50 I n salt w a t e r , Surface crack

Stress intensities ΔΚ MRarrl'2 100
■ , o : p H = 1.1, Aerated
z • , o : p H = 6 . 8 , Aerated
A,*:pH=6.8,Deaerated

Fig.4 Crack growth behaviors for the

small surface cracks.

AKeff=7MFW4<
In sail water pH=1.1 . Surface crack

- · - tAKeff = 3^1^™^
-o-:*Keff = 5 -
-^:*Keff = 7 ··
\\t ' ' 101
2a m

Fig.7 Effect of the severeness of the

environment on the relation
between (da/dN)cf/(da/dN)f and
crack length 2a.

Fig.6 Effect of crack length on crack

growth rates of the small surface
cracks in the acid solution.
WS8g5

SMALL FATIGUE CRACK GROWTH BEHAVIOUR OF HIGH STRENGTH STEEL

UNDER VARIABLE LOADING IN DISTILLED WATER

M.NAKAJIMA*, Y.KATO** and T.SHIMIZU*

* Dept. of Mechanical Engineering, Toyota College of

Technology, Eisei-cho 2-1, Toyota, JAPAN
** Dept. of Mechanical Engineering, Daido Institute of
Technology, Daido-cho 2-21, Minami-ku, Nagoya, JAPAN

ABSTRACT

Small fatigue crack growth characteristics under variable loading were

investigated on high strength steel in room air and in distilled water. Two
types of loading sequence were used: one is repeated two-step variable
loading under load control and the other is Hi-Lo two-step loading at
constant stress intensity factor range. It was found that retardation
cycles depended strongly on both crack length and environment. Retardation
cycles in both environments increased markedly with increasing crack length
until it reached a constant value corresponding to long crack data, and it
was smaller in distilled water than in room air.

KEYWORDS

Corrosion fatigue; Chemically short crack; Variable loading; Small crack;

Retardation; High strength steel; Distilled water.

INTRODUCTION

Small fatigue cracks whose growth rates are markedly accelerated in

corrosive environments, even if crack length is long in mechanical and
microstructural sence, are termed chemically short cracks (Gangloff,1981).
In recent studies, it has been confirmed that SCC properties of small cracks
are responsible for the chemical crack size effects (Nakajima et al.,1990).
However, many studies have focused on the small crack growth characteristics
under constant load amplitude (Minoshima et al.,1989, Nakai et al.,1989),
while the growth behaviour under variable loading has not been studied. In
825
826
this study, the growth behaviour of small cracks is investigated under
repeated two-step variable loading and under Hi-Lo two-step loading in
distilled water.

EXPERIMENTAL PROCEDURES

The material used in this study was a high strength steel SNCM439 (AISI4340)
tempered at 200°C. The chemical composition (wt.%) is 0.40C, 0.27Si,
0.68Mn, 0.008P, 0.006S, 0.05Cu, 1.72Ni, 0.78Cr, 0.15Mo and balance Fe. The
0.2% offset yield strength and the tensile strength are 1519MPa and 1926MPa,
respectively.

Tests were conducted on a rotating bending fatigue testing machine at a

cyclic frequency of 1Hz in room air and in distilled water (pH:5.6—6.1,
dissolved oxygen:7.9^8.2ppm) under freely corroding condition. Two types
of loading sequence were used: one is
repeated two-step variable loading Q2 05 , l8
under load control and the other is a mm ° ' ' ~1 '
Q2 Ο.β I 1.7
Hi-Lo two-step loading at constant
stress intensity factor range. The 10° Distilled water
loading conditions of repeated two-
step variable loading are listed in
Table 1. Hi-Lo two-step loading tests
were performed at four crack lengths "ÖIÖ4
under the condition of AK H =HMPa/m
and AK L =7MPa/¥. For comparison, long
crack data (>5mm) were obtained using E
E
CCT type specimens under axial loading
at the same test conditions as small IÖ5 Long crack
cracks. Crack length was measured by
replicating method. The stress
intensity factor K for small surface o Small crack
cracks was calculated with the IÖ1 ΔΑ 250 MPa
analytical solution developed by O· 4 0 0 MPa
Newman and Raju (Newman,1979). 7777Z Γ/oNaCI sol.

_l I I I I I I I I
RESULTS AND DISCUSSION 10' 5 10 20 50
ΔΚ MPaym
Figure 1 shows the small fatigue crack
growth characteristics under constant Fig.1. da/dN-ΔΚ relations under
stress amplitude in distilled water. constant stress amplitude
in distilled water.
Table 1. Loading programs σ H <^> σ L Room a i r D i s t i l i e d water
of repeated two- (MPa) N„ NL N„ NL
step loading. 2
400 <F> 200 10 2
10 4
10 3x10 3
600 <=> 200 10 2
10 4
Ί0 2
3x10 3
 827
For comparison, long crack data are represented by solid line, and small
crack data in 1%NaCl solution are indicated by hatched band. In distilled
water, small cracks grow faster than long cracks in the region below
15MPafm. However, the growth rates of small cracks in distilled water
decrease in the region below lOMPafm" as compared to the data in 1%NaCl
solution. This is considered to be attributed to the difference in SCC
behavior of small cracks between both environments (Nakajima et al.,1990).

The relations between da/dN and Δ Κ under repeated two-step loading in room
air are illustrated in Fig. 2 (a) and (b). The loading conditions are given
in each figure. The solid line and the hatched band indicate long crack and
small crack data at constant stress amplitude, respectively. As shown in
Fig.2 (a), in low Δ Κ region small crack growth rates at lower stress level
tend to lie on the extrapolated line of hatched band, but the growth rates
decrease with increasing Δ Κ as compared to those at constant stress
amplitude. This behaviour is due to retardation in crack growth produced by
higher stress level. On the other hand, at higher stress level the
acceleration of growth rates takes place. The observed acceleration is
considered to be due to the increase of crack opening displacement (Jono et_
aj^.,1990). Similar behaviour for the tests under variable loading has been
reported by other researchers (Takashina et al.,1990). In Fig.2 (b),
remarkable retardation is observed in growth rates at lower stress level,

a mm
02 Q3 0.5 LO

3
ισ
3
\0 \— Room air Room air

/·

ICH ισΐ
.92

E ο0Φ E
E 10* E
6><S> ισ'
o L o n g crack
F<8 WA Small crack ■8
• OH ■ 4 0 0 MPa
ισ< NH = IO 2 cycles ισ'
• OH = 6 0 0 MPa
NH = IO 2 cycles
O OL = 2 0 0 M P Q o OL = 2 0 0 MPa
OOCCEO nO
N L = 10 4 cycles N L - 1 0 4 cycles

ia7J 5 10 20 50 ισ7 -<üCPönpxTflaift

10 20 50
ΔΚ ΜΡαΤπΤ Δ< MPaym
(a) 400MPa 4Φ 200MPa (b) 600MPa Φ> 200MPa

Fig.2. da/dN-ΔΚ relations under repeated two-step

loading in room air.
828
being due to higher stress level (a H =600MPa) than in Fig.2 (a). On the
other hand, small crack growth rates at higher stress level show a
considerable scatter, but are approximately consistent with the data at
constant stress amplitude.

Figure 3 (a) and (b) represent the relations between da/dN and Δ Κ under
repeated two-step loading in distilled water. The solid line and the
hatched band indicate long crack and small crack data at constant stress
amplitude in distilled water, respectively. In Fig.3 (a) and (b), the
retardation in crack growth at lower stress level is not observed below a
crack length of 0.5mm, and with increasing crack length the growth rates
decrease as compared with those at constant stress amplitude. On the other
hand, the growth rates at higher stress level show a significant scatter
with increasing crack length, and also decrease as compared with those at

a mm a mm Q3 0.5
i 1
10
1
L5
1
0.3 0.5 Q3 Q5 10 U5

iai- Distilled water 10 h - Distilled water

Long crack - L o n g crack .

Wfl Small crack T
IUfi Small crack r r t W ^ L ·

icr ισν
3>
o

Εΐσ'
1/Φ
i o I/
lief
Wf ··
> °<L· · · 0
o°SQ)»o O O
σ
•8 7D oo
ICH • ÖH = 4 0 0 M P a
NH = 102 cycles
ioi I I • OH = 6 0 0 MPa
N H " IO 2 cycles
o ÖL = 2 0 0 MPa o OL - 2 0 0 MPa
NL«3xlO s cycles N L = 3 X I 0 3 cycles

ia7J ia7J 5 10 20
_J L
5 10 20 50 50
ΔΚ MPav/m AK MPav/m
(a) 400MPa <Φ 200MPa (b) 600MPa <^> 200MPa

Fig.3. da/dN-ΔΚ relations under

0.1mm repeated two-step loading
i 1
in distilled water.

Fig.4. Crack branching under

repeated two-step loading
in distilled water.
(2C=1.299mm, a=0.575mm)
 829
constant stress amplitude. Figure 4 shows crack branchings and deflections
under repeated two-step variable loading in distilled water. As is
generally known, crack branching and deflection decrease the crack driving
force (Suresh,1983). Therefore, it is considered that the decrease and
scatter in crack growth rates with the increase in crack length are
attributed to crack branchings and deflections. Comparing Fig.2 (b) with
Fig.3 (b), it is found that retardation is more remarkable in room air.

The results above mentioned indicate that less retardation occurs in small
crack region and in distilled water. In order to clarify the effects of
crack length on retardation behaviour, tests were conducted under Hi-Lo two-
step loading at constant stress intensity factor range. Figure 5 (a) and
(b) show crack growth curves in room air and in distilled water,
respectively. Crack length indicated in the figure is the size at which
stress intensity factor range is changed. Hi-Lo two-step loading test
results in both environments show that retardation cycles (N D ), which is
defined as the number of cycles while crack being stationary, increases with
increasing crack length. Furthermore, retardation behaviour is not observed
at the smallest crack length of 0.3mm in distilled water. Retardation
cycles is represented as a function of crack length in Fig.6. It is found
that retardation cycles in both environments increases markedly with
increasing crack length until it reaches a constant value corresponding to
long crack data, and at a given crack length retardation cycles is smaller
in distilled water than in room air.

0.5 Distilled water

▼ ' a)a=n.7rrwn
a)o=0.3mm
EO.I
E
0.8 . t . ■ ■ , , .

■ · i . . . . | . . . 1 ' tl MPaym — 7 MPa/m

^
/ m — 7 MPaTm 1
.0.5 &£
1 ^__oo-o-<
Γ0.5 b)a ' 0.5 mm
II MPa · · 1 ♦♦'
w s
b) a 0.5mm
. . . . 1 . . . 1 ,1 §0.1 .♦ΓΓ. . . 1 . .

υ " 1 1 * "■" ■ "

. . 1

1.0 c)a=I.Omm

1 ♦
* ♦ cr„
O σ^
. 1 . . ... . 1 . i . . 1 . .
0.6
2 3 2 3
Number of cycles 4
N (xio ) Number of cycles N (xio4)

(a) In room air (b) In distilled water

Fig.5. Crack growth curves under Hi-Lo two-step loading.

830
CONCLUSIONS ICf
\-
Small crack growth behaviour under
variable loading was investigated in I04
room air and in distilled water. The
results are as follows:
(1) Under repeated two-step loading in
[—
room air, crack growth rates of small ' /
cracks at lower stress and higher 1 o Room air
ΙΟΊh—
stress levels decreased and increased
1 · Distilled water
respectively, as compared with those
at constant stress amplitude.
ΙΟΊ[-
(2) In distilled water, the decrease
in crack growth rates at lower stress , 1
J—m 1 ..! „.I... 1 1
level was not observed below a crack
0.2 0.5 I 2 5 10
length of 0.5mm, while crack growth
Crack length a mm
rates at higher stress level decreased
as compared with those at constant Fig.6. Relations between retardation
stress amplitude, which was attributed cycles (ND) and crack length.
to crack branchings and deflections.
(3) The retardation cycles in both environments increased markedly with
increasing crack length until it reached a constant value corresponding to
long crack data, and it was smaller in distilled water than in room air.
(4) Retardation is less remarkable in small crack region and in distilled
water.

REFERENCES

Gangloff,R.P.(1981). The Criticality of Crack Size in Aqueous Corrosion

Fatigue. Res.Mech.Lett..1,299-306.
Jono,M.,A.Sugeta and M.Sugihara (1990). Observation of Small Surface Fatigue
Crack Growth Behavior under Varying Loading Using Image Processing
Technique. Proc.JSME..No.900-50.31-36.
Minoshima,K.,T.Sugiyama and K.Komai (1989). The Influence of Crack Length on
SCC Crack Growth Behavior of High-Strength Steel under Dynamic Loading
Conditions. Trans.JSME.,Α55,689-696.
Nakai,Y.,H.Akagi,Y.Kitamura and K.Ohji (1989). Short Surface Crack Growth of
a High-Strength Low-Alloy Steel under Cyclic Loading in 3.5%NaCl Solution.
Trans.JSME.,A55,1724-1732.
Nakajima,M.,Y.Kato and Y.Kitaoka (1990). Corrosion Fatigue Characteristics
of Small Surface Cracks in a High Strength Steel. Proc.Int.Conf.Fatigue90,
2,1611-1616.
Newman,J.C.Jr.(1979). A Review and Assessment of the Stress-Intensity
Factors for Surface Cracks. ASTM STP687,16-42.
Suresh,S.(1983). Crack Deflection:Implications for the Growth of Long and
Short Fatigue Cracks. Metall.Trans.,14Α,2375-2385.
Takashina,N and H.Misawa (1990). Acceleration and Retardation of Crack
Propagation in High Strength Steel under Variable Loading. J.JSMS.,39,70-
75.
 WS8g6

FATIGUE CRACK INITIATION AND PROPAGATION IN TI-6AL-AV ALLOY

UNDER HYDROGEN CHARGING

Keijiro NAKASA, Masaaki HORITA and Jianping LIU

Faculty of Engineering, Hiroshima University,

Higashi-Hiroshima, 72Λ Japan

ABSTRACT

The effect of hydrogen charging on the fatigue crack initiation

and propagation of Ti-6Al-4-V alloy was investigated in 3% NaCl
and H p S O , w a t e r s . The n u m b e r of c y c l e s to f a t i g u e c r a c k
i n i t i a t i o n , N-, was d e c r e a s e d by h y d r o g e n charging when the
apparent stress intensity factor Δ K & is large, but when ΔΚ
is s m a l l Nj_ was i n c r e a s e d . The crack p r o p a g a t i o n rate was
d e c r e a s e d by h y d r o g e n charging. The r e s u l t s were d i s c u s s e d by
the hydride formation behavior.

KEYWORDS

T1-6AI-4.V alloy; fatigue crack; hydrogen charging; hydride.

INTRODUCTION

T i t a n i u m and T i t a n i u m a l l o y s h a v e many e x c e l l e n t m e c h a n i c a l
properties, such as specific strength, corrosion and corrosion
f a t i g u e r e s i s t a n c e , c o m p a r e d with s t e e l s and a l u m i n u m a l l o y s .
H o w e v e r , when the t i t a n i u m a l l o y s are exposed to hydrogen
environments, e.g. high temperature and high pressure hydrogen
g a s , H 2 S g a s , h y d r o g e n gas w h i c h is g e n e r a t e d by c o r r o s i o n
r e a c t i o n , the a l l o y s can be e m b r i t t l e d by the f o r m a t i o n of
h y d r i d e (Paton et a 1. 1 9 7 Λ ; N a k a s a et a 1. 1 9 9 0 ) . M o r e o v e r , many
structural members and machine parts usually receive repeating
stress, and there are some papers (Pittinato, 1972; Moody et al.
1982) which report the detrimental effect of hydrogen on crack
propagation velocity. In the present research, the fatigue crack
initiation and propagation of Ti-6A1-^V alloy were investigated
under the cathodically hydrogen charging condition in order to
examine the f a t i g u e c h a r a c t e r i s t i c s a s s o c i a t e d with h y d r i d e
formation.

831
832
EXPERIMENTAL METHOD

The Ti-6Al-AV alloy was solution treated at 1223K, which is

lower than the $ transus and higher than the martensite start
(Ms) temperature, for 3·6 ks, followed by aging at 823K for
14»4ks. The optical micros trueture consisted of a mixture of
primary granular a-phase and acicular a + 3 phases which were
changed from martensitic a' -phase during aging.

Fig.1. Experimental apparatus.

The fatigue test under hydrogen charging was carried out by

using a testing machine shown in Fig.1. The CT-type notched
specimen was immersed into 3% NaCl or HoSO, aqueous solution (1
Nol) kept at 303K. The specimen surface was coated by scotch
tape except the crack propagation region of 8mm width, and the
current density, i c , of 500, 2000 and 3000A/m 2 was applied
between the specimen and an anodic Pt wire. The tension-tension
repeating stress with stress ratio R = K m i n / K m a x = 0 · ' ! was applied
just after the immersion and instantaneous hydrogen charging of
specimen. Because the stress intensity factor K can not be
defined for notch, the apparent stress intensity factor K was
used to express the crack initiation behavior from notch tip by
substituting the notch length for the crack length. The
frequency of repeating stress was 0.1Hz for the fatigue test
under charging and 1Hz for the test in air, respectively.

The number of cycles to crack initiation, N · , was obtained by

extrapolating the measured crack length a vs. number of cycles N
curve to a=0mm, while the crack propagation rate da/dN was
calculated from the gradient of a vs. N curve over the crack
propagation distance of at least 3mm after the crack growth of
2mm from notch tip to avoid the effect of repeating history
before crack nucleation on the crack growth hereafter.

In order to analyze the hydride formation on notch and specimen

surface, a micro-area X-ray diffraction apparatus (JE0L-MAP2,
beam diameter was 100 micron meter) with a position-sensitive
proportional counter was used.
 833
RESULTS AND DISCUSSION

Figure 2 shows the relationships between range of apparent

stress intensity factor Δ Κ & and the number of cycles to crack
initiation N. in HoSO, water. The N^ is smaller in I^SO, water
than in air where ΔΚ is large, but when AK.a is small the N^
is rather long in H 2 S0y water than in air. There seems to be
only a small effect of i c on the N ^ The similar tendency was
observed for the specimen tested in NaCl water. Figure 3 shows

Time, 11 s
60.
10* 10* 106
i ' r-
In IN H2S0«water
O50h
Θ /c= 500 A / m 2
Φ /c=2000A/m2
<K>
• /c=3000A/m2
\ Θ · fr\ In a i r
°2
σ£2θ|- fl=0.1 r<»-_

f =0.05 Hz

_L J_
102 103 10* 105
N u m b e r of c y c l e s

Fig.2. Relation between range of apparent

stress intensity factor and number of cycles.

I A«

4Ju
KKJ
500
-300
40

30 40
29
1000 h
ULX.
500 30 40

40 A0
T ILA
30 40 (b) 30 40

Fig.3. M i c r o - a r e a X - r a y d i f f r a c t i o n a n a l y s i s , ( a ) ΔΚ&
=^8MPam 1 / 2 , i =2000A/m 2 , c h a r g i n g time t c = 1 5 k s ,
(b) Δ K=20MPam^ / 2 , i =3000A/m 2 , t = 2 0 0 k s .
834
the typical examples of micro-area X-ray diffraction analysis,
where a phase(hcp) is the titanium phase ( the peaks from
3 phase are very weak), and γ (TiH-| c c _-| QQ ; f cc) and öphases
(TiHojfct) are the hydrides· According to" ?he Fig.3(a), when
charging time is short, there exists some amount of hydride on
side surface of specimen and notch corner but there is no
detectable hydride near the center of notch root. The reason
will be perhaps that the hydrogen gas bubbles stayed in the
center of notch root and prevented the solution of hydrogen
atoms into material. When the hydrogen charging time t c is long
or N^ is large (Fig.3(b)), on the other hand, a large amount of
hydride was formed also near the center of notch surface.

There seems to be two factors which affect the fatigue crack

initiation under charging condition. One is the destruction of
brittle hydride phase due to the stress repeating, which will
decrease the fatigue crack nucleation life by the formation of
micro-crack as a stress concentrator. Another is the generation
of compressive stress near notch surface by the formation of
hydride, which will prevent the repeating slip and prolong the
fatigue crack initiation life. Because the formation of hydride
results in about 15% of volumetric expansion under stress free
state, the compressive stress will be large. These two factors
will compete each other depending on the charging time, i.e. the
decrease in N^ at larger ΔK will be explained mainly by the
destruction of hydride at notch corner ( not the center of notch
r o o t ) , while the increase in N · at smaller Δ K w i l l be
attributed mainly to the existence of compressive stress due to
the formation of a large amount of hydride and the cracking of
hydride on notch surface will be difficult under such a small
repeating strain.

Figure 4- shows the relations between range of stress intensity

factor Δ K and crack propagation rate da/dN in I^SO, water.
The da/dN are smaller in I^SO, water at larger ΔΚ range than
in air. In order to find the reason, the crack closure
characteristics was examined. Fig.6 shows the relation between
range of stress intensity factor Δ K and crack opening ratio
U= K
( max- K op)/( K max- K min)= A K eff/ Δ K obtained in air. and in H 2 S0^
water from the relation between load and strain which was
measured by the strain gage stuck in front of crack tip, where
K is the stress intensity factor when the crack opening
starts. The opening ratio is smaller under charging condition
than in air, especially when ΔΧ is large. By using these
values, the relation between ΔΚ and da/dN were replotted as
the relation between the effective range of stress intensity
factor, A ^eff» anc* <*a / d N. Fig.5 gives the results, which
shows that the both data in air and in HpSOy water lie on the
same straight line. Thus, the decrease in da/dN under hydrogen
charging is explained by the existence of a certain kind of
closure phenomenon.

In order to clarify the reason for the crack closure, the

fracture surface was analyzed by the micro-area X-ray
diffraction method, but no hydride was detected on the fatigue
fracture surfaces, perhaps because the hydrogen bubbles which
stayed between narrow crack walls prevented the sufficient
amount of solution of hydrogen atoms for the formation of
 835
hydride. Next, because there was actually hydride on specimen
side-surface as was shown in Fig.3, after removing the specimen
surface by more than 0.5mm, which was the maximum depth of

IQ- 10"

In IN H2SO« water
ff=0.1 ^
O /c= 500 A / m 2
9 ,c = 2000 A / m 2 t -O- I n air 9
• /c = 3000 A / m
2
/

—_ n air / φ · |io-31
|_ /
o
X» h
Φ
o ,Φ

JlO"
σ
L '· I10- I
o
In IN H2SO« water

Φ /c= 5 0 0 A / m 2
oa /?= 0.1 σ
| Q /c=2000 A / m 2
/= 0.05 Hz
• /c=3000 A / m 2
o
o
\0 1 1 1 1 L ισ'ΐ 1 1 1 1 -U
10 20 30 40 50 60 10 20 30 40 50 60
Range of stress intensity factor Range of effective stress
ΔΚΙ MPa/m intensity f a c t o r , ΔΚ,ηΙ MPa/m

Fig.4· Relation between range Fig.5. Relation between

of stress intensity effective range of
factor and crack stress intensity
propagation rate. factor and crack
propagation rate.

1.0.

o 0.9|
o
9 0.8|
In IN H2SO4 w a t e r
• 0.7| fl=0.1 O /c= 500 A/m2
o
-O- In air Q /c=2000 A/m2
i 0.6| • /c=3000 A/m2
\_
o
0.5l _L I JL
20 30 40 50
Range of stress intensity factor
ΔΚ I M P a / m

Fig.6. R e l a t i o n b e t w e e n r a n g e of s t r e s s intensity
f a c t o r and c r a c k o p e n i n g r a t i o .
836
hydride, the crack closure were measured again. The increase of
crack opening ratio was observed by the removing of the
hydride, which means that the existence of "hydride-induced
crack closure" near specimen surface is one of the important
reason for the observed crack closure phenomenon. But, the crack
opening ratio U does not perfectly recover to the U in air even
after the removal of hydride, especially when ΔΚ is large where
hydride formation is small because of the shorter charging time
or crack propagation time.

According to the fractography, the fatigue fracture surface in

air reveals striation pattern in primary granular α-phases. On
the fatigue fracture surface under charging condition, however,
the striation pattern is not clear and the relatively deep and
slender grooves are observed, which may be formed by the
intergranular de lamination of acicular a and 3 phases. This
grooving can result in the "roughness-induced crack closure"
with an additional effect that the concave and convex portions
of fracture surface were expanded by the solution of hydrogen
atoms and they can never be fitted again each other during
unloading. Thus, the "hydride-induced crack closure" near
speciaen surface and the "roughness-induced crack closure" on
fracture surface are the main reasons for the crack closure
typical for the crack propagation under hydrogen charging.

CONCLUSION

The fatigue crack initiation and propagation behaviors were

investigated on the T1-6AI-4.V alloy under hydrogen charging in
3% NaCl and HpSO, waters. The results obtained are as follows:
(1) The number of cycles to crack initiation N ^ is smaller
both in NaCl and HnSOy waters than in air when the range of
apparent stress intensity factor Δ K is large, but it is longer
when ΔΚ& is small. The reasons will be that the hydride formed
on notch corner fractures to nucleate micro-crack when AK a is
large and the compressive stress due to the hydride formation
suppresses the crack initiation when AK a is small.
(2) The fatigue crack propagation rate da/dN measured in
both environments are smaller than that in air. The relations
between the effective range of stress intensity factor ^^ e ff
and da/dN lie on one straight line independently of the
environments. The main reason for the above result appears to be
the hydride-induced crack closure near specimen surface.

REFERENCES

Moody,N.R. and W.W.Gerberich(1 982). The effect of hydrogen on

fatigue and dislocation behavior of an a/3 titanium alloy.
Fatigue of Engineering Mat. & Struc, 5_, 57-70.
N a k a s a,K., K.Kiyose, and J.Liu(l990). Relation between bending
strength and hydride formation in hydrogen-charged Ti-6A1-4.V
alloy. J. Japan Inst. Metals., 54, 532-538.
Paton,N.E. and J.C.Williams, Ed. by I.M.Bernstein and
A.W.Thompson(l974·)· Effect of hydrogen on titanium and its
alloys. Hydrogen in Metals, ASM, 4.09-4-31.
Pittinato,G.F.(1972), Hydrogen-enhanced fatigue crack growth in
T1-6AI-4.V ELI weldments. Metal. Trans., 3A, 235-2Λ3-
 WS8g7

ON CORROSION FATIGUE OF FRICTION WELDED BUTT JOINT

H. NAKAYAMA*, Y. OH-UE*, Y. MUKAI** and K. OGAWA***

* Faculty of Junior College of Automobile Industry, Osaka Sangyo

University, Nakagaito, Daito-shi, Osaka, 574, Japan
** Faculty of Engineering, Osaka University, Suita-shi, Osaka, 565,
Japan
*** College of Integrated Arts and Science, University of Osaka
Prefecture, Mozu-umemachi, Sakai-shi, Osaka, 591, Japan

ABSTRACT

The present paper describes the characteristics of the fatigue strength and the
fatigue life distribution of S25C/S25C friction welded butt joint in artificial seawater.
It is revealed that the corrosion fatigue strength of the joint shows a trend to take the
lower value than that of the base metal in long life region, presumably depending on
high sensitivity of the material near the weld interface to aggressive environment.
And furthermore, statistical evaluation of corrosion fatigue lives indicates that, in the
case of the joint, the lower is the stress level the smaller is the scatter of fatigue lives
in contrast to the case of the base metal. Such fatigue behaviors composed of two
phases seem to be affected by the corrosion pits generated near the weld interface.

KEYWORDS

Fatigue strength; fatigue life distribution; friction welded joint; corrosion fatigue.

INTRODUCTION

Friction welded butt joints have come into wider use as structural elements;
propeller shaft, valve shaft of automobile structure and so forth. But, the reliability of
this type of joint has been supported only by empirical knowledge accumulated up
to the present, and the problem on fatigue behaviors of this joint remains open still.
It is an urgent theme to systematize the strength and the fracture processes of
friction welded joints in fatigue to establish a valid design concept taken into
account of their service conditions(Nakayama et al., 1981,1883, 1987, 1989).

Corrosion fatigue properties also must be discussed, for some of the joints are used
under pollutive environments. Therefore, corrosion fatigue tests in artificial
seawater were carried out on friction welded butt joint specimen composed of a
structural carbon steel, JIS.S25C. And the results were discussed from two points of
view; one was the characteristics of fatigue strength and another was the fatigue life
distribution.
837
838

Ν=3660 rpm

P 2 =100MPa

2 2 t2=10sec
Ρ1 =60MPa/ Total upset; 62=8.7mm
.Ε <Λ

3°- .8sec
Heating upset; δ^δ.θιτιηι
' P ,_; Preheating pressure
ph
Time t
Fig. 1. Schematic illustration of friction welding process

50
-IHB 80
130
Weld interface
Fig. 2. Shape and sizes of specimen

MATERIAL, JOINT AND EXPERIMENTAL PROCEDURE

0.23%C carbon steel (JIS. S25C) supplied as hot rolled bars with a diameter of
16mm was used as an experimental material. These rods were friction welded
under welding conditions illustrated in Fig. 1 after the annealing treatment of 870C,
Ihr., F.C. The joint efficiency in the meaning of static tensile strength was confirmed
to exceed 100% ; the breaking strength of the joint was 587MPa and that of the base
metal after the annealing treatment was 465MPa. Then, the joints were machined to
the spcimen shape indicated in Fig.2, where the weld interface was just at the notch
root. Stress concentration factor due to the notch is 1.39 under bending.

A macrophotograph of the joint shown in Fig. 3 indicates the weld interface and the
heat affected zone clearly. Figure 4 shows the hardness distributions near the
interface measured with a micro-Vickers hardness tester. This indicates that the
hardness at the location corresponding to the notch root is about twice of that of the
base metal. Then, the residual stress distribution in longitudinal direction on the
interface determined by X-ray diffraction profile, shown in Fig. 5, indicates that the
surface layer is highly compressed. Figures 4 and 5 suggest that the fatigue
strength of the joint is much higher than that of the base metal.

Cantilever type rotating bending fatigue testing machine equipped with a corrosion
chamber was used to conduct a series of experiments. Rotating rate in ordinary
atmospheric environment is about 2200 rpm and that for corrosion fatigue tests is
about 620 rpm. Fatigue tests were censored at 10 7 stress cycles. In corrosion
fatigue tests, circumferential U-notch was located just at the center of corrosion
chamber with the capacity of 600 cc, where the temperature and the circulating
volume of the artificial seawater were 283±2K and 340 cc/min, respectively.
 839

30 l·

15mm
J 20
Fig. 3. Macrophotogragh of joint
'co'
Q.

S- i o -

-10h
!200♦ · β CO
Λ Δ ^Δ ΔΛ Α
φ θ ^ Δ Δ ^ ΔΑ Φ -20
Οο OB
• C
£ 150 ίοθ-
y
Ü
> S°*eo8 -30

ό
Ö 100 I I I I I I -40 h
0 5
Distance from the weld interface d (mm)
Fig. 5. Residual stress
Fig. 4. Hardness distribution distribution on
near weld interface weld interface

EXPERIMENTAL RESULTS AND DISCUSSION

Distribution of Corrosion Pits in Artificial Seawater

Prior to fatigue tests, corrosion pit distribution was investigated by immersing both
the joint and the base metal plate specimens into artificial seawater, and the results
are shown in Fig. 6. The number and the depth of corrosion pits were observed on
four locations of the width of 1 mm, designated as A, B ,C and D in Fig. 6. The
observations indicate the generation of a large number of deep pits on the side
edge area "D" normal to the radial direction, in other words, the plane normal to the
fiber flow direction in the forging stage with the pressure P2 as illustrated in Fig. 1.
And this area corresponds to the notch root area of the joint specimen. On the other
hand, the generation of corrosion pits was scarcely observed for the base metal.

Results of Fatigue Tests

Results of a series of fatigue tests are shown in Fig. 7. S-N curves in this figure are
840

• (D)|

•A 40
1 *1
0
• (D)

• o

•
Ü 0
^Γ
* K
1 ·
i
o 8• 1O n Λ ^o o o
• ol
QLO

•••1
z (C) (C)
E 20
δ.
o O °On*n o oo
j§ 40
E *·• · (B)
z E (B)
| 201 ♦ ^4
• •
1
0c
> υ-φ ·
OoL (A)
^ϋ
o
n(
Γσ***« $fio
0 1 2 3 0 I 2
Distance from the weld interface d (mm) Distance from the weld interface d (mm)

Fig. 6. Observations of corrosion pits; locations for observation(left),

number of pits(center) and maximum depth of pits(right).

- O - Base material
- ♦ - Friction-welded T

232

1 * 2 2 2

ΤΓ2« i
>& 2 V rI^-3
<ferl \ 2 JJ In ordinary atmospheric
-o T] environment ·—
-o -Cm

\
IfS^ F
N n^2
\
'Tf \\ x

1 i
I *
! U?2 1\ ^ 2°^· · \
2 22
■M
—- - ■O
\
2 2
\
k.

! 1 1 II v 2
iv U
25

irk RW £rL&
In artificial seawater
23 2 2 2 M 1 0

MINI!
o5 I06 I0 7
Number of stress cycles to failure N

Fig. 7. S-N curves in ordinary atmospheric environment

and in aritificial seawater.
 841

Number of stress cycles to failure N

Fig. 8. Fatigue life distributions in ordinary atmospheric environment.

99.9
Π Ra«P matprial
99
- · Friction-welded ^ -<
<£ 90 i )i u

50

r
r^ # J¥ J L
/w ?l °A°/ • <
Ξ 10
5
n 5 Ϊo
,OQ~" o

In artifici al sea wat er

1
I0Ö 10'
Number of stress cycles to failure N

Fig. 9. Fatigue life distributions in artificial seawater.

those for P = 50%, where P is the fatigue failure probability discussed in the
following section. Results in ordinary atmospheric environment shown in upper half
part of Fig. 7 indicate that the fatigue strength of the joint is higher than that of the
base metal in a whole experimental range. But the joint specimen shows the larger
scatter of fatigue lives than that of the base metal specimen, presumably depending
on a slight difference in metallurgical situation near the weld interface. Fatigue
strengths in artificial seawater shown in the lower half part of Fig. 7 indicate that
though the fatigue strength of the joint specimen is higher than that of the base
metal specimen at relatively low stress cycles range, fatigue strengths of both
specimens take almost the same value in high stress cycles range near 107 cycles.

The corrosion fatigue behaviors of the joint clarified in this study gives the following
suggestion; the fatigue strength of the joint becomes lower than that of the base
metal even in low stress cycles region when loading frequency is less than 620
842
rpm because of the time-dependent property of corrosion fatigue. This is one of the
important fatigue properties of the friction welded butt joint.

Distribution of Fatigue Lives

Characteristics of fatigue life distribution are evaluated by assigning 10 or more

specimens at several stress levels, and results were discussed by assuming that
the fatigue life distribution obeys 3-parameter Weibull distribution function with the
saturated fracture probability, and failure probability P was determined by mean
rank method.

Distribution of fatigue lives in ordinary atmospheric environment shows that, in the

case of the base metal specimen, the scatter of fatigue lives becomes large in
accordance with the increase in fatigue life as a common trend of metallic materials.
But such a trend is scarcely observed for the joint specimen and the scatter is large
even at high stress level. Figure 9 indicates different distribution characteristics from
those in Fig. 8; (1) the scatters of fatigue lives at respective stress levels are almost
the same and are smaller than those in ordinary atmospheric environment in the
case of the base metal specimen; and (2) the smaller scatter is observed for the
joint specimen in comparison with that for the base metal as a whole, even at low
stress level.

CONCLUSIONS

Major conclusions obtained in this study are summarized as follows:

(1) Results of the immersion tests to investigate the generation of corrosion pits
indicated that a large number of deep pits generated on the plane normal to the
fiber flow direction, which corresponds to the surface of notch root of fatigue
specimen.
(2) Friction-welded joint specimen showed abrupt decrease in fatigue strength in
artificial seawater when compared with the results of base metal specimen.
(3) Though the joint specimen showed the larger scatter of fatigue lives than the
base metal specimen in ordinary atmospheric environment, the lower is the applied
stress the smaller is the scatter of fatigue lives of the joint specimen in artificial
seawater.

REFERENCES

Nakayama, H., Y. Oh-ue, K. Ishii and K. Ogawa (1981). Statistical fatigue strength
characteristics of friction welded butt joint specimen composed of 0.45%C carbon
steel. Jour. Soc. Mat. Sei., Japan. 3Q, 180-186. (in Japanese).
Nakayama, H., M.Hanano, Y. Oh-ue, K. Oh-hira and K. Ogawa (1983). Statistical
fatigue characteristics of friction-welded butt joint composed of commercial base
pure aluminium. Proc. 26th Japan Congr. Mat. Res., 147-153.
Nakayama, H., M. Aritoshi, K.Okita and W.Kishimoto (1987). Fatigue strength and
fatigue crack growth characteristics of SUS304/SUS304 friction welded butt joint.
Proc. 30th Japan Congr. Mat. Res., 99-105.
Nakayama, H., Y. Oh-ue, K. Ogawa and A. Hasui (1989). Fatigue strength
characteristics of S35C/S35C friction welded butt joint. Proc. 32nd Japan Congr.
Mat. Res., 75-82.
 WS8g8

THE ANOMALOUS BEHAVIOR OF FATIGUE CRACK GROWTH UNDER

CATHODIC PROTECTION IN SEAWATER

WU XINHUA ZHU ZIYONG KE WEI

Institute of Corrosion and Protection of Metals

Academia Sinica, Shenyang , 110015 , China

ABSTRACT

In ocean engineering , cathodic polarization is usually applied to protect corrosion . CaC0 3 and
Mg(OH)2 deposits will occur in certain protective potential ranges and affect crack growth process .
The distribution of deposit and its retarding effect on crack growth have not been quantified yet. In
this paper , the behavior of crack growth under cathodic protection in sea water was investigated;
deposit thickness distribution and its variation with crack growth are shown . Moreover , a new
model based on deposit growth law is proposed which explains the anomalous crack growth behav-
ior under cathodic protection in sea water .

KEYWORDS

Fatigue crack growth ; sea water ; cathodic protection ; deposits ; retardation .

INTRODUCTION

Marine structure is often cathodically protected . However , because of the existence of

Ca"1-1", Mg** ions in sea water , CaC0 3 , Mg(OH) 2 deposits will occur in certain potential range
and therefore modify the crack growth process . R. Van et al. ( 1983 ) and Hiroyuki Masuda et
al. ( 1988 ) studied the effect of the corrosion product wedging in the crack on the crack growth
behavior of a CT specimen by the Back Face Strain method . However, it is difficult or even impos-
sible to measure the Back Face Strain, e. g. in solution , high temperature environments etc . . W. H.
Hartt et al. ( 1985 ) tried to overcome this problem with a "deposit growth law" and proposed a
criterion that deposits have an effect on crack growth only when the deposit thickness is equal to or
larger than the minimum half crack tip opening-displacement . Up to now , although the studies
are based on the effects of deposits , the effects of the distribution of deposit on variations in crack
propagation are still not clear . In this paper , the results of fatigue experiments in sea water will be
discussed with regard to the cathodic polarization and deposit thickness distribution . Moreover , a
new model based on a "deposit growth law" is proposed , which explains the anomalous crack
growth behavior relative to cathodic polarization at each of the potentials .

EXPERIMENTAL

WFG36Z steel and A537 Cl 1 steel were used for fatigue test . Their chemical compositions (in
843
844

Fig. 1 . Crack growth rate curves at different potentials

(a) for WFG36Z steel (b) for A537 Cl 1 steel

wt%) and mechanical properties were as follows :

WFG36Z: C 0.16 , Si 0.34 , Mn 1.36 , P 0.009 , S 0.018 , Cu 0.08 , Al 0.026 , Nb 0.015 ;
σν 401.8(MPa) , στ 549.8(MPa), δ 34.0(%) , ψ 67.5(%);
A537C11: C 0.13 , Si 0.46 , Mn 1.48 , P 0.012 , S <0.05 , Cu 0.018 , Mo 0.18 , V 0.057 , Cr 0.04 , ay
365(MPa), στ 548(MPa) , δ 32.8(%) , ψ 70.5(%) .
The corrosion fatigue tests were carried out on a servohydraulic fatigue machine in load control.
Pmax= 16 KN , Pmin = 0 . The stress waveform was sinusoidal and the frequency was 10Hz . The single
edge notched specimens were 290mm in length , 36mm wide and 6 mm thick . Crack length was
measured with a travelling microscope in air; or with potential drop technology in solution .

A specimen bath was attached to the testing machine , in which circulated artificial sea water was
made according to ASTM DH 1141—75 . In the cathodic protection test, the specimen was coverd
by epoxy resin and the centre bared width was 7 mm for crack growth .

RESULTS

Figure 1(a) shows the influence of cathodic potential on crack growth rate of WFG36Z steel. When
the protection potential moves negatively from —800 to —850 mV ,the crack growth rate decreases .
When the potential moves further to —900 mV , the growth rate decreases in the initial stage of crack
growth and then has a steep increase . When the potential reaches -950 mV , the growth rate rises
again and is much larger than that at —900 mV or —850 mV . When the potential is rather more nega-
tive , eg . —1500 mV , the crack growth rate returns to a very low level and the general behavior of
propagation is the same as that at -900mV .

Figure 1(b) shows the similar influence of cathodic potential on crack rate of the A537 Cl 1 .

Figure 2 shows the influence of environment on crack growth rate; and the results in air , in freely
corroding condition , and at potential of-850 mV are compared . In ocean engineering , the protec-
tion potential is usually -850 1000 mV , and our results indicate that -950 1000 mV is a sen-
sitive fracture range for these materials in sea water . Repeating tests also show that the proper pro-
tection potential range is in the ranges of-800 to -900 and -1100 to -1500 mV . Therefore the shift
of protection potential in engineering must be controlled .

The effects of sea water on crack growth rate are different from that of 3.5% NaCl solution which
are shown in Fig. 3 . In 3.5% NaCl solution , the crack growth rate simply increases with Δ Κ and
shows the usual characteristic of fatigue crack growth . While in sea water , the growth process is
more complicated and the crack growth rate in the initial growth stage is much smaller than that
 845

Fig. 2 . Crack growth rate curves Fig. 3 . Crack growth rate curves in
under different conditions 3.5% NaCl and sea water

in 3.5% NaCl. In the later stage , the growth rates in both solutions become similar . The results
clearly indicate that the calco-magnisium deposits retard crack growth in sea water and the study of
the cathodic protection problem with a 3.5% NaCl solution instead of sea water is not very suitable .

DISCUSSION

Mechanism of crack growth

In sea water, hydrogen ( Andreson , 1981 ) and calco-magnisium deposits ( Philipponneau,

1981) will be produced in certain cathodic potential range . The hydrogen may cause hydrogen
embrittlement and accelerate crack growth ; on the contrary , calco-magnisium deposits may wedge
in a crack and decrease the effective Δ Κ , and hence retard crack growth .

Cottis R. A. ( 1985 ) studied the hydrogen permeation in a 3.5% NaCl solution at different potentials
and found that when the potential was more negative than -900 mV , the hydrogen permeation cur-
rent steeply increased . Theory and experiment verified that the direct diffusion of hydrogen is driven
by the hydrostatic tensile stress gradient ( Marichev , 1982 ) . Its equilibrium concentration C de-
pends on the initial C0 , i. e. C = C0 exp (σά\ / 3RT) , where σή is the sum of the main stresses ,
and v is the partial molar volume of hydrogen in steel . The idea of the ''critical concentration" of
hydrogen , which leads to the loss of the cohesive bond in the lattice , was also developed . At the
corrosion fatigue crack tip , if R > 0 , an average axial stress field always exists and makes the
hydrogen diffuse toward the front of the crack tip . Under constant load , the more negative the pro-
tection potential, the larger the initial concentration C0 is , and the easier hydrogen embrittlement is.
However , When pH > 8.3 and 9.3 ( Philipponneau, 1981 ), CaC0 3 and Mg(OH)2 will precipitate,
and the more negative the potential, the larger the amount of deposits will be accumulated on crack
walls and hence cause the effective minimum stress to increase and the effective Δ Κ to decrease .

Within the potential range of —850 to —900 mV , the crack growth retardation caused by depos-
its dominates the process of growth . However , a more negative potential may lead to hydrogen
embrittlement and the growth rate curves show a platform stage at -950 mV and -1000 mV . The
deposit not only decreases the effective Δ Κ but also restrains the diffusion of solution ( including
H + ) toward the crack tip and thus reduces the effect of hydrogen . All these factors will result in a
repid decrease in crack growth rate , e .g . for the -1250 mV and —1500 mV cases .
846

Fig. 4 . Schematic of crack faces Fig. 5 . The distributions of deposits

and deposits on crack wall at different
crack length

The thickness of deposit film will approach saturation as time goes on and the hydrogen diffusing in-
to the crack tip also becomes less and less with crack growth rate . Thus only the mechanical factor
controls the propagating crack , and the growth rates under different electrochemical conditions tend
to be the same .

In the later stages of crack growth , the plastic zone near the crack tip becomes larger . This results in
the blunting of the crack tip and zigzag path which makes the measuring error increase .

The distribution of deposits on crack walls

At a -850 mV cathodic protection potential, the calco-magnesium deposits growth law in sea water
is Y = 6.28x 10~3 logt - 2.6 x 10"2 (mm) ( Hartt et al.y 1985 ) , where Y is deposit film
thickness(mm); t is the time for which deposits have grown (sec .) . As shown in Fig. 4 , the deposit
film thickness at location X is:

Y(x) = 6.28 x 10"3 log{[N(a)-N(x)] / f} - 2.6 x 10~2 (x = 0 - a)

where N(a) is the cycle number when crack length is a(mm) , N(x) is the cycle number when crack
length is x (mm) . In Fig. 5 , dashed lines are Y(x) vs x (x = 0 ~ a) plot. If the abscissa is thought to
be the crack wall . Y(x) is the deposit film distribution on the crack wall when crack length ap-
proaches a(mm) . The solid lines indicate the crack centre lines at closure .

The distribution of deposits in Fig. 5 shows that it is not the deposits at the crack tip that retard
crack growth as reported in the literature but the deposits at the crack walls do it . In fact, at the
crack tip , the growth time of deposits is so short that the deposit film is very thin , may even not be
produced . Therefore the retardation can only be caused by the wedging of deposits on the crack
walls.

The Effect of Deposits

We start from an assumption that the deposit film is compact and hard enough that crack closure
would not influence the film thickness at any point in the crack and we consider it as the threshold
condition of crack growth retardation that the deposit film thickness Y(x) equals the crack minimum
half opening-displacement V ^ x ) .
 847

Fig. 6 . Variations of Kmax and Fig. 7 . Crack growth rate as a

Kmincfl(x) with crack length function of intensity factor
ranges Δ Κ and Δ Κ Λ

As mentioned above , the significant point for crack closure is the tangential point of the crack centre
line ( solid lines Vmin(x) in Fig. 5 ) to the distribution curves of deposits(the dashed lines Y(x)) . It is
also clearly shown in Fig. 5 ( at —850 mV ) that all the tangential points in the whole process of crack
growth are near the point a = 5.14 (mm) , at which the deposit film thickness just equals the maxi-
mum, corresponding to the longest time of deposit growth . Evidently it is also the crack length at
which cathodic protection has been applied .

It is worth noting that not all effective points necessarily correspond the thickest points of film . A
more negative potential or a faster growing of the deposit will result in the effective point moving
towards the crack tip . If the film thickness at any location reachs the maximum half opening—dis-
placement , the crack growth will be stopped completely .

According to D. Brock's report ( Hartt et al., 1985) , a crack produces the minimum half
opening-displacement Vmill(x) at location X , here

v
m!BW = ^m5n(x)(a2-x2)l/2/E (1)

thus

^ ^ « = ν„1η(χ)Ε/(32-χ2),/:! (2)

the effective minimum stress intensity factor Kmiacff (x) :

K . (x) = σ . Jx) V^a~ (3)

miaeffv ' mineffv ' v
'

The calculated Kmineff (x) for different crack lengths and Kmax are shown in Fig. 6 .

It is clearly shown that AK c f f has a minimum at certain crack length , that is to say , the retarding
effect of a deposit on crack growth reaches a maximum , and the crack growth rate reaches a
848
minimum, which is clearly shown by the d a / dN — Δ Κ curve in Fig. 7 . Replacing Δ Κ with ΔΚ βίΓ
calculated by the proposed model, a new growth rate curve , d a / d N ~ Δ Κ ^ , is shown by the
solid circle curve . It is found that the d a / d N vs Δ Κ ^ curve represents the normal corrosion fa-
tigue crack propagation characteristic . This means that the model properly reflects the eflect of the
deposit.

CONCLUSION

Both WFG36Z and A537 Cl 1 steels have the same optimum protection potential range , i. e. -800 to
-900 mV . The range of-950 to -1000 mV is harmful for crack propagation .

The thickness of the deposit film in a growing crack decreases from the crack mouth to the crack tip .
When the crack closes, the deposit film on both walls increases the effective minimum stress intensity
and retards crack growth .

The anomalous behavior of crack growth is due to the effect of deposit and can be explained by the
model proposed in this paper .

REFERENCES

Van , R . , H . L . Ewalds , W . A . Schultz and A . Punter (1983) . Anomalous fatigue crack growth
retardation in steels for offshore application . In: Corrosion Fatigue, ASTM STP801 ( T . W .
Crooker and B . N . Leis , Eds .), pp64-80 , American Society for Testing and Materials .

Masuda Hiroyuki , Saburo Matsuoka , Satoshi Nishijima and Masuo Shimodaria (1988) . The role
of corrosion in fatigue crack propagation for structural alloy in 3% NaCl solution. Corrosion
Science, 28,433-447 .

Hartt, W . H . and Wei Mao (1985). Growth rate of calcareous deposits upon cathodically polarized
steel in seawater . In: Corrosion' 85, International Corrosion Forum , Vol. 6, 317 , Boston .

Andreson , R . E . (1981). Cathodically protected steel in sea water; polarization curves and cathodic
reactions . In: Metallic Corrosion , 8th ICMC , Vol. 77, ppl333- 1339 . Dechema , Germany .

Philipponneau , G . (1981) . Contribution to the study of magnesium calcium deposit occuring dur-
ing steel protection in sea water . ibid, 1327-1332 .

Cottis , R . A . (1985) . The application of hydrogen permeation measurements to the study of corro-
sion fatigue crack growth in steels . Materials Science Forum , Electrochemical Methods in Corro-
sion Research Proceedings of an International Symposion ( G . E . Murch , ed . ) , Vol . 8 ,
pp243-252 . Switzerland .

Marichev , V . A . (1982) . Hydrogen embrittlement of construction materials . Werkstoffe und

Korrosion, 33 ,1—14 .
 WS9a1

ADVANCES FOR ONE-PIECE PANEL VEHICULAR COMPONENTS IN SMC MOULDING

Tsuneo Hirai

Department of Mechanical Engineering, Doshisha University,

Karasuma-Imadegawa, Kamigyo-ku, Kyoto 602 Japan.

ABSTRACT

Products moulded from composite prepreg materials are prone to several

problems during manufacture such as sink marks, warpage and weld lines. To
overcome the faults in practice it is necessary to analyse the in-mould
flow behaviour of the sheet moulding compound (SMC) during the unsteady
forming process. The purpose of this investigation is to develop a design
procedure for preventing above faults, applying CAD system. The paper gives
a review of investigation made at Doshisha University into flow charac-
teristics of composite materials.

KEYWORDS

SMC moulding; sink mark; weld line; charge ratio; one-piece panel

INTRODUCTION

When composite materials of Class-A SMC are compression moulded to produce

ribbed panels for vehicles, problems can arise due to the development of
fibre orientation during flow, resulting unstable deformation.

FORMULATION AND SOLUTION PROCEDURE

The unsteady flow state occurring during a press forming process should be
analysed using a Lagrangean description, but a simpler analysis will be
used employing a progressive step-by-step formulation method (Hirai, 1986)
and an Eulerian description. The modelling of the mechanical behaviour
during deformation is achieved as follows, see Fig.1.

Rheology of Composite Materials in Compression Moulding.

At the first step the deformation state does not depend on the compression
3
4
r a t e of the punch, but i s governed by the eigen mode of deformation state
before i n i t i a t i o n of flow.

[Κ][ψ]=[Μ][ψ][Ω 2 ] (1)

[<p]=U>j] ( j = 1 , 2 , . . . n ) , and [fi 2 ]=diag. [CÜJ2]

where [K] is the stiffness matrix and [M] is the mass matrix. Also [Ω ],
[ω·] and [ψ] are eigenvalue, natural frequency and mode matrix respec-
tively. The first mode should be used to analyse the subsequent process.
The practical case of forming a T-shaped component from a flat blank is a
typical practical case and a result is shown in Fig.2. The sequence of
deformation is simulated by linear incremental analysis. The dots shown in
the figure indicate where the reaction forces at the nodal points show
stress-free conditions. The phenomenon indicates the possibility of micro-
buckling in laminae at the surface. The asymmetry of the dotted nodal
points suggest a tendency for any subsequently formed weld line in the rib
section to undulate or 'snake'.

C Start ) Problem

Eigenvalue Analysis

Estimation of Boundary Asymmetric

Condition by 1st Mode State Deformation

Initiation of
Linear Incremental Analysis
Weld Line

H Thermal Diffusion

Estimation of Initial Viscosity

Flow Analysis

NO Initiation of
Surface Sink

Filling Flow Analysis Surface Sink

by Matrix Component
■
f
Chemical Diffusion Warp
(
'
Q End )

Fig.1 Flow chart of compression moulding.

 5
Since the flow state of a composite material depends on the fibre orienta-
tion, which results in different flow resistance in directions normal and
parallel to the flow, homogeneous orthotropic pseudo-plastic equations are
derived and used as governing equation to analyse the flow state.

pUjU^j.+p^-y^u^O (2)

(3)

where y i (J 2 )=K i /3(AJ 2 /3) n " 1 and K

i = a ij K j
In this case the constitutive equation is obtained by the assumption of the
following non-Newtonian;

°eq= K ^ e q ) n U)
The method of weighted residuals is used to solve the equations. Numerical
results for flow states during moulding at constant room temperature are
shown in Fig.3, as an example of unsteady flow using the progressive step-
by-step method. In the figures it is evident that the flow swings around
the rib corner, as shown by ringed vectors. The flow state suggests that
there is a resin rich region in the product. To prevent or minimise faults
in the product, the thermal diffusion condition achieved by using a
preheated die reduced the tendency, shown by the ringed vectors in Fig.3 to
form a resin rich region.

Aspects of Surface Sink Formation

In order to determine the flow characteristics of the composite, the ratio

of the pseudo-plastic viscosities % / Κ ^ is given a high value, to repre-
sent a highly anisotropic flow resistance. The velocities increase towards
the centre of the rib channel. A surface sink mark might be produced during
the final stage of moulding as resin flows down into the lower corners of
the rib through the orientated reinforcement composed by flow state, after
the flow front reaches at the lower mould. (Hirai, 1987) The stress state
distribution indicates a large region under elastic loading with high
hydrostatic pressure around rib part. The condition is verified by the ex-
perimental result shown by Fig.4. The lines A and B in the figure for SMC

Fig.2 Deformation state obtained by

linear incremental analysis.
}
fflrffc ~^_3. "Θ. \
0 I 2 (mm/sec)
0 Î0 20 30(mm)

Fig.3 Flow state.

6

FLOW OF CONPOSITE

Fig.4 Pressure measurements for SMC

and isotropic resin compound.
(b) Flow state
in rib part

Fig.5 Flow state and distribution

of flow velocities.

shows two drops in pressure opposite the rib, the first corresponds to the
initial surface sink, creating the possibility of a weld line and the
second occurs when the resin flows to fill the bottom corners of the rib
channel. The presence of anisotropic flow resistance accounts for the
phenomenon.

The flow resistance is high in the plate and low in the rib channel. At the
inlet to the channel, flow resistance is dependent on fibre orientation.
The flow vector distribution and flow front state are shown in Fig.5. The
tendency for surface sink is indicated by the figures and verified by the
experimental results shown below in Fig.11. (Hirai and Yamabe, 1990)

EFFECT OF RIB CONFIGURATION AND CHARGE PATTERN ON FLOW STATE

SMC is used in the manufacture of automobile parts because of advantages of

weightsaving, corrosion resistance, lower cost and greater freedom of
design. However, the problem of sink marks on panel faces opposite stiff-
ening ribs must be overcome.
 7

It might be possible to improve a sink mark fault by altering the con-

figuration of the charge of SMC and its position in the mould. Normally in
SMC moulding the charge ratio is kept considerable smaller than the full
case but this might lead to an unsymmetric flow in the rib when the flow
pattern on to the rib parts has an asymmetric configuration. Since impor-
tant requirements of vehicular components are rigidity and strength, it
might be desirable to mould symmetrically, as indicated in Fig.6. (Hirai et
al., 1988) The rigidity and strength of an asymmetrically moulded rib are
very low, especially on the resin rich side.

Relationships between surface quality and rigidity are shown in opposite

condition. It is evident that sink marks persist in the final product with
symmetric flow, but disappear in asymmetric flow.

1.0 Symmetric rib

Fiber rich
side

"0 0.5 1.0 1.5 2.0

Non dimensional deformation by span length 6/1» X10~ 1

Fig.6 Relation between bending load and deflection.

USING UPPER BOUND APPROACH FOR SMALLER CHARGE RATIO

It might have a tendency to apply a SMC compression moulding to smaller

charge ratio of prepreg material in order to improve a surface quality
overcoming the faults in practice such as sink mark. The purpose of this
investigation is to develop a design procedure using CAD system to control
charge pattern and design configuration of mould with ribs.

When small charge ratio is applied in the process, the branching flow ought
to set up flowing into sequent plain mould and perpendicular rib canal.

Upper Bound Consideration at the Branching Flow Domain

It should be considered the kinematically admissible velocity field in the

domain, since surface traction by in-mould flow from the plane channel part
of mould is equivalent to the resistance caused by narrowed plane channel
and distortion into rib part. When the flow front states near the rib part
as shown in Fig.7, the solution for flow state could be obtained by upper
bound approach. Material flow behave to hold the equilibrium of flow resis-
8
tance, considering the behaviour dependent on the incremental deformation
caused by progressive punch stroke in the domain. Considering admissible
velocity field along the boundary, the following equation is supposed ac-
cording to hold the equilibrium between the surface traction of inlet from
flow front and resistance into in-mould plane channel and distorted flow to
rib part in indicating the viscosity in both direction of plane and or-
thogonal rib channel shown as x and y.

_L3I* = _ l a * v (5)
μχ 9χ y y "5y~

where μ and μ are the coefficient of above directions and 9ρχ/3χ and
dpv/^y sh° w the pressure gradient.

Fig.7 Analytical model at branching flow domain.

Results and discussion

Flow behaviour filling up into rib part differs from the case of near full
charge in flow state. The progress of flow front in the plate shaped chan-
nel advances into the direction of subsequent plane mould at the crossing
domain with rib, and a branching flow originates into rib part after the
advancing of the process, since it might be smaller resistance against the
flat mould caused by becoming narrow dependent on punch stroke than that of
distortion filling into rib part at the domain. In the case, the curvature
of entrance part of rib have an effect on the flow behaviour, then the
branching flow might begin in earlier step.

As existence of fillet part suggests a tendency for initiation of weld line

as mentioned above in the case of hundred percentage of charge, the problem
should be arisen when flow front progresses across through rib part.

The behaviour might give good effect for sink mark formation in order to
follow consequence of flow at the behind space in rib part. The tendency
for surface sink and weld line are indicated by the numerical results shown
as Fig.8 and verified by the experimental results shown in Fig.9· When flow
front passes over the rib part after progress of punch stroke, the resis-
tance in the plane channel direction grows higher and process of filling up
into rib is originated earlier. Since the originated sink mark flow into
 9
flat mould constructed as weld line, it might be improve a surface quality
but. the weld line is remain in oblique direction. Though surface quality is
promoted for smaller charge ratio, the rigidity and strength become very
low evaluation caused by asymmetrically mould rib.

(ilium»»»»
ira 0 10 20 30 DnnO
I 1 1 I

0 20 40 Cmm/secD
(a) Without fillet radius (b) With fillet
at rib entrance radius at rib entrance

Fig.8 Velocity vectors obtained by upper bound approach.

(a) Without fillet radius (b) With fillet radius

at rib entrance at rib entrance

Fig.9 Experimental results for filling flow states.

MINIMISING SINK MARKS BY MEANS OF COUNTER PUNCH PRESSURE

Based on the foregoing analysis of the sink mark mechanism, attempts were
made to minimise or eliminate the marks. Since the flow velocity increases
towards the centre of the rib, it is assumed that the volume of the un-
filled lower corners of the rib is related to a measurement of the height
of the curved free surface at the corner. Measurements of surface sink are
then related to height of the curved free surface for different operating
conditions with the aim of minimising the sink.

The method investigated used a die with a counter punch operating in the
rib channel which moved down during the press action, creating a back pres-
sure just less than the punch pressure. (Hirai, 1988) The arrangement is
shown in Fig.10, with a counter punch. Surface roughness measurements
across the face opposite the rib are shown in Fig.11. These were obtained
using a counter punch operated by oil pressure. The results confirm that
the application of back pressure is effective in improving surface quality.

The effectiveness of flow front restriction caused by back pressure control

depends on the height of the curved free surface at the unfilled lower cor-
10
ners of the rib and the horizontal velocity vector component at the
entrance to the rib. Typical results from analysis using controlled back
pressure are shown in Fig.12. The above factors are'indicated in the figure
as deviator factor for the former and effect of swing for the later respec-
tively in connection with the velocity of punch stroke. The most satisfac-
tory result is obtained for condition B2, which uses a stepped back pres-
sure pattern.

i
O 1
/////////////
y//////
i *
5

3
θ 2
;
P > Pb
1
Pb Λ1

Fig.10 Configuration of mould 2 3

with counter punch.

3.Oh « \

2.0 h i j 2.0

G1 G 2
DISTANCE DISTANCE
A1 : Without back pressure
(a) With back- (b) Without back B1 : High value of back pressure
pressure pressure during the process
B2 : With back pressure
by s t e p p a t t e r n
Fig.11 Surface roughness of part of
moulded with or without back
pressure by counter punch. Fi£.12 r
j.-ieorGticH."l. oonsirlsrfvtion on
the controlling system.

CONCLUSION

The progressive flow state of a composite material during a compression

moulding process has been analysed numerically by assuming the flow to be
anisotropic. The results obtained by the Progressive Step-by-Step Method
developed in this paper are shown to be in good agreement with experiment.

REFERENCES

Hirai, T. (1986). Rheology of Carbon Fibre Composite Prepreg Materials.

In Development in Reinforced Plastics-5, (G. Pritchard, ed.) pp. 233-65.
Elsevier Applied Science Publishers Ltd., London.
Hirai, T. (1987). Proc. of ICCM-VI, London, pp 1-121-30
Hirai, T., T. Katayama, M. Yamabe and K. Watanabe (1988) Int Symp. on
FRP/CM, Nanjing, 1/section 5-c
Hirai, T. (1988). Advancing with Composites, Int Conf. on C M . , Milan,
pp 505-12
Hirai, T. and M. Yamabe (1990). Design concept for one piece panel
vehicular components in SMC compression molding Composite Structures,
U, 3-U
WS9a2

THE EFFECT OF FIBRE PRE-TENSION

ON RESIDUAL STRESSES IN FIBRE COMPOSITES

JANG-KYO KIM, YIU-WING MAI and BRIAN COTTERELL

Centre for Advanced Materials Technology
Department of Mechanical Engineering, University of Sydney
Sydney, NSW 2006, Australia

ABSTRACT

The residual stresses resulting from fibre pretension is estimated from a simple model. The principal effect
of fibre pretension is to improve the mechanical bonding at the interface which promotes factional
resistance during fibre pull-out. The fibre pull-out stresses are approximately estimated by superimposing
the additional residual clamping stress at the interface due to fibre pretension. Comparison of the theory
with experimental results on steel wire-epoxy matrix model composites shows a reasonable agreement,
particularly for the frictional pull-out stress after complete debonding.

KEYWORDS

Fibre composites; residual stresses; fibre pretension; interfacial debonding; fibre pull-out.

INTRODUCTION

The principle of advanced fibre composites is the stress transfer from the matrix to the fibre across the
interface. Residual stresses always exist in fibre composites which arise from matrix shrinkage during the
curing process, particularly for polymer matrix composites, and differential thermal contraction between
fibre and matrix when cooling from the cure temperature. These stresses, if too large, are detrimental to
the mechanical performance and structural integrity of fibre composites since they increase the tendency
for fibre buckling, matrix microcracking and interfacial debonding. They can also cause severe transverse
cracking, delamination and warping in cross-ply laminates even in the absence of external loads (Kim and
Mai, 1991). Therefore, much effort has been made to minimise these residual stresses, e.g. by adding an
expanding monomer into a polymer matrix (Piggott et al., 1985) which has additional effect of improving
fracture toughness in some carbon fibre-thermoset matrix composites. However, these stresses are
beneficial in some circumstances and play an important role for the improved mechanical adhesion at the
interface which in turn allows such a failure mechanism as frictional fibre pull-out to take place more
properly during fracture. The present work describes a simple model to predict the residual stresses
resulting from the pretension which has been applied to the fibre during the curing process. The
significance of fibre pretension on the interfacial debonding and frictional pull-out behaviours are studied
on a model composite. The potential applications of this technique to practical composites are also described.

11
12

ANALYSIS OF FIBRE PULL-OUT

Figure la shows the configuration of a partially debonded fibre (with radius a) which is located at the
centre of a coaxial cylindrical shell of matrix (with an outer radius b) with embedded fibre length L. In
the fibre pull-out experiments, the composite is fixed at one end (z=0) and a tensile stress is applied at
the other end of the embedded fibre. An improved analysis has been developed by the authors (Zhou et
ah, 1990) of the fibre pull-out stresses based on a concept of fracture mechanics where the differential
strain energies stored in the fibre and matrix at both bonded and debonded regions with respect to the
incremental debond length are equated to the interfacial fracture toughness Gic. The simplified form of the
partial debond stress σ/ and the initial frictional pull-out stress after complete debonding afr are given:

σάρ = σ0 + (σ - σ0) [exp{X (L-z)} - l]/[exp{\ (L-z)} + φ] (la)

ofr = 1 [exp(X L) - l]/[exp(X L) + φ] (lb)

z _0
r z . L-z (debond length) .
Ί' 1 h — I — H
(a) " L 1 ^ z=-L/2 z=0 z=L/2

Fig. 1. Schematics of (a) partially debonded fibre and (b) pretensioned fibre
in a fibre pull-out model.

σ0 is the stress at the boundary between the bonded and debonded regions which can be approximately
determined from the following equation for debonding as z-^L. i.e.
m
σ0 = [2 τ a Gic / F] (2a)

F is a complex function of material constants, geometric factors as well as the bond length z relative to
the total embedded length L. In Eqs la and lb, λ is the reciprocal length giving the effective friction shear
stress transfer distance and "a is the asymptotic debond stress for long embedded length. These parameters
are related to the coefficient of friction at the interface μ and the residual clamping stress q0 due to
differential thermal contraction between fibre and matrix by:

λ = 2μk/a (2b)

σ = - ( V k) (1 + φ) (2c)
α v
where φ = (yloi)(vJvù and k = (av{ + γ Ο / { ( 1 - d + 1 + ^ + 2 γ } . α = E^/Iif (Young's modulus
ratio of the matrix to the fibre), y = a2/(b2 - a2) (fibre volume fraction), and j>f and vm are the fibre and
matrix Poisson ratios respectively.

If a pretension σρ1 is applied to the fibre during curing as shown in Fig. 1(b) and upon release (or
 13
unloading) of the pretension after cure, residual stresses are developed in the fibre and matrix. These
residual stresses can be estimated from considering the unloading process analogous to the fibre push-in
process (which is the reverse of fibre pull-out). Using the stress equilibrium equations and simplifying
assumptions under plane strain deformation similar to those formulated in the previous study (Gao et al.,
1988, Zhou et al, 1990) and for the boundary conditions for the fibre axial stress afz after the release of
pretension (i.e. σ? = [(α/γ')/(1 + α/γ')] σρ1 at z — 0 and az = 0 at z = ± L/2), the residual stresses σ{ζ
in the fibre and amz in the matrix normalised with the pretension σ^ are given by:

- {(α/τ')/(1 + α/γ')} exp(-n L/2) + (A2/A,) {exp(-n L/2) - 1}

of I apt = exp(nz)
exp(n L/2) - exp(-n L/2)

{(α/γ')/(1 + a/Y)} exp(n L/2) - (A2/A,) {exp(n L/2)} - 1]

+ exp(-nz) + (A2/A,) (3a)
exp(n L/2) - exp(-n L/2)

* m z /a p t = y (a f Va pt -l) (3b)

where
2 [ γ ' - a - 2k'(apf - 7 V J ]
A, = - n 2 = (3c)
a'2 (1 + pj [2 T'(b2/a'2) ln(b/a') - 1]

2 [γ' - a - 2k'(ai/f - γ'ί/J]

A2 = (3d)
a' (1 + O [2 <y'(b2/a'2) ln(b/a') - 1]
2

Similarly, the residual clamping stress q, due to Poisson expansion of the fibre after release of pretension
normalised again with apt is given:

q, / apt = - k' [(1 - φ')(σΓ7σρ1) + φ'] / (1 + φ>) (3e)

In Eqs 3a to 3c y\ φ\ k' and all other relevant parameters should be determined based on the effective
fibre radius in the pretensioned state a' = a(l - i/fCrpt/Ef).

As tension is applied to the fibre at both embedded ends z = ± L/2 (i.e. axial symmetry against the mid
plane z = 0) these stresses are changed differentially and reach constant values along the embedded length
as before the release of the pretension when the external stress is equal to the pretension apt. Therefore,
the existing analysis for the pull-out model without pretension can be modified to determine the pull-out
stresses for the fibres with pretension by assuming that with these stresses the system is in mechanical
equilibrium. However, if tension is applied to the fibre at one end z = L/2 while the other embedded end
z = -L/2 is fixed as in the fibre pull-out test of the present study, the analysis becomes very much
complicated and the solution for the fibre stresses is not available. However, a simple solution can be
obtained if it is assumed that the principal effect of fibre pretension is to increase the residual clamping
stress at the interface and the residual stresses afz and amz in the axial directions are neglected. Therefore,
while other interfacial properties and pull-out parameters remain the same as those without pretension, the
clamping stress q, is super-imposed on the existing radial stress at the interface which affects mainly the
asymptotic debond stress F given in Eq 2c. To a first approximation, taking its mean value q*, over the
whole embedded fibre length L, the asymptotic debond stress σ' for the pretensioned fibre is given:

? = - [(% + ϊ ) / k') (i + ΦΊ (4)

Hence, approximate solutions for the partial debond stress σ / and the initial frictional pull-out stress σ{τ
for the pretensioned fibre are determined by simply replacing <Fwith σ' in Eqs la and lb with the correct
boundary between z = 0 and z = L instead of between z = -L/2 and z = L/2.
14

RESULTS AND DISCUSSION

Model composite specimens for pull-out tests were made from stainless steel wires embedded in an epoxy
resin. The surface of the wire was carefully prepared to obtain reproducible condition in a method similar
to that reported previously (Glavinchevski and Piggott, 1973). The matrix material was an epoxy resin
Araldite GY 260 (Ciba Geigy, Australia) and curing agent piperidine in the ratio of 100:5 by weight, cured
for 16 hrs at 120°C. Elastic constants and radii of the constituents are: Ef = 179 GPa, Έ^ = 3.0 GPa, vf
= 0.3, vm = 0.35, a = 0.275 mm and b = 6.5 mm. The wires were subjected to tension which
corresponds to a strain 0.5% during curing using a special fixture fitted to the mould. After complete cure
the tension was released as the specimens were removed from the mould. Pull-out tests were conducted
on an Instron testing machine with a cross-head speed 0.5 mm/min. The maximum debond stress ad* and
the initial factional pull-out stress σ{τ were determined based on the force values at the points just before
and after the instantaneous load drop in the pull-out force versus displacement record.

(a)
1

U0.8
VO
N ^ 0.6
VO
0.4
L/2 =
0.2 v 10 mm
s
\ 2 mm\ mm >*>.(^
n S?
4 6 8 10 4 6 8 10 0 2 4 6 8 10
z (mm) z (mm) z (mm)

Fig. 2. (a) Fibre axial stress afz, (b) matrix axial stress amz and residual
clamping stress q, (normalised with pretension apt) plotted as a function
of the distance z from the mid-plane for the steel wire-epoxy matrix
model composite.

The normalised residual stresses in the wire, matrix and interface which are predicted based on Eqs. 3a
to 3e for the steel wire-epoxy matrix composite are plotted as a function of the distance from the mid-plane
in Fig. 2. It is noted that the wire is placed in tension and the matrix in compression in the axial direction,
while the interface is placed in compression in the radial direction after release of the pretension. The
gradient of all these stresses increases as the embedded length L is decreased, an indication of possible
interfacial debonding for very short L even in the absence of an external stress if apt is large.

Based on the instability conditions for debond process described in a previous paper (Kim et al., 1991),
the maximum debond stress σά* and the frictional pull-out stress σ{τ are calculated for the model composite
containing wires with and without pretension and these predictions are compared with experimental results
as shown in Fig. 3. The simple theory predicts that the maximum debond stress σα* is almost independent
of whether the fibres are pretensioned or not for both the uncoated and coated wires, an indication that a
small increase in 7? due to the superimposition of q, does not influence significantly ad* for the range of
L used. This prediction is in good agreement with the experiment for the uncoated wires. In contrast, the
experimental ad* values are slightly higher than the prediction for the coated wires with pretension. This
seems to be partly attributed to the fact that the coating of finite thickness in a paste form is squeezed out
by the matrix shrinkage during cooling from the cure temperature, promoting direct contact between the
wire and epoxy at the asperities of wire rough surface. Upon release of the pretension, the coating is
 15
further squeezed out increasing the area for direct contact. With regard to the initial fnctional pull-out
stress afr after complete debonding, the agreement is good for both uncoated and coated wires with and
without pretension. The theory predicts that the rate of increase in afr due to pretension becomes smaller
as L is increased, which is a direct result of the low q, values for long L as noted from Fig. 2c. The above
experimental and theoretical comparisons generally indicate that the effect of pretension is more
pronounced for fibres with weak interfacial bonding (GK = 35 J/m2 for the release agent coated wires) than
those with strong bonding (GK = 1 3 1 6 J/m2 for the uncoated wires). However, it should be emphasised
here that the simple analysis for the fibres with pretension does not lend any rigorous support to the
validity of the fibre pull-out stresses. In particular, the debond criterion given by Eq. 2a may not be
accurate due to the neglect of residual stresses in the axial direction.

2.5

4 8 12 16 4 8 12 16
L (mm) L (mm)

Fig. 3. Comparisons between experiments and theories of (a) the maximum

debond stress ad* and (b) initial fnctional pull-out stress ou as a function
of embedded fibre length L for the steel wire-epoxy matrix model
composite. Experiments: uncoated wires O without and # with
pretension; release agent coated wires Q without and ■ with
pretension. Theories: wires without pretension; wires with
pretension.

It is worth noting that the experimentally determined parameter σ predicts the residual clamping stress due
to differential thermal contraction of the fibre and matrix q0 = -8.85 MPa and -7.28 MPa respectively for
uncoated and release agent coated wires. For the coefficients of thermal expansion of the wire and matrix
a f = lxlO r5o /C and a m = 5xlO"5o/C respectively and the temperature difference between the cure and the
ambient ΔΤ = 100°C, these values are in good agreement with the value -8.69 MPa estimated from the
elasticity theory proposed by Harris (1978):

(« m - α,) ΔΤ E,,,
<k> (5)
(1 + α,ΔΤχΐ + amAT)(ii(l - vf) + 1 + cm + 2 γ ]

Although some difficulties are expected to apply pretension to the fibre in practical composites, potentials
of this technique can be identified from the finding that pretension increases the mechanical bonding at the
interface which controls the fnctional resistance during fibre pull-out. It is intuitive that the beneficial
effect of pretension is most useful for composites with weak interfacial bonding, particularly for ceramic
matrix composites where the bonding is mainly mechanical in nature. The improved fnctional resistance
can ameliorate the crack growth resistance (or R-curve) behaviours of the composite in fibre bridging
during fracture process. Another important property of the composite with fibre pretension would be the
16
triaxial compressive stresses remained after cure in the matrix material. Although these stresses may cause
microcracking in the matrix and interfacial debonding in severe cases, it can reduce the permeability and
diffusivity of moisture into the composite under humid and/or acid environments and thus can avoid, to
some extent, the degradation of long-term mechanical properties. This argument can be partly supported
by the work of Pollard et al. (1989) who found that hydrostatic compressive pressure applied to glass fibre-
polyester composites in sea water reduced slightly the diffusivity of water molecules. The exact
mechanisms of this behaviour is yet to be clarified, but it appears that the compactness of the molecular
structures in the matrix has been promoted under compressive pressure.

CONCLUSION

A simple model has been developed to predict the residual stresses resulting from pretension which is
applied to the fibres during curing of the fibre composites. Fibre pull-out tests on steel wire-epoxy matrix
model composites showed that fibre pretension does not affect much the maximum debond stress ad* for
uncoated wires, but it increases slightly σά* for release agent coated wires. The latter is explained by the
squeezing or spreding of the coating in a paste form due to the release of pretension which increases the
apparent contact area between the wire and matrix. The principal effect of fibre pretension is to promote
the mechanical bonding at the fibre-matrix interface which in turn improves the frictional resistance during
fibre-pull-out. This is potentially useful for composites with weak interfacial bonding, particularly in
ceramic matrix composites. A reasonable agreement is obtained for the pull-out stresses between
experimental results on the steel wire-epoxy matrix model composite and a simple theory which has been
developed based on a existing debond theory by superimposing the residual clamping stress at the interface.

ACKNOWLEDGEMENTS

The authors with to thank the Australian research Council for continuing support of this work which forms
part of a larger project on "Development of high strength and high fracture toughness composites with
controlled interfaces."

REFERENCES

Gao, Y.C., Y.W. Mai and B. Cotterell (1988). Fracture of fibre-reinforced materials. /. Appl. Math. Phys.
(ZAMP), 39, 550-572.
Glavinchevski, B. and M. Piggott (1973). Steel disc reinforced polycarbonate, /. Mater. Sei., 8, 1373-
1382.
Harris, B (1978). Shrinkage stresses in glass/resin composites. /. Mater. Sei., 13, 173-177.
Kim, J.K., C. Baillie and Y.W. Mai (1991). Instability of interfacial debonding during fibre pull-out.
Scripta Metall. Mater., in press.
Kim, J.K. and Y.W. Mai (1991). High strength-high fracture toughness fibre composites with interface
control- a review. Comp. Sei. Technol., in press.
Piggott, M.R., P.S.Chua and D. Andison (1985). The interface between glass and carbon fibres and
thermosetting polymers. Polym. Comp., 6, 242-248.
Pollard, A., R. Baggott, G.F. Wostenholm, B. Yates and A.P. George (1989). Influence of hydrostatic
pressure on the moisture absorption of glass fibre-reinforced polyester. J. Mater. Sei., 24, 1665-1669.
Zhou, L.M., J.K. Kim and Y.W. Mai (1990). Interfacial debonding and fibre pull-out stresses: a new
model based on the fracture mechanics approach. Proc. Symp. 8th Austr. Fract. Group (Y.W. Mai,
ed.), Sydney Univ., Sydney, pp. 184-185.
 WS9a3

THE EFFECT OF IMPREGNATED FIBRE BUNDLES

ON THE FRACTURE BEHAVIOURS OF CFRP

JANG-KYO KIM and YIU-WING MAI

Centre for Advanced Materials Technology
Department of Mechanical Engineering, University of Sydney
Sydney, NSW 2006, Australia

ABSTRACT

The fracture behaviours of carbon fibre reinforced plastic composites (CFRP) were investigated using
specimens containing bundle fibres which were impregnated with polymers before being incorporated into
an epoxy resin matrix. Of particular interest were the beneficial energy absorption mechanisms which are
augmented by the bundle impregnation during fracture. Results showed that fibre bundling can improve
transverse impact fracture toughness of the composite by approximately 100% as compared to the
composite with uniformly distributed fibres for a given total fibre volume fraction, without any reduction
in flexural strength. The fracture toughness correlated approximately with the frictional fibre pull-out work
which was predicted based on the bundle strength and fibre pull-out length data.

KEYWORDS

CFRP; fibre bundle; fracture toughness; tensile strength; fibre pull-out; statistical analysis.

INTRODUCTION

Fibre composite technology is based on taking advantage of the high specific strength and modulus of
fibres by dispersing them in a resin matrix which acts as a binder and transfers stresses to the fibres across
the interface. In addition to strength and stiffness, another important property of a composite is its specific
resistance to fracture or fracture toughness. It is well known that the fracture toughness of a composite is
not simply the sum of the weighted contributions by the constituents, but is governed more importantly
by the extent of energy absorption processes through various toughening mechanisms. Since a critical
design criterion in fibre composites is sufficient fracture energy absorption capability, particularly in impact
loading situations, there have been a number of attempts to improve the composite fracture toughness
without significant loss of stiffness and strength. A comprehensive review on these toughening methods
and the various factors which would affect the efficiency of enhancement of toughness is given recently
by Kim and Mai (1991).

The review suggests that the use of large diameter fibres can improve fracture toughness of brittle fibre-
ductile metal matrix composites. This is explained in terms of the increased volume of ductile matrix

17
18
material involved in shear flow at the fibre-matrix interface which gives rise to the fibre pull-out force
proportional to the fibre diameter. Large diameter fibres may also be beneficial for brittle fibre-brittle
matrix composites through the ameliorating effect of increasing critical transfer length, provided that these
fibres can retain the same properties as the smaller diameter fibres. It is well known that the tensile
strength and modulus of many types of fibres show a systematic decrease with increasing fibre diameter.
Fila et al. (1972) demonstrated that tough composites with fibre bundles of large diameter and uniform
strength could be produced in a bundle impregnation technique. However, no comparison was made with
composites of uniform fibre distribution and the toughness result was correlated basically with the stress
redistribution energy after fibre breakage both for glass and carbon fibre-polyester composites. The present
work describes an attempt to enhance the fracture toughness of composites using carbon fibres in an epoxy
matrix, by adopting the principle of large diameter fibres. The fracture toughness and strength of the
composite with impregnated bundles are compared to the composite with fibres of relatively uniform
distribution. The implication of microscopic observation of the fracture surface is also described.

EXPERIMENTAL WORK

The fibre used was a carbon fibre Grade HTA (Toray, Japan) in the form of 12K tow and of diameter 7
μνα. The matrix material was an epoxy resin Araldite G Y 260 (Ciba Geigy, Australia), a diglycidal ether
of bisphenol A (DGEBA), and curing agent piperidine in the ratio of 100:5 by weight. Bundles of fibres
were impregnated with polymer solutions in a method similar to that recommended by the specification
(ASTM D2343). The imprégnants were made from epoxy resin (EP, the same material as the matrix
material for the composite) and polycarbonate resin (PC) which were diluted with acetone or dissolved in
méthylène chloride respectively to ensure complete wetting of individual fibres in a bundle. Any excess
imprégnant was wiped out using felt wipers before winding on a fixture. The wet bundles were cured to
produce rigid fibrous rods of diameter approximately 0.8mm.

The unidirectional continuous fibre composites were produced either by hand lay-up of prepregs for fibres
of uniform distribution or on a split-frame mould for impregnated bundle fibres. The prepregs were
fabricated using a prepreg machine (Mai and Castino, 1984) where fibres were laid up on the periphery
of a drum onto which the matrix material was subsequently applied. The impregnated bundles were secured
into the holes of Teflon dams in the mould. The randomly oriented fibre composites were also produced
using chopped fibres (both with and without bundle impregnation) of length approximately 30 mm in an
open mould. Before moulding the unimpregnated chopped fibres were distributed uniformly in a water bath
and dried completely. All these composites were placed in a vacuum oven with pressure -100 kPa for 1/2
hr to evaporate entrapped air bubbles, followed by cure for 16 hrs at 120°C.

Tensile specimens of the fibre bundles both with and without impregnation were mounted on cardboard
frames as recommended by the specification (ASTM D3379), which were then loaded over a fixed gauge
length 20 mm by using rubber-backed jaws. Flexural strength of unidirectional fibre composites was
determined in three-point flexure of unnotched specimens with a span-to-depth ratio of 30:1. Tensile and
flexural tests were conducted on an Instron testing machine at a cross-head speed of 0.5 mm/min. The
fracture toughness of composites was evaluated using a Zwick impact tester of total span 40 mm at an
impact velocity 2.93 m/s on a specimen 12mm wide and 55mm long with a notch of depth about 2 mm
made in the width direction of the centre span. The fracture surface was characterised and pull-out length
was measured on impact test specimens using an optical stereo microscope and a scanning electron
microscope (SEM).

RESULTS AND DISCUSSION

The transverse impact fracture toughness values for composites with uniform fibre distribution are
compared with those with impregnated bundles in Figs. 1(a) and 1(b). Impact fracture toughness increases
approximately linearly with increasing Vf for the range of small Vf used. The EP-impregnated fibre bundles
impart a toughness value approximately twice that for the composites with uniform fibre distribution for
 19
a given Vf for both the composites with unidirectional continuous and short randomly oriented fibres. The
large increase in toughness appears to be attributed to the ameliorating effect of increasing the fibre pull-
out length, proportional to the critical transfer length, by the bundles of large diameter shown in Table 1.

Fig. 1. Impact fracture toughness of CFRP with (a) unidirectional continuous

fibres and (b) short randomly oriented fibres as a function of fibre
volume fraction Vf: O uniform fibre distribution; · EP-impregnated
bundles; Δ PC-impregnated bundles.

The reason for the only marginal improvement in fracture toughness for the unidirectional composites with
PC-impregnated bundles, otherwise the improvement being as large as 100% for short bundle composites,
seems to be related to the flexibility of PC and, to a less extent, incomplete wetting of the individual fibres
with PC. It was normally observed that the apparent diameter of these bundles in the cured composite was
greater than that measured before moulding, particularly in the central area of the mould. This indicates
that during curing under high temperature some amount of molten epoxy resin has penetrated into the PC-
impregnated bundles which were slightly sagged between fixed ends of the mould. This reduced somewhat
the efficiency of the effect of bundle impregnation. The beneficial toughening effect of bundle impregnation
is not accompanied by any reduction in flexural strength: in fact the strength values for composites with
impregnated bundles are even slightly higher than those composites of uniform fibre distribution for a
given Vf as shown in Fig. 2. This favourable result is despite the adverse effect of premature failure of
impregnated bundles in the compressive face which triggers fracture of the whole specimen in bending due
to the large stress concentration.
300

Fig. 2. Flexural strength of CFRP of unidirectional continuous fibres as a

function of Vf. Symbols as in Fig. 1.

The statistical variation of bundle fibre strength σ* is described by the cumulative probability P developed
20
by Weibull (1952):

Ρ ^ ) = i . S(<l·) = 1 - exp [- (<Τ/σ»οη (1)

where S is the cumulative probability of survival, and m and σ^ are the Weibull modulus and the
characteristic strength of the fibre bundle respectively. Eq 1 is also applied to describe the probability of
a fibre pull-out over a particular distance I (Beaumont and Anstice, 1980) by replacing ob and σ^ with i
and £0. The characteristic parameters thus determined and the arithmetic mean values a* and £ are
summarised in Table 1. The pull-out lengths for unimpregnated fibres were measured from the composite
with fibres of uniform distribution. The details of the statistical variation of these properties are omitted
here. Table 1 proves that bundle impregnation can improve the tensile strength of the bundle as well as
uniformity of the strength. The strength values for the impregnated bundles shown were calculated on the
basis of the total cross-sectional area of the bundle including the imprégnant with average fibre volume
fractions 78% and 81% for the EP- and PC-impregnated bundles respectively. If the impregnated bundles
are regarded as composite rods, the mean values of net fibre strength in bundles would become 2.28 GPa
and 2.16 GPa respectively according to the rule of mixtures prediction. These values are about 25%
greater than those (i.e. gross tensile strength of the impregnated bundles) given in Table 1. The measured
pull-out lengths of the EP-impregnated bundles are almost an order of magnitude longer than those for
individual fibres with similar data scatter.

Table 1. A summary of Weibull parameters for tensile strength of

bundle and fibre pull-out length

Fibres Tensile strength (GPa) Pull-out length (μιη)

m σ*Ό ob m ÎQ i

Unimpregnated bundle 13.8 1.73 1.67 2.03 110 94.8

Ep-impregnated bundle 18.4 1.84 1.79 1.67 764 664

PC-impregnated bundle 21.2 1.80 1.76

Typical fracture surfaces of uniformly distributed fibre composites shown in Figs. 3(a) and 3(b) are
characterised mainly by short pulled out individual fibres and some degree of matrix deformation between
reinforcing fibres. In sharp contrast, significantly long pull-out bundles are shown for composites with
impregnated bundles in Figs. 3(c) and 3(d). Evidently, the impregnated bundles act more or less as single
fibres of large diameter with minor longitudinal splitting. It is also interesting to note that the pulled out
bundle shows a rough top surface consisting of small bundle fibres, an indication of some energy
absorption during fracture of the bundle. The clean matrix fracture surface with semi-circular patterns
around the bundle (Fig. 3(c)) is a direct result of localised rapid and brittle fracture with little deformation,
the so-called "micro-pop in" phenomenon (Kunio et al, 1981). Further development of fracture is
suppressed by the presence of the bundle acting as a rigid obstacle and requires significant matrix
deformation leaving very rough fracture surface behind the bundle. Similar semi-circular crack patterns
are also shown in Fig. 3(d). The matrix material around the bundles is fragmented in this composite
probably to allow pull-out of inclined bundles of large diameter which are not perpendicular to the
advancing crack. This observation is similar to the report by Hing and Groves (1972) that in addition to
the fibre pull-out, fracture of randomly oriented ductile fibres in a brittle matrix requires extra energy
absorption mechanisms including fragmentation of matrix, enhanced frictional work near the exit point of
the fibre from the matrix.

The fibre pull-out work (R^) has been shown to be a dominant source of the fracture toughness of CFRP
(Beaumont and Harris, 1972; Kim and Mai, 1990). An upper bound estimate for R^ for unidirectional
 21
continuous fibre composites is made assuming that fibre pull-out length I varies between zero and half the
critical transfer length (iJ2) with a mean value of i JA:

R^ = v f & tc I 12 = Vf & ί I 3 (2)

&_ is tensile strength of individual fibres for composites with uniformly distributed fibres. Its mean value
& is estimated from the relationship developed by Coleman (1958):

ob/or = (l/m) ,/m exp(-l/m) / Γ(1 + 1/m) (3)

where Γ is the gamma function. If the WeibuU modulus for individual fibres m is taken, to a first
approximation, as 4 (which is a reasonable value since very brittle fibres like carbon fibres normally show
a large amount of scatter (Hull, 1981)), Eq 3 gives approximately 0.6. Hence, & is estimated to be 2.79
GPa which corresponds to 86% of the value (3.23 GPa) specified by the manufacturer. Eq 2 can also apply
to the composite with impregnated bundles, when relevant properties of the bundles are used. The effective
volume fraction of bundle is slightly higher than the total volume fraction of fibre Vf due to the effect of
imprégnant in bundles. The contribution of pull-out work of small bundle fibres on the top surface of the
impregnated bundle is neglected as compared to that of the impregnated bundle.

Fig. 3. SEM photographs of the impact fracture surfaces for composites with
(a) unidirectional continuous and (b) short randomly oriented fibres of
uniform distribution, and for composites with (c) unidirectional
continuous and (d) short randomly oriented EP-impregnated bundles.

The Rpo value for V f =0.06 predicted using the relevant data given in Table 1 is 5.3 kJ/m2 for composites
with uniform fibre distribution. For simplicity only mean values are used in the calculations. This value
is considered to be in good agreement with the experimental result shown in Fig. 1 for the same Vf.
However, for the same Vf the estimated Rp,, value for composites with EP-impregnated bundles gives 24
kJ/m2 which is almost twice the experimental result. This appears to be associated with the overestimate
22
of ί for the bundle. It should be noted that measurement of Î using a microscope cannot account for the
variation over the whole area of the bundle. Another reason would be some degree of longitudinal splitting
of the bundle which reduces the effective surface area for the frictional pull-out.

Apart from the improvement in fracture toughness, bundle impregnation has other advantages. Fibre
slackening can be reduced significantly by applying slight tension during winding and subsequent curing
of impregnated bundles. Confining the distribution of fibres in a bundle can also avoid, to some extent,
the fibre misalignment which might otherwise result in some reduction in compressive strength (Wisnom,
1990). Provided that all the fibres are properly wetted by the imprégnant, twisting of fibres within a bundle
seems not to deteriorate mechanical properties of the composite. However, fibre bundling may introduce
unreinforced weak gaps between large bundles which are detrimental to the overall mechanical performance
and structural integrity of the composite. This problem may be reduced to a minimum by placing individual
fibres between bundles. This technique seems to be practically feasible particularly for short fibre
composites in such processes as spray moulding, injection moulding, etc.

CONCLUSION

Fibre bundling can favourably used to improve fracture toughness of fibre composites without sacrificing
strength properties. The results on CFRP show that for composites with polymer impregnated bundles the
impact fracture toughness increases by 100% compared to composites with fibres of uniform distribution
without any loss of flexural strength in the range of small Vf studied. The impregnated bundles act as
single fibres of huge diameter increasing effectively the fibre pull-out length. Statistical analysis also
demonstrates that bundle impregnation can improve the tensile strength of the bundle as well as uniformity
of strength distribution.

REFERENCES

ASTM D2343-67. Tensile properties of glass fibre strand, yarns and rovings used in reinforced plastics.
ASTM D3379-75. Tensile strength and Young's modulus for high modulus single-filament materials.
Beaumont, P.W.R and P.D. Anstice (1980). A failure analysis of the micro-mechanisms of fracture of
carbon fibre and glass fibre composites in monotonie loading. /. Mater. Sei., 15, 2619-2635.
Beaumont, P.W.R and B. Harris (1972). The energy of crack propagation in carbon fibre-reinforced resin
systems. /. Mater. Sei., 7, 1265-1279.
Coleman, B.D. (1958). On the strength of classical fibres and fibre bundles. /. Mech. Phys. Solidsy 7, 60-
70.
Fila, M., C. Bredin and M.R. Piggott (1972). Work of fracture of fibre-reinforced polymers. J. Mater.
Sei., 7, 983-988.
Hing, P. and G.W. Groves (1972). The strength and fracture toughness of polycrystalline magnesium oxide
containing metallic particles and fibres. J. Mater. Sei., 7, 427-434.
Hull, D. (1981). In: An Introduction to Composite Materials, pp. 127-142. Cambridge Univ. Press,
Cambridge, 127-142.
Kim, J.K. and Y.W. Mai (1991). High strength-high fracture toughness fibre composites with interface
control- A review. Comp. Sei. Technol., in press.
Kim, J.K. and Y.W. Mai (1990). The effect of interfacial coating and temperature on the fracture
behaviours of unidirectional KFRP and CFRP. submitted to /. Mater. Sei.
Kunio, T., M. Shimizu and S. Sohmiya (1981). Role of local fibre distribution at notch tip in the fracture
toughness of FRP. Proc. ICF 5, Vol. 1, 495-502.
Mai, Y.W. and F. Castino (1984). Fracture toughness of Kevlar-epoxy composites with controlled
interfacial bonding. J. Mater. Sei., 19, 1638-1655.
Weibull, W. (1951). A statistical distribution function of wide applicability. Trans. ASME Series E, J.
Appl. Mech., 18, 293-296.
Wisnom, M.R. (1990). The effect of fibre misalignment on the compressive strength of unidirectional
carbon fibre/epoxy. Composites, 21, 403-407.
 WS9a4

DELAMINATION CRACKS ORIGINATING FROM TRANSVERSE

CRACKING IN CROSS-PLY LAMINATES UNDER PLANE STRAIN
BENDING AND ANTIPLANE SHEARING

YJ. KIM, T.W. KIM and S. IM

Department of Mechanical Engineering Korea Advanced Institute of

Science and Technology, P.O.Box 150, CheongRyang, Seoul, Korea

ABSTRACT

Based upon the Stroh formalism for anisotropic elastic materials and upon the method
of eigenfunction expansion, the stress redistribution due to delamination cracks
originating from transverse cracking is examined for cross-ply laminates under plane
strain bending and antiplane shearing. The structure of solution in the form of series
expansion is determined from the eigenvalue equation resulting from appropriate near-
field conditions. To complete the solution, use is made of the singular hybrid finite
element method. The fracture mechanics parameters, such as, stress intensity factors
and energy release rates are calculated, and the stability of crack growth is examined for
varying ratios of ply thickness in terms of the energy release rate.

KEYWORDS

Hybrid finite element method; stress intensity factors; energy release rates; stability.

STATEMENT OF THE PROBLEM AND BASIC EQUATIONS

Consider cross-ply composite laminates, [90/0] s subjected to bending or antiplane

shearing. As the load increases, there will occur numerous transverse cracks running
parallel to the fiber orientation of the 90° ply, with an approximately uniform spacing
along the length of the laminates. These cracks, terminating perpendicularly to the ply
interface because of the stronger 0° ply, tend to develop into delamination cracks along
the interface as the load increases further. We will examine fracture behavior of the
laminate containing such interfacial cracks under plane strain bending or antiplane
shearing. To simplify the problem, we assume that the cracks are uniformly arranged
with the configuration symmetric about the mid-plane, as shown in Fig.l, so that the
overall arrangement is obtained by repetition of the representative unit cell. We take a
23
24

Fig. 1. Delmination cracks originating from transverse cracking in

[90/0] s under plane strain bending and antiplane shearing

rectangular Cartesian coordinate system with origin at one of the crack tip. We choose
the Xi axis to be along the length of composite laminates while the x 2 axis is taken to be
along the direction of the laminate thickness, and then the x3 axis becomes along the
laminate width, which is parallel to the cracks(see Fig.l). Each ply of the composite
laminates lies in a plane parallel to the x r x 3 plane, and the ply orientation Θ is defined to
be the counterclockwise angle, viewed from the top, that the fiber direction makes with
the Xj axis. We assume that the laminate dimension in the x 3 direction (laminate width)
is sufficiently large compared with the laminate thickness and that the laminate is
assumed to be in the state of plane strain bending or antiplane shearing on the x r x 2
plane. Let Ui, σ φ e y denote the Cartesian components of displacement, stress and
strain, respectively. For deformations that depend upon two coordinates xx and x 2 only,
we have the governing equations of equilibrium equation, strain-displacement relation
stress-strain relation :

q w + σί2>2= 0 , 6y = (Uij+ Uj ■)/2 , o y = C ijkl % , (l.a,b,c)

where Cijkl are the 4-th order stiffness tensor, and comma indicates the partial
differentiation with respect to x{. Introducing the "collapsed" representation, we may
write the stress-strain relation as

σί = ς ^ . , e^SyOj. (2-a,b)

Ci and Si are the stiffness and the compliance matrix, and the two indices for the stress
and the engineering strain are collapsed as follows : (l,l)-*-(l), (2,2) -**(2), (3,3) -*-
(3), (2,3) -^(4), (1,3) -*-(5), (1,2) +(6). For orthotropic materials likes [90/0]s, and [0/
90]s laminates, we have
 25

^-14-Ci5-C 1 6 -C24-C25-C2 6 -C34-C35-C3 6 -C45-C 4 6 -C5 6 -0 . (3)

For such materials, the displacement component u3 is decoupled from uu u2, that is, the
antiplane shearing is decoupled from the plane strain deformation. To determine the
solution structure for the present problem, we use the so-called Stroh formalism(Ting,
1986). Following Ting(1986), we can show that the general solution takes the form for
the present problem,

u a = v akf(zk), zk = X! 4-^ x2 (k=l ,2,3,4) (4.a,b)

df(zk)
σ
αβ= T aßk"^"" > Taßk= (caßyi +M-kcaßy2)vYk for plane strain bending (4.c,d)

u 3 = vg, g(C, ) , ζι =xl +vz x2 (? =1,2) (5.a,b)

σ
3α= τ3α/ $r ' τ3α/ =
^ 3 α 3ΐ + v/ C3a32^ v3/ for antiplane shearing, (5.c,d)

where summation is implied on repeated Greek indices; μ,,, ν, are the eigenvalues to be
determined, and f(zk), g ^ ) are functions of zk, ζ . Substituting equations (4.c) and (5.c)
into equation (l.a), we obtain the equations for plane strain bending and antiplane
shearing:

D«ßUOν^ = 0, D ^ û O = C a l ß ^ k ( C a l ß 2 + C ^ ) + μ, 2 Ο α2β2 , (6.a,b)

Dsaty ) v3 = 0, D33ÎV, ) = Cmi+\t (C3132 + C3231) + V^Qaaa . (6.c,d)

For the existence of nontrivial solutions, we have

detBVjO] = Ό φ(μJ = 0, det[D33(v/ )] = D33(v/ ) = 0 , (7.a,b)

and the solutions of the quartic equation and the quadratic equation yield the two pairs
of complex conjugate eigenvalues,

μα+2= μ« (<*=1,2) v ! = v2 . (8. a,b)

ASYMPTOTIC EIGENFUNCTION EXPANSION AND SINGULAR

HYBRID F.E.M. SOLUTION

We assume the power type eigenfunction for f(z k ), g(Q ) as given by (Ting, 1986)
°° 00

C n+ D
fkfek> = Σ *n 4 V (δη+l), g(Ç, ) = Σ / ηζ/δη+1/ « n + 1 ) , (9.a,b)
n=1 n=1
(k=l,2,3, 4) (7 =1,2)
which leads to the expression for the displacement and stress field
26

| 1®
/

"r
s I / te
^
S1 1
Λ
70=ί te
ΝΊ Φ

□
\α.
ΤΊ V
Ml \
v! 1 _Λ
^
Tan6o= 0.5 Hybrid Element Regular Element

Fig. 2. Typical mesh configuration for the plane strain bending and
antiplane shearing of [90/0] s laminates

u
a =2uCkn V
ak z
k n
Mön+U σαβ - ^ Μ α ι x
aßk z k (10.a,b)
n=l n=l (k=l,2,3, 4)

u
3 = A D / n v
3f S/ n
MOn+lJ, σ
3 α - A D / n ^ α / ζ/ % x (10.C,d)
n=l n=l (I = 1 , 2 )
where the superscript m=l,2 indicates the upper and the lower ply, respectively. Here
the eigenvalues δη are to be determined from the so called "near-field" conditions
around the crack tip, including the traction or displacement conditions on the crack
surface and on the ply interface. The coefficients Ckn or D, n are dependent upon the
associated eigenvalues δη, and it can be determined within an arbitrary constant when δη
is obtained. We assume that the two plies are rigidly bonded along the rest of the ply
interface. Then the near field conditions for the plane strain bending may be written as

σ 2 2 (1) (χι,0 + ) = σ 2 2 (2) (χ 1 ,0') = 0,σ 1 2 (1) (χ 1 ,0 + ) = σ12(2)(χ1,0") = 0 (ll.a,b)

(on the crack surface, χχ < 0 ) ,

[σ22(Χι, 0)] =[σ12(χ!, 0)] = 0 , [Ul(Xl, 0)] = [u2(xlf 0)] = 0 (12.a,b)

(on the interface, xi > 0 ) ,

where the bracket [ ] denotes the discontinuity of the quantity in it across the ply
interface, for example, [σ22(χ!, 0)] = σ22 (1) (x1? 0 + ) - σ22 (2) (x1? 0" ). The similar
conditions can be written for the antiplane shearing, which is omitted here because of
space limitation. To take only the real part of equations (10.a,b) for convenience, we
may introduce, say for C kn (a) ,
 27

Fig. 3. Energy release rate versus the length of delamination crack

under a fixed bending and shearing loading in [90/0] s

Ckn(a) = l/2( γ1ν - iY2v)bkn(a) for complex δη, Im[5J > 0

α )
^ = 1/2γ 3ν ΐΟ α) for real δ η , (13)

where b kn (a) is obtained from the foregoing near-field conditions and γ1ν, γ2ν> γ3ν are
constants to be determined from the remote boundary conditions through matching with
the aid of the hybrid F.E.M..

NUMERICAL RESULTS AND DISCUSSION

In this section, we determine the unknown free constant γ 1ν , γ2ν> γ3ν through the hybrid
F.E.M to complete the solution. We will discuss the nature of near-tip singular fields in
terms of stress intensity, and the fracture behavior of delamination cracks, including the
stability of crack growth and the effects of ply thickness upon the energy release rates.
For numerical computation, we use the following material data for the graphite epoxy
T300/5208,
E L =134GPa, Ep =E z =10.2GPa, 0 ^ = 0 ^ = 5.52 GPa , 0 ^ = 3 . 4 3 0 1 ^
v L T = v L Z = 0 . 3 , v^=0.49.
To determine the free constants and thereby complete the solution, we match the near-
field solution (10.a,c) with the remote boundary conditions, comprising the remaining
conditions other than the near-field conditions, through singular hybrid F.E.M., wherein
the crack up region is modeled as a singular element into which the asymptotic
solution is embedded, and the other region as the displacement-based regular finite
elements. The details of this formulation are not described here because of limitation of
space available, but interested readers may be referred(Wang and Yuan, 1983; Im and
28

Table 1. Comparision of two methods

1/2
unit : [GPa(mm)
Antiplane shear Pure bending
(No. of eigenvalues) Κπι/γ 0 Kj/Oo Κι/θο
Collocation method 40 -1.0634
(100 collocation station) 60 -1.0634 _ _
80 -1.0634 _ _
(No. of elements) (No. of elements)
Hybrid F.E.M 41 -1.0523 39 1.3265 1.0445
(15 eigenvalues) 47 -1.0615 47 1.3274 1.0442
53 -1.0629 55 1.3277 1.0441

Kim, 1989). To confirm the solution, the present hybrid F.E.M. solution is compared
with the boundary collocation solution in terms of the stress intensity factor for the
loading of antiplane shear in Table 1. We find an excellent agreement between the two
solutions (the relative difference is less than one percent). Fig.3 shows the stability of
crack growth in terms of energy release rates under a fixed load condition for the plane
strain bending and for the antiplane shearing, respectively. It reveals important features
regarding the growth of delamination cracks originating from transverse cracking in
cross-ply laminates. When we assume the failure criterion based upon the critical
energy release rate, G=GC (G c is a material constant), we see that for bending any
delamination crack will undergo unstable growth until the crack length reachs a critical
value associated with the maximum G, and it will continue to grow under a fixed
loading until the energy release rate decrease to the critical value G c . Thus there exists
an inherently built-in crack arrest mechanism for the plane strain bending. The similar
result was reported for extensional loading(Kim and Im, 1991). For the antiplane
shearing, on the other hand, G versus crack length curve is relatively flat other than
large values of G for vanishing crack length. It is worthwhile to note that energy
release rate does not go to zero for vanishing crack length under antiplane shearing
because the stress singularity for the transverse cracks(which is obtained as the
delamination cracks vanish) is stronger than the square root singularity under the
antiplane shearing(Im and Kim, 1989).

REFERENCES

Im, S and Kim, T.W. (1989). Stress field near transverse cracks under extension or in-
plane shear in cross-ply composite laminates. _KSME_J., 3, 121-129.
Kim, T.W.and Im, S. (1991). Delamination crack originating from transeverse cracking
in cross-ply composite laminates under extension. To appear in Int. J. Solids
Structures.
Ting, T.C.T. (1986). Explicit solution and invariance of the singularities at an interface
crack in anisotropic composites. Int. J. Solids Structures, 22, 965-983.
Wang, S. S. (1983). A hybrid finite element approach to composite laminate elasticity
problems with singularities. J. Appl. Mech., 50, 835-844.
WS9a5

PROPERTIES OF INTERMINGLED CARBON/PEEK 3-D

WOVEN COMPOSITES
M.H. MOHAMED, N.F.N. MACHFUD, and H. HAMOUDA
Department of Textile Engineering, Chemistry, and Science,
College of Textiles and the Mars Mission Research Center
North Carolina State University
Raleigh, North Carolina 27695-8301, U.S.A.

ABSTRACT
The presence of voids is one of the major problems associated with resin infil-
tration techniques when using 3-D woven preforms. Efforts to reduce the voids
invariably result in the creation of microcracks. In this paper, the use of
PEEK fibers intermingled with carbon fibers into a multi-layer preform is dis-
cussed. Influence of processing parameters, such as temperature, pressure,
and consolidation time, on the composite properties is presented. One of the
issues emphasized is the effect of pressure on buckling of the Z-reinforcement
fibers and the bending behavior.

INTRODUCTION
Thermoplastic composites offer many advantages such as improved environ-
mental resistance, increased interlaminar toughness, and enhanced damage
tolerance. Among the new resins, Polyether-ether ketone (PEEK) has been
proposed as a matrix for structural composites. PEEK can also be welded,
reprocessed, and indefinitely stored at room temperature (Kenny et al., 1989).
On the other hand, PEEK has higher viscosity than thermosetting resins. The
high viscosity of PEEK makes it more difficult to be impregnated into a 3-D
preform. To overcome this difficulty, the hybrid yarn technique appears very
promising. During this process, the reinforcing fibers are woven together
with thermoplastic fibers. PEEK resin already in the preform is consolidated
by the application of heat and pressure. Different combinations between
pressure, temperature, and time will result in different void content in the
composites and different shapes of the Z yarn. The void content dictates the
properties of the composite. Voids can be starting points for crack propagation
in composites. In addition, expansional mismatch between fibers and matrix
causes residual stresses which manifest themselves in unusual thermal
expansion behavior, premature plycracking, delamination, and warping of
unsymmetrical laminates (Kim et al., 1989).

29
30

3-D MULTI-LAYER FABRIC FORMATION

There are many ways to incorporate the reinforcing fibers into composites.
One of them is 3-D weaving. In 3-D weaving, several layers of warp and filling
yarns are stacked and held together by Z yarns to achieve thickness.
Thus 3-D fabrics not only have a three-dimensional shape, but also have yarns
in all three directions (Mohamed et al., 1988). 3-D structures are produced by
means of several techniques (Mohamed, 1990). The structures used in the
present study were produced using a manually operated experimental rig
shown in Figure 1, which follows a process similar to that of traditional
weaving. The warp yarns (X-direction) are arranged in multiple layers. Each
two layers form a fixed shed. The filling yarns (Y-direction) are inserted into
the sheds by a number of needles equally spaced from each other. Z yarns
which are controlled by two or more harnesses are arranged parallel to the
warp yarns with the required frequency for the specific structure. An auto-
mated machine using the same principles of the above rig has been described
by Mohamed et al. (1989). This machine is capable of producing 3-D thick
walled shapes.
Structures obtained by the above process are 3-D orthogonal weaves with
doubled filling yarns (Mohamed et al., 1989), as shown in Figure 2. Since there
is no interlacing in the internal structure, there is little or no yarn crimping
(i.e., the yarns remain straight). The interlacing occurs only at the surfaces
where the yarns change direction.

CONSOLIDATION PROCEDURE FOR CARBON/PEEK

In order to determine which combination of process parameters produces the
best results, several consolidation treatments were used. The treatments are
combination of pressure, temperature, and time. Consolidation pressure was
set at three different levels; 250, 375, and 500 psi. Consolidation temperature
was set also at three different levels; 700, 750, and 800°F. Consolidation time
was set at three different levels; 30, 60, and 90 minutes. Each sample was set
in the mold by placing it between two platens of a press. The consolidation
pressure was held constant during consolidation. For each different pressure
the temperature was raised up from 100°F to the desired level at 50°F intervals.
In order to obtain an even heat distribution, the temperature was kept for two
minutes before allowing it to increase again. When the temperature reached
the desired level, it was maintained for the desired duration (30, 60, 90 min-
utes), and then reduced to room temperature during a 20-minute period.

TESTING PROCEDURE
The consolidated samples were tested on an Instron tester. Three points
bending test was applied to the samples, the span length of the tester was two
inches with support diameter of 0.5 inch. Twenty pounds full scale load with
0.02 inch per minute crosshead speed was used to measure bending modulus
of the samples. A 500 lbs full scale load and 0.1 inch per minute crosshead
speed were used to measure the bending strength of the samples. Consoli-
dated samples were cut one inch long in the warp direction. Each sample
 31
was molded in Polyester resin. The molded samples were polished from the
roughest grind to the finest alumina particles. These samples were then
examined by light microscopy.

RESULTS
The consolidated samples were examined using a microscope. The X- and Y-
direction cross sections are shown in Figure 3. It can be seen that the matrix
distribution is not similar for each treatment, especially when using different
pressure for consolidation. The higher the applied pressure, the more uni-
form is the matrix distribution. For all treatments, the voids tend to be concen-
trated in the body of the yarn and at the spaces of the orthogonal arrangement.

The voids are spread out not only in the empty spaces between yarns, but also
in the body of the yarns (X, Y, and Z). The size and frequency of the voids are
reduced by increasing the consolidation pressure; the best result was obtained
at 500 psi pressure. On the other hand, the smaller the applied pressure, the
straighter are the Z yarns.
Figure 3 shows that the shape of the Z yarns changes for different pressure:
the Z yarns at 500 psi bend at several points. The Z yarns, shown in Figure 3,
are bent both in the X-Z plane and the Y-Z plane. This is due to the empty
spaces in an orthogonal arrangement of yarns. The Z yarns bend toward the
empty available spaces when the sample is compressed during consolidation.

Bending Modulus and Bending Strength

The effect of processing variables on the mechanical properties are discussed
in the following: The effects of consolidation temperature are shown in Figure
4; both the bending modulus and bending strength increase with the increase
of the processing temperature.

The effects of consolidation time are depicted in Figure 5; both the bending
modulus and bending strength corresponding to 250, 375, and 500 psi
treatments increased when the consolidation time was extended from 30 to 90
minutes. This could be attributed to the better fiber and matrix bonding which
occur after the initial 30 minutes of consolidation. Thus the bending modulus
and bending strength are controlled by the length of time during which the
matrix remains at a temperature higher than its melting point provided that
other processing parameters are kept constant. Figure 6(a) illustrates the
relationship between the consolidation pressure and bending modulus. Figure
6(b) shows the relationship between consolidation pressure and bending
strength. Both bending modulus and bending strength increase with the
increase of consolidation pressure. The increase of bending modulus from 250
to 375 psi consolidation pressure is very substantial, but the increase of
bending modulus from 375 to 500 psi is not large. Figure 3 shows the various
aspects of cross section specimens. The higher the pressure applied during
the consolidation process, the more uniform is the distribution of the matrix in
the cross section. According to Maekawa et al. (1989), the bending modulus
and bending strength linearly decrease as void volume contents increase.
Furthermore, Maekuma et al. (1989) mentioned that the bonding between the
32

fibers and matrix was developed further if the fibers are dispersed in the
matrix. The results obtained in this work confirm their findings.

CONCLUSIONS
Within the range of temperature, pressure, and time investigated here, it is
clear that the modulus of elasticity and the bending strength are increased
with the increase of the three parameters. The effect of consolidation time on
the final properties appears to be more important than that of the temperature
provided the temperature is above the melting point of the matrix. Pressure
plays an important role in determining the matrix distribution and the void
content. The higher the pressure, the better is the PEEK distribution within
the composite. The only disadvantage of high pressure is the increased buck-
ling of the Z-yarns which may affect the impact resistance of the composite.

ACKNOWLEDGEMENTS
This work is partially supported by NASA under grant No. NAGW-1331 to the
Mars Mission Research Center.

REFERENCES
Kenny, J., D'Amore, A., Nicolais, L., Iannone, M., and Scatteia, B. (1989).
Processing of amorphous PEEK and amorphous PEEK based composites.
SAMPE Journal, 25(4), July/August.
Kim, K.S., Hahn, H.T. and Croman, R.B. (1989). The effect of cooling rate on
residual stress in a thermoplastic composite. J. Composite Technology and
Research, 11(2), 47-52, Summer.
Maekawa, Z., Yokoyama, A. and Hamada, H. (1989). Mechanical properties of
comingled yarns composite. Proc. 1st Japan International SAMPE
Symposium, November 28-December 1, 1989.
Maekuma, H., Kubomura, K , Ohsone, H., Tsuji, N. and Herai, T. (1989). A
study of processing of thermoplastic powder impregnated carbon fiber
prepreg. Proc. 1st Japan International SAMPE Symposium, November 28-
December 1,1989.
Mohamed, M.H. (1990). Three-dimensional textiles. American Scientist, 78,
530-541, November-December.
Mohamed, M.H., Zhang, Z. and Dickinson, L. (1988). Manufacture of
multilayer woven preforms. Advanced Composites and Proc. Techn.;
ASME-MD-Vol. 5.
Mohamed, M.H., Zhang, Z. and Dickinson, L. (1989). 3-D weaving of net
shapes. Proc. 1st Japan International SAMPE Symposium, November 2 8 -
December 1,1989.
 33

Z yarn

filling

Fig. 1. 3-D weaving apparatus. Fig. 2. 3-D orthogonal structure.

Fig. 3. Warp yarn cross-section: (a) 250 psi; (b) 375 psi; (c) 500 psi;
Filling yarn cross-section: (d) 250 psi; (e) 375 psi; (f) 500 psi.
34
60-

50-
7-\
40-
6
30- Press. 250
5
Press. 250 Press. 375
20- Press. 375 Ή Press. 500
Press. 500
10· 3

650 700 750 800 850 650 700 750 800 850
Temperature ( ° F ) Temperature ( F)
(a) (b)
Fig. 4. (a) Relationship between bending modulus and con-
solidation temperature; (b) Relationship between
bending strength and consolidation temperature.

60 Ί
8. 8
Jt 50 H
o j 2 7
*. 40-j
LU j
| 30 J- Press. 250
O I- Press.375
Press. 500

o-
30 60 90
Time (mn)

(a) (b)
Fig 5. (a) Relationship between bending modulus and con-
solidation time; (b) Relationship between bending
strength and consolidation time.

50
Q-

o
§ 30

% 20
■σ
o Time. 30
E
? 10 Time. 60
Time. 90
0
20Ό 25 0 3 00 350 400 450 500 55 0 200 250 300 350 400 450 500 550
Pressure (psi) Pressure(psi)

(a) (b)
Fig. 6. (a) Relationship between bending modulus and con-
solidation pressure; (b) Relationship between bending
strength and consolidation pressure.
 WS9a6

COMPOSITE PLATE OPTIMIZATION - SINGLE PARAMETER PROBLEMS ?

Joachim L. Grenestedt
Japan National Aerospace Laboratory, Airframe Div.
Jindaiji Higashi-machi 7-44-1, Tokyo 182, Japan

ABSTRACT
A number of results concerning layup optimization of composite material plates are presented The layup
was the same over the whole plate. There was supposed to be no coupling between in-plane stresses and
out-of-plane deformation, but otherwise full degree of freedom was given to the ply angle variation
through the thickness. The object functions were, respectively, free vibration frequency, buckling load,
or deflection under a pressure perpendicular to the plate surface. By numerical simulations of a large
number of rectangular orthotropic plates with various loadings and boundaries was it seen that the
optimal designs always were angle-ply laminates (+/-oc), thus governed by a single parameter.

Bounds based on energy theorems were used for showing that for clamped plates with one symmetry do
non-zero bending-twisting coupling stiffnesses never make the plate perform better, so the optimal
design is orthotropic, and, as said, numerical simulations showed that the optimal orthotropic layups
were angle-ply.
An example of a non-symmetric loading of a non-orthotropic laminate is presented, shear buckling of a
rectangular plate. Numerical optimization lead to an off-axis unidirectional layup, thus again leaving
only a single parameter for the optimization task, the off-axis angle.
One orthotropic configuration whose optimal layup is not an angle-ply is presented, the round plate
under circular symmetry, whose optimal layup is isotropic.

KEYWORDS
Composite material, plate, optimization, vibration, buckling, bending deflection

GOVERNING EQUATIONS
In the present study are the laminates supposed to lack coupling between in-plane stresses and out-of-
plane deformation (By=0). Examples are symmetric layups. The governing differential equations are
thus un-coupled and only the out-of-plane equations are needed. The elastic constants needed are the six
bending stiffnesses, D u , D12, D22, Ü66, Di6, and D26.
With the operator L(w) defined as
35
36

L ( w ) = ^4 4 D161 6 3| ^ + 2 v^12 + 2 D ^ 4D *"

ax ôx ay "Way 2 ^axay3
+

+D
a*w
2 2 T - 4T
ay (D
do the governing equations take the following form :

vibration L(w) = ρω 2 w, Q)

ôw XT owl d
buckling L(w) = — XTNvx — + N , — + — LN y^ay + N** ^
dx k a x ^ ö y j ay dx (3)
bending deflection L(w)=p, p= pressure. (4)

The object function is the square of the lowest vibration frequency, ω2, for the vibration optimization
task.
For the buckling optimization is it supposed that all loads are increased proportionally and independent
of the layup,

(Ν,,Ν,,Ν,,ΜΝ',,Ν;,^! (5)

where primed quantities are some reference loads. The load factor y when instability occurs is taken as
the object function.

For a plate subjected to forces perpendicular to the surface is the object function defined as

ΓΓ pwdxdy
R =
Π |p|dxdy
(6)
which is a weighted average deflection. The pressure p is supposed to have the same sign (positive or
negative) over the whole plate.

ELASTIC CONSTANTS
The optimal layups were searched through all possible combinations of the elastic moduli, i.e. there was
no limitation such as a fixed number of plies. The six bending stiffnesses are not independent but
functions of four lamination parameters, which can describe any possible layup, (Tsai and Hahn, 1980),
WitoW 4 :

12 ^ 2 2 3r *2 *
Wiu3,4] ïT Icos2a,cos4a,sin2ot,sin4ajz dz = ^ Icos2oc,cos4a,sin2a,sin4ajz dz ,
=
(7)

where a is the layup angle, which is a function of the z coordinate. Tsai and Hahn, 1980, normalized
the lamination parameters differently. The bending stiffnesses take the form
 37
D; I = U 1 + U 2 W 1 + U 3 W 2 ,

D ; «U, - U2W, + U3W2, D1111 =D n , Ώηη ^D«,

D;=U 4 -U 3 W 2 , D111^, D^-D*.
D*« = i ( U , - U«) - U 3 W 2 , D1122 = A 2 D 2222 = ^
ijU iik 1
D* =iU 2 W 3 + U3W4, D =D =Ό™ -D* ,
D^ ="5U2W3 - U3W4, other terms aie zero, (g\

where Dy*=12Dij/h^ and h is the thickness of the laminate, U1-U4 are linear combinations of the on-
axis moduli of a lamina and can be considered as material constants. IW^ is a two-dimensional bending
stiffness tensor.
Throughout this paper were three material systems used, carbon/epoxy (T300/5208), aramid/epoxy
(Kevlar 49/epoxy) and glass/epoxy (Scotchply 1002), Tsai and Hahn, 1980.

ORTHOTROPIC LAMINATES
In this case are D i6 and D26 zero, leaving only two optimization parameters, Wi and W2. In some cases
can closed form solutions be obtained, e.g. for a simply supported plate with the dimensions a and b is
the lowest free vibration frequency

2 π4
ω - — Ai-^4 + 2(A2 + 2 D 6 6 ) i i r + D 2 2 i ·
(9)
This expression is linear in the bending stiffnesses, and these are linear in the non-zero lamination
parameters Wi and W2, so obviously will the optimal design be found on the border of the allowable
region of these lamination parameters. This border corresponds to an angle-ply laminate (+/-<x)
according to Miki, 1985, and the optimization task has become a single parameter problem.
Using brute force and a lot of numerical calculations has it been seen that the same holds (i.e. that the
optimal design is an angle-ply laminate) for rectangular orthotropic plates with a number of different
boundary conditions, e.g. (SSSS, SCSC, CCCC) concerning vibration optimization, (SSSS, SCSC,
CCCC, SSSF) concerning uniaxial homogeneous compression, (SSSS, SCSC, SSCC, CCCC)
concerning bending deflection under a constant pressure, and (SSSS, CCCC) œnœrning homogeneous
shear buckling. The four capital letters represent the boundary conditions of the four edges, S=simply
supported, C=clamped, F=free edge. In each case were approx. ten plate aspect ratios a/b investigated,
and three material systems.

ENERGY THEOREMS AND BOUNDS

Vibration

Using Hamiltons theorem, the vibration frequency ω is found for the deflection function that minimizes

JTwdxdy
2
2
ω =—
P II w 2 dxdy
(10)
where the strain energy per area is
38

W = - D^ w,jj Wjy = {orthotropic part ) + 2

a2W ^ (?w ^ &w]
16 Q 2 26 2
dxdy d
(11)
An approximate w(x,y), fulfilling the boundary conditions, will overestimate the vibration frequency.

Buckling

The critical load factor γ is found for the deflection function w(x,y) that minimizes

2JTwdxdy
' J(N' x (wJ 2 + N;(w^) 2 + 2N;w,w^)dxdy

The absolute value of the true load factor γ will be smaller than any estimate obtained by using an
approximate deflection function which fulfils the boundary conditions.

Bending Deflection

Using Clapeyrons theorem is it seen that the object function R can be written as

IT pwdxdy JTwdxdy
Ί 2
"JJ^^~" ] | |p|dxdy
|p|dxdy " 2 JJ|p|dxdy
(13)
The deflection function w(x,y) is obtained by minimizing the potential energy

U= IT Wdxdy - IT pwdxdy = --^R (T|p|dxdy

JJ JJ 2 JJ (14)

An approximate deflection function w(x,y) will result in a potential energy U larger than the true value,
so the true deflection R will be larger than the approximate deflection. A lower bound on the deflection is
thus obtained.

CLAMPED PLATES, ONE SYMMETRY, EFFECTS OF D i 6 AND D26

We suppose that the deflection function wort(x,y) of an orthotropic laminate has at least one symmetry or
anti-symmetry, which is often the case when the loads and boundaries have at least one symmetry (there
are exceptions). We further suppose that the boundaries are clamped. We can then get bounds on the
object functions of a laminate with non-zero bending-twisting coupling stiffnesses Di6 and/or D26 by
substituting the deflection function of an orthotropic laminate with identical Du, D12, D22, and Ü66
stiffnesses in Eq. ( 10)-(14) for the non-orthotropic laminate. Since it was supposed that the boundaries
were clamped do the orthotropic deflection function wort(x,y) fulfil the boundary conditions of the non-
orthotropic laminate (the deflection and its normal derivative are zero on the edges).
Because of the symmetry/anti-symmetry of the approximate deflection function wort(x,y) do the terms
multiplied by Di6 and D26 in the strain energy, Eq. ( 11), vanish when integrated over the plate, so these
approximations yield identical object functions as for the orthotropic laminates. Since our tasks were to
 39
maximize vibration frequency, maximize buckling load, or minimize bending deflections,
respectively, is it seen that for neither task are non-zero bending-twisting coupling stiffnesses ever
beneficial.

A NON-SYMMETRIC EXAMPLE - SHEAR BUCKLING

Non-zero Di6 and D26 terms give a rectangular plate a preferred direction of shear - in one direction will
the shear buckling load be higher than for the corresponding orthotropic laminate, and in the other
lower. Using finite difference calculations and optimization by non-linear programming was it seen that
the optimal layup for all length/width ratios was off-axis unidirectional, i.e. this is also a single
parameter optimization task, the parameter being the off-axis angle. For further details see Grenestedt,
1990.

ROUND PLATE
With the same arguments as was used to show that Di6 and D26 are not beneficial for clamped plates
with one symmetry will it now be showed that round clamped plates with such loadings that the
deflection of an isotropic laminate is a function only of the radial coordinate, is the isotropic layup
optimal. For isotropic layups are all lamination parameters zero.
It is sufficient to show that the strain energy for a non-isotropic plate when the deflection function of an
isotropic plate is assumed is the same as that of the isotropic plate, and then use the bounds described
above. First, it is clear that Di6 and D26 terms are not beneficial since the round isotropic plates have the
earlier stated symmetries, and they are therefore set to zero.
The strain energy per area in general curvilinear coordinates is expressed as

wW"J-Iil-H*4£S§f»-S1 (15)
where a vertical dash represents covariant derivation, and entities with a dash above are entities in the
curvilinear coordinates Θ1. The bending stiffness tensor jy^^ is constant in Cartesian coordinates θ*.
Using lamination parameters the strain energy expression takes the form

ddld& ,
w
οθ^θ 1 bj (16)
With polar coordinates

(17)
do the covariant derivatives of the isotropic deflection function take the form

(18)
and the coordinate transformation coefficients are
40

aff2"
1 cosS2 -^rsinü 2
ae dQ1

dQ2 *-«■.
inS 2
sin
Lao2 ae2J (19)
Eq.(18) and (19) in (16) gives

I ΛΧ
7

T = W
\2
I c o s ^ e ^ - s i n ^ e 2 ) ] , and
' 2
(20)

[cos 2 (26 2 )-sin 2 (2ë 2 )j.

■k-i e,J (21)
The total strain energy is the integral of Eq. (16) over the plate, but the integrals of Ti and T2 are zero
(integration over 2π of the terms containing "2 are zero) so the strain energy is the same as that of
the isotropic plate, which was what had to be shown to prove that the isotropic layup is optimal.

SUMMARY AND CONCLUSION

Optimization of rectangular composite plates concerning maximization of fundamental free
eigenfrequency, maximization of buckling load, and minimization of deflection under pressure
perpendicular to the surface was studied. A large number of numerical simulations for rectangular plates
were performed. The results suggest that the optimal layups always are angle-ply (+/-oc) when effects of
non-orthotropy are neglected (i.e. Di6 and D26 are zero). In the case of shear buckling were the Di6 and
D26 stiffnesses included, and numerical optimization revealed that the optimal layups were off-axis
unidirectional laminates (a).

One example was presented for which the optimal layup is neither angle-ply nor off-axis UD, the round
plate under symmetric conditions for which the optimal layup is isotropic.

ACKNOWLEDGEMENTS
The author acknowledges Peter Gudmundson for the round plate idea, and Tokio Kasai for
computational consultations.

REFERENCES
Grenestedt, J.L. (1990). Layup Optimization against Buckling of Shear Panels. Structural Optimization
(to be published).
Miki,M. (1985). Design of Laminated Fibrous Composite Plates with Required Flexural Stiffness. In:
Vinson,J.R. and M. Taya (eds.), ASTM STP864.387-400. Philadelphia: ASTM.
Tsai, S.W. and H.T. Hahn (1980). Introduction to Composite Materials. USA: Technomic Westport
CT.
 WS9a7
STRENGTH OF METAL-FRP BONDED JOINTS
UNDER THERMAL CYCLE

Takao MORI *
Qiang YU **
Masaki SHIRATORI **

* Advanced Technology Research Center, NKK

Corporation, 1-1 Minamiwatarida-cho,
Kawasaki-ku, Kawasaki, 210 Japan.
** Dept. of Mechanical Engineering, Yokohama
National University, 156 Tokiwadai,
Hodogaya-ku, Yokohama, 240 Japan

ABSTRACT

This paper presents a set of results in numerical and experimental analyses

on the thermal fatigue strength of metal-FRP bonded joints. Numerical
analyses, thermal conduction analyses and thermal stress analyses were
performed by FEM. A prototypical thermal cyclic testing apparatus for metal-
FRP bonded joints was fabricated, and experimental analyses were carried out
under several levels of thermal cycle by using the apparatus. It has been
found that remarked thermal-stress concentrations at the ends of the
adhesive layer, and the thermal fatigue strength of the joints can be well
explained by the maximum equivalent thermal stress at the adhesive layer.
Besides, the residual strength of the joints affected thermal cycle
decreases in proportion as the number of cycle.

KEYWORDS

Metal-FRP Bonded Joint, Thermal Stress, Mises' Equivalent Stress, Stress

Concentration, Thermal Cycle, Fatigue Strength

INTRODUCTION

The authors have been proposed a strength criterion for the metal-FRP bonded
joints that a fracture of the joint occurs when a maximum equivalent stress
at the adhesive layer reaches a critical value at both room temperature and
low temperature (Shiratori et al., 1988, Mori et al. 1990). At low
temperature, the equivalent stress has to contain the thermal stress
resulting from a difference of material properties between metals and FRP.
It is also very important to consider thermal stress for the strength of
metal-FRP bonded joints under thermal cycle.

In this paper, thermal conduction and thermal stress analyses were conducted
to estimate stress distribution Aluminum-CFRP bonded joints under thermal
cycle. Then a prototypical thermal cycle testing apparatus was fabricated to
gain enough experimental data in a short time and the thermal cyclic tests
for the joints were carried out under several levels of thermal cycle to
41
42
confirm the thermal fatigue strength. An equivalent stress concept gave
good agreement to experimental results.

NUMERICAL ANALYSES

By using a finite element method (FEM), thermal conduction analyses and

thermal stress analyses were conducted on a combination of joint
constituents;
Al-CFRP : Aluminum alloy a-5083 and uni-directional CFRP
(Torayca T-305 + epoxy) made by hot press method

Table 1 Physical properties

Temperature Material Young' s Shear Poisson* s Cofficient of

modulus modulus ratio thermal expansion
(°C) (GPa) (GPa) (1/°C)
Aluminum 70.6 20.5 0.33 2.2X10" 5
Adhesive 0.20 0.07 0.30 4. 2 X 1 0 -75
23 x: 109 xy: 3.8 xy: 0.35 4.0X10- 5
CFRP y : 7.6 y z : 0. 33 3.2X10- 5
z : 7.6 zx: 3.8 zx: 0.024 2.8X10-"
Aluminum 80.4 27.0 0.33 2.2X10- 5
Adhesive 4.60 1.93 0.30 4.2X10- 75
-100 x: 116 xy: 4 . 5 xy: 0. 35 4.0X10" 5
CFRP y : 10.3 y z : 0. 33 3.2X10" 5
z : 10.3 z x : 4. 5 zx: 0.024 2.8X10"

Table 1 shows t h e p h y s i c a l p r o p e r t i e s of c o n s t i t u e n t m a t e r i a l s a t room

t e m p e r a t u r e ( 2 3 e C ) and a t -100°C. The a n a l y z e d j o i n t s were s i n g l e - l a p joints
a s shown F i g u r e 1.

ΧΊΟ |
Off'l
Δffy
AdhesiveN 2C o Dff z
OL
• r xy
/ ■
'
x Off
Al • ^ο^, i ! I ^ c
CFRP r^£2?:*l£?roco o e o e w e w o cyxDC<£^^osrft\>-

I 2c 3 j "~*-·*.
j

2C=12.5 ti =3
l+2C=100 t2 =3 j
x -15 —
h=0.05
I
x/c

Figure 1 Single-lap bonded joint Figure 2 Thermal stress distributions

along adhesive layer
 43
Figure 2 shows the distribution of stresses due to the temperature change
from 23*C to -100*C. Because of a great difference between the coefficient
of thermal expansion of Aluminum and that of CFRP, shear stress and Mises'
equivalent stress have considerable concentrations at the edges of adhesive
layer. Here the maximum equivalent stress is defined as the average of
stress at the region (l-2)h from the edge, where h is the thickness of the
adhesive layer. The maximum equivalent stress is effected by the thickness
of Aluminum plate and it increases as the plate becomes thicker. Thus
different levels of the maximum equivalent stress in the adhesive layer can
be gained at the same thermal cycle condition by changing the thickness of
Aluminum plate.

A PROTOTYPICAL THERMAL CYCLE TESTING APPARATUS

Thermal cycle test has been often conducted by using several methods such
as; (1) immersing test specimens in a hot bath and a cool bath repeatedly,
(2) heating and cooling test specimens repeatedly in the same bath. Both
methods need a long time for one cycle, so it will be difficult to gain
enough test data for examining a basic criterion in thermal fatigue
strength.

Since the coefficient of thermal expansion for the fiber direction of CFRP
is nearly zero irrespective of temperature, the thermal cycle test of
Aluminum-CFRP bonded joints can be performed by cooling and heating only the
Aluminum plate. Besides, Aluminum has a very large thermal conductivity and
a small specific heat, so the time of thermal cycle tests can become shorter
with this method.

RDwer ^ Diffusing pipes Setting plates

)Spong\ Test spec±nen /

[ob o o\\Z^
Base plate
Fancqp
Nonconducting layer

Figure 3 Thermal-cycling test apparatus

The prototypical apparatus based on the above idea is shown in Figure 3 (L.
F. Coffin et al., 1954). Heating is accomplished by allowing the Aluminum
plate to serve as its own heater and by passing current through it, and
cooling is accomplished by radial nitrogen gas using a diffuser consisting
of a closed-end tube with several radial holes. The Aluminum part of the
joint specimen is attached between two setting plates, which are supported
by springs,, so that the Aluminum part can make a free thermal expansion
horizontally. Braided power cables are attached directly to these setting
plates. From the electrical resistance of Aluminum and maximum heating rate
desired, a current transformer with a secondary winding, supplying 2.0 volts
44
at 1000 amperes, is required. A solenoid-operated valve is used to supply
the nitrogen gas coolant to the diffuser during the cooling phase. A
thermocouple, measuring the temperature of the point A as shown in Figure 1,
is connected to the temperature controller. The temperature amplitude is
controlled by the temperature controller and the time-delay relays. When the
temperature of the point A reaches the lower limit of the temperature
amplitude, cooling nitrogen gas stops and heating starts after some
interval. This apparatus can test 6 specimens at the same time.

THERMAL CYCLE PATTERN

The temperature distribution in the adhesive layer is not uniform during

thermal cycles. This would effect the thermal stress distributions in the
adhesive layer. Then, non-steady state thermal conduction and thermal stress
analyses ought to be performed to evaluate the thermal stress distributions
in the adhesive layer accurately.

The temperature distributions in the adhesive layer were analyzed for the
cooling and keeping phases. The boundary conditions were defined as that the
surface of ALuminum plate has a constant coefficient of heat transfer and
that of CFRP plate was a insulating layer. This is because the thermal
conduct of CFRP is so slight that its effect on the adhesive layer can be
ignored. The results of analyses are shown in Figure 4. For the cooling
phase (from 0 to 70 seconds), the temperature has a nonflat distribution in
the adhesive layer. But it can be removed by giving a lower limit keeping
phase (from 70 to 100 seconds). The temperature distribution at 100 seconds,
after a 30 seconds keeping phase, is almost uniform along the length of
adhesive layer and becomes near steady-state. The time of both cooling and
keeping phase depend on the thickness of Aluminum plate. The longer keeping
time is necessary to gain a uniform enough temperature distribution for the
thicker Aluminum plate joint.

Figure 4 Effect of time on temperature Figure 5 Effect of time on thermal stress

distribution over adhesive layer distribution over adhesive layer

The distributions of thermal equivalent stress in the adhesive layer are

shown in Figure 5. The thermal stress distribution at 100 seconds represents
good agreement with at steady-state. Therefore, the thermal cycle pattern,
 45
which contains keeping phase, was decided appropriately.

EXPERIMENTS

In order to confirm thermal fatigue strength of Al-CFRP joints, thermal

cycle tests were carried out for single-lap joints(the thickness of Aluminum
plates are both 3mm and 6mm) under three thermal cycle patterns(from room
temperature to -100 °C, -125eC and -196°C). Table 2 shows the number of
cycles to failure. The numbers decrease as the temperature range becomes
larger and the thickness of Aluminum plate becomes thicker.

l£ r
Table 2 Cycles to failure
0 ti=3mm
10 i O
D ti=6mm
-
0
8 D
□ o -
o
temperature t i = 3mm t i = 6mm Q_
D
amplitude 5
6 ' D° O -
23—100°C 3.93X10' 2.72X10' o O
1.04X10* 4.65X10' D 0
7.63X10'
1.48X10*
2.12X10* 9.81X10'
4 - D □ o ° J
D
7.16X102 Q
23—125°C 0
1.03X10' 2 □ \
1.98X10' a
D

23—196°C 1.46X102 9.31X101 0 i_

L5
Π Œ)
md
2.43X102 4.82X101 10 z
5x10* 10 5x10s 104
Cycles

Figure 6 Residual stregth after

thermal cycling

Figure 6 shows the relationship between the residual strength of the joints
at room temperature and the numbers of thermal cycles. The strength is
defined by nominal stress sf=P/s, where P, s are the breaking load and the
area of bond respectively. In this series of tests, the lower temperature
was -100 *C and the upper temperature was 20 *C. The residual strength
decreases as the numbers of cycles become larger and the thickness of
Aluminum plates become thicker.

THERMAL FATIGUE STRENGTH

The static strength of metal-FRP bonded joints can be well estimated by the
maximum equivalent stress in the adhesive layer. Figure 7 shows the
relationship between the maximum thermal equivalent stresses in the adhesive
layer by numeric analyses and the numbers of thermal cycles to failure by
experiments. The relation, which compares to S-N curve, is represented as
only a near line irrespective of the thickness of Aluminum plates and the
temperature ranges. Therefore, thermal fatigue strength of Al-CFRP joints
can be estimated by the maximum equivalent stress concept.
46

300 —r— 1 1
eti=6mm, 23—196*C
© ti=3mm, 23—196*C
β Ö • ti=6mm, 23—125*C
0 Q «>ti=6mm. 23—lOO'CJ
200 <Mi=3mm. 23—100*c]

·· ·
c c CD J
lo 100 0 ΦΦ9 1

I « 1 1 . _

10' 10e 10' 104 10e 10e

Cycles t o failure

Figure 7 Relationship between O and

cycles to failure

The difference of the residual strength at room temperature after thermal

cycles between Aluminum thickness 3mm and 6mm can be explained by the
maximum equivalent stress as well as the thermal fatigue strength. The
numbers of thermal cycles give a damage to the residual strength, so it is
very important to consider the effects of thermal cycles.

CONCLUSIONS

In order to examine the thermal fatigue strength of metal-FRP bonded joints,

a prototypical testing apparatus was fabricated and both numerical and
experimental analyses of Al-CFRP single-lap bonded joints under several
thermal cycles were carried out. Thermal fatigue strength of bonded joints
can be well estimated by the equivalent stress concept as well as static
strength of the joints at both room temperature and low temperature, and S-N
curve by using maximum equivalent stress becomes only a linear line
independent on joint thickness and temperature ranges. And residual strength
of bonded joints are also affected by thermal cycles. It is very important
to consider thermal stresses under thermal cycles for applying metal-FRP
bonded joints to structural elements.

REFERENCES

(1) L.F.Coffin and R.P.Wesley, Apparatus for study of effects of cyclic

thermal stresses on ductile metals. Trans. ASME, Vol.76,1954,923.
(2) Shiratori, M. and Mori, T. Stress analysis and design of metal-FRP
bonded joints. Trans. Jpn. Soc. Mech. Eng., Vol.54, No.503,A(1988), P.1404.
(3) Mori,T., Yu, Q., Takehana,S., Shiratori,M., Low-temperature strength of
metal-FRP bonded joints. Trans. Jpn. Soc. Mech. Eng., Vol.56, No.523(1990-
3), P.437.
(4) 0da,J. and Nayuki,T. The finite element method for adhesive bonded
structures and its applications. Trans. Jpn. Soc. Mech. Eng., Vol.50,
No.450(1984-2), P.242.
(5) Sugibayashi, T. and Ikegami, K. Trans. Jpn. Soc. Mech. Eng., Vol.50,
No.451(1984-3),P.373.
 WS9bi Interphase Engineering
of
High Performance, Polymer Matrix Composites

Hatsuo Ishida
Department of Macromolecular Science
Case Western Reserve University
Cleveland, Ohio 44106-1712

INTRODUCTION
High performance composite materials have attracted an intense interest among mate-
rials scientists during the past few decades as a novel group of materials which were suitable
and often desirable alternatives to metallic materials. At first, there was some resistance to use
composite materials in critical applications due primarily to a lack of availability of engineering
data. In recent years, the recognition of high performance composites as reliable materials is
no longer a dominant obstacle for their application. In fact, such critical applications such as
those found in the aerospace community have advanced the performance of the products be-
yond what metallic materials can potentially achieve. However, the traditional trial-and-error
developmental approach remains to be a problem. Furthermore, the majority of composite
research, including high performance composites, is done from a mechanical point of view,
while the fundamental molecular and chemical aspects of the materials are mostly ignored.

High performance composite materials consist of two very dissimilar materials. The
modulus and strength ratios of the reinforcing fiber and the matrix resin are usually much
higher than those of typical commodity composite materials. It is now well recognized that the
fiber/matrix interface/interphase plays an important role in the mechanical and physical prop-
erties of composites. At this point, we must clearly define the terms "interface" and
"interphase". An interface is the hypothetical plane at the border of two dissimilar materials,
and only when two materials are completely immiscible due to chemical or physical reasons
can this plane be clearly defined. Usually, few materials exist which meet the criterion for a
true interface, except when the chemical bonds connecting these two phases exist; these bonds
are often included in the concept of an interface. Bulk materials near the interface usually show
slightly different structures and properties from those further away from the interface due to the
physical and chemical interactions with the surface of another phase, giving rise to a gradient
structure. This interfacial region is termed "interphase." Specifically, an interphase is
comprised of a distribution of corresponding materials of unspecified thickness which depends
on the chemistry and processing conditions of the system. Schematic diagrams of these two
concepts are shown in Figure 1.

The concept of interphase was, to the author's knowledge, introduced by Sharpe in

1971 in relation to the adhesion of coating materials. (1) The concept was later applied to
composite materials in late 1970's by Manson and Sperlin (2) and Ishida and Koenig (3). The
importance of the interphase is noteworthy especially in relation to the historical debate of the
reinforcement mechanisms of composites. Traditionally, the chemical bonding theory (4),
47
48

restrained layer theory (5), deformable layer theoryt (6), and many others have been proposed
in order to explain the role of the interface in reinforcing the composite. Only the chemical
bonding theory has received an overwhelming amount of supportive evidence. The other
theories were short lived because of evidence opposing their mechanisms. However, the
chemical bonding theory alone was insufficient to explain all observed phenomena, and was
later modified by adding the interpenetrating theory (7,8). This newly added theory suc-
cessfully explained the fact that the monolayer surface treatment of the reinforcing fiber does
not exhibit optimum strength in spite of the fact that the monomolecular equivalence coverage
is, in theory, sufficient to obtain maximum concentration of chemical bonds between two
phases.

A. Interface B. Interphase

Figure 1. Schematic diagram showing concept of interface and interphase in composite

materials. It should be noted that interphase can exist in any phase. The diagram shown
here indicates only matrix interphase. Also, the interphase/bulk boundary is drawn for
the purpose of clarity. The interphase usually consists of materials with structural
gradience so that the interphase/bulk interface is a diffuse boundary.

Along with the improved manufacturing technology of composite materials, the use
environments and subsequent requirements of the composites are much more severe than be-
fore. In order to manufacture composites suitable for the increased demands, complex
chemical and mechanical designs must be made. The commonly used trial-and-error approach
is no longer capable nor suitable for coping with such complexity, since the number of trials
will be astronomically large with the increased number of parameters. It is the purpose of this
paper to discuss a scientific way of manufacturing composites through systematic
interface/interphase studies. We term this approach as "interphase engineering".
Interphase engineering begins with an atomic/ molecular understanding of the inter-
face/interphase. Thus, controlling the interface/interphase structures is possible through ex-
tensive chemical knowledge. Finally, tailoring the desired composite properties is done in
combination with the understanding of the structure/property relationship. In this paper, ex-
amples of a general interphase engineering approach with special emphasis on high perfor-
mance composites will be shown, although different systems are chosen in each category in
order to demonstrate the breadth of the research.

INTERPHASE ENGINEERING
A. Understanding the Interface/Interphase Structure

Characterization of the surfaces of reinforcing materials has made remarkable advances

in the past decade. Surface spectroscopic techniques such as x-ray photoelectron spectroscopy
(XPS), Auger photoelectron spectroscopy and secondary ion mass spectroscopy (SIMS) have
been used extensively to study carbon fiber surfaces. Atomic or near neighbor information can
 49
be readily obtained by these techniques and important insights have been obtained. Since there
techniques probe the uppermost few nanometers of a surface, they are truly effective in
elucidating the nature of the surface. Another class of techniques utilized are molecular
spectroscopic techniques, including infrared, Raman and nuclear magnetic resonance
spectroscopy (NMR). There techniques are useful for examining larger scale actrivity such as
that found in an interphase. In this paper, a few examples of the application of vibrational
spectroscopic techniques on the characterization of high strength fiber surfaces will be
described. It should be noted that many techniques stated above are not in a strict sense
interface techniques. Some of them are surface-sensitive techniques and others are bulk-
sensitive techniques. However, with careful sample preparation, information from the
interfacial region can be emphasized and the structure of the region studied. The coating of a
very thin layer of matrix material on the reinforcing fiber is one such approach.

Studying the surface of carbon fibers has long been done by techniques such as XPS,
and nearest neighbor information has been reported. Extensive application of this technique to
the study of carbon fiber surfaces has provided us with rich information . We now know that
the surface is covered with hydroxyls, carbonyls, carboxylic acids, and lactones. The appli-
cation of vibrational spectroscopic techniques to the carbon fibers study of provides very im-
portant insights toward adhesion at the fiber/matrix interface since adhesion is more directly
correlated with molecular structure variation. Nonetheless, vibrational spectroscopy has rarely
been utilized in this area because of the great difficulty in observing surface species, which is
caused by the high absorption of the probing radiation. Recently, this difficulty has been
overcome by the application of Fourier transform infrared (FT-IR) attenuated total reflection
(ATR) spectroscopy. Optimum optical conditions were theoretically calculated (9) and the
surface species of the nitric acid oxidized carbon fibers studied (10) as shown in Figure 2.
Due to the enhanced intensity of the surface species by adopting a special optical configuration,
newly formed polar groups on the surface could be observed. Reduction of the carbon fiber
surface caused the expected elimination of bands which correspond to the polar groups as
indicated in spectrum B. Later, this technique was applied to the study of epoxy polymeriza-
tion near the carbon fiber surface (11). It was found that, when an epoxy primer was cured
around carbon fibers with different levels of surface oxidation, the polymerization of epoxy
resin can be accelerated where the concentration of surface polar groups is relatively low. On
the other hand, the polymerization was retarded for high concentrations of surface species.
This was attributed primarily to the preferential adsorption of the catalyst near the fiber surface.
Similar examples of preferential adsorption of amine catalysts of epoxy resins have been
reported for various composite and coating systems (12-15).

OXIDATION TIME (HOURS)

Figure 2. Comparison between the integrated intensity of the ester group (solid line) and
the carbonyl group of the surface species of oxidized carbon fibers (dotted line) as a
function of oxidative treatment of the fibers.
50

Another example of the surface study of reinforcing fibers is the application of diffuse
reflectance spectroscopy to poly(para-phenylene terephthalamide) fibers, otherwise known as
aramid fibers (16). Aramid fibers are considered to have a skin-core structure and the
molecules at the fiber surface are highly oriented. Adhesion of the matrix resin to the fiber is
poor due to inadequate molecular mixing and low chemical reactivity. A surface treatment is
sought that will increase the number of surface functional groups. Hydrolysis, for example,
may be useful for an epoxy resin matrix since the hydrolysis products of aramid fiber are
primary amine and carboxylic acid. In order to study the chemical reaction occuring at the
fiber surface, Fourier transform infrared diffuse reflectance spectroscopy (DRIFT) has been
utilized. A difficulty arises due to the abundance of information obtained from the bulk of the
fiber rather than the surface region alone. A new technique termed KBr overlayer diffuse re-
flectance spectroscopy was applied for the study. This technique involves covering the aramid
fiber surface with a layer of KBr powder of several particles thickness. By diffusing the angle
of incident light, the surface selectivity was dramatically increased. Representative spectra are
shown in Figure 2 where briefly hydrolyzed aramid fibers are examined with varying amounts
of KBr overlayer. The phenyl mode of the hydrolysis products at 883 cm"1 is enhanced as the
amount of the KBr overlayer is increased indicating the improved surface selectivity of the
technique. It also indicates that the hydrolysis is confined to the near-surface region, thus
avoiding damage to the bulk of the fiber.

Different samples necessitate different techniques for optimizing the ability to study the
surface region. Similar to the case with aramid fibers, very high molecular orientation and
crystallinity at the fiber surface make ultra-high modulus polyethylene fibers unfavorable for
adhesion with most matrices. Since polyethylene fibers are weak absorbers but strong
scatterers in the infrared, we have applied Fourier transform infrared diffuse transmittance
spectroscopy to their study (17).

950 900 850 800 750

WAVENUMBERS (CM"1)

Figure 3. Diffuse reflectance spectra of Kevlar-49 fibers hydrolyzed for 20 min in 10 %

by weight NaOH solution at ambient temperature with varying amounts of KBr
overlayer: (A) 60 mg KBr, (B) 40 mg KBr, (C) 20 mg KBr, and (D) no KBr.

Diffuse transmittance has long been regarded problematic in infrared spectroscopy due to its
loss of energy. Improved sensitivity and energy collection efficiency revived the usefulness
of what was once regarded as a troublesome technique. Due to the elimination of the specular
reflectance which causes spectral distortion in DRIFT, the perturbation caused by the molecular
orientation is essentially eliminated. Even a small orientation effect is large enough to disturb
surface studies since the information from the surface region is so small. The very high
sensitivity of this technique allowed the detection of the formation of carbonyl groups on
 51
polyethylene fibers after surface treatment by fuming nitric acid at 85 °C for 30 seconds.
Ordinarily, it requires a few hours of treatment at this condition to detect the formation of
carbonyl groups.
While the optimum technique must be sought for a particular system, it is clear that
we now have techniques which allow molecular characterization of reinforcement surfaces.
For more information concerning surface FT-IR techniques, a review article has been reported
elesewhere (18). Accurate determination of the surface structure is the starting point of
subsequent structural control of the interphase which is described in the following section.
B. Controlling the Interface/Interphase Structure
Surface treatments of reinforcing fibers can be regarded as attempts to control the in-
terfacial structure. Silane treatment of glass fibers, electrochemical oxidation of carbon fibers,
plasma treatment of aramid fibers, and corona discharge treatment of ultra-high modulus
polyethylene fibers all attempt to add surface reactivity towards matrix resins. These effects
are well documented in the literature (19, 20). In this paper, emphasis is placed on the
structural control of the interphase.
Thermoplastic-matrix composites are the subject of recent interests. While the chemical
bonding theory is frequently used to explain the reinforcement mechanism of thermoset-matrix
composites, chemical reactivity of a thermoplastic matrix towards the fiber surface is an
exception rather than a rule. Thus, thermoplastic-matrix composites require a different
reinforcement mechanism than chemical reaction with the surface. An important recent
recognition is that, for a composite with a semicrystalline matrix, the formation of a tran-
scrystalline zone provides a reinforcement mechanism. While the role of the transcrystalline
zone for the mechanical properties of composites has been a subject for controversy, there
seems to be a recent consensus that such a structure is favorable for improved mechanical
properties (21). However, the majority of studies of transcrystal formation have been from
qualitative points of view.
One of the useful quantitative approaches is the use of the heterogeneous nucleation
theory (22). However, this theory, as applied to transcrystal formation, makes use of the
measurement of nucleation rate as well as the growth rate of the transcrystals. While the
growth rate can be readily measured, the nucleation rate often cannot be measured due to the
massive nucleation at the fiber surface; however, these properties are known to be inversely
related. According to the theory of heterogeneous nucleation, the nucleation rate can be written
as:
I =I o . e x p ( - ^ ) . e x p ( - 1 6 ^ A g 5 ) [1]
kl
kTAT 2 Ah f ¥
where I is the nucleation rate at time t, Io a constant nucleation rate, k Boltzmann's constant, T
crystallization temperature, Δφ the activation energy of nucleation, Ahf the heat of fusion per
unit volume of crystal at the equilibrium melting point Tm°» and f the correction factor ex-
pressed by 2T/(Tm° + T). The energies, σ, ae, and Δσ, are defined in Figure 4.
Once heterogeneous nucleation has occured, the surface of the nucleus will grow by
adsorption and crystallization of polymer molecules. This process is also referred to as
secondary nucleation. The activation energy, Δφ, has a much smaller contribution to the
overall nucleation rate than the term due to thefreeenergy difference Δσ. This is particularly
true at low supercooling where the mobility of polymer chains is still high.
The subsequent growth process does not involve Δσ since no new surface is created.
Two cases, or regimes of growth, can be distinguished (23). In regime I, the completion of a
new layer is rapid compared to the rate of nucleation, whereas in regime II, multiple nucleation
52
occurs at the substrate surface before a layer is completed. The net growth rate, g, is ex-
pressed as:
Δφ. . βσσ 6 Τ&
g = go . exp ( - p £ ) . exp ( - -£ ) [2]
kT
kT ΔΤ Ahff
where go is a constant growth rate and bo is the thickness of a new layer, bo can be related to
the Miller's indices of the polymer unit cell (for PE, bo = duo), β is a constant reflecting the
growth regime: for regime I, β=4, whereas for regime II, β=2. Regime II is observed at higher
supercooling since it requires a higher nucleation rate, due to limited chain mobility.

Melt

Figure 4. Diagram defining the parameters used for heterogeneous nucleation theory.

Equations [1] and [2] indicate that the nucleation rate is a function of l/ΤΔΤ2 whereas
the growth rate depends on l/ΤΔΤ. A plot of In I + Δφ/kT versus l/ΤΔΤ 2 should yield a
straight line whose slope, K^ is proportional to σσ β Δσ. Similarly, a plot of In g + Δφ/kT ver-
sus 1/ΤΔΤ should yield a straight line whose slope, Kg> is proportional to σσ β . A combined
nucleation and growth experiment thus yields estimates of σσ β Δσ and σσ β from which Δσ is
obtained. The value Δσ gives a quantitative assessment of the ability for a given reinforcing
fiber and matrix system to form a transcrystalline zone. Using this approach, one can quanti-
tatively evaluate the interphase morphology in the semicrystalline thermoplastic matrix com-
posite.

Figure 5 shows the kinetic study of the growth of transcrystals and spherulites (24). It
is interesting to note that there is a temperature window of several degrees where the growth
rate of the transcrystal is substantially large while the growth rate of the bulk spherulites is
almost zero. If a composite material was cooled from the melt and annealed within this tem-
perature window very carefully, it is possible to manufacture an all-transcrystal composite
material. Indeed, we have succeeded to prepare ultra-high modulus polyethylene fiber rein-
forced polycaprolactone with transcrystals impinging upon each other. In spite of the limita-
tion of the fiber-to-fiber distance, which was approximately 400 μπι, the thickness of the
transcrystal was around 200 μιη which is much thicker than is ordinarily reported.

C. Tailoring the Properties of Composite Materials

One of the aims of interphase engineering is to tailor the mechanical and physical
properties of a composite material with a systematic understanding of the interphase structure
and ability to control its structure. In order to achieve this task, knowledge of struc-
 53

ture/property relationships is indispensable. The following example is an attempt to manufac-

ture a composite material with improved toughness without sacrificing strength or rigidity. It
has been reported that the introduction of ductile layers near the reinforcing fiber surface
improves toughness of composites (25,26). We have also taken a similar but more systematic
approach. A glass bead-filled high density polyethylene composite was prepared by a two roll
mill. The samples were subjected to mechanical, rheological, morphological, and molecular
characterizations. Theoretical predictions of the modulus and loss tangent were also performed
based on the properties of the individual materials.

2000

Ώ 1500
£
a 1000
.2
o
3
T3
►5 500

0
44 48 52 56
Temperature (°C)

Figure 5 - Temperature dependency of the induction time for a) massive bulk nucleation
(pure PCL matrix) and b) transcrystallization (PCL/PE composite). Notice the large
difference for the temperature associated with each process, at a given induction time.

This allowed us to design a certain composite structure with experimental verification. It was
found that when an elastomer is distributed as spheres, the loss tangent is much smaller than
when it is coated uniformly around the glass beads. The thin coating of the elastomer is thus
more effective in dissipating the fracture energy than the phase separated elastomer phase away
from the filler surface. Additionally, introduction of a thin coating at the surface may also
change the interfacial fracture mechanism. For very brittle materials such as glass and carbon
fibers, protection of the surface might also improve the toughness. Figure 6 shows the impact
strength of the glass bead-filled polyethylene plotted against the modulus of the composite.
Ordinarily, when the toughness improves, the rigidity is sacrificed as shown below by the
solid curve, where no interfacial treatment of the filler was given. The addition of an elastomer
which has no preferential affinity toward the filler surface was of little help. However, when a
maleic anhydride modified rubber is combined with an amine-functional silane coupling agent
treated filler, preferential adsorption of the rubber takes place and a simultaneous improvement
in toughness and modulus is achieved.

CONCLUDING REMARKS
The demanding requirements imposed on modern composite materials require that a
more systematic approach be applied toward their studying and manufacturing. We propose an
approach termed "interphase engineering" which calls for the understanding of inter-
face/interphase structures, controlling the structure of the interfacial region, and finally design
of the properties of the composite. With an outburst of composite interface studies, especially
in the past several years, there are already indications of successful interphase engineering in
composite research.
54

5
0 2 4 6 8
IMPACT STRENGTH (kJ m"2)

Figure 6. Storage modulus G' plotted against Izod impact strength for a Si02-filled
polyethylene (PE) composites. (O) PE and PE/Si02 composites; (n) multicomponent
composites with <t>si02= 0.20 and ethylene-propylene diene (EPDM) rubber volume
fractions of 0.001, 0.01 and 0.03; and ( ^ ) multicomponent composites and <t>si02= 0.20
and maleic anhydride modified EPDM volume fractions of 0.001,0.01,0.03, and 0.10.

REFERENCES
1. L.H. Sharpe, 162 nd Meeting, American Chemical Society, Div. Org. Coat. Plast.
Chem. Preprints, 31, 201 (1971)
2. J.A. Manson and L.H. Sperling "Polymer Blends and Composites", Plenum, New York
(1976) p.442.
3. H. Ishida and J.L. Koenig, Polymer Eng. Sei., 1978
4. E.P. Plueddemann, J. Paint TechnoL, 40, 1 (1968).
5. C.A. Kumins and J. Roteman, J. Polym. Sei. Part A, 1, 527 (1963).
6. P.W. Erickson, A.A. Volpe and E.R. Cooper, Proc. 19th Ann. Tech. Conf., Reinf.
Plast. Div., API, Section 21-A (1964).
7. E.P. Plueddemann, "Silane Coupling Agents," Plenum, New York (1982) p. 134.
8. K.P. Hoh, H. Ishida and J.L. Koenig, Polym. Comp., 11, 121 (1990).
9. C. Sellitti, J.L. Koenig and H. Ishida, Appl. Spectrosc, 44, 830 (1990).
10. C. Seilitt, J.L. Koenig and H. Ishida, Carbon, 28, 221 (1990).
11. C. Sellitti, J.L. Koenig and H. Ishida, J. Polym. Sei. Phys. Ed., 28, 1121 (1990)
12. P.W. Erickson, J. Adhesion, 2, 131 (1970).
13. R.L. Patrick, W.G. Gehman, L. Dunbar and J.A. Brown, / . Adhesion, 3, 165 (1971).
14. T. Hirai and D.E. Kline, / . Comp. Mat., 7, 160 (1973).
15. J. Nigro and H. Ishida, / . Appl. Polym. Sei., 38, 2191 (1989).
16. E.G. Chatzi, H. Ishida and J.L. Koenig, Appl. Spectrosc., 40, 847 (1986)
17. A. Taboudoucht and H. Ishida, Appl. Spectrosc, 43, 1016 (1989).
18. H. Ishida, Rubber Chem. TechnoL, 60, 497 (1987).
19. "Composite Interfaces," H. Ishida, Ed., Elsevier Science, New York (1986).
20. "interfaces in Polymer, Ceramic, and Metal Matrix Composites," H. Ishida, Ed.,
Elsevier Science, New York (1988).
21. B.S. Hsiao and E.J.H. Chen, in "Controlled Interphases in Composite Materials," H.
Ishida, Ed., Elsevier Science, New York (1990).
22. B. Wunderlich, "Macromolecular Physics", Vol. 2, Chapt. 5, Academic Press, New
York (1976).
23. J.D. Hoffman, G.T. Davis and J.L Lauritzen in "Treatise on Solid State Chemistry",
Vol. 3, Chap. 7, N.B. Hannay, Ed., Plenum New York (1976)
24. H. Ishida and P. Bussi, J. Mat. Sei. (in press).
25. R.E. Lavengood and M.J. Michno, Jr., Proc. Div. TechnoL Conf., Eng. Prop.
Structure Div., SPE (1975) p.127.
26. L.D. Tryson and J.L Kardos, Proc. 36th Ann. Conf., Reinforced Plast./ Composites
Inst., SPI, Section 2-E (1981).
 WS9b2

EFFECTS OF REINFORCING FIBER AND MATRIX RESIN

ON DELAMINATION FATIGUE CRACK PROPAGATION
IN CF/EPOXY LAMINATES

Hideki Sembokuya*, Masaki Hojo**, Takahira Aoki***

Kiyoshi Kemmochi**, and Hiroshi Maki*

* Faculty of Engineering, Takushoku University, 815-1, Tate-machi, Hachioji,

Tokyo 193, Japan
** Industrial Products Research Institute, AIST, Μ Γ Π , Higashi, Tsukuba 305, Japan
*** Institute of Engineering Mechanics, University of Tsukuba, Tennodai, Tsukuba 305,
Japan
ABSTRACT

Mode I delamination fatigue crack propagation behavior was investigated with

unidirectional CF/epoxy laminates made from Toray T300/#3601, T800/#3601,
T300/#3631, and T800/#3631 prepregs. The fatigue crack growth behavior of
laminates tested here was mainly controlled by the matrix resin. The
delamination fatigue crack growth rate of laminates with #3601 epoxy resin
was almost the same without respect to the fibers. On the other hand, the
threshold value of crack growth for the T800/#3631 laminates is slightly
larger than that for the T300/#3631 laminates. The relative contribution of
the maximum stress and the cyclic stress was derived by the analysis of the
stress ratio dependency proposed by authors. The energy release rate cor-
responding to the free-edge delamination onset for the quasi-isotropic
laminates was calculated for the T300/#3601 laminates. The results were com-
pared with the threshold values of the energy release rate range for
delamination fatigue crack propagation. Contribution of fibers and matrices
to the fatigue crack growth behavior was discussed on the basis of the frac-
tographic observation.

KEYWORDS

Composite materials; delamination; fatigue; carbon fiber; crack propagation

INTRODUCTION

Fatigue fracture of carbon fiber reinforced plastic (CFRP) laminates is

primarily caused by interlaminar fracture or delamination. Interlaminar
fracture is considered to be caused by cohesive fracture of matrix or in-
terfacial debonding between fibers and matrices. Thus, the toughness of
matrix and the strength of interfacial bonding are the important factors for
improving the resistance of fatigue fracture of CFRP.

In the present study, mode I delamination fatigue crack propagation tests

were carried out for four kinds of CF/epoxy laminates. The effects of the
reinforcing fiber and the matrix on the delamination fatigue crack growth
55
56
Table 1. Constitution of laminates and mechanical properties.

Fiber/ Constitution Elastic Interlaminar fracture toughness

Matrix of laminate modulus(MPa) Energy release rate, G I C (N/m)

T300/#3601 (0). 138 90

T800/#3601 (0), 162 80

T300/#3631 (0). 136 160

T800/#3631 (0)64 166 170

Elastic modulus: in fiber direction

Thickness = 8 mm

behavior was investigated. The mechanism of delamination fatigue fracture

was discussed on the basis of the stress ratio dependency and fractographic
observations.

EXPERIMENTAL PROCEDURE

The laminates were made from four kinds of Toray prepregs (T300/#3601,
T800/#3601, T300/#3631, and T800/#3631) which consist of carbon fibers (T300
and T800) and epoxy resins (#3601 and #3631). The constitution of the
laminates and the mechanical properties are shown in Table 1 (Maekawa et
al. ). Double cantilever beam (DCB) specimens (width = 20 mm) were used for
the delamination fatigue crack growth tests (Hojo et al., 1987). Fracture
mechanics parameters are calculated by using analytical compliance method
(Kageyama and Hojo, 1990).

A computer-controlled servohydraulic fatigue testing machine (Shimadzu; max-

imum capacity = 9.8kN) was used for the delamination fatigue crack propaga-
tion tests. The stress ratio, R, of the minimum to the maximum load was kept
constant (R=0.2 and 0.5). The frequency of stress cycling was 10 Hz.

EXPERIMENTAL RESULTS AND DISCUSSION

Delamination Fatigue Crack Propagation Behavior

Figure 1 shows the relations between the maximum energy release rate, G m a x
and the crack propagation rate, da/dN for the T300/#3601 and T800/#3601
laminates. Figure 2 shows the same relations for the T300/#3631 and
T800/#3631 laminates. The exponents of the power functions in the region
-8,
where 10~ö
<da/dN<10 -10 m/cycle are quite large. Thus, the values of G m at
the rate of 1 0 ~ 1 0 m/cycle are considered as threshold values here. For the
laminates with #3601 matrix (Fig. 1 ) , the effect of the reinforcing fiber on
the threshold values is negligible when compared at the same R value. The
threshold values are larger for higher R values. For the laminates with
#3631 matrix (Fig. 2 ) , the effect of the reinforcing fiber on the threshold
values was observed under the same R value. The threshold values of the
T800/#3631 laminates are slightly larger than those of the T300/#3631
laminates. Figures 1 and 2 showed that the threshold values for the
laminates with #3601 matrix are smaller than those for the laminates with
#3631 matrix under the same R value.

Figure 3 shows the relations between the energy release rate range, AG and
 57
the crack propagation r a t e , da/dN for I ' ' 1 ' L ' 1 ' 1 ' 1 ·■

a l l laminates· The e f f e c t of the r e i n -

10"'
forcing f i b e r on the threshold values I R T300/
3601
of AG i s s i m i l a r t o t h a t in the Gmax~ | 0.2 o ψ
da/dN r e l a t i o n . The e f f e c t of s t r e s s 0.5 o
o ·
o o
r a t i o i s r e l a t i v e l y small. Figures 1-3 T800/ ♦ ·
show t h a t d e l a m i n a t i o n f a t i g u e c r a c k Γ R
3601 ♦♦8
p r o p a g a t i o n for t h e s e l a m i n a t e s is \ 0.2 ♦ <>♦ · ]
mainly c o n t r o l l e d by the matrix r e s i n s 0.5 • <>♦ £
r a t h e r than the reinforcing f i b e r s . 0+ · j
MO" r <>♦ 9 H
Effect of S t r e s s Ratio ♦ · 1

Authors (Hojo e t a l . , 1987) proposed \ .

o
that the equivalent s t r e s s i n t e n s i t y ■S10'
range, ΔΚ should be used t o c o r r e l a t e { * *
• -1
t h e growth r a t e under d i f f e r e n t R o
v a l u e s i n s t e a d of Gmav, ΔΘ, and t h e o
A A % \
stress intensity range, ΔΚ. ΔΚ is >io"l·
d e f i n e d by
AK eq = ΔΚ (1-R)~Y (1)
1 ■ 1 ! 1 1 I 1 1 1 1 . hi
10
50 100
= A K 1 ^ *maxY (2) Maximum energy release rate, Gmax(N/m)

where ^ is the maximum stress inten- Fig. 1. G m a x vs. da/dN

sity factor. Parameters γ and 1-γ indi- for #3601.
cate the contribution of the maximum
stress and the cyclic stress on the
crack growth rate, respectively. The -—«—i ■ i ' i ' i ■i ■i ■ i i i i i
value of γ varies between 0 and 1. o o
o o J
10"7
In order to determine the γ values, the So o ·· 1
1
threshold values of ΔΚ are plotted /$> ° · 1
against (1-R) in Fig. 4. Since γ values • # .
0 *°
are larger than 0.5 for all laminates, id*
A
s* ·
the contribution of the maximum stress
o° ♦♦ °° ·· 1
is large in fatigue crack propagation
mechanisms, γ values for the laminates
with #3601 (0.82 for T300 and 0.88 for <>♦ 9) A
id*
T800) are larger than those for the
<>♦*§· J
laminates with #3631 (0.74 for T300 and Φ
8 ·
0.66 for T800). Thus, the contribution <>♦ o ·
8
of the cyclic stress is relatively
larger for the laminates with #3631. io-'° o J
o*
o ·
Comparison of Energy Release Rate
Between DCB and EDT Specimens
io-M R
H
T 3 0 0 / T800/ -\
3631 3631
O'Brien (1982) proposed the edge 0.2 o ♦
delamination tension (EDT) test which 0.5 o ·
dealt with the growth of free-edge m"« . 1 . 1 . 1 . 1 . 1 . 1. 1 1 1 1 1
d e l a m i n a t i o n in qua si-isotropic 50 100 150
laminates in order to evaluate inter- Maximum energy release rate, Gmax ( N / m )
laminar fracture toughness. Thus, it is
Fig, 2
· G max v s · d a / d N
interesting to investigate the relation
for #3631.
between the growth threshold of
58
delamination fatigue crack growth ~i—»- J ' 1 ' 1 '1 Ί 1 1
tests by using DCB specimens and the "
onset of delamination of EDT - R T300 * °o J
specimens under fatigue loading. In - 0.2 o
0.5 o £> · 1
our previous study of tension-tension
fatigue tests for CFRP laminates oo
R T800 • ♦
(Nagasawa, et al, 1990), we conducted L10" 8 - 0.2
I* }
§<>♦
fatigue tests of the T300/#3601 - 0.5 •
quasi-isotropic laminates of lay up <9o ♦
of (+45/-45/0/90)2s to obtain an S-N «>♦ · ♦ .
curve of onset of delamination. 8» H
-L <£>♦ o

During free-edge delamination growth,

the value of the energy release rate •I
€
♦
increases and then reaches a Sl<T
saturated value. The saturated values fc&A 9>·
<?!
for the quasi-isotropic T300/#3601
L
•o <>♦
o ·
laminates are computed by using Kondo o
and Aoki's method (1987). Since the %
first free-edge delamination was ob- ho- r • -
served at the inner (0/90) interface, 3601 3631 '
the a s y m m e t r i c delamination
propagated at the inner (0/90) inter- I ■ 1 , 1 ■ 1 i 1 i 1 i 1 1
_J L.
face was assumed. It can be predicted 40 80 120
that the mode I component is dominant Energy release rate range, AG(N/m)
in the total energy release rate be-
cause the inner (0/90) interface is F i g . 3 . AG v s . da/dN.
close to the surface of symmetry. The
contribution of residual thermal
stresses are included in the calcula-
tion. Here, the temperature dif-
ference, ΔΤ, equals -157 K. The 1.0
energy release rate corresponding to
the onset of delamination was calcu-
lated under these conditions. The
calculated results are compared with
the threshold values of the energy 0.5
release rate range for the delamina-
tion fatigue crack propagation tests
by using the unidirectional DCB
specimens in Table 2.

The values for the DCB fatigue crack 0.2 r

propagation tests are smaller than T300/36O1
T800/3601
0.82
that for the EDT fatigue tests at
T300/3631
0.88
each R value. These saturated values
T800/3631 0.7Λ
for the EDT tests seem to be overes-
0.1 0.66
timated because there was no artifi- 0.2 0.5 0.8 1.0
cial defect in the specimen tested
Stress ratio parameter, 1 - R
here. If the energy release rate was
calculated with small defect in stead
of the saturated values, the agree- F i g . 4. Threshold value
ment will become much better. More of ΔΚ v s . 1-R.
detailed study is necessary in order
to explain the differences quantita-
tively.
 59
Table 2. Comparison of values of energy release rate range.

rv <- ρηηΗίΗΛη Constitution Energy release rate range, AG (N/m)

Test condition ^ l a m i n a t eg R = oa R = 0 >2 R = 0 #3

DCB fatigue ( Q) 4 3 i 2* 4 3 #5 4 U0
64
test

EDT fatigue (+ 4 5/-45/0/90) oc 64.0 67.2* 71.3

zs
test

* Extrapolated value or interpolated value.

Fractographic Observation

Figure 5 shows the macroscopic fracture surfaces of all laminates tested

here. The arrow shows the crack growth direction. The fracture surfaces of
the T300/#3601, T800/#3601 and T300/#3631 laminates are smooth. For the case
of the T800/#3631 laminates, the traces of fiber bridging is clear. The
fiber bridging is considered to increase crack growth resistance (Hwang and
Han, 1988). This observation agrees with the fact that the threshold value
of the T800/#3631 laminates is larger than that of the T300/#3631 laminates.

Figure 6 shows the scanning electron micrograph (SEM) of interlaminar frac-

ture surface for the T300/#3601 laminates. This micrograph is characterized
as a matrix dominant surface. Though a few exposed fibers can be seen, the
interfacial bonding is generally good.

Figure 7 shows the fracture surface of the T300/#3631 laminates. About 70%
of the fracture surface is characterized as a matrix dominant surface. In
the remaining fracture surface, interfacial debonding and exposed fibers
were observed. For the laminates with #3631 matrix, the fracture surface is
more rough than that with #3601 matrix. Slight ductility was observed for
the laminates with #3631 matrix with higher magnification. These facts agree
with that the γ values for laminates with #3631 matrix are smaller than
those with #3601.

crack growth
direction

i i
10 mm

Fig. 5. Fracture surfaces of DCB specimens.

60

Fig. 6. SEM for T300/#3601. Fig. 7. SEM for T300/#3631.

(R=0.5, near threshold) (R=0.5f near threshold)

CONCLUSION

1. Mode I delamination fatigue crack propagation was mainly controlled by

matrix resin for the T300/#3601, T800/#3601, T300/#3631, and T800/#3631
laminates. For the laminates with #3631, the threshold values of the
T800/#3631 laminates was slightly larger than that of the T300/#3631
laminates.
2. The analysis of the stress ratio dependency indicated that the contribu-
tion of the maximum stress was large in delamination fatigue crack propaga-
tion for all laminates used in the present study. The contribution of the
cyclic stress for the laminates with #3631 was relatively larger than that
for the laminates with #3601.
3. Fractographic observation indicated that fiber bridging was evident for
the T800/#3631 laminates. This observation supported the experimental result
that the threshold value of the T800/#3631 was larger than that of the
T300/#3631 laminates. Scanning electron micrographs also showed that the
delamination fatigue crack behavior was mainly controlled by matrix resin.

REFERENCES

Hojo, M., Tanaka, K., Gustafson, C. G., and Hayashi, R. (1987).

Composite Sei. Tech., 2j)» 273-292.
Hwang, W. and Han, K. S. (1988) J. Composite Materials, 22_, 396-430.
Kageyama, K. and Hojo, M., Proc. Japan-US Conf. Composite Materials
(to be published).
Kondo, K. and Aoki, T. (1987). Composite Structures 4, 2^,
Damage Assessment and Material Evaluation, Marshall, I., H., ed., 241-257.
Maekawa, Z., Hamada, H., Hojo, M., and Ishibashi, S. (to be submitted)
Nagasawa, C , Sembokuya, H., Hojo, M., Kemmochi, K., Endo, K., and Maki, H.
(1990). Advanced Composite Materials, Proc. 1st France-Japan Seminar on
Composite Materials., Bathias, C. and Uemura, M., ed., 149-156.
O'Brien, T. K. (1985). ASTM STP775, Riefsnider, K. L. ed., 140-167.
 WS9b3

EFFECTS OF ELECTROLYTE ON THE STRUCTURE OF

PYROLYTIC GRAPHITE SURFACES IN ANODIC OXIDATION

M. NAKAHARA and K. SHIMIZU*

Composite Materials Research Laboratories

♦Polymers Research Laboratories
Toray Industries, Inc., 3-2-1, Sonoyama
Otsu, Shiga 520, Japan

ABSTRACT

Anodic oxidation effects on the structure of the basal and edge surface of pyrolytic graphite
have studied by laser Raman spectroscopy, and by a gas-phase chemical modification method
coupled with X-ray photoelectron spectroscopy. Surface covering fractions have also been
studied by α-epichlorohydrin monolayer formation. In the case of the edge surface, hydroxyl
groups are added without the destruction of its structure with a mild treatment. With more
severe treatment, carboxyl groups are added and this addition is also accompanied by the
destruction of the basal and edge surface structures. It is found that anodic oxidation in an
alkaline electrolyte has a wider permitted range of treatment, in which hydroxyl groups can be
added without destroying the edge surface structure, than that in an acid electrolyte.
Finally, it is confirmed that both carboxyl and hydroxyl groups can make covalent bonds with
epoxy groups of a-epichlorohydrin.

KEYWORDS

Anodic oxidation; electrolyte; adhesion; graphite; carbon fibre; epoxy resin.

INTRODUCTION

Oxidative surface treatment of carbon fibers (CFs) increases the interlaminar shear strength
(ILSS) of CF-epoxy matrix composites (Drzal et al., 1982 ; Norita et al., 1986). In
particular, an anodic oxidation method is preferably applied in industrial processes because
of the shorter oxidation time and the superior processing control possibilities (Fitzer et al.
1988).

In order to optimize anodic oxidation of CFs, the effects of the kind of electrolyte on the
adhesion between CFs and epoxy resin, and on the structure of CF surfaces have been
investigated. For example, Ehrburger and Donnet (1980) have performed anodic oxidation
experiments on CFs in HN0 3 and NaOH, and suggested that the presence of stronger acidic
groups (COOH and OH) on CF surfaces results in the strong interfacial bonding of the
composites and the treatment of CFs in NaOH yields comparatively stronger acidic groups.
Kozlowski and Sherwood (1985), using X-ray photoelectron spectroscopy (XPS), have shown that
the amount and type of surface oxides varies considerably depending upon the pH of the
electrolyte, and suggested that different oxidation mechanisms work at different pH values.
Harvey et al., (1987) have examined the effects of a variety of factors including the kind of

61
62
electrolyte on the ILSS of composites, and concluded that the rise in ILSS with surface
treatment is not dependent upon the 0/C ratios or the amount of carboxyl functionality present
on the CF surface, inferring that mechanical keying of epoxy resin to the CF surface plays an
important role in forming the fiber-resin bond. On the other hand, Fitzer and Rensch (1990)
have carried out the anodic oxidation of CF surfaces in acid and alkaline electrolytes, and
reported that the adhesion improvement by the treatments between CFs and epoxy resin is mainly
due to the chemical interaction at the interface, and NaOH electrolyte improves the adhesion
much better than an acid type electrolyte such as H 2 S0 4 . As mentioned above, the
mechanism of the improvement in interfacial adhesion by anodic oxidation is still a
controversial subject. One of the reasons for this is that the extremely complex structure of
CF surfaces makes it difficult to understand the adhesion mechanism.

Therefore, a study on anodic oxidation has been performed by using the basal and edge surfaces
of pyrolytic graphite (PG) as a model CF surface (Nakahara et al., 1990). In this paper the
effect of anodic oxidation on the basal and edge surfaces of PG in acid and alkaline
electrolytes is described with respect to the physical and chemical properties of their
surfaces and the reaction of surface chemical groups added to their surfaces with
fl-epichlorohydrin. In addition, the interfacial adhesion between CFs and epoxy resin is
discussed based on the data obtained in this study.

EXPERIMENTAL PROCEDURE

PG from Union Carbide Corporation is used in the present study. Mirror-polished edge surfaces
of PG, which are parallel to the c-axes of graphite crystallites, are prepared by the method
of Katagiri et al.(1988). Basal surfaces, which are perpendicular to the c-axes of graphite
crystallites, are prepared by cleaving PG. These surfaces are ultrasonically rinsed three
times in trichloroethylene, acetone and distilled water in that order, and then dried at 100t.

The basal and edge surfaces are oxidized anodically in sulphuric acid and tetraethylammonium
hydroxide (EAH) solutions (0. IN). When NaOH is used as an alkaline electrolyte, sodium
remains on the surfaces even after washing in distilled water. The same phenomenon has been
reported for CFs by Kozlowski and Sherwood (1985). If sodium exists on the surfaces of PG in
the form of NaOH, errors may appear in the quantitative analysis of hydroxyl groups (C-OH).
Thus in this study EAH solutions free from sodium is used as an alkaline electrolyte instead
of NaOH which is most common as an alkaline electrolyte.

The specific electric charge (electric charge (C) per unit area (m2 )) is controlled by
changing the current density with a potentiometer (Hokutodenko HJ-2010), keeping the treatment
time at 10 sec. Anodic oxidation is carried out in four steps: 50,125,500 and 5000 Cm -2 on
the basal and edge surfaces. After the surface treatments, the surfaces are again rinsed in
distilled water and dried at 100t.

Laser Raman spectroscopy is used to characterize the structural changes of the oxidized
surfaces. Raman spectra of the surfaces are measured by using a double-grating monochromator
(Jobin Yvon Ramanor U-1000) with a cooled photomultiplier tube (Hamamatsu R-1104).

XPS is used to determine the oxygen contents present on the basal and edge surfaces. A
spectrometer (SSI SSX-100-206) with a monochromatized ΑΙΚαι. 2 X-ray anode (hp =1486. 6eV) is
used for XPS measurement in a vacuum of 3 x 10"9 torr. Photo emitted electrons are measured
at 35 degrees to the basal and edge surfaces. Moreover, a gas-phase chemical modification
method coupled with XPS (Nakayama et al., 1988) is used for detecting hydroxyl and carboxyl
groups on the basal and edge surfaces. Trifluoroacetic anhydride is used to label hydroxyl
groups. Trifluoroethanol and dicyclohexylcarbodiimide are used to label carboxyl groups.

Chemical treatment of both unoxidized and oxidized surfaces with α-epichlorohydrin is carried
out by refluxing the basal and edge surfaces in contact with α-epichlorohydrin for 10h. After
the chemical treatment, the surfaces are ultrasonically rinsed for 15 min in acetone and
distilled water and dried for 30 min at 100t. The fraction (q) of the surface covered by an
fl-epichlorohydrin monolayer is estimated by using the method proposed by Waltersson (1985).
 63
RESULTS AND DISCUSSION

The Raman spectra of the unoxidized and oxidized edge surfaces of PG in the acid electrolyte
are shown in Fig. 1(a). Two Raman bands are observed at 1580 and 1355 cm-1. In the case of
the acid electrolyte, a marked change in the spectra is recognized in the range 500 to 5000
Cm-2. On the other hand, in the case of the alkaline electrolyte, any changes in the spectra
is not recognized up to 5000 Cm -2 . A change in the spectra for the basal surfaces shows also
the same tendency as the case for the edge surfaces. The intensity ratio (R) of the 1355 cm -1
band to the 1580 cm -1 band of PG can be related to the amount of defects, such as the edges
and lattice vacancies of the graphite basal planes, in the surfaces of PG(Tuinstra and Koenig,
1970; Katagiri et al., 1988). Fig. 1(b) shows the change in R as a function of the specific
electric charge for the edge surface of PG. Any changes in R for the alkaline electrolyte are
not recognized in the range 0 to 5000 Cm-2, whereas the increase in R for the acid electrolyte
is recognized in the range 500 to 5000 C m 2 . These results suggest that with the acid
electrolyte the structure of the basal and edge surfaces is destroyed at 5000 Cm-2, unlike the
case with the alkaline electrolyte. Consequently, it is proved that the effect of an alkaline
electrolyte on the surface strcture is different from that of an acid one.

1/
15000 Cir2
1.2

1.0

1 °· 8
^ 0.6
500 Cm"2

J
G 0.4
Jnoxidized 1
0.2

-L -i_L -L
1800 1600 1400 1200 1000 0 ' 10 2 10 3 10 4
Wave number(cm_1) Specific electric charge (Cm -2 )

Fig. 1. Raman data: (a) Raman spectra of the unoxidized and oxidized
edge surfaces of PG measured with incident laser radiation
polarized parallel to the edge surface for the acid electrolyte,
;(b) change in R as a function of the specific electric charge
with the unoxidized and oxidized edge surfaces for ( O ) the
acid electrolyte and ( # ) the alkaline electrolyte.

A quantitative analysis (Nakayama et al., 1988) determining the amount of hydroxyl and
carboxyl groups present on the basal and edge surfaces of PG has been carried out. Fig. 2(a)
shows the change in 0/C, -C00H/C, and -OH/C ratios with the edge surface as a function of the
specific electric charge for the acid electrolyte. The amount of carboxyl groups increases
with increasing specific electric charge. The increase is especially large when the specific
electric charge increases from 500 to 5000 Cm -2 . In the basal surface, a marked increase of
the amount of carboxyl groups is not found up to 500 Cm"2, and the amount of carboxyl groups
increases rapidly in the range 500 to 5000 Cm -2 (Nakahara et al., 1990). As stated above,
the Raman spectral results indicate that the basal and edge surface structures are destroyed
at 5000 Cm-2. The rapid increase in the amount of carboxyl groups at the basal and edge
64

Specific electric charge(Cm ~ 2 ) Specific electric charge(Cm ~ 2 )

Fig.2. Relation between the amount of oxygen-containing groups and

the specific electric charge for (a) the acid electrolyte
and for (b) the alkaline electolyte.

surfaces in the range 500 to 5000 Cm-2, is considered to be related to the destruction of
their surface structure. A large quantity of carboxyl groups is expected to be added at the
discontinuity of broken basal and edge surface structures. The increase of the amount of
hydroxyl groups is not recognized up to 5000 Cm -2 for the basal surface (Nakahara et al.,
1990), but recognized in the range 125 to 500 Cm -2 for the edge surface. On the other hand,
the amount of hydroxyl groups shows a rapid decrease in the range 500 to 5000 Cm-2.
Therefore, in the anodic oxidation of the edge surface in the sulphuric acid electrolyte, it
is possible to add a large quantity of hydroxyl groups on the edge surface without destroying
its structure.

The change in 0/C, -C00H/C, and -OH/C ratios with the edge surface as a function of the
specific electric charge for the alkaline electrolyte is shown in Fig. 2(b). No increase in
the amount of carboxyl groups is found up to 5000 Cm-2. As mentioned above, the structure of
the edge surface with the alkaline electrolyte is found to be free from destruction up to 5000
Cm -2 . The degree of surface destruction seems to be related to the increase in the amount of
carboxyl groups. The amount of hydroxyl groups, on the other hand, increses with incresing
specific electric charge. Therfore, with the alkaline electrolyte, it is seen that hydroxyl
groups can be added on the edge surface without destroying its structure up to at least 5000
Cm -2 . This treatment level is higher than that of the acid electrolyte.

From the results described above, it is seen that the surface structure and the species of
surface chemical groups added by the anodic oxidation have a close relationship. That is to
say, when the edge surface is oxidized anodically without destruction of the structure,
hydroxyl groups are added on the edge surface. On the other hand, hydroxyl groups are not
added on the basal surface by anodic oxidation. Carboxyl groups are added on the basal
surface only when the basal planes at the surface are destroyed by anodic oxidation.

Surface covering fractions (q) for the basal and edge surfaces treated with a-epichlorohydrin
plotted against the totalamount of hydroxyl and carboxyl groups is shown in Fog. 3. It can be
seen that the increase ofq increase with increasing total amount of these groups. This result
indicates that a-epichlorohydrin can be covalently bonded through its epoxy groups to hydroxyl
or carboxyl groups on the basal or edge surface.
 65
0.6
O : basal surface
□ : edge surface

0.4

er
OH(~80X)
0.2
COOH(~90X)

0 0.05 0.10 0.15

{[-OH]+[-COOH]}/C

Fig. 3. Relation between the fraction (q) of the surface covered by an

ff-epichlorohydrin monolayer and the total amount of hydroxyl
and carboxyl groups.

The edge surface, having many hydroxyl groups, is considered to be very important in improving
the shear strength of CF-epoxy matrix composites. This is because hydroxyl groups at the edge
surface form covalent bonds with both epoxy groups and internal carbon atoms bound by strong
covalent forces to preserve the hexagonal array. On the other hand, the basal and edge
surfaces, having many carboxyl groups, are not considered to be so important in improving the
shear strength of the composites. The reason is as follows. In the case of the basal surface,
carboxyl groups at the basal surface form strong covalent bonds with epoxy groups, but the
atoms at the basal surface form weak Van der Waals bonds with internal basal planes. In the
case of the edge surface, carboxyl groups at the edge surface also form strong covalent bonds
with epoxy groups, but the bonding between carbon atoms bonded with carboxyl groups at the
edge surface and internal ones becomes weaker through the partial destruction of sp2 bonds
between the carbon atoms.

The rise in the ILSS of the resulting CFs and epoxy resin matrix composites by anodic
oxidation may be considered as occurring because the functional groups described above at the
edge surface can form covalent bonds with epoxy groups. The amount of the functinal groups
(-0H, -C00H) added in the alkaline electrolyte at 5000 Cm ~Z is smaller than that added in the
acid one at 500 Cm"2 as seen from Fig. 2. Judging from only the amount of the functional
groups, the acid type electrolyte is expected to be more efficient in increasing the ILSS of
the composites than the alkaline one. Fitzer and Rench (1990), however, have reported that an
alkaline electrolyte improves the adhesion between CFs and epoxy resin matrix much better than
an acid one. This suggests that there are some other factors to be considered in addition to
covalent bonds with functional groups in improving the ILSS of the composites. This matter
will now be discussed.

It is well known that clouding in alkaline solutions occurs during anodic oxidation of CFs.
On the other hand, the anodic oxidation of PG in the alkaline electrolyte used in this study
gives no clouding of the alkaline solutions. PG has a much narrower 1580 cm * band and much
smaller 1355 cm -1 band compared with the 1580 enr1 and 1355 cm"1 band of high strength PAN-
based CFs (Fitzer and Rozploch, 1988). From these characteristics of Raman bands, it can be
seen that PG has much more graphitized structure than PAN-based high-strength CFs. Highly
graphitized structure such as PG seems not to be readily attacked by anodic oxidation in the
alkaline electrolyte. The clouding of the solutions is considered to be closely related to
the presence of less graphitized and weakly bonded structure in the CF surface layer.
Probably, during anodic oxidation in an alkaline electrolyte, the less graphitized structure
66
is removed from the CF surfaces into the alkaline electrolyte, causing the clouding of the
alkaline solutions. When an alkaline electrolyte removes the weak structure from the CF
surfaces during the treatment and adds the functional groups mentioned above on the newly
appeared strong surface structure, the ILSS of the composites may increase rapidly. On the
other hand, in the case of the acid electrolyte, a part of the functional groups is possibly
added on the edge surface damaged by anodic oxidation and the edge sites of the weak structure
initially present in the CF surface layer. In this case, it seems that the rise in ILSS
cannot be related to only the amount of the functional gruops.

CONCLUSIONS

Anodic oxidation in the alkaline electrolyte, in which hydroxyl groups can be added without
destroying the edge surface structure, has a wider permitted range of treatment than that in
the acid electrolyte. Hydroxyl groups can form covalent bonds with epoxy groups. Thus the
edge surface is considered to have a very important role in improving the shear strength of
CF-epoxy matrix composites. The amount of hydroxyl groups added by treating with the alkaline
electrolyte is smaller than that with the acid electrolyte. Carboxyl groups are added to the
basal and edge surfaces in the range 500 to 5000 Cm -2 for the acid electrolyte, where the
structure of the surface is destroyed, and also form covalent bonds with epoxy groups. In
this case, the bonding between atoms located in the surfaces and the inside will become weaker
when the amount of carboxyl groups on the surfaces increases. Therefore, in the range of
higher specific electric charge, the basal and edge surface structures, having many carboxyl
groups, may reduce the shear strength of the composites.

ACKNOWLEDGMENTS

The authors would like to thank Mr. G. Katagiri and Mr. Y. Nakayama of Toray Research Center, Inc.
for the analysis of PG surfaces by laser Raman spectroscopy and XPS respectively.

REFERENCES

Drzal,L. T., M. J. Rich and P. F.Lloyd( 1982). Adhesion of graphite fibres to epoxy matrices: l.The
role of fibre surface treatment. J. Adhesion, 16, 1-30.
Ehrburger, P. and J.B. Donnet( 1980). Interface in composite materials. Phil. Trans. R. Soc. Lond., Α294
495-505.
Fitzer, E. and F. Rozploch(1988). Laser Raman spectroscopy for determination of the C-C bonding
length in carbon. Carbon, 26, 594-595.
Fitzer, E., H. Jager, N. Popovska and F.V.Sturn( 1988). Anodic oxidation of high modulus carbon
fibres in sulphuric acid. J. Appl. Electrochem., 18, 178-182.
Fitzer, E. and H. -P. Rensch(1990). In:Composite Interfaces(H. Ishida, ed. ), pp. 241-254. Elsevier, New
York.
Harvey, J., C. Kozlowski and P. M. A. Sherwood(1987).X-ray photoelectron spectroscopic studies of
carbon fibre surfaces. J. Mater. Sei., 22, 1585-1596.
Kozlowski,C.and P.M.A.Sherwood(1985).X-ray photoelectron-spectroscopic studies of carbon-fibre
surfaces: Part 5.-The effect of pH on surface oxidation. J. Chem. Soc., Faraday Trans. 1 , 81,
2745-2756.
Nakahara,M., Y. Nakayama, G. Katagiri and K. Shimizu(1990). Anodic oxidation effects on pyrolytic
graphite surfaces in acid. J. Mater. Sei., in press.
Nakayama, Y., T.Takahagi, F.Soeda, LHatada, S.Nagaoka, J.Suzuki and A. Ishitani( 1988). XPS
analysis of NH 3 plasma-treated polystylene films utilizing gas phase chemical modification
J. Polvm. Sei. Polvm. Chem. Ed., 2(L 559-572.
Norita, T., J. Matsui and H. S. Matsuda(1986). In:Composite Interfaces(H. Ishida and J. L. Koenig, Ed. )
pp. 123-132. Elsevier, New York.
Tuinstra, F. and J.L. Koenig(1970). Raman spectrum of graphite. J. Chem. Phys., 53, 1126-1130.
Waltersson, K. (1985).ESCA studies of carbon fibres: Part Π - surface reactions of carbon fibres
with epoxides. Coma Sei. Tech., 22, 223-239.
 WS9b4

MICROMECHANICAL INVESTIGATION OF FIBER

REINFORCED POLYMERS

C. G. MAROTZKE
Bundesanstalt für Materialforschung und
- prüfung (BAM)
Unter den Eichen 87, D 1000 Berlin 45

ABSTRACT
In fiber reinforced materials containing short fibers, the
mechanical properties are influenced by local stress distribu-
tions. By means of an idealized model of the composite mate-
rial, the stress field in the vicinity of the fiber is analyzed
using the finite element method. It is shown that the interface
is extremly loaded by shear stresses at the fiber ends. These
shear stresses can initiate a local failure of the interface.
Since additional radial stresses are active at the fiber end, a
further stress transfer due to friction is possible after a
delamination of the fiber. The influence of a partial debonding
of the interface on the stress transfer between fiber and
matrix is studied, simulating the extension of an interface
crack. To this end, a contact element algorithm is employed.

KEYWORDS

Fiber reinforced materials; micromechanics; interface crack;

finite element method; single fiber pull-out test.

Introduction
The mechanical properties of the interface between fiber and
matrix play an important role in the mechanics of composite
materials. This is due to the stress transfer between the two
phases, paticularly in the case of short fiber reinforced
materials. However, in materials reinforced by endless fibers,
this problem also arises in the case of broken fibers, which
can be due to the processing of the material, or due to the
statistical strength of the fibers. The stress distribution in
the vicinity of the fiber ends is very inhomogeneous. Within
the linear theory of elasticity, even stress singularities
arise here. In real materials, these stress singularities re-
sult in severe stress concentrations (Marotzke, 1990), whose

67
68
intensity depends on the mechanical properties of the two
constituents and on the bonding conditions. As these stress
concentrations can initiate local failure, which can lead to a
global failure of the composite material, an investigation of
the stress field in the vicinity of the fiber is needed. This
is done with the aid of a finite element analysis for a
perfectly bonded fiber and for a partial delamination due to an
interface crack, starting at the fiber end. Results are shown
for a thermoplastic matrix reinforced by glass fibers.

Since there is no possibility of a direct measurement of the

stresses, due to the microscopical scale, a theoretical
investigation has to be performed. Therefore, some simplifying
assumptions concerning the material behaviour and the bonding
conditions have to be made. It is well known from physical
investigations that the mechanical properties of the polymer
matrix in the boundary layer next to the fiber deviate from
that of an undisturbed material. This may be owing to a change
of the morphology near the fiber or due to the diffusion of
coupling agents from the fiber surface. Single fiber pull-out
tests, conducted by Hampe (1987) at the 'Bundesanstalt für
Materialforschung und -prüfung' (BAM), revealed the influences
of the coupling agents as well as of the temperature treatment
on the mechanical properties of the boundary layer. As there
are no material data available for the boundary layer, the
properties of the undisturbed matrix are assumed to be also
valid near the interface. Both materials are regarded as
linear-elastic, homogeneous, isotropical and perfectly bonded
together. The fibers are assumed to be perfectly cylindrical.

Short Fiber Composite Model

The investigation of the stress transfer between fiber and ma-

trix has to be carried out using a simplified model. This model
consists of a single finite fiber in the center of the next
neighbouring, hexagonally arranged fibers (Fig.l). The model-
ling of the surrounding fibers as discrete fibers, requires a
three-dimensional finite element analysis. Confining the fiber
volume fraction to about 25%, the neighbouring fibers can be
considered by distributing their stiffness over a ring of
corresponding stiffness at the distance of the fibers.

real system

displacement u
\ matrix ; single fiber
idealised
system

ring with distri-

L/2 buted stiffness
of neighbouring
Finite- Element System fibers

Fig. 1. Schematic outline of the short fiber

composite model
 69
The model so obtained is axisymmetrical and requires only a
two-dimensional analysis providing axial loading. The system is
loaded by an axial tension, which is applied by a uniform
displacement of the axial boundaries. The element net chosen
consists of 24 elements in the radial direction and of 46
elements in the axial direction.

Stress Transfer in the Composite Model

Utilizing the short fiber composite model, the stress transfer

is studied on the example of a glass fiber polycarbonate system
with a stiffness ratio of 32, a length to diameter ratio of 36
and a fiber volume fraction of 2.1%. Corresponding to the
stiffness ratio, the axial stresses in the fiber are signi-
ficantly higher than those in the matrix (Fig.2). However, it
has to be considered that the strength ratio of fiber and
matrix is almost of the same order as the stiffness ratio.

Fig. 2. Axial stresses in the glass fiber

composite model

The axial stresses in the fiber reach a maximum in the middle

of the system. Leading up to the fiber end, the axial fiber
stresses decrease with an increasing slope. This means that
high interfacial shear stresses are active in this region. At
the fiber end, the stresses in the matrix increase, due to the
transfer of the remaining fiber force through the fiber end.

Most of the fiber load is transferred to the matrix by

interfacial shear stresses (Fig.3). The shear stresses reach
their maximum at the fiber surface and decrease very rapidly in
the radial direction. In the last third of the fiber, an
extensive increase is seen, so that the matrix in this zone is
not only stressed by high axial stresses, but also by high
shear stresses. These stress concentrations can either lead to
a plastic yielding of the matrix, when the matrix is ductile
and the strength of the interface is sufficiently high, or to a
local failure due to a matrix crack or a debonding of the
70
interface. Similar phenomena could be observed by comparison
of experimental data with numerical results in single fiber
pull-out tests (Marotzke and Hampe, 1990). Depending on the
fiber surface treatment, two types of failure could be
observed, fiber debonding after matrix yielding and brittle
cracking of the interface.

Fig. 3. Shear stresses in the glass fiber

composite model

Propagation of an Interface Crack

With a view to the reliability of structural parts, it is

interesting to study the change of the stress distribution in
the vicinity of the fiber, due to the extension of an interface
crack, in order to find out, whether it leads to an augmen-
tation or to a reduction of the loading of the boundary layer.
To this end, an interface crack, starting at the fiber end, is
simulated. A contact element algorithm is employed to prevent
the penetration of the phases into each other and to take into
account the stress transfer due to friction. Owing to the
different thermal expansion coefficients of fiber and matrix,
shrinkage stresses arise in composites with thermoplastic
matrices during the cooling process, which promote a stress
transfer after debonding, by building up radial compressive
stresses in the interface. This effect is less pronounced for
low fiber volume fractions. Therefore, the shrinkage stresses
are neglected in this study. To simulate the propagation of the
crack, in each time step the links between one pair of elements
are released, so that the contact elements become active. For a
crack of about a quarter of the fiber length, 20 time steps are
performed, including up to 3 0 equilibrium iterations.

In Fig.4, the axial fiber stresses are plotted for the perfect-
ly bonded fiber, for the case when only the circular area at
the end of the fiber is debonded and for several phases of an
interface crack, running along the fiber. A friction coeffici-
ent of 0.7 is assumed for the interface. During the extension
of the crack, the fiber is continously unloaded. In the
 71
debonded zone, only small remaining fiber stresses are active.
They decrease almost linearly up to the fiber end, whereby the
slope flattens with increasing crack length.

σζζ [N/mm z ]

1
interfacial crack length / diameter ratio

perfectly bonded -

debonded fiber end -

fiber end

axial coordinate z \pm)

Fig. 4. Axial fiber stresses for different

phases of an interface crack

The corresponding interfacial shear stresses (Fig.5) reach

their maximum in the case of a debonded fiber end. With further
propagation of the crack, the maximum of the interfacial shear
stresses decreases to the amount of the perfectly bonded
system. In the contact zone, only small shear stresses are
built up due to friction, which diminish during the crack
extension. The zone of the maximum interfacial shear stresses
moves from the fiber end to the crack tip without a
considerable change of its intensity. That means that the
loading of the interface by shear stresses is of the same order
for a perfectly bonded fiber as for an interface crack.

r yz [N/mm z ]

1 débonded fiber end

k
A interfacial crack length / diameter ratio
A 0.32
\ / 0.64
\Y / ,0.36
perfectly
Jbonded ΛΑ \ / \ A Λ .-—1.60

0 2 1 24 8 3 B < 0 6 2 7
axial coordinate z [pm]

Fig. 5. Interfacial shear stresses for diffe-

rent phases of an interface crack
72
The radial stresses in the interface vanish over almost the
whole fiber length, except at the fiber end and in the debonded
region (Fig. 6 ) . Here, in the case of a perfectly bonded fiber
and of a debonded fiber end, high compressive stresses arise.
When the crack starts to run along the fiber, they are strongly
reduced and then decrease with further crack propagation. The
low radial stresses are limiting the stress transfer through
the debonded interface. Therefore, the influence of the
friction coefficient on the stress transfer is not important
for the investigated material combination.

Oyy [N/mm*]

100 -i

axial coordinate z [//ml

Fig. 6. Interfacial radial stresses for diffe-

rent phases of an interface crack

Conclusions

In fiber reinforced materials, severe stress concentrations

arise at the fiber ends, which can give rise to a debonding of
the interface. The propagation of an interface crack leads to a
shift of the zone of the shear stress concentrations from the
fiber end to the crack tip, without a considerable change of
its intensity. The delamination of the fiber end yields to an
unloading of the fiber but not to an unloading of the boundary
layer. That means that a total failure of the interface is
probable after initiation of an interface crack, when the
behaviour of the materials is brittle.

REFERENCES
Hampe, A. (1987). Grundlegende Untersuchungen an faserver-
stärkten Polymeren. Amts- und Mitteilungsblatt der BAMf
18, 3-7
Marotzke, C. (1990). Micromechanical investigation of fiber
reinforced materials by finite element analysis. In:
Struceng and Femcad ( A. Niku-Lari, Ed.), pp. 95-100
Marotzke, C., A. Hampe (1990). Finite element analysis of the
single fiber pull-out test. In: Struceng and Femcad
( A. Niku-Lari, Ed.), pp. 131-136
 WS9b5

DEFORMATION BEHAVIOR OF COMPOSITE INTERPHASE

NORIO SATO and TOSHIO KURAUCHI

Toyota Central Research & Development Laboratories, Inc.

Nagakute-cho, Aichi-gun, Aichi, 480-11, Japan

ABSTRACT

Deformation behavior of interphase in polymer matrix composite was studied by

means of in situ failure analysis by SEM, acoustic emission measurement,
dynamic viscoelastic property measurement, and thermo-acoustic emission
measurement which were proposed by the authors. Microvoiding, shear yield-
ing, and microcracking occurring in the interphase around the fibers were
found to play an important role for the toughening mechanism of the
composite.

KEYWORDS

Composite interphase; Microvoiding; Shear yielding; Microcracking; Toughening

mechanism; In situ failure analysis by SEM; Acoustic emission measurement;
Viscoelastic analysis; Thermo-acoustic emission measurement; Sheet molding
compound.

INTRODUCTION

Deformation behavior of the interphase around fibers in the polymer matrix

composite is considered to affect the fatigue durability of the composite.
Figure 1 shows a typical example of deformation behavior of the interphase
around fibers in a composite when subjected to an external load. Matrix
microviding, shear yielding, and microcracking are observed in the interphase
in the vicinity of the interface between the fiber and matrix. The micro-
failure is accumulated in the composite due to repeated loading applied to
the composite, which is considered to be responsible for fatigue of the
composite. Therefore, it is very important to clarify the deformation behav-
ior of the interphase for developing durable composite. In this study, some
novel methods to study the behavior are proposed and the relationship between
the deformation of the interphase and fatigue property of the composite is
discussed. The composite used here is a sheet molding compound (SMC) con-
sisting of a vinylester resin and randomly dispersed chopped-strands of glass
fibers (volume fraction of 40%).

73
74

Fig. 1. Deformation behavior of the interphase,

Microvoiding and shear yielding were generated
before interfacial Microcracking.

DEFORMATION OF INTERPHASE OBTAINED BY

IN SITU MICROFAILURE ANALYSIS

In order to examine the microfailure process of the interphase when the

composite is subjected to a load, in situ failure analysis by SEM (Sato et
al., 1985) was carried out. For the analysis, a composite specimen was
subjected to a bent load with a small bending device in a SEM apparatus, and
then SEM observation was carried out on the side surface of the specimen
under load to examine the deformation and microfailure of the interphase.
The observation was repeated with stepwise increase of the load until the
composite failed, so that detailed deformation behavior of the interphase as
well as morphology of microfailure could be obtained.

Figure 1 shows a typical example of the deformation behavior of the inter-

phase of an SMC composite under load, which shows microvoiding and shear
yielding of the matrix in the interphase and microcracking at the interface.
At first, microvoiding was observed to occur in the matrix in the vicinity of
the interface and to spread into the matrix region. Then, shear yielding of
the matrix was observed to occur in the matrix region between fibers. Then,
microcracking occurred at the interface, separating the matrix from the
fiber. The interfacial microcracking was observed to grow in the matrix
region and also to propagate to the interface of the neighboring fibers. So,
the microcrack grew to a large one, leading to final failure of the compos-
ite.

Fig. 2. DeforMation behavior of the interphase,

interfacial Microcracking was generated
without Microvoiding and shear yielding.
 75
Figure 2 shows an example of the deformation behavior of the interphase for
another SMC composite. For this composite, the sizing agent treated on the
fiber surface was different from that of the former one. In this case, the
interfacial microcracking occurred in a brittle manner without the occurrence
of microvoiding and shear yielding in the interphase. So, it was found that
the sizing agent strongly affects not only the bond strength at the interface
but also the deformation behavior of the interphase. From fatigue test of
these composites, the former composite was found to exhibit better fatigue
property than the latter one. Therefore, it is considered that microvoiding
and shear yielding of the interphase play an important role for the toughen-
ing mechanism for this type of the composite.

MICROFAILURE BEHAVIOR DETECTED BY

ACOUSTIC EMISSION MEASUREMENT

Figure 3 shows a typical example of acoustic emission behavior of an SMC

specimen under a three-point bending test with its load-deflection curve.
The emission was found to occur at a load fairly lower than the ultimate one
and to increase rapidly with the load. This result indicates that the micro-
failure in the composite begins to occur at a relatively low load and in-
creases with the increase of the load. The emission origin, however, was not
clarified only by the acoustic emission measurement. Then, the result of the
emission behavior was interpreted by comparing with the microfailure process
obtained by the in situ failure analysis (Sato et al., 1988). As a result,
it was found that the emission is associated with the interfacial microcrack-
ing shown in Figs. 1 and 2, not with microvoiding nor shear yielding of the
interphase. Then, it became possible to detect the occurrence of the inter-
facial microcrack sensitively by the acoustic emission measurement.

20000 '
o
o O
10000 ®
LU
<
0 20 40
Deflection ( m m )

Fig. 3. Load-deflection curve and acoustic emission

behavior under three-point bent test.

Figure 4 shows the emission behaviors with the increase of the applied bent
load for four kinds of SMC specimens among which the type of sizing agents
for the fibers was different. The start point of the emission was shifted
from lower load to higher one due to the xype of the agents. This result
indicates that the behavior of interfacial microcracking is strongly affected
by the type of the sizing agents. There was a tendency that the composite
which yielded the interfacial microcracking without microvoiding and shear
yielding in the interphase showed the faster start of the emission against
the bent load, on the other hand, the one which yielded microvoiding and
76
shear yielding in the interphase before the occurrence of the interfacial
microcracking showed the slower start of the emission. Furthermore, it was
found that the composite which showed the slower start of the emission showed
better fatigue property. Therefore, the emission behavior of the composite
was found to be strongly related to the fatigue property of the composite.

c
O
Ü
"c
Φ
>
LJJ
LU
<

500 1000
Load (N)
Fig. 4. Difference of the acoustic emission behavior
due to the type of the sizing agent.

VISCOELASTIC PROPERTY OF THE INTERPHASE

The composite is subjected to dynamic load of high level in the practical

uses, so that the viscoelastic property of the composite against the dynamic
load is considered to relate to the fatigue property of the composite. In
order to study the viscoelastic property of the composite under the dynamic
load of high level, a high power dynamic viscoelastic instrument was made
(Sato et al., 1990).

Figure 5 shows a typical example of the viscoelastic property which shows the
stress dependence of the storage modulus, dissipation factor, and temperature
rise until the composites failed. The storage modulus slightly decreased,
the dissipation factor remarkably increased, and the temperature slightly

1 12
-α
O ~
OC
1
Î&
o ^
° """*^£^>^Λ
I 8 ^^«^
03

\*s
0.12
V-"^ y·
1—0-10
^^1>
? o
^*^L^ B
£ | 0.08
^Z~^\^
ΑΤ^^*\^-*-*\
*£m**^\ _J—>—*^^ \
5 0.06
J&£~*-~*-
0.04
■f
§ — 20
«£>
S i - " 10 ^r^L·^·
= w
t τ-τ^ρϊ^ΤΎ^τ .I
50 100
Stress C MPa )

Fig. 5. Stress dependence of the viscoelastic property

of the composite and difference of the property
due to the type of the sizing agents.
 77
increased with the increase of the dynamic stress applied to the composite.
This change of the viscoelastic property of the composite is considered to be
resulted from the change of the viscoelastic property of the interphase due
to the occurrence of microvoiding, shear yielding, and microcracking. The
figure also shows the difference of the viscoelastic property due to the type
of the sizing agents treated on the fibers. It was found that the dissipa-
tion factor strongly depends on the type of the sizing agents. There was a
tendency that the composite which showed the lower value of the factor showed
the slower start of the acoustic emission, and that the one which showed the
higher value of the factor showed the faster start of the emission. Further-
more, the composite which showed the lower value of the factor showed better
fatigue property. Therefore, the viscoelastic property of the composite is
considered to be strongly affected by the deformation behavior of the inter-
phase and there is considered to be a relationship between the viscoelastic
property and fatigue one.

THERMAL MICROCRACKING OF INTERPHASE DETECTED BY

THERMO-ACOUSTIC EMISSION MEASUREMENT

When the composite is subjected to a thermal cycle, thermal stress is induced

due to the difference of the thermal expansion coefficient between the fiber
and matrix, which is sometimes responsible for the occurrence of microcrack
at the interphase. Acoustic emission occurring at that time is called ther-
mo-acoustic emission (Sato, et al., 1988).

Figure 6 shows the thermo-acoustic emission behavior of an SMC composite

consisting of carbon fibers. The composite was heated from room temperature
to 200 C and then cooled to room temperature. The emission was mainly ob-
served in the cooling period, which is considered to be associated with the
interfacial failure induced by the residual thermal stress. The interfacial
failure, however, was hardly observed by SEM examination. The emission is
presumed to come from very small interfacial microfailure.

The figure also shows the change of the emission activity due to the amount
of the sizing agent treated on the fibers. The activity was found to de-
crease with increase of the agent. The reason of the decrease is considered
as follows. The sizing agent is diffused into the matrix in the vicinity of

Fig.6. Thermo-acoustic emission behavior and

difference of the behavior due to the
amount of the sizing agent.
78
fibers in the curing process of the composite, which is responsible for the
formation of the interphase whose modulus is slightly lower than that of the
matrix resin. The residual thermal stress around fibers is relaxed due to
the presence of the soft interphase, so that the occurrence of the interfa-
cial microcracking is suppressed. This is the reason why the emission activ-
ity decreased with increase of the agent. The stress relaxation through the
interphase is considered to be very important mechanism to suppress the
microfailure at the interphase. The mechanism is available not only for the
thermal loading but also for mechanical loading to the composite. The dura-
bility of the composite is expected to be enhanced by the stress relaxation
mechanism through the interphase. The thermo-acoustic emission measurement
is considered to be used to obtain some information about the deformation
behavior of the interphase by the thermal stress.

CONCLUSION

The methods for analyzing the deformation mechanism of the interphase in the
composite were presented and some obtained results were reported. The mecha-
nism has still remained obscure, however, it is obvious that the interphase
has an important role for the fatigue durability of the composite. Further
study for the interphase is considered to become much more important for the
development of the composite for the structural applications.

REFERENCES

Sato, N., T. Kurauchi, S. Sato and 0. Kamigaito (1985). In Situ Observation

of Fracture Process in Short Glass Fiber Reinforced Thermoplastic Composite
ASTM STP 868, 495.
Sato N., T. Kurauchi, and 0. Kamigaito (1988). Reinforcing Mechanism by
Small Diameter Fiber in Short Fiber Composite. J. Comp. Mater., 22, 850
idem (1990). Novel Methods to Study the Deformation Behavior of Composite
Interphase. Proceedings of 5th Japan-US Conference on Composite Materials,
to be published,
idem (1988). Detection of Damage in Composite Materials by Thermo-Acoustic
Emission Measurement. J. Comp. Mater., 22, 447
 WS9b6

CHARACTERIZATION OF CARBON F I B E R SURFACE

RELATING TO I N T E R F A C I A L ADHESION I N COMPOSITES

Y. SAWADA, A. SHINDO* and Y. NAKANISHI

Government I n d u s t r i a l Research I n s t i t u t e of Osaka

1-8-31 Midorigaoka, Ikeda, Osaka 563, Japan
(«present address: Corporate Research & Development Laboratory, Tonen Corp.
1-3-1 Nishi-Tsurugaoka, Ohi, Irma, Saitaia 354, Japan)

ABSTRACT

Methods for evaluating the surface activity and surface roughness were
investigated on PAN-based carbon fibers. The specific surface areas were
determined by krypton adsorption measurements at -195°C on the carbon
fibers degassed at 100°C and 950°C. After the krypton adsorption
measurement, the carbon fiber was degassed again at 950°C, and then oxygen
chemisorption was measured at 300°C and an adsorbing time of 24 hours. The
active surface area was determined from the amount of chemisorbed oxygen,
and the ratio of active surface area to the surface area from the krypton
adsorption at a degassing temperature of 950°C was calculated as an active
surface area rate. Concentration of oxygen atoms on the fiber surface and
relative amount of the boundary carbon atoms in the fiber skin were
measured by XPS and Raman spectroscopy, respectively. They varied
depending on the active surface area rate. Surface roughness was evaluated
using the geometrical surface area obtained from optical diffraction
diameters of the fiber and the specific surface area at a degassing
temperature of 100°C. The interfacial shear strength in the composite
increased with increasing active surface area rate.

KEYWORDS

carbon fiber, surface area, active surface area rate, surface roughness,
krypton adsorption, oxygen chemisorption, XPS, Raman spectra, interfacial
shear strength, CFRP

INTRODUCTION

Carbon fiber reinforced plastics have high potential for the application to
structural materials, because of their high specific strength and modulus.
Such mechanical properties of the composites are brought about mainly from
the high strength and high modulus of the carbon fibers. In such a case,
the mechanical properties of the composites depend, to a large extent, on
the interfacial adhesion, and are in need of the optimum interfacial

79
80
strength between the carbon fiber and the matrix.

On the surface of the high performance untreated carbon fibers, the

graphitic basal planes are arranged in parallel to the surface. Therefore,
the carbon fiber exhibits poor adhesion to most thermosetting resins, and
consequently the composites fail to display their potential mechanical
properties which can be expected to be brought about from reinforcing
effectively with the carbon fibers. Therefore, commercially available
carbon fibers have been usually subjected to the surface treatment by
oxidation, which is to have the effect of increasing the surface activity
and roughness of the fiber surface.

By the way, it is generally accepted nowadays that in the epoxy matrix

composites carbon fibers adhered with the matrix primarily by the chemical
coupling through the oxygen-containing functional groups combining with the
carbon atoms protruding on the periphery of the graphitic basal planes. On
the other hand, on the fiber surface many wrinkles or ridges run nearly
along the fiber axis. They join to each other here and there and are
undulating in height. In addition, pits or depressions are probably formed
on the fiber surface by the surface treatment. Such uneven features of the
fiber surface are thought to increase the interfacial adhesion.

As mentioned above, the surface properties of the carbon fibers have a

marked influence on the display of the potential mechanical properties of
the composite. Accordingly, in the study on the mechanism of the
interfacial adhesion in the composite, the surface properties of the carbon
fibers must be first evaluated. This paper describes measurements of
specific surface area, active surface area, amount of boundary carbon atoms
and surface roughness performed to characterize the carbon fiber surface,
and a measurement of interfacial shear strength to demonstrate their
usefulness to understanding the interfacial behavior of the composites.

EXPERIMENTAL

PAN-based carbon fibers with or without surface treatment, and without

sizing supplied by manufacturers were used. They were chosen from high
strain types of carbonized fibers and the high modulus types of graphitized
fibers.

The specific surface areas were measured by the BET method using krypton
gas as adsorbate. A continuous carbon fiber yarn of about 1 g was washed
with distilled water and dried in air at 120°C. Subsequently it was
degassed at 100°C in a precision volumetric adsorption apparatus, and then
a krypton adsorption isotherm was measured. After that, the carbon fiber
was degassed again and heated in vacuo up to 950°C, and then another
adsorption isotherm was measured. The specific surface areas were
calculated from these data in a relative pressure range of 0.1-0.35.

After the measurement by the adsorption isotherms, the carbon fiber was
heated again up to 950°C and then cooled down to 300°C in vacuo. At that
temperature oxygen gas at 1.8-1.9 Torr was admitted to bring into contact
with the fiber. The amount of chemisorbed oxygen was measured after the
fiber sample had been held for 24 hours under the condition.

The concentration of oxygen chemisorbed on the fiber surface was evaluated

from the areas of the peaks of C l g and 0 l g by X-ray photoelectron
 81
spectroscopy (XPS), with a bundle like sample, correcting for the elemental
sensitivities.

To obtain information of the crystallograhic structure in the fiber skin,

Raman spectra were measured using bundle like fiber samples. The ratio of
the intensities of two peaks at 1365cm" and 1580cm" was evaluated. The
ratio is to be directly related to the amount of boundary carbon atoms,
including the peripheral carbon atoms and other relatively unstable carbon
atoms.

Densities of the carbon fibers were measured using a density gradient

column which was made up of ethanol and bromoform. On some of the carbon
fibers densities were also measured from the weight when the fibers were
immersed in various kinds of fluids such as a 0.5 percent aqueous solution
of sodium acetate, ethanol, benzene, acetone or a silicone oil to compare
the influence of the penetrating power.

Optical maximum and minimum diameters at a cross section of the carbon

fiber were measured from the Fraunhofer diffraction pattern of a He-Ne
laser beam. The influence of the reflection from the fiber surface on the
pattern was corrected(Perry et al., 1974). From the mean optical
diameters, the geometical surface area per unit length of a single
filament, SAL, was calculated, being based on the assumption that the
filament was a column having the circular or elliptical cross section with
the diameters obtained. Next, another surface area per unit length of the
filament, SA-^QQ, was calculated from the specific surface area at a
degassing temperature of 100°C, weight per unit length of the fiber yarn
and filament number in the yarn. From these data, surface roughness was
calculated by the equation:
R = ( SA 1 0 0 - SA L ) / SAL. (1)
The interfacial shear strengths in the carbon fiber reinforced epoxy or
polyimide composites were measured using dumbbell shaped specimens having a
single filament, which were prepared in a silicone mold. The specimen was
stretched until the number of the fragments of filament fractured in the
resin was saturated, under a transmitted light microscope with polarized
light illumination, and the length of the fragments was measured. The
critical transfer length, L c , is obtained by the equation(Ohsawa et al.,
1978):
Lc = 4 L / 3 (2)
where L m is the mean fragment length. The interfacial shear strength, T ,
is calculated according to the equation(Kelly et al., 1965):
-C «( 5 f / 2 )( T x d x d m i n / Lc / Ls ) (3)
where Ç"f is the fiber tensile strength at a gauge length of L c . The
tensile strength, 6~f was estimated from the single filament strengths at
gauge lengths of 5, 10, 20 and 40 mm, applying Weibull statistics. And
d
max a n d dmin a r e t n e °Ptical maximum and minimum fiber diameters. L g is
the circumference of the circular or elliptical cross section with the
diameter obtained, and is calculated from an approximate equation:
L
s = ^ x dmax x I ! - U/4)e 2 - (3/64)e4 - (5/256)e6 ]. (4)
where e is defined by the equation:
e
= A J < W 2 - dmin2 / < W <5>

RESULTS AND DISCUSSION

82
Surface Activity of Carbon Fibers

Fig. 1 shows some of the krypton gas adsorption isotherms obtained for the
carbon fibers degassed at 100°C and 950°C. The specific surface areas
estimated from the isotherms are shown in Table 1. There can be seen
increases in specific surface area with the rise of degassing temperature
and the surface treatment. The increments of specific surface area by
surface treatment of the carbonized fibers are larger at a degassing
temperature of 100°C. However, those of the graphitized fibers are larger
at a degassing temperature of 950°C. This difference probably reflects the
difference in shape of pits or depressions formed by the surface
treatments.

In Figs. 2 and 3, the amount of chemisorbed oxygen on a carbon fiber (X550-

S), obtained at different temperatures and initial oxygen pressures, are
shown as a function of chemisorbing time. The initial pressure is the
pressure which the oxygen gas is to exhibit if the gas is introduced into
the vacant sample container. The amount of chemisorbed oxygen increases
with rising temperature, and the higher the initial oxygen pressure is, the
larger the amount of chemisorbed oxygen becomes, though it was not
saturated even at 16 hours. The amounts of chemisorbed oxygen at a
chemisorbing time of 24 hours at 300°C and at an initial oxygen pressure of
1.8-1.9 Torr were evaluated, then, to obtain the relative values of surface
activity for the carbon fiber. From the amounts, the specific active
surface areas were calculated on the assumption that all of the chemisorbed
oxygen formed carbonyl groups with the peripheral carbon atoms of the
graphitic layer planes in the surface. The ratio of the specific active
surface area to the specific surface area for the fiber degassed at 950°C
was calculated as the active surface area rate. They are also shown in
Table 1.

The oxygen concentration obtained by XPS and the intensity ratio of the two
peaks of the Raman spectrum are plotted against the active surface area
rate in Figs. 4 and 5, respectively. The oxygen concentration increases
linearly with increasing active surface area rate for each type of carbon
fiber. The intensity ratio of Raman peaks for the graphitized fiber
increases with increasing active surface area rate, but the variation in
the intensity ratio brought about by the surface treatment is very little
for the carbonized fiber.

Surface Roughness of Carbon Fibers

The densities evaluated by immersing the carbon fiber in various kinds of

fluid did not show a meaningful difference between the fluids.
Furthermore, there was seen no meaningful deference between the cross-
sectional areas measured from the mean optical diameters and from the
weight per unit length, filament number and density of the yarn.

The surface roughness of the carbon fibers are shown in Table 1. There are
seen increments of the surface roughness brought about by the surface
treatment.

Relationship between Surface Properties of Carbon Fibers and Interfacial

Shear Strength
 83
The interfacial shear strength in
the composite increases with

°-° 1
increasing active surface area 0.5 [■
rate, as shown in Fig. 6. The
other measures of surface activity ho
□* 1

such as the surface oxygen o

o 0.4
concentration estimated by XPS and
the intensity ratio of the Raman nd
ω ^
spectra also indicated & 0.3 L y
u
o ΓΓ1 AX* ^o
relationships with the interfacial
shear strength, but they showed
CO
T3 \
difference between the types of
1

rk
carbon fibers. (
0 -p*--

SUMMARY , ,
u
1 1
Methods for evaluating the surface 0 0.2 0.4 0.6 0.8 1.
activity and roughness of carbon Relative pressure (P/P0)
fibers were studied. It was able
to demonstrate that the Fig. 1. Krypton adsorption
measurements of the gas adsorption isotherms at -195°C.
were useful for characterizing the • ; X550-S,degassed at 100°C
O ; X550-S,degassed at 950°C
surface of the carbon fiber as
■ ; M40-S, degassed at 100°C
reinforcement for resin matrix a ; M40-S, degassed at 950°C
composites.

Table 1. Characterization of carbon fiber surface by gas adsorption

o
Surface area (m /g)
Active sur face area Sui"face
Fiber after degassing
at 100°C at 950°C
(m2/g) (%) Roughness {%)

Carbonized fiber
X550-U 0.442 0.603 0.046 7.7 21.
X550-S 0.495 0.630 0.085 13.4 36.
ST3-U 0.382 0.473 0.025 5.2 14.
ST3-S 0.404 0.488 0.049 10.0 23.
Graphitized fiber
M40-U 0.404 0.526 0.014 2.7 17.
M40-S 0.571 1.182 0.126 10.7 61.
HM40-U 0.421 0.496 0.013 2.6 26.
HM40-S 0.453 0.592 0.052 8.8 37.

REFERENCES

Kelly,A and W.R.Tyson(1965). High strength materials(V.F.Zackay,ed.),p.578.

Wiley.
Ohsawa,T., A.Nakayama,, M.Miwa and A.Hasegawa(1978). Temperature dependence
of c r i t i c a l fiber length for glass f i b e r - r e i n f o r c e d thermosetting r e s i n s .
J.Appl.Polym.Sei.,22,3203-3212.
P e r r y , A . J . , B.Ineichen and B.Eliasson(1974). Fibre diameter measurement by
l a s e r d i f f r a c t i o n . J.Mater.Sei.,9,1376-1378.
84

S 0 .10
\
Β^
0 08 *A°
PC v^Ä 0.15 6tot*
^o*
cd fc^ οΠ
<D
PC* ,QO1
πα°
u ο,θθ
cd
0 06 0.10 Χ.891ΤΤΟΓΓ
nd
ω
J-l .«/^ϊ??."3ϋ-
0. 04
rû
O
0.05
πΡ 0.7826ΤΟΓΓ

IfiP •H

o. 0 2 ^ # · · · · · · ^ · · ; · ΐ 5 ^ Γ Γ e
0
0 5 10 15 20
0 JL·
0 5 10 15 20 Chemisorption time at 300°C (h)
Chemisorption time (h) Fig. 3. Dependence of oxygen
F i g . 2 . Dependence of oxygen chemisorption on initial
c h e m i s o r p t i o n on t e m p e r a t u r e oxygen pressure and time;
and t i m e ; sample:X550-S. sample:X550-S.

25

20

15
</ o

y
^
10
o
bt) 5

1 1 1 1 11 1 1 1 1 1 1 1 1 1 1
"0 5 10 15 5 10 15
A c t i v e s u r f a c e a r e a r a t e {%) A c t i v e s u r f a c e a r e a r a t e {%)
F i g . 4 . R e l a t i o n s h i p between s u r f a c e F i g . 5 . R e l a t i o n s h i p between
oxygen c o n c e n t r a t i o n i n t e n s i t y r a t i o of Raman
e s t i m a t e d by XPS and a c t i v e peak and a c t i v e s u r f a c e
surface area r a t e . area r a t e .
O ; X550, Δ ; ST3, · ; M40, A ; HM40 O ; X550, Δ ; ST3, · ; M40, A ; HM40

II« •
F i g . 6. I n t e r f a c i a l s h e a r s t r e n g t h
Interfacial

as a f u n c t i o n of a c t i v e
surface area r a t e .
strength

O ; untreated carbonized/polyiiide
yu
- Δ/8' •
a
;
;
surface treated carbonized/polyiiide
untreated carbonized/epoxy
Δ ■ ; surface treated carbonized/epoxy
1 1 1 1 1 i 1 1 1 I I I 1 11 Δ ; untreated graphitized/epoxy
) 5 10 15 A ; surface treated graphitized/epoxy
Active surface area rate (*)
WS9b7

Study on Interface of Thermoplastic Composite Laminate

made of Co-woven Fabrics

Tsuneo Hirai*, Tsutao Katayama*, Shimpei Ito**,

Hirokazu Inoguchi***, Masahiro Shinohara****,
and Masayoshi Ogawa****

* Faculty of Engineering, Doshisha University,

Karasuma-Imadegawa, Kamigyo-ku, Kyoto
** Nitto Boseki Co., Ltd., Toyo-Hamacho Bldg., 2-9-5,
Nihombashi-Hamacho, Chuo-ku, Tokyo
*** Nitto Boseki Co., Ltd., Electronic Material Research
Laboratory, 20 Ipponsugi, Sakurashimo, Fukushima
#**# Graduate Student, Doshisha University,
Karasuma-Imadegawa, Kamigyo-ku, Kyoto

ABSTRACT

Thermoplastic resin trends to be applied to the matrix of the continuous

fibre reinforced composites. But it is difficult to impregnate reinforce-
ment strands with melted resin because of its high viscosity. Therefore,
to improve the defect, co-woven fabrics have been developed.
In this paper, the adhesive condition at the matrix/fibre micro interface
of co-woven fabric laminates is estimated by comparing with that of film
stacking laminates under immersion tests in hot water. Consequently, it is
shown that this co-woven structure is effective for the impregnation with
matrix resin and the adhesive condition at the micro interface.

KEYWORDS

Thermoplastic composites; adhesive condition; co-woven fabrics; film

stacking; immersion test; impregnation with matrix resin.

INTRODUCTION

Recently, fibre reinforced thermoplastic (FRTP) composites are widely used

and drawing public attentions because these composites have the potential
to offer high impact resistance, high fracture toughness, benefits of
decreased manufacturing cost and so on. However, in application of the
thermoplastic resin to continuous fibre reinforced composite materials, it
is difficult to impregnate reinforcement strands with melted resin due to
its high viscosity and there are some areas where can't be filled up with
the melted resin, or some voids in the composites. Mechanical properties
of these thermoplastic composites are much affected by these defects.
Therefore, to improve such defects, co-woven fabrics have been developed.
These fabrics have the structure that cold-stretched fibrous thermoplastic
resins are coupled with reinforcement strands and the fibrous resins and
reinforcement strands are co-woven. When the co-woven fabrics are applied
to composites, it is expected that impregnation with melted resin will be
easy and the adhesive condition at the matrix/fibre micro interface will

85
86

be better by this structure.

In the previous paper (Hirai et al., 1990), to evaluate the adhesive con-
dition at the micro interface, glass/nylon co-woven fabric laminates were
immersed in hot water and the adhesive interface of the laminates was
degraded. If the adhesive condition at the micro interface of the
laminates is not better, the interface seemed to be degraded faster and
mechanical properties of the laminates seemed to be lower. Therefore,
after the immersion test, the mechanical properties of co-woven fabric
laminates were obtained and the adhesive condition at the micro interface
was discussed. But the nylon resin absorbed water well and dissolved in
water well, so it was not easy to make clear whether the lowering of
mechanical properties is due to the degradation of the adhesive interface
or the dissolution of the matrix resin.

In this paper, instead of nylon resin, polyetherimide (PEI) resin was used
as a matrix and the immersion test was performed. To make clear the effect
of co-woven structure on the interfacial condition at the micro interface,
mechanical properties after the immersion test of co-woven fabric
laminates were compared with those of glass/PEI film stacking laminates.

EXPERIMENTAL PROCEDURE

Test Specimen

In f a b r i c a t i n g composite Glass fiber Glass cloth

laminates, two types of
l a m i n a t i o n method a r e
applied. One method uses
co-woven f a b r i c , c o n s i s t
of fibrous PEI r e s i n and
T-glass f i b r e , (TEXXES®
hybrid f a b r i c , Nitto
Boseki C o . , L t d . ) and
these fabric are
laminated. Another
method is the film
stacking method t h a t PEI
film and T-glass Co—woven fabric Film stacking
cloth are laminated a l -
t e r n a t e l y . Fig.1 shows Fig.1 Schematic drawing of laminate
a schematic drawing of constructions.
laminate constructions.
Each laminate i s press-moulded a t 350°C and 0.5 MPa in the matched metal
d i e . The a p p l i e d f i b r e weight f r a c t i o n i s 5Λ (%) in both t y p e s of
laminates.

Immersion Test under Hot Water Environment

To estimate the impregnation with matrix resin and the adhesive condition
at the matrix/fibre micro interface, the immersion test under the constant
temperature at 80°C are performed. This is called the "constant
environment" here. Besides to promote the degradation of adhesive inter-
face, the immersion test under another environment are carried out. In
 87
this environment, temperature varies cycli-
cally between 70°C and 90°C. This is called
the "cyclic environment" here. Fig.2 shows
the relation between the environment tem-
perature and time in the unit cycle. Both
types of the laminates are immersed in each
type of the environment. After the set im-
mersion time, absorption properties such as
the weight ratio, W r , the dissolution loss,
W , and the water absorption ratio, ¥ w , are
obtained. Because both laminates have the Time (min.)
same fibre weight fraction, the absorption
properties seem to be much affected only by Fig.2 Relation between the
the impregnation with matrix resin or the environment tempera-
adhesive condition at the micro interface. ture and time in
the unit cycle.
The weight ratio, Wr, is obtained as
follows;

W r = (Wg-W^/W-, (1)

where W-j is the weight of matrix resin in the specimen before immersing
and W2 is the weight of matrix resin in the wiped specimen after immers-
ing.

The dissolution loss, ¥ , is obtained as follows;

W e = (W3-W1)/W1 (2)

where ¥0 is the weight of matrix resin in the dried specimen after immers-
ing.

Therefore the water absorption ratio W w is obtained as follows by eq. (1)

and eq. (2);

W w = (Wg-W^/Vl·, = ¥ r -W e (3)

Then to estimate the adhesive condition at the matrix/fibre micro inter-

face, the three point bending test is carried out in conformity with JIS
K7055 at every immersion time and the flexural strength retention is
determined.

RESULTS

Immersion Test under the Constant Environment

The absorption properties and the flexural strength retentions in co-woven

fabric laminates are compared with those in film stacking laminates under
the constant environment.

Absorption Properties Fig.3 shows the relation between the absorption

properties and the immersion time under constant environment. In this
figure, the water absorption ratio increases as the immersion time goes
by. The dissolution loss is almost constant until 200 hours and comes to
88

decrease after 200 hours. Because PEI resin comes to dissolve after this
resin is saturated with water for 200 hours in these specimen. And the
water absorption ratio of film stacking laminates has higher value than
that of co-woven fabric laminates. The difference of the water absorption
ratio between two types of laminates until 200 hours is due to the ad-
hesive interface condition. Because the impregnation with matrix resin of
film stacking laminates is worse than that of co-woven fabric laminates,
so there are some voids in the laminates and the adhesive condition at the
micro interface of film stacking laminates seems to be worse. The impreg-
nation would be confirmed by the retention of the flexural strength.

Flexural Strength Retention Fig.4 shows the relation between the flexural
strength retention and the immersion time under the constant environment.
The flexural strength retention decreases until 200 hours, and this reten-
tion decreases more steeply after 200 hours. The flexural strength reten-
tion of film stacking laminates is lower and decreases earlier than that
of co-woven fabric laminates. Until 200 hours, the difference of the
retention between two types of laminates is due to the adhesive condition
at the matrix/fibre micro interface.

120
Water absorption
Q (Co—woven) O Co—woven fabric
Δ Film stacking
φ (Film stacking) 2° ^
H , lOOf

Of
Dissolution loss i
Δ (Co—woven)
* (Film stacking)

60
<

40
10 100 1000 10000 10 100 1000 10000
Immersion time (hr.) Immersion time (hr.)

Fig.3 Relation between the ab- Fig. 4. Relation between the

sorption properties and flexural strength reten-
the immersion time under tion and the immersion
the constant environment. time under the constant
environment.

Immersion test under the Cyclic Environment

To promote the degradation of the adhesive interface, the immersion test

under the cyclic environment are carried out for both types of laminates.
And the absorption properties and the flexural strength retention of each
laminates are compared. Besides these properties under the cyclic environ-
ment are also compared with those under the constant environment.
 89
Absorption Properties Fig.5 shows the relation between the absorption
properties and the immersion time under the cyclic environment. In this
figure, there are hardly any differences between constant environment and
cyclic environment until 200 hours. Therefore the cyclic environment has
no effect on the absorption properties until the matrix resin comes to
dissolve. After 200 hours, the dissolution loss of the matrix resin be-
comes so large that it is not clear whether the difference between the
water absorption ratio under the cyclic environment and that under the
constant environment is due to the degradation of the adhesive interface
or due to the dissolution of the matrix resin.

Flexural Strength Retention Fig.6 shows the relation between the flexural
strength retention and the immersion time under the cyclic environment.
Also in this case, the flexural strength retention has the same tendency
as under the constant environment. But the flexural strength retention of
film stacking laminates decreases earlier than that of co-woven fabric
laminates and the difference of the retention between co-woven fabric
laminates and film stacking laminates is larger than that under the con-
stant environment. If the adhesive condition at the matrix/fibre micro in-
terface is worse, the adhesive force at the micro interface seems to
reduce easily because of the difference of thermal expansion coefficients
between the glass fibre and the matrix resin under cyclic environment.
120
Water absorption
O Co—woven fabric
Q (Co—woven) Δ Film stacking
$ (Film stacking) 8 o
X

- 1 lOOf

£ 80
of
Dissolution loss
o Λ (Co—woven)
a i (Film stacking)

60l·
<

-2 40
10 100 1000 10000 10 100 1000 10000

Immersion time (hr.) Immersion time (hr.)

Fig.5 Relation between the ab- Fig.6 Relation between the

sorption properties and flexural strength reten-
the immersion time under tion and the immersion
the cyclic environment. time under the cyclic en-
vironment.

CONCLUSION

In this paper, to estimate the interfacial conditions at the matrix/fibre

micro interface of co-woven fabric laminates, the immersion test under the
90
hot water environment is carried out. And following results are obtained.

(1) The water absorption ratio and the flexural strength retention under
both environments seems to be affected by the impregnation with the matrix
resin and the adhesive condition at the micro interface until the matrix
resin comes to dissolve.

(2) When the adhesive condition at the matrix/fibre micro interface is

worse, the flexural strength retention under the cyclic environment
decreases earlier and is lower than the flexural strength retention under
the constant environment. Under the cyclic environment, the water absorp-
tion ratio seems not to be affected by the cyclic change of temperature
until the matrix resin comes to dissolve. So this cyclic environment is
slightly effective to estimate the interfacial condition at the micro in-
terface until the matrix resin comes to dissolve.

(3) When co-woven fabrics are applied to the continuous fibre reinforced
laminates, the impregnation with matrix resin and the adhesive condition
at the matrix/fibre micro interface are better than those of film stacking
laminates. Therefore this co-woven structure is effective for the impreg-
nation with matrix resin and the interfacial condition at the micro inter-
face.

REFERENCES

Hirai, T., T. Katayama, S. Ito, H. Inoguchi and J. Araki (1990). Study on

micro-interface of FRTP laminate made of fibrous thermoplastic resin and
reinforcement strands in hot water environment. Journal of the Society of
Materials Science, Japan, 39i 989-995· (in Japanese)
 WS10a1

FATIGUE CRACK GROWTH CHARACTERISTICS OF METAL MATRIX

COMPOSITES
Kazumi HIRANO

Mechanical Engineering Laboratory, Agency of Industrial Science and

Technology, MITL
Namiki 1-2, Tsukuba-shi, Ibaraki-ken 305, JAPAN.

ABSTRACT

One of the most important and urgent problems is to characterize the fatigue damage tolerance
behavior for a wide use of advanced metal matrix composites (MMCs) for primary aerospace,
aeronautic and automotive structural applications. The final goal of this study is to establish the
new concepts of material design for high performance (high strength, high toughness and high
durability) MMCs. In this paper, current R&D trends on advanced structural composite materi-
als in Japan were generally reviewed, and the fatigue crack growth characteristics covering the
threshold stress intensity factor range AKth, which is one of the most important fracture mechan-
ical properties for ensuring the composite structural integrity, were investigated for whisker-
reinforced high-strength aluminium alloy, continuous fiber-reinforced aluminium and titanium
alloys matrix composites on the basis of fracture mechanics and fractography.

KEYWORDS

Fracture Mechanics; Metal Matrix Composite; Fatigue Crack Growth Characteristics;

Threshold Stress Intensity Factor; Fatigue Failure Mechanism.

INTRODUCTION

The significance of understanding the fatigue damage tolerance behavior has been recognized for
ensuring the composite structural integrity, because research and development (R&D) on ad-
vanced composite materials technology is more and more active and mature with the aim of
practical use. In particular, one of the most important and urgent problems is to characterize the
fatigue crack growth(FCG) characteristics for a wide use of the advanced composite materials
for primary aerospace, aeronautic and automotive structural applications. The final goal of this
study is to establish the new concepts of material design for the high performance(high strength,
high toughness and high durability) composite materials. In this paper, current R&D trends of
the advanced structural composite materials in a field of aeronautics and aerospace technologies
in Japan was generally reviewed, and a few of my current research (Hirano et al., 1988-91)
would be introduced for fracture mechanical characterization. FCG characteristics covering the
threshold stress intensity factor range ΔΚ^, which is one of the most important fracture mechan-
ical properties, were investigated in order to ensure the fatigue damage tolerance behavior for
whisker-reinforced high-strength aluminium alloy, continuous fiber-reinforced aluminium and
titanium alloys matrix composites on the basis of fracture mechanics and fractography.
93
94
CURRENT R&D TRENDS OF ADVANCED STRUCTURAL COMPOSITE
MATERIALS IN JAPAN

The most interesting and candidates for the advanced structural materials in a field of aeronautic
and aerospace technologies are summarized in Fig. 1 (SJAC Report, 1989). Recently, in our
country, several R&D national projects have also performed on these advanced structural mate-
rials. Project on both polymer matrix composites(PMCs) and MMCs had carried out for the past
eight years in the Basic Technology Projects for the Future Industries under the sponsorship of
Ministry of International Trade and Industry. Project on intermetallic compounds (IMC), fiber
reinforced these matrix composites(IMCs) and carbon-carbon composites(C/Cs) have started in
1989. Research on the basic technology for the development of Functionally Gradient Materi-
als(FGMs) for relaxation of thermal stress has also been done under the sponsorship of Science
and Technology Agency. In these projects, we have researched and developed the technologies
for advanced materials testing, and performed fracture mechanical characterization for the high
performance materials at an ultra-high temperature (Hirano et ai, 1990).

Fig. 1. Current R&D trends of advanced structural materials and its temperature capability.

WHISKER-REINFORCED HIGH-STRENGTH ALUMINIUM ALLOY

MATRIX COMPOSITES

MMCs are generally considered to be attractive as structural materials because of their superiority
over PMCs for the high-temperature application as well as their high specific strength and mod-
ulus. In particular, discontinuously reinforced MMCs are attractive in that they exhibit essen-
tially isotropic properties and can offer distinct technological advantages over continuously rein-
forced MMCs, as well as cost advantages, due to lower fiber costs and the ease of their fab-
ricability using standard metal working practices. One of the most important mechanical proper-
ties of structural materials is durability (fatigue life, damage tolerance safety). However, very
little data have been reported on the fatigue damage tolerance behavior (Logsdon et al., 1986).

Relationships between da/dN and ΔΚ

Fatigue crack growth rates da/dN as a function of ΔΚ are shown in Fig. 2 for silicon carbide
whisker-reinforced aluminium alloy matrix composite (SiCw/2025Al). The figure indicates that
the da/dN are uniquely related to ΔΚ in the logarithmic diagram, and the da/dN-ΔΚ relationship
can be expressed by Paris-Erdogan's rule (Paris et ah, 1963) in the range of da/dN > 10 9 m/
 95
cycle. The slope of the logarithmic plots is large compared with those of the ordinary metallic
materials. This is due to both the difference in fatigue failure mechanism and the lower fatigue
fracture toughness AKfc (identical to plane-strain fracture toughness Kj c (Hirano et al., 1989)),
which is determined at final fast fracture during the fatigue crack growth test. And it is found
that the da/dN-ΔΚ relationships are deviated from the linear expression with decreasing ΔΚ, and
consequently the da/dN approaches to ultra-low value. That is to say, there truly exists AKth for
whisker-reinforced aluminium alloy matrix composite. It can also be seen that there is a remark-
able dependence of the FCG characteristics on stress ratio R. The higher R have the larger fa-
tigue crack growth rates. Eventually, the AKth decreases with increasing stress ratio.

Effect of Specimen Orientation. It is also found from Fig. 2 that there is a remarkable depen-
dence of the FCG characteristics on specimen orientation, and da/dN for L-T orientation are
lower by one or two orders of magnitude than those for T-L orientation at the same ΔΚ value.
This is remarkably reflected in the ΔΚ^ value. It is concluded here that there is a remarkable
anisotropic property in the FCG characteristics, and the FCG resistance for the L-T orientation
is superior to that for the T-L orientation. However, it should be noted here that the mixed-mode
(Modes I and II) fracture occurred in the L-T orientation as shown in Fig. 3. It is necessary for
the further research to quantitatively evaluate the FCG resistance for the L-T orientation.

10-:
F" SiC /2025
w
io-(
p R=0.05
10""

io-£ u !0

Mixed mode
io-<

io-1
-

—
iW 0 L-T
D T-L
io-1
~
\° " <£U24-l3 Mode I
0 °
I I I I ! , iJL_
5 10 50
ΔΚ MPaym

Fig. 2. Fatigue crack growth rates as a Fig. 3. Schematics of macroscopic fatigue

function of ΔΚ for SiCw/2025Al. crack growth path.

Influence of Matrix Metal on FCG. Figure 4 shows that the da/dN for SiCw/7075Al at the
same ΔΚ value are higher than those for SiCw/2025Al. In particular, there is a remarkable dif-
ference near the threshold. The AKth value determined at da/dN =10 10 m/cycle is nearly 1.6
MPam 1 / 2 for SiCw/7075Al, on the other hand is about 4.0 MPam 1 ' 2 for SiCw/2025Al. In
summary, the FCG resistance for SiCw/7075Al is inferior to that for SiCw/2025Al.

A comparison of the da/dN-ΔΚ relationships indicates that the da/dN for SiCw/7075Al at the
same ΔΚ value are higher than that for unreinforced 7075A1 alloy, and the FCG resistance is
inferior to that for the matrix metal. In particular, it is noticeable both in the lower growth rates
region near the threshold and in the higher growth rates region. The whisker reinforcement of
7075Al alloy is not always effective to improve the FCG characteristics for the T-L orientation,
and rather reduces the FCG resistance. On the other hand, the FCG rates are lower for the
SiCw/2025Al vis-a-vis the unreinforced matrix until a ΔΚ level is reached where the lower
96

O Vf=17.1%
Δ Δ Vf=19.0%

X
■ 4
CO 0.6 ' Δ
E Δ S Cw/
v * ^ ^ 2C 25-T6
Q. 0.4
O

'
ΡΔ *Δα_ΔΑ *tA Δ

Γ
ο op^ Δ

Kmax MPaVm

Fig. 4. Influence of matrix metal on FCG Fig. 5. Plots of Kop/Kmax against K max .
characteristics.

fracture toughness of the reinforced alloy once again predominates. In particular, AKth for the
reinforced alloy is superior to that for the unreinforced matrix metal. It is considered to be pri-
marily due to the fatigue crack deflection and the crack bowing mechanisms.

Crack Closure Characteristics

Ratios of crack opening stress intensities Kog to maximum stress intensities K m a x are plotted
against K max in Fig. 5. It can be seen from this figure that the Kop/Kmax values are nearly con-
stant in the higher K m a x region, and rapidly increase with decreasing K max . It is also presumed
from the fractographic examinations of both fracture surface and fracture path that is due to the
plasticity-induced, fracture surface roughness-induced and fretting oxides-induced crack clo-
sures. In particular, it is supposed to occur the crack closure due to both the roughness of frac-
ture surface and the mixed mode deformation resulted from the zig-zag fracture path near the
threshold. It is also found that the Kop/Kmax values for SiCw/7075Al are considerably lower
than those for SiCw/2025Al.

Plots of the da/dN against the effective stress intensity factor range AKeff determined from the
measurements of the crack closure show that the da/dN-AKeff relationships covering the ultra-
low crack growth rates near the threshold region can be expressed by the power law, although
there is a little scatter. The da/dN-AKeff relationship for SiCw/7075Al except near the threshold
agrees relatively well with that for SiCw /2025Al. It is concluded here that the influence of the
matrix metal on the FCG characteristics can be rationalized by the concept of the crack closure,
although it is fairly questionable in measuring Kop, especially near the threshold.

Fractographic Examinations

Fatigue cracks predominantly propagated in the matrix metal near the threshold, and the whiskers
were not appeared on the fracture surface as shown in Fig. 6. Fatigue striation patterns which
characterize the fatigue fracture mechanism cannot always be clearly observed even at Stage lib.
 97

(a) SiCw/7075Al (b) SiCw/2025Al

Fig. 6. Fractographs of fatigue fractured surface near the threshold.

The monotonie fracture mechanism, that is, quasi-cleavage, dimple, joining of voids and cavi-
ties, and interfacial fracture patterns, rather than cyclic fracture mechanism are mainly observed.
In particular, the quasi-cleavage patterns are observed for SiCw/7075Al due to low tensile
ductility, on the other hand the ductile aspects like dimple pattern for SiCw/ 2025A1. These
fractographic examinations are essentially identical to the difference of the FCG resistance be-
tween SiCw/7075Al and SiCw/2025AL The whisker reinforcement for the FCG resistance in
2025Al alloy is presumed to be due to both the less preferential alignment and the compatibility
between whisker and the matrix metal.

CONTINUOUS FIBER-REINFORCED METAL MATRIX COMPOSITES

Macroscopic Features of FCG Behavior

A summary of the observed path of fatigue fracture in the unidirectionally continuous fiber
(SICCVD) reinforced MMCs is presented in Fig. 7. Crack propagation path is found to be
dependent upon the matrix metal and the fiber/matrix interface characteristics. It is a great differ-
ence that the longitudinal fatigue crack growth did not occur in the case of Al alloy matrix com-
posite, on the other hand, in the case of Ti alloy matrix composite both the longitudinal and the
mixed-mode (Modes I and II) FCG behaviors occurred with breaking the reinforcement fibers.
A weak interface and great difference of mechanical properties between the reinforcement fiber
and the matrix metal led to interfacial debonding within the plastic zone at the crack tip in the case
of SICCVD/A1 alloy and caused the crack to propagate the fiber/matrix interface. A strong inter-
face and a relative little difference of mechanical properties allowed little debonding and crack
propagated with the fiber breakage in the case of SiCcvr/Ti alloy.

Transverse FCG Characteristics

There are remarkable influences of both stress ratio and matrix metal on the transverse FCG
characteristics. Effect of stress ratio on the da/dN-ΔΚ relationship is certainly rationalized by the
concept of crack closure. Effect of matrix metal on the da/dN-ΔΚ relationship, especially near
the threshold, is also successfully rationalized by a parameter of ΔΚ/Ε (Hirano et al, 1988).

A schematic illustration is summarized in Fig. 8 for the presumption of the transverse FCG char-
acteristics. The da/dN-ΔΚ relationship covering the near-threshold can be successfully presumed
in terms of parameter AK/(1-Vf) from that for the matrix metal by considering the degradation of
fracture toughness Kc.
98

SiCWAlalloy]-

AKfc

I I '

T-orientation
w
Mixed mode L-orientation
Z
•o
CO

SiCcvp/Ti alloy)—

uk High ΔΚ

- da/dN-AK(Matrix metal)

T-orientation
Ψ
Mixed mode L-orientation
ΔΚ/d-Vf)

Fig. 7. Schematics of macroscopic features of Fig. 8. Schematic illustrations of the trans-

FCG behavior for unidirectional verse FCG characteristics and the
MMCs. plastic zone size at a crack tip.

Transverse FCG Characteristics

There are remarkable influences of both stress ratio and matrix metal on the transverse FCG
characteristics. Effect of stress ratio on the da/clN-ΔΚ relationship is certainly rationalized by the
concept of crack closure. Effect of matrix metal on the da/dN-ΔΚ relationship, especially near
the threshold, is also successfully rationalized by a parameter of ΔΚ/Ε (Hirano et al, 1988).

A schematic illustration is summarized in Fig. 8 for the presumption of the transverse FCG char-
acteristics. The da/dN-ΔΚ relationship covering the near-threshold can be successfully presumed
in terms of parameter AK/(1-Vf) from that for the matrix metal by considering the degradation of
fracture toughness Kc.

Mixed Mode FCG Characteristics

Aluminium Alloy Matrix Composite. Stable crack growth can be achieved under the mixed
mode loading. The FCG rates db/dN for SÎCCVD/6061 Al are plotted as a function of maximum
J-integral (Jmax) in Fig. 9. The db/dN are uniquely related to J max . The relationships in the sta-
ble fatigue crack growth rate region (db/dN > 10 8 m/cycle), that is Stage lib, can be expressed
by the power law. It is also found that there is a remarkable influence of the matrix metal and the
interfacial properties on the mixed mode FCG characteristics. The FCG resistance for SiCcvD
/Al-4%Ti alloy is superior to that for SiCcvrV 6061 Al.

The solid line in this figure indicates the results for the transverse FCG test. There is little
difference in the FCG resistance between the mixed mode and pure Mode I loading conditions.
It is a reason that the fatigue crack growth are predominantly governed by the mixture of both
matrix metal and interfacial failures mechanism as shown from the fractographic examinations.
 99
Titanium Alloy Matrix Composite. Plots of db/dN for SiCcvD/Ti-15-3 against J m a x are also
shown in Fig. 10 along with data for the L- and T-orientations for a comparison. The figure
indicates that the db/dN are also uniquely related to J m a x in a case of Ti alloy matrix composite.
However, the FCG characteristics does not closely follow the normal power law and the db/dN-
Jmax relationship for the mixed mode loading condition deviates from the initial linear expression
as the J m a x level increases. This is caused by the transition of the fatigue failure mechanism
from the matrix metal failure with the fiber breakage to the matrix/fiber interface failure. Fatigue
fracture toughness Jfc determined at a unstable fracture is relatively identical to the T-orientations.
It can also be seen from Fig. 10 that the mixed mode FCG resistance is superior to that for T-
orientation. This is due to the fact that the mixed mode FCG occurred with the reinforcement
fiber breakage.

Longitudinal fatigue crack initially propagated from the machine notch with breaking the rein-
forcement fiber, and finally terminated the crack propagation due to the reinforcement fiber
bridging. Figure 10 also shows that the longitudinal FCG resistance is the most excellent. This
is successfully rationalized by taking into consideration the fiber bridging of the cracked sur-
faces.

Crack growth

IO"1
1
! SiCcvD/Ti-15-3
HT
O SiCcvD /A1-4T1 • O L-orientation
D SiCcvD /6061A1 r □ T-orientation
io-6 SiCcvD /6061A1 <§ Δ Mixed mode D
(Mode I) ΡΔ
& io'7 r Jjp
£ io-7
10»
I 10-
z
I io-9

10"

10' 10 100 1000 10000

10 100 1000
Jmax N/m Jmax N/m

Fig. 9. Relationship between db/dN and J m a x Fig. 10. Mixed mode fatigue crack growth
for AI alloys matrix composites. rates data as a function of J max for Ti
alloy matrix composite.
CONCLUSIONS

Current R&D trends of advanced structural composite materials in Japan were generally reviewed
and introduced a few of my current research concerning the fracture mechanical characterization
for advanced metal matrix composites, especially FCG characteristics. It is necessary for the
further research to establish the new concepts of material design for high performance MMCs.

ACKNOWLEDGMENTS
This research was supported by scientific research fund in the Project of the Basic Technology
for Future Industries under the sponsorship of the Ministry of International Trade and Industry.
100
I also wish to thank my colleagues who contributed their efforts to the accomplishment of this
experimental work.

REFERENCES
Hirano, K., F. Tamae and K. Nonaka (1988). Fracture mechanics of transverse fatigue crack
growth characteristics of advanced continuous fiber reinforced metal. Trans JSME., 54-501,
910-916 (in Japanese).
Hirano, K. (1988). Near-threshold transverse fatigue crack growth characteristics of unidirec-
tional continuous fiber reinforced metals. Proc. of 4th Japan-U.S. Conference on Composite
Materials, 633-642.
Hirano, K. and H. Takizawa (1989). Evaluation of fatigue crack growth characteristics of
whisker reinforced metals. Trans. JSME., SerA, 55-511, 373-379(in Japanese).
Hirano, K. and H. Nakazawa (1989). Fracture toughness of whisker reinforced aluminum al-
loys. Trans. JSME., SerA, 55-520, 2427-2433(in Japanese).
Hirano, K. and T. Sasaki (1990). Fracture toughness of advanced whisker reinforced metal
matrix composites. Proc. of Comp'90 to be published.
Hirano, K. (1990). Fatigue crack growth characteristics of whisker reinforced aluminum alloys.
Proc. of the 5th Conf. of Fatigue and Fatigue Threshold, 863-868.
Hirano, K. (1990). Mixed mode(I,II) fatigue crack growth characteristics of continuous SiCcvD
fiber reinforced aluminium and titanium alloys matrix composites. Proc. of 5th Japan-U.S.
Conf on Composite Materials, to be published.
Hirano, K. (1990). Strain measurements by image processing techniques and its application to
an ultra-high temperature tensile testings of carbon/carbon composites, ibid, to be published.
Hirano, K. and T. Suzuki (1990). Fracture mechanics of functionally gradient materials at an
ultra-high temperature. Proc. of the 1st Int. Symp. on FGMs, 313-319.
Hirano, K. (1991). Determination of fracture toughness for whisker-reinforced aluminium alloy
matrix composite using chevron-notched specimen. JSME Int. J., 34-310.
Logsdon, W. A. and P. K. Liaw (1986). Engng. Fract. Mech., 24-5, 737-751.
Paris, P. C. and F. Erdogan (1963). Trans. ASME, SerD., 85, 528.
R&D Project on Basic Technology for Future Industries organized by Agency of Industrial Sci-
ence and Technology. Composite materials (1981-88), High performance materials (1989-97).
SJAC Report on Trend Analysis for Next-Generation Space Plane (1989). Trend Analysis for
Development of Space Planes (Japan Association of Aeronautic and Space Industry).
Special Coordination Funds for Promotion Science and Technology organized by Science and
Technology Agency. Research on the basic technology for the development of functionally gra-
dient materials for relaxation of thermal stress (1987-91).
WS10a2

FATIGUE OF AN ALUMINIUM BASED METAL MATRIX COMPOSITE AT AMBIENT

AND ELEVATED TEMPERATURE

J.C. HEALY and CJ. BEEVERS

IRC in Materials for High Performance Applications

and School of Metallurgy and Materials,
University of Birmingham, Birmingham, B15 2TT, U.K.

ABSTRACT
The fatigue response of A356, a casting Aluminium-Silicon alloy, reinforced
with 20% volume fraction of silicon carbide paniculate was investigated at 23°C and 220°C at
stress ratios of 0.1 and 0.5. A closure effect, which was more marked at 23°C than at 220°C,
was observed in this material. Long crack growth at R = 0.1 and 220°C was faster than that
observed at 23°C for equivalent values of delta K. Elevated temperature long crack growth
was found to be matrix dominated compared to that at ambient temperature where SiC
paniculate played an important role in crack growth.

KEYWORDS

Fatigue; temperature; composite; crack growth; paniculate; closure.

INTRODUCTION

In recent years metal matrix composites have become increasingly attractive and
important engineering materials due to their high stiffness, superior strength and high cycle
fatigue properties, (McDaniels, 1985; Nair et al., 1985). Although providing less efficient
reinforcement than fibres or whiskers, discontinuous reinforced alloys have the advantage of
being isotropic and workable by conventional techniques. Despite the potential use of metal
matrix composites in the aerospace and automotive industries there is not, as yet, a
comprehensive data base relating to the fatigue and mechanical properties of these new
materials. This is particularly true at the elevated temperatures (200°C-300°C) at which these
materials might be expected to operate under service conditions if they eventually replace
conventional alloys. The purpose of this investigation is to address this problem by studying
long crack growth at both ambient temperature and at 220°C.

101
102

EXPERIMENTAL PROCEDURE

Material
The material used in this investigation was an aluminium silicon alloy, A356, reinforced with
20% volume fraction of SiC paniculate. It was tested in the as-received condition (cast and
extruded to 62 mm bar). The matrix composition is given in Table 1, and the microstructure
shown in Fig. 1. The silicon is more regularly shaped, grey in colour and considerably
smaller than the larger, darker and more irregular shaped paniculate.

Table 1 Composition of the matrix alloy as described in Product

Specification Duralcan F3A.203

Si Fe CÜ Mn Mg Ζϊϊ Ή Other M

6.5-7.5 0.15 max 0.2 max 0.1 max 0.3-0.45 0.1 max 0.2 max 0.05-0.15 Rem

The distribution and morphology of SiC paniculate were examined in both the transverse and
longitudinal direction in selected areas using an image analyser. The matrix was found to
contain 20% ± 2% of SiC paniculate with an aspect ratio in the range 2:1 to 5:1 and an
average size of 16μπι. The resultant mechanical properties measured at room temperature in
air in the longitudinal direction indicated UTS and 0.2% proof stress values of 382 MPa and
342 MPa respectively with a total % elongation at fracture of - 3 % and a Young's modulus of
~104GPa.

Fig. 1 Microstructure of A356+20% SiC paniculate.

Specimen Preparation

Specimens were initially polished on diamond discs with 125 μπι diamond down to 20 μπι
diamond, using water as a lubricant. This was followed by polishing on 6 μπι Kernet
lead/tin plate using diamond slurry. Final polishing was achieved using a fine (1 μιη) nylon
cloth with colloidal silica.

Long Crack Growth

Long through thickness fatigue cracks were grown in 8 mm thick compact tension (CT)
specimens in the L-R orientation at 23°C. A potential difference technique was used to
monitor crack growth and automated load shedding was carried out to determine crack
growth rates approaching threshold.

Long through thickness cracks, in single edged notched specimens lOx 1 0 x 3 8 mm, were
manually load shedded under three point bend at 23°C to near threshold growth rates prior to
 103
the cracks being grown out at constant load at 220°C. Elevated temperature crack growth
was monitored using a direct optical system (Healy etal., 1991).

All long crack testing was carried out in air, using Amsler Vibrophore fatigue machines at an
averageQfrequency of 100 Hertz. Tests were conducted at stress ratios (R) of 0.1 and 0.5 at
both 23°C and 220°C. Fracture surfaces were examined in a scanning electron microscope.

RESULTS

Long Crack Growth

Long crack growth data obtained at R = 0.1 and R = 0.5, at 23°C, are shown in Fig. 2. A
threshold stress intensity (AK th ) of 6.41 MPaVm was determined for R = 0.1 and 3.67
MPaVm for R = 0.5 at 23°C. From the R = 0.1 data, the estimated fracture toughness was
calculated to be approximately 17 MPaVm. There was an increase in growth rates with an
increase in temperature when plotted in terms of the alternating stress intensity. At R=0.1,
increasing the temperature from 23°C to 220°C resulted in a reduced resistance to crack
growth, with faster growth rates for all values of delta K at 220°C. At R=0.5 this was also
observed to a less marked extent in the near threshold region, but in the Paris regime crack
growth rates were actually slower at 220°C than at 23°C for the same nominal values of delta

I . i I , , , , i , , , , i ■ ■ . . I
5 10 15
Delta K (MPaVm)

Fig. 2 Fatigue crack growth at 23°C and 220°C.

Fractographv

The fatigue fracture surfaces at 23°C and 220°C are summarized in Fig. 3 for specimens
tested at R = 0.1 and R = 0.5 respectively. Crack propagation at 220°C was clearly matrix
dominated while at 23°C the SiC paniculate played a significant role in the growth process.
The extent of SiC particulate fracture has decreased with increasing temperature.
104

Fig. 3 Fatigue fracture surfaces at growth rates of approximately

1E-5 mm/cycle.(a) R=0.1,23°C (b) R=0.5, 23°C
(c) R=0.1, 220°C and (d) R=0.5, 220°C.

DISCUSSION

The microstructure in Fig. 1 shows the fairly even distribution of SiC particulate with some
alignment in the extrusion direction. The presence of surface and subsurface porosity was
associated with the clustering of the SiC particulate indicating incomplete consolidation of the
material during processing. Although this did not have an adverse effect on the high
threshold values obtained, such porosity could effect the initiation resistance of the material to
short fatigue crack formation.

Figure 2 compares the fatigue crack growth data obtained at ambient and elevated
temperatures. Looking first at the room temperature data. Crack growth rates were observed
to increase significantly with increasing stress ratio, to the extent that the data sets overlap
only when the R=0.5 data are approaches the fast fracture region. This effect, though not as
marked, has been previously reported by Logsdon and Liaw (1986) in 6061 reinforced with
25% SiC particulate at load ratios of 0.1 and 0.7. The relatively low fracture toughness and
high threshold of the present material made it difficult to conduct tests at R=0.7.
Consequently direct comparison between the present results and the results obtained by
Logsdon and Liaw (1986) cannot be made. The importance of the particulate in the crack
growth process is clearly reflected in the fracture morphology, Figs. 3(a) and (b). The
incidence of fractured carbides on the fracture surface increased with increasing values of
delta K. It should be noted, however, that carbide fracture ahead of the crack tip was not a
necessary condition for failure. Crack tip deflection at the particle/matrix interface was found
to extensive with the crack propagating around the particulate. Shang et al. (1988) and Biner
(1990) have demonstrated that such crack tip/particulate interaction can result in crack closure
and hence, to retardations in crack growth rates. These observations are clearly in keeping
with the present work. Figure 4 shows a typical crack tip profile, recorded at zero load for
material tested at 23°C and R=0.1, following carbide fracture. The degree of closure is
 105

significant. On this basis, if it is assumed that cracks propagated at high R (R=0.5) are
relatively closure free, the differences in growth rates can be rationalized in terms of a crack
closure based mechanism.

Fig. 4 Crack closure promoted by Fig. 5 Crack path at R=0.5, 220°C.

particulate cracking.

Extending these observations to the data obtained at 220°C it is apparent that, although the
stress ratio effect is reduced, the differences in crack growth behaviour at high and low R are
significant. Surprisingly little work carried out on the elevated temperature properties of
metal matrix composites. Mc Daniels (1985) studied the effect of temperature on the tensile
properties on unreinforced 6061 and 6061 with 20% vol. SiC particulate. It was found that
the discontinuous SiC/Al composites showed an advantage over conventional alloys at
elevated temperatures with a fall in ultimate tensile strength as test temperature was increased.
It was concluded that SiC/Al composites could probably be used effectively for long term
exposures to at least 204°C, and short term to 260°C. More recently Hasegawa (1990)
investigated the S-N behaviour of an unreinforced cast aluminium alloy (AC8A) and one SiC
reinforced, (SÎC/AC8A) from room temperature to 350°C. Similar to results obtained by Mc
Daniels (1985) the whisker reinforced material had superior strength over the temperature
range examined. This was attributed to an increased resistance to initiation in the reinforced
material. Couch and Bo wen (1990) investigated the fatigue crack propagation in 8090 with
16.6% vol. SiC particulate. It was found that at 250°C there was increased resistance to
fatigue crack growth. The fracture surfaces in Figs. 3(c) and (d) for R=0.1 and R=0.5 at
220°C are similar, with a matrix dominated mode of crack growth apparent. At 220°C the
cracks tended to avoid interaction with SiC particulate. Thus it could be argued that with the
increase in temperature and accompanying drop in strength which will occur, an easier path
for growth is found through the deformation present in the matrix.

Growth rates at R=0.1 were found to increase with an increase in temperature from 23°C to
220°C, for all values of delta K, Fig. 2. Examining the fracture surfaces in Figs. 3(a) and
(c), it would appear that the mechanisms of crack growth are different, with a matrix
dominated mode of growth at 220°C and strong interaction with the SiC particulate at 23°C.
The difference in growth rates could be due to the SiC particulate being a more effective
barrier to crack growth at 23°C than at 220°C, in addition to an increase in delta CTOD for the
same nominal value of delta K at 220°C due the fall in strength. At R=0.5 the crack growth
at 220°C were faster than at 23°C in the near threshold region, although at higher growth rates
the room temperature data were actually faster than that at 220°C. As at R=0.1 there is a
matrix dominated mode of crack growth at R=0.5 and 220°C and strong interaction with the
SiC particulate at 23°C. Crack growth at R=0.5 and 220°C showed marked deviation from
the normal to the stress axis, Fig.5, in comparison to crack growth at 23°C. This would
result in a longer actual crack length and reduced delta Keff. Both of these effects would
appear to have combined to reduce crack growth rates below those observed under similar
conditions at ambient temperature.
106

CONCLUSIONS

1. A strong closure effect was observed for long crack growth at 23°C.
2. The mechanism of crack growth at 23°C involved strong interaction with the SiC
paniculate which promoted crack closure and crack tip deviation.
3. A closure effect was also observed for long crack growth at 220°C which was less
marked than at 23°C.
4. The mechanism of crack growth at 220°C was matrix dominated with little evidence of
crack tip interaction with the SiC paniculate.
5. Increasing the temperature from 23°C to 220°C caused an increase in growth rates for
all values of delta K at R=0.1, and in the near threshold growth rates only at R=0.5.

ACKNOWLEGMENTS

This work is pan of a program supported by the EEC, under auspices of the Brite/Euram
program.

REFERENCES

S.B.Biner (1990). Growth of fatigue cracks emanating from notches in SiC paniculate
aluminium composite. Fatigue Fract. Engng. Mater. Struc, 13, 637-648.
P.D. Couch and P. Bowen (1990). Effect of temperature on fatigue crack propagation in
SiC paniculate reinforced al-base composites. To be published in.Fatigue 90 (H.
Kitagawa and T. Tanaka, ed). Proc. of the Fourth International Conference on
Fatigue and Fatigue Thresholds held 15-20th July, 1990.
N. Hasegawa (1990). Fatigue properties of SiC whisker reinforced aluminium cast alloy at
elevated temperature. In : Fatigue 90 (H. Kitagawa and T. Tanaka, ed), Vol.2, pp.
851-856. Proc. of the Fourth International Conference on Fatigue and Fatigue
Thresholds held 15-20th July, 1990.
J.C. Healy, L. Grabowski and C.J. Beevers. To be published in the International journal of
Fatigue in 1991.
S. Kumai, J.E. King and J.F. Knott (1990). Short and long fatigue crack growth in a SiC
reinforced aluminium alloy. Eng. Fract. Mech., 13, 511-524.
W.A. Logsdon and P.K. Liaw (1986). Tensile, fracture toughness and fatigue crack growth
rate properties of silicon carbide whisker and particulate reinforced aluminium metal
matrix composites. Eng. Fract. Mech., 24,131-151.
D.L. McDaniels (1985). Analysis of stress-strain, fracture, and ductility behaviour of
aluminium matrix composites containing discontinuous silicon carbide reinforcement.
Met. Trans. 16A, 1985, 1105-1115.
S.V. Nair, J.K. Tien, R.C. Bates (1985). SiC reinforced aluminium metal matrix
composites. Int. Met. Rev., 30, 1985, 275-290.
Product Specification Duralcan F3A.203, 8/1/89. Durai Aluminium Composites Corporation
10505 Roselle Street, San Diego, CA 92121, USA.
J.K. Shang, W. Yu and R.O. Ritchie (1988). Role of silicon carbide particles in fatigue
crack growth in SiC-particulate reinforced aluminium alloy composites. Mat. Sei. and
Eng. 102, 181-192.
WS10a3

Fatigue Crack Growth in Continuous Fibre Reinforced Titanium

Alloy Metal Matrix Composites.

P. Bowen, A. R. Ibbotson, C. J. Beevers.

School of Metallurgy and Materials / I.R.C. in Materials for High

Performance Applications, University of Birmingham, P.O. Box
363, Birmingham, B15 2TT, United Kingdom.

ABSTRACT

Crack growth rate per cycle, da/dN, does not have an unique relationship with the applied
alternating stress intensity range, ΔΚ, in continuous fibre reinforced titanium based metal
matrix composites. This is a direct consequence of crack bridging by intact fibres which results
in crack size dependent crack growth resistance. In the testpiece geometry considered, a single
dominant crack develops and grows through matrix regions first, leaving fibres bridging in the
crack wake. This results in decreased crack growth rates as the crack grows. The onset of first
fibre failure appears to be controlled by the applied stress intensity range, but care is needed to
define stable / unstable crack transition. The number of intact fibres bridging the crack is of
paramount importance in determining the onset of catastrophic failure.

KEYWORDS

Metal Matrix Composites; Continuous Fibre Reinforced; Crack growth resistance; TÎ-6A1-4V;
Silicon Carbide; Fibre Bridging.

INTRODUCTION

Interest has been expressed in the use of continuous fibre reinforced composites for aerospace
applications. These systems are highly anisotropic but there are still many opportunities for
their use in engineering components, utilising optimised uniaxial properties, and demonstrator
programmes with titanium alloy composites are under study. Composites based on titanium
alloy matrix materials such as Ti-15V-3Cr-3Al-3Sn (Ti-15-3) and TÎ-6A1-4V, and on titanium
aluminide matrix material, all reinforced with Textron SCS-6 silicon carbide fibres are now
available. This availability has stimulated much research effort, particularly in the USA
(Johnson, 1989; Johnson et al., 1990; Harmon and Saff, 1989; Cox and Marshall, 1990).

The assessment of crack growth under cyclic loading in such materials is at an early stage. A
feature of such materials is that the crack growth per cycle, da/dN, can decrease with increases
in nominal applied stress intensity range, ΔΚ, as a direct consequence of fibre bridging of crack
surfaces (Cotterill and Bowen, 1990; Ghosn et al.,1990; Bowen et al., 1991). It is inevitable
that size dependent crack growth rates will be exhibited in such systems, and accurate
modelling of effective stress intensities at growing crack-tips will be essential if fracture
mechanics parameters are to be used with confidence.

107
108

This present paper describes initial observations of fatigue crack growth in a TÏ-6A1-4V alloy
matrix reinforced with Textron SCS-6 silicon carbide fibres. Crack growth has been measured
by the use of modified direct current potential drop techniques, and individual fibre fracture has
been identified.

EXPERIMENTAL

All tests were carried out on single edge notched bend testpieces of nominal dimensions
(4x2x70 mm3). Cracks were grown by fatigue from a slot cut to a depth of 1 mm, so that the
crack depth to width ratio, a/W, was equal to 0.25. Cracks were grown perpendicular to the
direction of fibre reinforcement and parallel to the stacking direction of the fibres within a mat.
Tests were performed in three point bending with an overall span to width ratio, s/W, equal to
15.

An ESH servo-hydraulic testing machine fitted with a 1 kN load-cell was used at a frequency of
0.5 Hz. A constant load range (ΔΡ) was maintained during each section of every test. This
allowed the nominal stress intensity range, ΔΚ, to increase with crack length. Changes in crack
length were monitored using a direct current potential drop technique. Care must be taken to
ensure that calibration curves appropriate to the testpiece size under consideration are used
(Bowen et al., 1991). Additionally, single overloads were applied to testpieces in some tests.
Effects of stress ratio, R, on crack growth rates, da/dN, were considered. (R = CJmin/ CJmax).
Stress ratios of 0.1 and 0.5 were utilised.

Tests were performed on a Ti-6A1-4V alloy matrix reinforced with silicon carbide fibres in the
as-received condition (i.e. solution treated condition). The fibre diameter was of the order of
140 μπι and the fibre volume fraction was nominally 0.35. Polished metallographic sections
were studied optically, and fracture surfaces were examined on an ISI 100A scanning electron
microscope operating at 20 kV.

RESULTS

The dependence of crack growth rate, da/dN, on the nominal applied stress intensity range,
ΔΚ, is shown in Fig. 1(a), for a stress ratio, R, equal to 0.1. The curves are unusual since
da/dN decreases as the nominal ΔΚ increases, and care is needed when presenting and
interpreting data using a da/dN verses ΔΚ relationship alone. Therefore, data is also presented
for da/dN verses total crack length (including the cut notch), see Fig. 1(b). In this test
overloads of up to a nominal K^^ of 80 MPaVm were applied at point A, and did not promote
catastrophic failure. Subsequent crack growth rates were increased sharply, Fig. 1 (a) and (b),
but growth remained stable. No increases in crack length were observed on application of a
single event overload. (These results are discussed in more detail elsewhere (Bowen et al
1991)). Most importantly, overloads were applied only after the fatigue crack had grown to a
length of 1 mm (i.e. a total crack depth of 2 mm, including the cut notch).

Increasing the applied cyclic load range from 100 N to 125 N is seen not to effect the crack
growth rate markedly, see Fig. 2 (a) and (b), but it has a dramatic effect on the onset of final
failure. Catastrophic failure now occurs at a nominal applied stress intensity, ΔΚ, equal to 39
MPaVm, Fig. 2 (a).

For a cyclic load range, ΔΡ, of 100 N little effect of higher stress ratio, R, on crack growth
rates are seen, compare Figs. 3 (a) and (b) with Figs. 1 (a) and (b), but once again the onset of
final failure is promoted at smaller crack lengths - catastrophic failure now occurs at a total
crack length of 1.84 mm and at a nominal applied stress intensity, Kmax< equal to 64 MPaVm,
see Figs. 3 (a) and 3 (b). It is also apparent from Figs. 3 (a) and 3 (b) that the observed
behaviour is reproducible closely between testpieces.

It is important to note that in these systems using three point bending, a single dominant crack
results. Damage is localised only to regions close to the dominant crack as shown in the optical
 109

sections through the fracture surface, Fig. 4. There is an indication that an increased degree of
fibre pull-out is observed under fatigue loading, and this is confirmed fractographically, see
Fig. 5. It has also been possible in these studies to estimate the onset of first fibre failure,
Table 1, and also to estimate the number of fibres bridging during selected stable or unstable
events, Table 2.

DISCUSSION

The study has produced many interesting observations. From Table 1, it maybe deduced that
the incidence of first fibre failure appears to be characterised more accurately by the applied
nominal value of ΔΚ, rather than by the value of Kmax as perhaps would be expected (Cotterill
and Bowen, 1990). This is discussed elsewhere (Bowen et al 1991; Ibbotson et al 1991), but
remains an interesting observation here. This idea is also consistent with the limited effect of
stress ratio on crack growth rates, da/dN, compare Figs. 1 and 3, but care must be given to the
assessment of the onset of catastrophic failure. Note that for a similar cyclic load range of ΔΡ =
100 N, a high stress ratio (R = 0.5) promotes catastrophic failure at a crack length of 1.84 mm
(with seven bridging fibres) whereas stable crack growth occurs to a total crack length of 2.0
mm (prior to an overload of up to Kmax ~ 80 MPaVm) for a low stress ratio (R = 0.1).

Table 1 : Incidence of first fibre failure.

Test Condition Nominal applied ΔΚ Κ max

(MPaVm) (MPaVm)

R = 0.1,AP= 100 N 27 30

R = 0.1,AP = 125 N 31 35

R = 0.5, ΔΡ = 100 N 27 54

Table 2 : Stable / unstable crack growth events.

Test Condition Number of ΔΚ K^max Comment

fibres bridging (MPaVm) (MPaVm)
PaVm)
crack
R = 0.1,AP= 125N 8 35 39 Unstable
failure.
R = 0.1,AP = 100N 28 66 Stable (overload
to 180 N.
R = 0.1,AP = 100N 23 80 Stable (overload
to 220 N).
R = 0.1,AP = 100N 18 51 Stable (test
interrupted).
R = 0.5, ΔΡ = 100N 7 32 64 Unstable
failure.
The critical role of crack bridging by fibres can be seen in Table 2. The present results are
consistent with the occurrence of fatigue crack growth through the alloy matrix first, and that an
increased fatigue crack length leads to an increased number of bridging fibres. Crack growth
rates decrease because the effective local crack-tip stress intensity range at the growing crack-tip
falls. Also of interest is the observation of increased fibre pull-out lengths in regions failing by
fatigue compared to those observed in fast fracture regions, Fig. 5. This maybe attributed to
differences of behaviour due to the failure of fibres behind the crack-tip (i.e. bridging fibres in
the wake) compared with those that fail ahead of a dynamic, unstable crack.
110

A consequence of the study is a geometry dependent crack growth resistance. This is an

uncomfortable design parameter, but nevertheless the information given in Tables 1 and 2 may
still be of use in defining relatively crude operating limits, especially if it is accepted that the
study of the growth of a single dominant crack can provide a lower bound crack growth
resistance for multiple crack damage. In the present study, for the particular combination of
cut-notch and partly bridged crack considered, if applied ΔΚ levels are held below 27 MPaVm
then it may be suggested that fibre failure will not occur. Much further work is required to
substantiate such claims, but it is possible to see the use of failure maps which define critical
combinations of bridging fibres and applied nominal ΔΚ levels.

CONCLUSIONS
Crack growth resistance is dependent upon crack size in continuous fibre reinforced titanium
alloy composites.

Crack growth occurs through the matrix regions first, and the growth rate is dependent
critically upon the number of intact crack-bridging fibres. Therefore, as the fatigue crack length
increases, the effective stress intensity range at the crack tip can be reduced by fibre bridging,
and crack growth rates decrease despite an increase in the nominal applied stress intensity
range.

The onset of first fibre failure appears to be controlled by the applied stress intensity range, but
care is needed to define stable / unstable crack transitions since marked effects of stress ratios
and stress range can also be observed.

ACKNOWLEDGEMENTS

Support for one of the authors (ARI) from a SERC CASE award with Rolls Royce is gratefully
acknowledged. The support of M. V. Hartley, Rolls Royce, Derby, has been particularly
beneficial to the programme, and has included many useful discussions.

REFERENCES

Bowen P., Cotterill P. J., Ibbotson A. R. (1991)., "Fatigue Crack Growth in Continuous
Fibre Reinforced Metal Matrix Composites," in Inst. of Phys. Short Meetings Series, to be
published in February, London, UK.
Bowen P, Ibbotson A. R. and Beevers C. J.(1991)., "Characterisation of Crack Growth in
Continuous Fibre Reinforced Titanium based Composites under Cyclic Loading," in
Mechanical Fatigue of Advanced Materials, Engineering Foundation Conference, Santa
Barbara, California.
Cotterill P. J. and Bowen P.(1990), "Fatigue Crack Propagation in a SiC Fibre Reinforced Ti-
based Metal Matrix Composite," Fatigue 90, pp 2551 - 2556, Vol IV, Honolulu, Hawaii.
Cox B. N. and Marshall D. B.(1990), "Analogies between Bridged Cracks in Fatigue and
Monotonie Loading," Fatigue 90, pp 659 - 664, Vol II, Honolulu, Hawaii.
Ghosn L. J., Telesman J. and Kantzos P.( 1990),"Fatigue Crack Growth in Unidirectional
Metal Matrix Composites," Fatigue 90, pp 843 - 898, Vol II, Honolulu, Hawaii.
Harmon D. M. and Saff C. R.(1989), ASTM STP 102. Ed W. S. Johnson, pp 237 -
250,Philadelphia.
Ibbotson A. R., Beevers C. J. and Bowen P.(1991), "Crack Growth Resistance Under Cyclic
Loading in Continuous Fibre Reinforced Titanium Based Composites", submitted to
Scripta. Metall.. January, 1991.
Johnson W. S.(1989), ASTM STP 102. Ed W. S. Johnson, pp 194 - 221, Philadelphia.
Johnson W. S., Naik R. A. and Pollock W. D.(1990), "Fatigue Damage Growth Mechanisms
in Continuous Fiber Reinforced Titanium Matrix Composites," Fatigue 90, pp 841 - 850,
Vol II, Honolulu, Hawaii.
 Ill

Crack length (mm)

Fig.3 (a) ΔΚ vs da/dN (b) crack length vs da/dN for R=0.5,AP=100N

-ci
υ
O

8l
Fig.5 SEM micrograph
showing regions of increased
fibre pullout in regions of
fatigue crack growth (a -
fatigue, b - fast fracture)

&

Fig. 4 Optical section through a typical

fracture surface.
112

ιο-5
o s o°
-
<to

I Q "6
•A
A

40 45

1.0 1.2 1.4 1.6 1.8 2.0 2.2

Crack length (mm)

Fig.l (a) ΔΚ vs da/dN (b) crack length vs da/dN for R=0.1,AP=100N

a '

a P
%
^ (mm/cycle)
o

iio-6

Fig.2 (a) ΔΚ vs da/dN (b) crack length vs da/dN for R=0.1,AP=125N

WS10b1

DYNAMIC SHEAR STRENGTH OF SiC WHISKER REINFORCED

ALUMINUM ALLOY COMPOSITES

T. Yokoyama and K. Kishida

Department of Mechanical Engineering

Okayama University of Science, Okayama 700, Japan
"t"""" Department of Precision Engineering
Osaka University, Suita, Osaka 565, Japan

ABSTRACT

Dynamic shear strength of SiC whisker reinforced 6061-T6 aluminum alloy (

or SiCw/6061-T6 Al alloy ) composites are determined by means of a modified
torsional split Hopkinson bar apparatus. A specially-designed thin-walled
tubular specimen is used to eliminate the practical difficulties involved
in attaching the specimen to the Hopkinson bars with an epoxy cement. The
generation of a torsional loading pulse having a short rise-time is
achieved through the sudden release of a torque stored in the portion of
the incident bar. Reliable shear stress-strain data are presented at strain
rates of over 1500/s for the SiCw/6061-T6 Al alloy composite and the matrix
alloy. The experimental results show that the matrix Al alloy 6061-T6
itself is strain-rate independent over a range of strain rates in shear
from 10~ 3 to about 1700/s, whereas the SiCw/606l-T6 Al alloy composite
exhibits apparent strain-rate dependence.

KEYWORDS

Dynamic shear strength; SiC whisker; aluminum matrix composite; strain-rate

effect; Hopkinson bar; torsional impact testing

INTRODUCTION

Owing to the rapidly expanding applications of composite materials in the

aerospace and automobile industries, the mechanical behavior of composites
at impact loading rates has received much attention in recent years. Among
metal matrix composites, a SiC whisker reinforced aluminum alloy composite
is one of the discontinuous fiber reinforced metals which are undergoing
intensive development. The mechanical properties of SiC whisker reinforced
aluminum alloy ( hereafter designated as SiCw/Al alloy ) composites have
been investigated by several workers; see, for example, Divecha et al.
(1981), Rack et a^. (1982), Kloucek and Singer (1986), and Morimoto and
Ohuchi (1988). Nevertheless, the strengthening effects in view of the
dynamic mechanical properties of SiCw/Al alloy composites are not yet well
understood.
113
114
The objectives of the present study are to characterize the dynamic
stress-strain behavior in shear of SiCw/6061-T6 Al alloy composites and to
analyze the strengthening mechanisms due to the SiC whisker reinforcement.
A modified torsional split Hopkinson bar apparatus was developed for
determining the dynamic shear stress-strain characteristics of the
SiCw/6061-T6 Al alloy composite fabricated by a powder metallurgical method
using hot isostatic pressing. A specially-designed thin-walled tubular
specimen of short gage length was used to overcome the practical
difficulties involved in fixing the specimen to the loading bars with an
epoxy adhesive. A torsional loading pulse with a short rise-time was
generated by suddenly releasing a torque stored in the portion of the
incident bar through the rapid fracture of a notched bolt. Reliable shear
stress-strain data were obtained at strain rates above 1500/s for 20 vol.%
SiCw/6061-T6 Al alloy composites and compared with those obtained at
quasi-static strain rates. Subsequently, the static and dynamic shear
stress-strain relations for the unreinforced matrix material or the 6061-T6
Al alloy were determined to investigate the influence of the SiC whisker
reinforcement. In an effort to elucidate the strengthening mechanisms due
to the SiC whisker reinforcement from a microscopic point of view, the
fracture surfaces of the SiCw/6061-T6 Al alloy composite specimens were
examined with the help of a scanning electron microscope.

EXPERIMENTAL PROCEDURE

Experimental Apparatus

Figure 1 shows a schematic drawing of the modified torsional split

Hopkinson bar apparatus employed in the present experiments. The apparatus
consists essentially of two Hopkinson bars ( usually termed incident and
transmitter bars ) , a frictional clamping device, a torque pulley and
recording equipment. The specimen is placed between the incident and
transmitter bars of seamless steel tubes ( ASTM MT1020 ) with 20 mm outside
diameter and 8.8 mm inside diameter. The bars are supported by a series of

INCIOENT BAR TRANSMITTER BAR

300 ?°, . 300

ST0RE0-

£a
SPECIMEN
T0RQUE

B
^
GAGES INCIOENT GAGES TRANSMITTER GAGES

3SÉ ] ~ NOTCHED BOLT

CHANNEL STEEL 1

( DIMENSIONS IN MM )
INCIDENT BAR
ST0AC0-
TORQUE
GACtS mciocwT GAGES TAAHSHITUR GAGES
^SjU-PIYOT PL
D
■ BASE PLATE

STRAIN
CAGE
j m o GL
Fig. 2. Clamping device.

LIf 1ER | I MONÏTO

R | Γ^ 1

1 I f 11 »""» 1
I CHART
I RECORDER |
JL-—I
DIGITAL
STORAGE
i c p . i ii 1 . Fig. 1. Torsional split
JMCROCOHPUTER)
·
IOSCULOSCOK
I
Hopkinson bar system.
 115
V-blocks that allow the bars to rotate freely in either direction. A torque
is stored in the portion of the incident bar between the clamp and the
torque pulley. The clamping device for holding and releasing the stored
torque is depicted in Fig. 2. The clamp design consists of two arms with
hinged bottoms that press against the sides of the incident bar under the
action of the notched bolt ( AISI 1045 steel ). In this design, the clamp
arms are shaped to match the circumference of the incident bar. The stored
torque is released by further tightening of the clamp until the notched
bolt breaks. Upon release of the clamp, a sharp-fronted torsional loading
pulse of constant amplitude ( equal to one half of the stored-torque )
propagates down the incident bar toward the specimen. Simultaneously, an
unloading pulse of equal magnitude propagates back toward the torque
pulley. Figure 3 indicates a Lagrangian x-t diagram which illustrates the
details of the torsional wave propagation in the bars. The duration of the
loading pulse is the time required for the torsional pulse to travel twice
the distance between the clamp and the torque pulley. When the torsional
pulse (φ^) reaches the specimen, part of the pulse is reflected back (φχ)
and part is transmitted through the specimen ( <t>t) into the transmitter bar.

i
TORQUE PULLEY
INCIDENT GAGES _ TRANSMITTER
CLAMP GAGES

4 <V
ψ®ψ®
·.
•a

WÄ
5 1? im
5| 5
12.5

(DIMENSIONS IN M M ) SECTION A-A

Fig. 4. Configuration and

nominal dimensions of torsion
specimen.
Fig. 3. Lagrangian x-t diagram for
torsional split Hopkinson bar.

The incident, reflected and transmitted strain pulses were measured by two
sets of 90-deg rosette strain gages ( Kyowa, Type KSN-2-F3-11 ) mounted
diametrically opposite each other on the incident and transmitter bars. The
location of the strain gages was determined so that the continuous records
of each strain pulse could be obtained without interference from
reflections. The output signals from the gages were fed through a bridge
circuit to a dual-beam digital storage oscilloscope ( Iwatsu, Model
DMS-6430 ) with an 8-bit fast analogue-digital converter, where the signals
were digitized and stored at a sampling rate of 1 \is. The digitized data
were then transmitted to a 16-bit microcomputer ( NEC, PC-9801VM ) for
processing data.

Data Analysis
116
The shear strain γ, strain rate γ and stress τ in the specimen are obtained
from the torsional Hopkinson bar test records as follows:

= (r s c s /r b L)J o t [Φ i (t')-φ r (t')-Φ t (t')]dt^ (1)

= (Γ^/^ΜΦ^Ο-φ^Ο-φ^)], (2)

= (GbrsJb/2rbJs)[Φi(t)+Φr(t)+Φt(t)]. (3)

Here r is the radius, L the gage length, J the polar moment of area, c the
torsional wave velocity, G the shear modulus, and t the time from the start
of the pulse. The subscripts b and s denote the Hopkinson bar and the
specimen, respectively; and r g is the mean radius of the thin-walled
portion of the specimen ( see, Fig. 4 ). In the above derivations, it is
assumed that: (i) the plastic deformation is confined to the thin-walled
portion of the specimen and does not extend into the flanges; and (ii) this
deformation is uniform along the gage length. Equations (1) and (3) provide
the average strain and stress in the specimen as functions of time.
Eliminating time yields the stress-strain curve for the specimen at the
strain rate given through Eq. (2). In practice, the data reduction is
carried out with the aid of the 16-bit microcomputer system.

EXPERIMENTAL RESULTS AND DISCUSSION

Fabrication Method and Specimen Configuration

SiCw/606l-T6 Al alloy composites were fabricated by a powder metallurgical

technique using hot isostatic pressing. The fabrication process is
illustrated in Fig. 5. The microstructure of the SiC whiskers in an
extruded rod of the 20 vol.% SiCw/6061-T6 Al alloy composite is shown in
Fig. 6. The torsion specimen ( Fig. 4 ) is a short thin-walled tube with
integral octagonal flanges that fit into matching sockets in the ends of
the Hopkinson bars. In order to prevent any relative motion between the
sockets and the flanges, precise machining of each flange is needed to hold
the specimen flanges against the driving faces of the octagonal sockets.

SiC WHISKERS ALUMINUM ALLOY POWDERS

J

EXTRUDED RODS
Fig. 6. Microstructure of SiC
Fig. 5. Fabrication process of whiskers in extruded rod of
SiCw/6061-T6 Al alloy composite. SiCw/6061-T6 Al alloy composite.
 117
Torsional Split Hopkinson Bar Tests

A series of torsional impact tests was conducted using the modified

torsional split Hopkinson bar apparatus. Figure 7 presents typical
oscilloscope records from the torsional Hopkinson bar test on the
SiCw/6061-T6 Al alloy composite. The top trace gives the incident and
reflected strain pulses; the bottom trace gives the strain pulse
transmitted through the specimen. Figure 8 shows the resulting dynamic
stress-strain curve along with the corresponding static curve. The
SiCw/6061-T6 Al alloy composite is definitely strain-rate sensitive. Note
that a rapid decrease in the stress level of the static curve corresponds
to fracture initiation in the gage section of the specimen. Subsequently,
both quasi-static and impact torsion tests were performed to evaluate the
mechanical properties of the matrix alloy only. Figure 9 depicts the static
and dynamic shear stress-strain data for the unreinforced 6061-T6 Al alloy.
A comparison of Figs. 8 and 9 indicates that the static yield strength for
the SiC/6061-T6 Al alloy composite is improved by about 40 % by whisker
reinforcement. In contrast to the SiCw/606l-T6 Al alloy composite, the
matrix Al alloy 6061-T6 itself exhibits essentially no strain-rate
sensitivity, at least up to shear strain rates of approximately 1700/s.

In order to study the whisker reinforcement mechanisms, the fracture

surfaces of the SiCw/6061-T6 Al alloy composite specimens were examined by

Seep rate: 100 us/div.

Vertical scale
Top trace: 1003 με/div.
Bottom trace: 49 με/div.

Fig. 7. Typical oscilloscope records

from torsional Hopkinson bar test on
SiCw/606l-T6 Al alloy composite.
(Top trace: incident and reflected
strain pulses; bottom trace: trans-
mitted strain pulse.)

—T—
MATERIAL: SlCv»/6061-T6 * MATERIAL: 606I-T6
DYNAMIC f - 1559 DYNAMIC f - 1737 ( l / i )
STATIC f - 6.7E- 3 (1/.1 STATIC f - 4.8E-3 ( 1 / . )

Λ Ί
-
- K i1
1 i "
t 5
,
10 15 5 10 15
SHEAR STRAIN T (X) SHEAR STRAIN T IX)

Fig. 8. Static and dynamic shear Fig. 9. Static and dynamic shear
stress-strain curves for SiCw/6061 stress-strain curves for 6061-T6
-T6 Al alloy composite. Al alloy.
118

Fig. 10. SEM photographs of fracture surfaces of SiCw/

6061-T6 Al alloy composite specimens: (a) static torsion
pecimen; (b) dynamic torsion specimen.

means of a scanning electron microscope. Figure 10 represents the SEM

photographs of the fracture surfaces of the static and dynamic torsion
specimens. The SEM examination reveals that the fracture surface of the
static torsion specimen consists of small and shallow dimples indicative of
low localized ductility, whereas that of the dynamic torsion specimen
exhibits larger dimples indicative of greater localized ductility. This
observation is qualitatively consistent with the experimental results.

CONCLUSIONS

The shear stress-strain relations for the 20 vol.% SiCw/6061-T6 Al alloy

composite and the matrix alloy at strain rates exceeding 1500/s have been
determined by the use of the modified torsional split Hopkinson bar
apparatus. The test results of this study indicate that the matrix Al alloy
6061-T6 itself is insensitive to strain rate, at least up to about 1700/s,
while the SiCw/6061-T6 Al alloy composite displays a definite strain-rate
sensitivity. This is probably attributed to the dynamic interface
interactions between the SiC whiskers and the matrix alloy. This view is
supported by SEM observations of the fracture surfaces of the torsion
specimens.

REFERENCES

Divecha, A.P., S.G. Fishman and S.D. Karmarkar (1981). Silicon carbide
reinforced aluminum - a formable composite. J. Metals, 33, 12-17.
Kloucek, F. and R.F. Singer (1986). Influence of processing on the
mechanical properties of SiC whisker reinforced aluminum composites.
In: Proceedings of the 31st Int. SAMPE Symposium, 1701-1712.
Morimoto, H. and K. Ohuchi (1988). Influence of whisker volume fraction on
the mechanical properties of SiC whisker reinforced aluminum alloy
composites. Japan Inst. Light Metals, 38, 658-664. (in Japanese).
Rack, H.J., T.R. Baruch and J.L. Cook (1982). Mechanical behavior of
silicon carbide whisker reinforced aluminum alloys. In: Proceedings of
the ICCM-IV (T. Hayashi, K. Kawata and S. Umekawa, Eds.), 1465-1472.
WS10b2

ENDURANCE WEAR OF MULTIPHASE ALLOYS WITH TITANIUM CARBIDES

P.A. COULON
Steam Turbine Division
GEC Alsthom
90018 BELFORT, FRANCE

INTRODUCTION

The final low pressure stages of high-rating steam turbines usually consist of martensitic 12 %
chromium steel blades whose leading edges are protected from erosion caused by droplets of water
by a hard cobalt-based cladding. The use of titanium alloys, mainly Ti6AJ4V, by a number of
steam turbine manufacturers as a substitute for 12 % chromium steel for the outlet stages of
turbines, due to the reduced weight and corrosion-fatigue resistance of these alloys, allows the
height of blades to be considerably increased. With the same centrifugal stresses titanium allows
a 50 % increase in the height of blades. In parallel, the peripheral speeds at the end of the turbine
blade bodies increase in direct proportion. At present, speeds of up to 750 m/s are possible on
the most advanced machines. Since titanium does not have superior resistance to water droplet
erosion compared to that of the steel normally used (in fact slightly but not sufficiently superior),
it is inevitable that the leading edges will need to be protected.
As a matter of fact, GEC Alsthom has developed, for 3,000 rpm machines, the longest titanium
blade ever designed (Fig. 1). This blade, measuring 1.5 m long, will multiply the largest available
exhaust area so far obtained with steel blades by a factor exceeding 1.5.

PHYSICAL AND CHEMICAL CHARACTERISTICS OF THE TESTED TWO-

PHASE ALLOYS

The two-phase alloys in the test program (Ref. 1.2) are composed of a pprox. 1/3 weight of ti-
tanium carbide TiC (i.e. 45 % volume) (Fig. 2). The binding phase consists of between 30 and
45 % iron complemented by variable quantities of chromium, nickel, molybdenum and cobalt.
The chemical analyses of the 5 titanium carbide based grades arc shown in Table 1. The density
of these alloys is 6.6 g/cm-\ the modulus of elasticity is 290,000 N/mrn^, the shear modulus
115,000 N/mmf The thermal expansion coefficient is very close to that of titanium : approx. 9
x 10""PC*' between 20 and 100°C, 10"->°C"' between 20 and 400°C. The hardnesses are a function
of the tempering temperature. Transition from the "annealing" condition to the "quenched" con-
dition is a function of the holding temperature particular to each grade.
The five matrices tested are (see table 1 : analysis of grades AW, BN , FM, CU, DS) :
• One austcnitic matrix (CU) which was soon abandoned : insufficient hardness and an ex-
pansion coefficient incompatible with a titanium-base substratum.
• Two purely martensitic matrices (AW, DS) with satisfactory mechanical and physical char-
acteristics, but with a final hardening heat treatment incompatible with the coating deposit
cycle.

• Two chrome nickel base maraging matrices (BN, FM) whose properties were found to be
satisfactory. This study compares the behaviour of two maraging matrices (after ageing
treatment at 480°C/6h), one nickel-base, the other chrome-base.

119
120

E R O S I O N R E S I S T A N C E IN R E L A T I O N T O H A R D N E S S

Hardness is an essential parameter (but not the only one) of the resistance of the alloy deposit
to impact erosion.
Figure 3 outlines the main results of weight loss in time for alloys AW, BN, CU and DS, ob-
tained on Dornier installations (ref. 3.4).
For the envisaged application (very large titanium blades for last L P stage in steam turbines), at
peripheral operational speeds of 750 to 800 m/s the minimum hardness required is 58 H R C .
Figure 4 shows the hardness obtained in relation to the proportion (in weight) of titanium carbide
for various metal matrices. In addition to our results, Patel's findings have been noted (ref. 5).
If the level is set at 58-60 H R C , the nickel-based matrices are eliminated straight away (this is
not the nickel maraging which will be discussed later) leaving only "steel" matrices, including
"maragings" or "cobalt".
The minimum proportion of TiC for "steel" matrices is 22 % . For "cobalt" matrices, which were
also rejected because of their austenitic structure with a corresponding high expansion coefficient,
this proportion could be as low as 15 % (ref. 6, 7 and 8).
In this study, two "steel" matrices were tested, one a nickel maraging and the other a chrome
maraging, both with :

• A hardening (ageing) treatment compatible with the conditions of deposit and leading to
hardness values of 60 H R C (as was the aim).

• An expansion coefficient in relation to temperature (apparently) compatible with that of the

substractum (here TÎ6A14V).

MARTENSIT1C TRANSFORMATION DURING COOLING

Dilatometry showed that the bi-phase material Chrome and Nickel maraging matrices was subject
to structural transformation in the steel phase, causing radical and large variations in expansion
during cooling towards 200°C (Fig. 5). Even if expansion due to martensitic transformation only
compensates for the difference between the expansion coefficient of the Ti6A14V substratum with
that of the filler material, the fact that the filling was carried out at very low temperatures causes
high stresses (estimated at + 200, 250 MPa) on a deposit that is already very brittle. These
stresses explain the cracks found in the alloy (photo 6).
The "Nickel maraging" matrices is thus not appropriate for this application.

USE O F PRESTRESSING

Some precautionary measures are necessary to prevent the infortunate side-effects of martensitic
transformations during cooling after the depositing operations by projection, spray, welding or
brazing.
These transformations at around 200 or 300°C are radical, causing modifications in volume and
in thermal expansion coefficients.
Micro-crack s can be initiated and, at the very least, high residual tensile stresses can be induced
during these phases of transformation.
In order to avoid this, prc-stressing must be carried out in order to compensate for the stresses
brought about by the depositing. Pre-stressing can be either mechanical (bending of the blade)
or thermic (appropriate water cooling).

I M P A C T E R O S I O N TESTS

The tests were partly carried out on the Dornier installations ( F R G ) . The parameters are strictly
identical to the parameters used when working out the series of tests given on figure 3.

• diameter of the water droplet = 1.2 mm

• concentration of the volume of water = 4.5 x 10""

• surface tested = 78.5 m m 2

• pressure = 760 Torr.

• angle of incidence = 90°C

The erosion resistance of the two materials is satisfactory and conforms to the results expected.
Figure 7 expresses the time required to reach the erosion threshold in relation to hardness : the
incubation time of the nickel maraging matrices is slightly less than that of the chrome maraging
matrices. Figure 8 indicates the rate of weight loss dG/dt against hardness.
 121

DISCUSSION

No turbine constructor would deny that the inlet edges of very large steam turbine blades made
from Titanium alloys must be protected (refs 9, 10, 11, 12). Erosion by water droplets projected
at speeds of 700-800 m/s is a severe phenomenon^ capable of attacking the material seriously in
the short or middle term. Protection consisting of titanium carbide combined with a maraging
bonding material semi-hard, has been demonstrated. An alternative with titanium carbide alone
(too hard, therefore not ductile enough) or with a titanium carbide associated to a bonding ma-
terial without a point of martensitic transformation, i.e with a fcrritic or austenitic structure, is
not acceptable (too soil).

CONCLUSIONS

Hard, titanium carbide TiC based materials can be used for the protection of the large titanium
blades of steam turbines against erosion and abrasion. These materials can be found in different
forms : sintered then brazed or welded pellets, projection and hot rcfusion, laser, electron beam
etc...
The resistance of TiC alloys to erosion compares favourably with the materials traditionally used
on steel blades i.e. cobalt based alloys which are furthermore very difficult to combine with tita-
nium alloys.
Laboratory tests reinforced by the production of prototypes have justified the use of two-phase
titanium carbide based alloys on materials as sophisticated as the last stages of high-rating steam
turbines.
The characteristics of the titanium carbide anti-erosion coating will be as follows :
• Compatibility with the TÏ6A14V substratum
— no elements fragilizing the substratum in the deposit alloy
— thermal expansion coefficients close to those for the substratum through out the tem-
perature range.
• Hardness
— macro-hardness of the binary alloy * 60 I IRC
— micro-hardness of the bonding agent * 50 I IRC
• No acceptable structural transformations during the thermal cycles
• Fine grain size compatible with the type of projection

REFERENCES
(1) COULON, P.A.,"Coating for Last Row Steam Turbine Titanium Blading" ASM International
and EPR1 : Advances in Material Technology for Fossil Power Plant. Proceedings of Interna'
tional Conference 1-3 September 1987, Chicago, Illinois USA, PP 435-446.
(2) COULON, P.A., "The Resistance to Erosion of Multiphase Alloys with Titanium Carbide
Phase" Lubrication Engineering Vol. 44 N° 4 (April 1988) pp 345-352.
(3) SCIIROEDER, Dr, "Handbuch Regen Erosion" Dornier System GmbH, Koblenz BWB, AT
(Dec 1984)
(4) DORNIER System Liquid Impact Investigations, with the Mach 3 Rotating Arm Facility, An-
gewandte Forchung (1980).
(5) PATEL, MS., "Erosion-Resistant Alloy" UK Patent Application CR 2076019A (Jul 1980).
(6) SALTZMAN, G., A., "Carbides Add Muscle to PTA Antiwear Coatings" Metal Progress Feb
1986 pp 25-30.
(7) AUFDERHAAR, B., "TiC Wear Surfacing Powders" Metal Progress Vol 119 N° 7, 1981, pp
30-33.
(8) 1NCO ALLOYS International "Inco Alloy MS 250 a High-strength Maraging Steer - notice
technique 1986
(9) JAFFEE, R., I. "Titanium Steam Turbine Blading" presented at EPRI Titanium Steam Turbine
Blading Workshop Nov.9-10, 1988 Proceeding of the Conference.
(10) MORSON, A., WILLIAMS, J.C "Some Aspects of the Development of the Continuously cou-
pled 40-inch Titanium Last-stage Bucket" EPRI Workshop Nov. 88 see (8).
(11) YASUGA1I1RA, N., NAMURA, K., "Erosion Resistance of Titanium Alloys for Steam Turbine
Blades as measured by Water Droplet Impingement"', EPRI Workshop Nov. 88 see (8).
(12) DRAHY, /., "Water Droplet Erosion of Titanium Alloy Steam Turbine Blading" EPRI
Workshop Nov. 88 See (8).
122
Chemical analysis of the matrix of AW BN FM CIJ I)S
five titanium carbide based graded tested

TiC 33 32 31 34 32,8

C 0.7 0.4 0.02 0.5

Cr 12.5 14 18 12

TABLE 1 Mo 2.7 4.5 5 2 1.50

Cu 1 0.8 1 1 1

V 0.4

Al 1.5 1 0.2

Ni 0.52 4 18 12 0.6

Co 8 8 0.08

Ti 1 1

Nb 0.9

Fe 45 31 36 31 50.9

Structure of Maraging Maraging

the matrices Martensite Ni-Cr Mar- Ni Marten- Austcnitic Martensite
tensite site
HRC min 52 50 50 46 50
max 70 64 64 52 70

TITANIUM BLADING FOR 3 0 0 0 rpm TURBINES

Fig. 1
 123

40/WrriL 20 μ m
F l g . 2 : TWO-PHASE ALLOY MICROGRAPHS
LOSS OF WEIGHT WATER CONCENTRATION 4.5 X 10" 6 DROPLET DIAMETER 1.2 mm
INmg
i ; 18 C SURFACE OF TEST PIECE 78.5 mm 2
15 16A
16B 1 3 17
6
COBALT BASE ALLOY
9 CASTING
1 CASTING
6L FORGED 5? 18 B 10
10 FORGED
Ü«
J 3 ROLLED 5?
/"

TITANIUM CARBIDE
15 CU

1
16 BN
17 AW
/9 //
18 DS J/ / /
H BC = 6T .18 A

TIME OF EXPOSURE IN MIN

Flg. 3 : 5 10 15 20 25 30 35 40 45
IMPACT EROSION OF COBALT ALLOYS, NICKEL ALLOYS & BIPHASE
ALLOYS WITH TITANIUM CARBIDE BASE

Fig. 4 HARDNESS AS A FUNCTION OF TiC PERCENT

• · · COBALT MATRIX
% OF TiC xxx IRON MATRIX |ACC. TO PATEL
A ■ ■ ■ NICKEL MATRIX
100 -j
O O O IRON MATRIX ] ACC. TO COULON <f*

50 56 60 HARDNESS HRC
124

700 - I

TÏ6AL4V
CHROMIUM MARAGING
NICKEL MARAGING

EXPANSION
Fig. 5 :
COMPARISON OF BEHAVIOUR IN EXPANSION BETWEEN Ti 6 AL 4V
& TiC BASE WITH A Cr MARAGING MATRIX & A Ni MARAGING MATRIX

Flg. ï
IMPACT EROSION OF TITANIUM CARBIDE ALLOYS AS A FUNCTION
OF HARDNESS I THRESHOLD TIME

HRC| PARAMETERS : 600 m/s

DROPLET DIAMETER 1.2 MM .
70 WATER CONCENTRATION 4.5 x 10

THRESHOLD (TIME-MIN)

Fig. 8
IMPACT EROSION OF TITANIUM CARBIDE ALLOYS AS A FUNCTION
OF HARDNESS II LOSS OF WEIGHT RATE

Fig. 6 : CRACKS FOUND

IN THE BIPHASE ALLOY
WS10b3

TENSILE AND COMPRESSIVE PROPERTIES OF A

SiCw/60 6lAl COMPOSITE

L. GENG, C.K. YAO and D.Z. WANG

Department of Metals and Technology, Harbin

Institute of Technology, Harbin 150006» China

ABSTRACT

The tensile and compressive properties of a SiCw/606lM

composite made by squeeze casting method were measured at
different temperatures. The experimental results show that the
strength of the SiCw/606lAl composite is much higher than that
of the 606lAl, but the ductility of the composite is obviously
decreased as compared with the 6061^1. The tensile experimental
results show that the ratio of yeild strength to tensile
strength of the SiCw/606lAl composite is low, which indicates
that the deformation strengthening effect of this composite is
higher. With the increase of the temperature, the tensile
strength of the SiCw/606lAl composite is decreased at a lower
speed than that of the 6061^1 does. The compressive experimental
results show that with the increase of the temperature, the
compressive strength of the S i C w / 6 0 6 l M composite is decreased
at a higher speed than that of the 606lAl does. In the state of
compressive stress, the S i C w / 6 Q 6 l M composite exhibits a good
ductility. The critical reduction of the composite at room
l s
temperature is 15W, and that at 500T 50**· Because of the
rotation and break of some SiC whiskers during the compression,
there is a peek in the stre s s — strain curve of the composite.

KEYWORDS

Silicon carbide; whisker; aluminium; composite.

INTRODUCTION

125
126
The S i C w / A l c o m p o s i t e s are d i s c o n t i n u o u s r e i n f o r c e d c o m p o s i t e s ,
w h i c h can be p r o d u c e d by some c o n v e n t i o n a l m e t h o d s . T h e y exhibit
mechanical properties which are more modest than those
a c h i e v a b l e w i t h c o n t i n u o u s r e i n f o r c e m e n t s but still c o n s i d e r a b l e
higher than those of the unreinforced a l l o y ( D i v e c h a et a l . ,
1980)· F ° r e x a m p l e , they have a m o d u l u s m u c h h i g h e r than that of
a l u m i n u m and as h i g h as that of t i t a n i u m (Guo et a l . , 1989)· T h e
specific modulus ( modulus/density) of this composite is
increased by 50K c o m p a r e d w i t h a l u m i n i u m or t i t a n i u m ( M c D a n e l s
et a l . , 1982)· The s t r e n g t h , e s p e c i a l l y at h i g h t e m p e r a t u r e s , of
the S i C w / A l c o m p o s i t e s is g r e a t l y improved as c o m p a r e d w i t h that
of the m a t r i x a l l o y (Ma et a l . , 19 90)· The SiCw/Al composites
can also be shaped by s t a n d a r d m e t a l l u r g i c a l p r o c e s s e s such as
extrusion and rolling ( G e n g et a l . , 1 9 8 9 ) · The excellent
mechanicl p r o p e r t i e s of the S i C w / A l c o m p o s i t e s m a k e them ideal
m a t e r i a l s for a e r o s p a c e and u n d e r w a t e r s t r u c t u r e s (Burgam, 1 9 8 2 )

In this p a p e r , the tensile and c o m p r e s s i v e p r o p e r t i e s of the

SiCw/606lAl c o m p o s i t e at d i f f e r e n t temperatures were studied,
and the d e f o r m a t i o n b e h a v o u r s of the c o m p o s i t e w a s d i s c u s s e d .

MATERIALS AND EXPERIMENTAL PROCEDURE

The reinforcement used is ß - S i C w h i s k e r m a n u f a c t u r e d by Tokai

C a r b o n C o . Ltd., S h i z u o k a , J a p a n . The SiC w h i s k e r has a d i a m e t e r
of 0-l_l-0Pm ana
" a
length of 30~10Ol·11"- The matrix material
used is commercial 6061 aluminium alloy. The SiCw/6061Al
c o m p o s i t e , w i t h a w h i s k e r v o l u m e f r a c t i o n of 20**> w a s fabricated
by squeeze c a s t i n g m e t h o d .

B o t h the S i C w / 6 0 6 l M c o m p o s i t e and the 6061 a l u m i n i u m a l l o y were

T6 t r e a t e d , and then the tensile and c o m p r e s s i v e s p e c i m e n s were
m a c h i n e d from the c o m p o s i t e and the a l u m i n i u m a l l o y . The tensile
tests w e r e c a r r i e d out at room t e m p e r a t u r e , 20 0*C and 4θθΓ> and
the c o m p r e s s i v e tests w e r e done at 300Ϊ! f 400*C and 5 0 0"C - T h e
orientation of the w h i s k e r s in the c o m p o s i t e s b e f o r e and after
c o m p r e s s i o n w a s o b s e r v e d by s c a n n i n g e l e c t r o n m i c r o s c o p e ( S E M ) .

RESULTS AND DISCUSSION

T e n s i le Te s t

F i g . 1 shows the T y p i c a l s t r e s s - s t r a i n curves for SiCw/606lAl

c o m p o s i t e and 6 0 61AI a l l o y . It can be seen from this figure that
the ratio of y i e l d s t r e n g t h to tensile s t r e n g t h of the c o m p o s i t e
is about 0·6> a n Q 4 that of the 6 0 61^1 a l l o y is about 0·7· This
 127
600
SiCW8N1Al:UTSsSI2MP·
S YS=353MP«
500 jX E l . =2.15%

* 400 X
stress

I ^ ^~m\k\ :UTS=345MP·
-/ X YS=244MP«
// El.=7.14%
100 Fi g.j T e n s i l e s t r e s s - s t r a i n curves
' 1 / 1 1
of the T 6 - t r e a t e d S i C w / 6 0 6 1 A l
c o m p o s i t e and 6 0 6 1 ^ 1 .
0 0.5 1.0 1.5
strain % n
result i n d i c a t e s that it is e a s y for the p l a s t i c d e f o r m a t i o n of
the composite. D u r i n g the t e n s i l e p r o c e s s e s of the c o m p o s i t e ,
the s t r e s s d i s t r i b u t i o n in the c o m p o s i t e is not u n i f o r m . There
w i l l be a s t r e s s c o n c e n t r a t i o n in the m a t r i x a r o u n d the w h i s k e r ,
therefore, the local p l a s t i c d e f o r m a t i o n of the m a t r i x around
the w h i s k e r w i l l take p l a c e u n d e r a c o m p a r a t i v e l y lower tensile
load, w h i c h r e s u l t s in a lower y i e l d s t r e n g t h of the c o m p o s i t e .
W h e n the s t r e s s s u r p a s s the y i e l d s t r e s s of the c o m p o s i t e , more
and m o r e m a t r i x w i l l take part in the p l a s t i c d e f o r m a t i o n of the
c o m p o s i t e , and also b e c a u s e the m a t r i x a l l o y w a s s t r e n g t h e n e d by
plastic d e f o r m a t i o n , the load b e a r i n g a b i l i t y of the c o m p o s i t e
is i n c r e a s e d . O n the o t h e r h a n d , the a n g l e s b e t w e e n the axis of
some w h i s k e r s and the t e n s i l e d i r e c t i o n w i l l be d e c r e a s e d by a
few d e g r e e s due to the r o t a t i o n of some w h i s k e r s , and this will
lead to the i n c r e a s e of the t e n s i l e s t r e n g t h of the c o m p o s i t e .

F i g . 2 shows the t e n s i l e s r e n g t h and e l o n g a t i o n of the c o m p o s i t e

and the 6 0 61Al a l l o y at d i f f e r e n t t e m p e r a t u r e s . F i g . 2 ( a ) shows
that the s t r e n g t h of b o t h the c o m p o s i t e and the 6 0 61Al a l l o y is

(0
i 000 -
E ^ 10
£ 500

I8
engt

£ 300 <* 6
^ \
Ü 200 \
\ fc 4
<Λ - Μ \ Φ
2
1 1 1
100 200 300 400 100 200 300 400
temperature °C temperature X
(a) (b)
Fig.2 Tensile strength and e l o n g a t i o n of the T6~treated
S i C w / 6 0 6 1 A l c o m p o s i t e and 6 0 61AI at e l e v a t e d temperatures.
SiCw/606lAl; 606lAl
128

d e c r e a s e d w i t h the i n c r e a s e of the t e m p e r a t u r e . T h e s t r e n g t h of
the 60 61Al alloy decreased at high speed, and when the
t e m p e r a t u r e is 400Ü/ the t r e n g t h is o n l y no m o r e than too M P a ,
but the d e c r e a s i n g speed of the s t r e n g t h of the composite is
lower c o m p a r e d w i t h that of the 6 0 6 1 A l a l l o y , and from F i g . 2 ( a )
it can be seen that the strength of the c o m p o s i t e at 300Ü
e q u a l s to the s t r e n g t h of the 60 61Al a l l o y at room temperature.
The main reasons for this m a y be that the s t r e n g t h of the S i C
w h i s k e r is almost ont d e c r e a s e d b e f o r e 400Î!; and on the other
h a n d the S i C - A l i n t e r f a c e b o n d i n g s t r e n g t h is h i g h , e v e n at 400*C·

F i g . 2 ( b ) shows that the d u c t i l i t y of the c o m p o s i t e is m u c h lower

than that of the 60 6 1 A l , w h i c h is m a i n l y because that the
plastic d e f o r m a t i o n of the c o m p o s i t e is s t r o n g l y prevented by
the whiskers. with the i n c r e a s e of the temperature, the
ductility of the 60 61Al a l l o y is i n c r e a s e d , so it b e c o m e s easy
for the r o t a t i o n of the w h i s k e r s d u r i n g the p l a s t i c deformation
of the c o m p o s i t e , and t h e r e f o r e the t e n s i l e e l o n g a t i o n of the
c o m p o s i t e is i n c r e a s e d w i t h the i n c r e a s e of the t e m p e r a t u r e .

Compressive Test

Fig. 3 is the t y p i c a l compressive stress-strain curves for

SiCw/606lAl composite and 6061 Al a l l o y at 3oOTC and 400IC it
obviously shows that there is a p e e k in the curves of the
c o m p o s i t e , but no p e e k can be found in the c u r v e s of the 6 0 6 1 A l .
W i t h the i n c r e a s e of the c o m p r e s s i v e s t r e s s , the m a t r i x a l l o y in
the composite is strengthened, so the composite is also
strengthened, but on the o t h e r h a n d , the angle between the

Fig.3 Compressive stress-strain

curves of the T6~treated
SiCw/606lAl composite and
60 61Al m a t r i x at elevated
t empe r a t u r e s.
a
: 300ΐ!> c o m p o s i t e ;
b : 40θΓ> c o m p o s i t e }
c
10 20 30 : 300#C> 6 0 6 1 A I ;
strain % d: 400ÎS 6 0 6 1 A I .
 129

Fig.4 S E M p h o t o g r a p h s of the S i C w / 6 0 6 l M c o m p o s i t e ,
a. b e f o r e c o m p r e s s i o n ; b . a f t e r c o m p r e s s i o n .

whisker axis and the c o m p r e s s i v e d i r e c t i o n is i n c r e a s e d due to

the w h i s k e r s r o t a t i o n , and some w h i s k e r s w i l l b r e a k d u r i n g the
compressive d e f o r m a t i o n of the c o m p o s i t e , so the load bearing
ability of the c o m p o s i t e w i l l be d e c r e a s e d , t h e s e two opposite
a s p e c t s lead to the p e e k in the c o m p r e s s i v e s t r e s s - s t r a i n c u r v e s
of the c o m p o s i t e.

F i g . 4 is S E M p h o t o g r a p h s s h o w i n g the w h i s k e r d i s t r i b u t i o n in the
SiCw/606lM composite. F i g . 4 ( a ) s h o w s that the S i C w h i s k e r s
disperse randomly in the c o m p o s i t e b e f o r e the c o m p o s i t e is
compressed; and F i g . 4 ( b ) s h o w s that a l m o s t all the w h i s k e r s in
the c o m p o s i t e a f t e r b e i n g c o m p r e s s e d are p e r p e n d i c u l a r to the
compressive direction, and the l e n g t h of the w h i s k e r s is
obviously decerased, this result m e a n s that large amount of
w h i s k e r s are r o t a t e d , and m a n y w h i s k e r s , e s p e c i a l l y the longer
whiskers, are b r o k e n d u r i n g the c o m p r e s s i v e d e f o r m a t i o n of the
composite. This further improves that the p e e k in the
compressive c u r v e s of the c o m p o s i t e is due to the r o t a t i o n and
b r e a k of the w h i s k e r d u r i n g the c o m p r e s s i o n of the c o m p o s i t e

300 400 500 300 400 500

temperature °C temperature C
(a) (b)
Fig.5 Compressive strength and c r i t i c a l reduc t ion of the
T ß — t r e a t e d S i C w / 6 Q 6 j A l c o m p o s i t e and 6 0 61^1 a t e l e v a t e d
temperatures. composite; 60 6 1 A l .
130
F i g . 5 shows the c o m p r e s s i v e s t r e n g t h and the c r i t i c a l r e d u c t i o n
of the S i C w / 6 0 6 1 A l c o m p o s i t e and the 60 61Al a l l o y at different
temperatures. By the same reasons as that of the tensile
strength of the c o m p o s i t e , the c o m p r e s s i v e strength of the
composite is m u c h higher than that of the 6061^1 alloy,
e s p e c i a l l y at high t e m p e r a t u r e s , as shown in F i g . 5 ( a ) . F i g . 5 ( b )
shows that the c o m p o s i t e has a good d u c t i l i t y w h e n it is in
compressive stress s t a t e , and the c r i t i c a l r e d u c t i o n reach 50W
a
* 500Ü· W h e n the c o m p o s i t e is in the c o m p r e s s i v e stress state,
it is difficult for the microcracks to initiation and
p r o p a g a t i o n , so the c o m p o s i t e e x h i b i t s a good d u c t i l i t y .

CONCLUSIONS

B e c a u s e the S i C w / 6 Q 6 l M c o m p o s i t e has a high p l a s t i c d e f o r m a t i o n

strengthening effect, the ratio of the yield s t r e n g t h to the
tensile s t r e n g t h is lower c o m p a r e d w i t h the 6 0 6 l M a l l o y . The
composite has a high tensile s t r e n g t h , especially at high
temperature. the tensile s t r e n g t h of the S i C w / 6 0 6 l M composite
at
300*0 equals to that of the 6061^1 alloy at room t e m p e r a t u r e .

Because the rotation and b r e a k of the whiskers during the

c o m p r e s s i v e d e f r o m a t i o n of the c o m p o s i t e , there is a p e e k in the
c o m p r e s s i v e s t r e s s - s t r a i n curve of the c o m p o s i t e . The composite
has a higher c o m p r e s s i v e s t r e n g t h than the 6 0 61^1 alloy d o e s , it
e x h i b i t s a good d u c t i l i t y w h e n it is in c o m p r e s s i v e stress state,
and the c r i t i c a l r e d u c t i o n of the c o m p o s i t e reach 50W at 500Γ·

REFERENCES

Divecha, A. P. and F i s h m a n , S.G. C19 8 0 ) · Progress in the

D e v e l o p m e n t of SiCw/Al A l l o y s , 12th N a t i o n a l SAMPE Technical
C o n f e r e n c e , O c t o b e r 7-9, 6 5 6— 6 6 3-
Guo, S.Q., H a n , G . H . and Y a o , C.K. (1989)· M i c r o s t r u c t u r e s and
P r o p e r t i e s of S i C w / A l C o m p o s i t e s , Acta Metallurgica Sinica
( E n g l i s h E d i t i o n ) , Series B, j , 19 8~194 -
M c D a n e l s , D . L . and H o f f m a n , C.A. (1982)· N A S A - T M - 8 3 6 1 0 ·
M a , Z.Y. and Y a o , C.K. (1989)· M i c r o s t r u c t u r e and P r o p e r t i e s of
S i C w / 6 0 6lAl C o m p o s i t e , Materials C h e m i s t r y and P h y s i c s , ^ 5 ,
463-471·
Geng, L., Jiao, C.G. and Y a o , C.K. (1989)· Some E f f e c t s of Hot
Rolling on the M i c r o s t r u c t u r e and Properties of SiCw/Al
Composite, P r o c . jst Japan International SAMPE Symposium,
Nov.28* 997-1001-
Burgam, P. M . ( 1982)· The Push to A d v a n c e d Composite,
M a n u f a c t u r i n g E n g n e e r i n g , D e c e m b e r , 37—42·
 WS10C1

Dislocation Punching in Aligned Fiber Metal Matrix Composites

M. Taya* and K. E. Lulay

Department of Mechanical Engineering University of Washington
Seattle, WA 98195 U.S.A.

T. Mori

Department of Materials Science and Engineering,

Tokyo Institute of Technology
4259 Nagatsuda, Midori-ku, Yokohama, 227 Japan

Abstract
Punching of dislocations that relax the high stress field induced by the coefficient
of thermal expansion mismatch between fiber and matrix is studied analytically by
use of Eshelby's model. The punching distance in the matrix after punching are
obtained for a short fiber and long fiber metal matrix composites.

Keywords

Dislocation punching, CTE mismatch, metal matrix composites, Eshelby's model.

Introduction
Strengthening of metal matrix composites (MMCs) has been attributed to "back
stress" induced as a result of plastically deforming matrix resisting fillers that can
deform elastically. Among composite models, the back stress model based on
Eshelby's method (Eshelby, 1957) is considered most general in that it can treat
three-dimensional problem associated with a short and long fiber composites
(Taya, 1991). In most composite models, however, it has been assumed that the
mechanical properties of the matrix metal in a MMC are the same as those of the
unreinforced metal. Taya and Arsenault (1987) pointed out that there exists a large
gap between the experimental results of composite yield stresses (a y c ) and the
predictions based on the existing composite strengthening models which use the
above assumption. The gap was recently attributed to negligence of the fact that
the dislocations are generated in the matrix due to punching to relax the high
stress field induced by the coefficient of thermal expansion (CTE) mismatch
between the filler and matrix, and the dislocation so generated enhance the matrix
flow (or yield) stress in a MMC prior to external loading (Arsenault and Shi, 1986 ;
Taya and Mori 1987 ; Taya et al., 1991). Taya et al. (1991) confirmed by both
experimental and analytical studies that the strengthening observed in SiC
particle/6061 Al matrix composites quenched is attributed maily(about two-thirds)
to the dislocation punching driven by CTE mismatch and the strengthening due to
back stress is only one-third of the total strengthening. In the case of an aligned
short fiber MMC, Taya and Mori (1987) found analytically that as fiber aspect ratio

* Department of Materials Processing, Faculty of Engineering

Tohoku University, Sendai, 980, Japan

131
132
increases the punching of dislocations along the fiber axis becomes more difficult
and at and beyond a certain aspect ratio, the punching would not take place along
the fiber direction. Then, it would be reasonable to assume that for a long fiber
MMC, the punching can take place along the plane transverse to the fiber axis. In
this paper, an attempt is made to review the dislocation punching models associated
with aligned short and long fiber MMCs. First, the case of a short fiber MMC is
examined, and then followed by the case of a long fiber.

Short Fiber MMC

Consider a short fiber MMC where short fibers of prolate ellipsoidal shape are
aligned along the xß-axis and otherwise distributed uniformly in a matrix metal.
When a MMC is subjected to temperature change during cool down from high
temperature to room temperature, ΔΤ(< 0), CTE mismatch strain (a*) can be induced
within fiber (Ωι) with the corresponding eigenstrain eij defined by

< - ■
(1)
where oc* = (ocf-ocm)AT (2)

and where otf and ccm and CTE of the fiber and matrix, respectively, and 6ij is
Kronecker's delta. The eigenstrain given by eq.(l) is equivalent to making arrays
of prismatic dislocation loops adhered to the matrix-fiber interface | Ωι | , Fig. 1(a)
where the major and minor axes of the short fiber are denoted by c and a,
respectively. In order to relax the high stress field induced in and around a short
fiber, one can assume that the arrays of prismatic dislocation loops punch out
along the fiber axis (the x3-axis) with the punching distance c', Fig. 1(b). The
eigenstrain corresponding to the punching to c', Fig. 1(b) is given by

a* 0 0
eu = 0 a* 0 in Ωι (3)
0 0 0

0 0 0
eij = 0 0 0 in Ω2 (4)
0 0 a*c/c

where the punched-out region including the fiber domain is denoted by ^ 2 ·

Punching criterion

The criterion for determining punching distance c' is given by (Taya and Mori,
1987)
_ au_aw
dc' 3c' (5)
Where U is the total potential energy of a composite and W is the work done by the
motion of the dislocation loops during the punching.
Total potential energy U

The total potential energy of a composite which is equal to the strain energy in
absence of external load is given by
U= lfaij(eij-e;j)dV
(6)
L
SO
 133
where c\j and eij are the internal stress and strain induced by eigenstrain eij
defined by eqs.(3) and (4), dV is the volume element and D is the domain of the
composite. In order to calculate U, one must evaluate the stress and strain field
which will be solved by use of Eshelby's method (Eshelby, 1957 ; Mura, 1987). To
facilitate the analysis, we assume that the interaction between fibers are
negligible, which is valid for small volume fractions of fiber. The case of large
volume fractions have been given elsewhere (Lulay, 1990). First consider an
2*
inclusion Ω2 with eij which is embedded in the matrix without fibers (Ωι). Then
2*
the stress due to eij is given by
Oij = Cijkl (e2kl -4*i> (7)
2 çp- 2*
e
where kl" 5klmn emn (8)
and where e|i is the strain induced by e|*i , Sy mn is the Eshelby's tensor related to
Ω2 which is a function of fiber aspect ratio c/a and the matrix Poisson's ratio v.
Cijkl in eq.(7) is the stiffness tensor of the matrix. Next introduce an Ω^ with Gjki
1*
(the stiffness tensor of the matrix) and eigenstrain eij into Ω2. Then the total stress
within Ω1 is given by
+ —
°»j ^y Q'-ijkl
j k l (^klmn
' ^ητη " ^kl + ^ ι - t^\)
= Qjkl (Sklmn ^ητη " Cy + e k j - e k l ) (9 y

where e|a is the strain induced by introducing Ω1 into Ω 2 and it is related to a

fictitiously introduced eigenstrain eij defined only inside Ωι
1 _ ς, 1 1**
e
kl ~ 5klmn emn (10)
It is noted that the stress field defined by the second equality in eq.(9) is valid for
f
the entire composite domain D, for the inhomogeneity Ω1 with Cijkl is converted to
an equivalent inclusion Ωι with Cijkl- It is also noted in the above equations that
once the fictitious eigenstrain eij is solved from eq.(9) the stress and strain field
within Ωι and Ω2 are calculated. For example, from eqs.(7) and (9), aij is expressed
1**
in terms of eij
<*ij = Cijkl (sklmn emn " \ \ ) ^ jj

The strain energy of the composite U per unit volume is simplified as (Taya and
Mori, 1987)
TT 1 r r^ /c2 1** l
**\ 2
* 1 c 2 2* 1 r 2 1*
U = - i - fiCijkl
J ( S k l m n ^ m n " e k l ) e iiJj " 7 Ϊ2 σ
ϋJ e i1J
j " Γ" f l c ij e
ij
2 " 2 2
e
fiCijkl ( S k l m n kl " ekl ) e
ij
(12)
where f 1 and f2 are the volume fraction of fiber (Ω1 ) and Ω 2 , respectively and
f2=(c7c)fi.

Work done bv the motion of dislocation loops W

The average work (W) by the motion of a dislocation loop at X3=z during the
punching is
134

\ν = 2πΕ(1 - i £ ) 1 / 2 z ( £ l - 1 )bk
c2 c
(13)

where b and k are Burgers' vector and friction stress in shear. The total work done
by 2N dislocation loops at z, W is then becomes

W = 2Y 2π3(1 - ^ i ) 1 / 2 z„ ( ^ - 1 )bk
ηίι c2 c
(14)
where z n is the location of the nth dislocation loop. By using the limiting sequence,
N -> oo , and keeping Nb=ca* constant, one can convert the summation to
integration
W=2 2na (1 - 3Î. ) 1/2 ζ(— - l)ka*dz
n2 C
Jo c

(15)
per unit volume
(16)
Upon substitution of eqs.(12) and (16) into (5), one can obtain the equation to
solve for the punching distance c' normalized by c (=ξ)

(17)
f !* 2*
where Η(ξ) is a function of ξ (=c'/c) and known parameters : Qjki, Cij kl, eij, eij, fi
and c/a, and its explicit expression is given elsewhere (Taya and Mori, 1987).
In order to examine the dependency of the punching distance c' on several
parameters, we have conducted a parametric study to find that c'/c decreases with
increase in c/a. Fig.2 show the results of c'/c vs. c/a for SiC /Al matrix composite
with ΔΤ = -200°C and k/μ = 0.001. Fig.2 indicates that at and beyond a certain value
of fiber aspect ratio(critical fiber aspect ratio), the punching along the fiber axis
is no longer possible. Lulay (1990) calculated the critical fiber aspect ratio ((c/a)*)
more accurately by accounting for the interaction between fibers for SiC/6061 Al
composite with AT=500°C to obtain (c/a)* =72. By using the criterion that the strain
energy of the punching mode along the X3~axis is lower than that along the xi-x2
axes, Lulay concluded that the punching along the plane transverse to the fiber
axis would be preferred for c/a > 72. In the following the transverse punching in
a long fiber MMC will be stated.

Long Fiber MMC

Consider the cross section of a typical long fiber in a long fiber MMC, and look at
the stage of the punching to the circular domain with r, shown as fine dash circle
in Fig.3 where the radius of the circular domain corresponding to the final stage
of punching indicated by large dash line is denoted by a'. The eigenstrain before
punching is the same as in the case of a short fiber MMC and given by eq.(l). After
1*
punching to radius r, the eigenstrains in the domain of fiber (Ωι) eij and in the
punched out domain(Q2) given by
0 0 0
0 0 0 in (18)
0 0 a
 135

e5 = e*(r) 0 1 0 in Ω 2 (19)
0 0 0
where
e*(r) = (a/r)22ct* (20)

In the following, we will calculate the strain energy of a composite, U and the
work done by the motion of dislocation lines W. Then by using eq.(5), The
punching distance a' will be obtained. To facilitate the analysis, the stiffness of the
fiber is made equal to that of the matrix, but the interaction between fibers will be
accounted for. The case of accounting for the stiffness of the fiber as well as the
interaction between fibers will be given elsewhere (Taya and Mori, 1991).

Stress field

The problem of calculating the stresses within Ωι and Ω2 is reduced to that of two
inclusions. First the case of a single fiber imbedded in infinite matrix is
considered, for the extension to finite volume fractions of fiber is straight
forward, which will be considered later. Let the internal stresses due to Ω1 with eij
2* 1 2
and that due to Ω2 with eij be denoted by aij and ccij, respectively. By applying
eq.(7) to eqs.(18) and (19), one can calculate the internal stresses given by
for Ωι
σ α σ α
<*îl
11 = 22 = - 7 Τ ^ Τ * > 33 = - 7 Γ ^ Τ *
(1-V) (1-V) 21) (
and for Ω2
11 22 3i v
(1-ν) V ' (1-ν) a'' ( 2 2)

The average of the stresses in the matrix, <cij>m can be calculated by using Mori-
Tanaka theory (Mori and Tanaka, 1973).

< Sij > m = -fi σ-j - f2 Crfj (23)

By substituting eqs.(21) and (22) into (23) and noting that f2=f(a/a') 2 , one arrive at

(24)

Strain energy U

First we shall calculate the strain energy per unit fiber Uf which is given by

(25)

Where Ui is the self energy associated with Ωί.υι (with i,j=l,2, m) is the interaction
energy between Ωί with the stress induced by Ωj or the matrix (j =m )· The details
are given elsewhere (Mura, 1987). There energies per unit volume are :
136

Ul 2 = - fx o?j eî/ (26)

UIlm = -fi<a ij > m ei;/2

U?m = -f 2 <o ij > m 4*/2

From eqs.(18) - (22), (24) - (26), the total strain energy of the composite per unit
volume, U is given by

v
(1-v) a' ( 27)
Work done bv the motion of dislocation lines W

The number of dislocation lines per unit length of fiber, n(r) when punching to r
is given by
W(r)
w
b (28)
where e*(r) is given by eq.(20) and b is Burgers' vector. The work done by the
motion of a single dislocation line from r to r + 6r, ÔW i is given by

ÔWi = nkbôr (29)

where k is the friction stress in tensile mode, and n is given by eq.(28). The work
done by all dislocation lines per unit fiber when they moved from a to a', Wi is

-r
calculated as

Wi= | nkbdr = 2n&2ka*\n(^-)

(30)
The work per unit volume of the composite, W is obtained by multiplying Wi by
fl/0ra 2 ), thus

W= 2f!ka*ln£) (31)

Punching distance a'

The punching distance a' can be obtained by substituting eqs.(27) and (31) into (5),
resulting in
a
(1 -v) k (32)

In order for eq.(32) to be valid, the strain energy defined by eq.(27) must be
positive,i,e.,
l + (r-) 2 (l + 2 v ) - 2 f i ( l + v ) > 0
This is valid always if 1 - 2fi(l + v) > 0, i,e, fi <
1
2(1 + v)
then the punching is possible. Even if fi > !
2(1 +v)
the punching is still possible with the upperbound on a', a* given by

a* = afi" 1/2 (34)

 137
Denoting the number of fibers per unit area by N

l W = fi (35)
N7c(a*)2=l (36)

Thus, eqs.(35) and (36) yields eq.(34). When a' = a*, the strain energy U, eq.(27)
still remains non-negative. In summarizing the above, when

μ(1 + 2v) a , < !

k(l - v) (37)

the punching is not possible, since it would lead to a'< a as seen from eq.(32).
When
ϋί1±Μ α ·>1
Ml - v) (38)

and also eq.(34) is valid, then the punching can always take place with the
punching distance given by eq.(32). When eq.(38) and eq.(37) are valid, the
punching can take place, but the punching distance is bounded by a* given by
(34), which is a decreasing function of fi. As an extreme case when the volume
fraction of fiber fi becomes 1, eq.(34) provides a* = a, i,e., no punching is expected.

Acknowledgement

This work was supported in part by the AFOSR Contract (89-0059) to the University
of Washington and also by the Grant from Alcan International to Tohoku
University

References

Arsenault R. J. and Shi,N. (1986). Dislocation generation due to differences in

coefficients of thermal expansion, Mater, Sei. Eng, £_L, 175-187.
Eshelby, J.D. (1957). The determination of the elastic field of an ellipsoidal
inclusion, and related problems, Proc. Roy, Soc. London, A 2 4 1 . 376-396
Lulay, K.E (1990). Strengthening of metal Matrix composites by quenching, PhD
dissertation. University of Washington.
Mura, T. (1987). Micromechanics of defects in solids, 2nd ed. Martinus Nijhoff. The
Hague.
Mori, T. and Tanaka, K. (1973). Average stress in matrix and average energy of
materials with misfitting inclusions, Acta Metall. 2J_, 571-574
Taya, M. (1991). Strengthening mechanisms of metal matrix composites, overview,
Mater/Trans. JIM, 3 2 , 1-19
Taya, M and Arsenault, RJ. (1987). A comparison between a shear lag model and an
Eshelby type model in predicting the mechanical properties of a short fiber
composite, Scripta Metall. 2 i , 349-354.
Taya, M, Lulay, K.E. and Lloyd, D, J.(1991). Strengthening of a paniculate metal
matrix composite by quenching, Acta Metall. Mater., 1 £ , 73-87.
Taya, M. and Mori, T. (1987). Dislocations punched-out around a short fiber in a
short fiber metal matrix composite subjected to uniform temperature change, Acta
Metall, 1£, 155-162.
Taya, M. and Mori, T. (1991). Dislocation punching in a long fiber metal matrix
composite, to be submitted.
138

(a} (b)
Fig. 1 Dislocation punching model for a short fiber MMC

x2

y ^

'1 ty^
SiC/Ai Composite
A T « - 2 0 0 eC , - . 0 . 0 0 1 y

Γ
!|\ xV (
ISiià ^
WEEK >
■Hi ' Xi
1

\\ y 1
\
\ /
y /
2a
10 20 30 2r
Fiber Aspect Rotio,-^-
2_a; *

Fig. 2 Punching distance c"

vs. fiber aspect ratio Fig. 3 Dislocation punching
c/a. model for a long fiber
MMC.
 WS10C2

COMPUTATIONAL MODELING OF Al-Cu MATRIX,

SiC REINFORCED COMPOSITE MATERIALS

P.E. MCHUGHf, R.J. ASAROt, C F . SHIHf

fDivision of Engineering, Brown University,

Providence, RI 02912, USA
{Department of AMES, University of California, San Diego,
La Jolla, CA 92093, USA

ABSTRACT

Computational mechanics has become increasingly concerned with the analysis of com-
plex deformation processes and failure in material microstructures. In the work de-
scribed in this article we use what, in light of this trend, we may call Computational
micromechanics to study metal matrix composite materials, in particular materials with
Al- 3 wt % Cu matrices reinforced with SiC particles. We focus on the evaluation of the
performance of the microstructure, viz. deformation behavior, development of strength-
ening mechanisms and failure mechanisms. We employ various methods to evaluate this
performance, viz. variation of microstructural parameters such as 1) matrix properties,
2) volume fraction of reinforcement and 3) microstructural morphology; change in load-
ing state; relation of macroscopic constitutive behavior to microscopic behavior using
stress strain curves; introduction of the effects of processing, the residual stresses present
due to working and temperature change. The modeling involves a detailed description
of the material microstructure where individual matrix grains and reinforcing particles
are represented and incorporates a physically based, rate dependent, crystallographic
theory of plastic slip in the context of finite deformation kinematics. The theory is
implemented using the finite element method.

KEYWORDS

Composite; metal matrix; reinforcement; strength; failure; hydrostatic stress; computa-

tion; finite element.

MODEL DESCRIPTION

The constitutive theory that is used in the following analyses is a rate dependent plastic,
finite deformation, crystallographic theory (Asaro 1979, 1983). Within the single crystal
framework, the plasticity is described solely by continuum shear flows that occur along
139
140
the various slip systems of the crystal. The elasticity and rigid motions of the crystal
are also accounted for. The rate constitutive relations resulting from the theory are im-
plemented in the finite element context via the one step, explicit rate tangent method of
Pierce et al (1984). The details of the theory and numerical method are given in Harren
et ai. (1988), Harren and Asaro (1989) and McHugh et al (1989a, 1989b). An enhanced
version of the theory which incorporates deformation due to temperature change and
the corresponding numerical method is detailed in McHugh et al (1991). Figure 1
shows the finite element microstructural model used in the composite simulations. It
is an extension of the polycrystal model of Harren et al (1988) and Harren and Asaro
(1989) and is detailed in McHugh et al (1989a, 1989b, 1991).

Fig. 1. Geometry of microstructural model, \ unit cell.

The model consists of 27 grains (or single crystals). An idealized slip system geometry
is used; three slip systems with equivalent constitutive properties are arranged to form
an equilateral triangle whose angle of orientation with respect to the reference axes is
randomly chosen so that each grain has its own randomly assigned lattice orientation.
The material shown in Fig. 1 constitutes one-fourth of a unit cell which means that
the actual periodic poly crystalline unit is obtained by reflecting the grains shown in
Fig. 1 across the left edge and then reflecting both groups across the bottom edge. The
lattice is assumed to deform in plane strain. Periodic boundary conditions are applied
so that tensile and compressive loading histories are constrained to be orthotropic. The
periodicity condition requires that the edges of the one-fourth unit cell remain straight
and aligned with the coordinate axis and support no shear stress. We require that the
total load in the horizontal direction be zero and prescribe a uniform normal velocity on
the top boundary. The initial conditions correspond to zero stress and strain. As regards
material properties, isotropic elasticity and Taylor isotropic hardening plasticity (Taylor
1938) are assumed. The matrix hardening properties were obtained from the data of
Chang and Asaro (1981) for tensile deformation of Al-Cu single crystals. The crystals
were age hardened to produce microstructures containing a nominal solid solution (S-S),
GP-II zones and θ'. The model consists of two phases with individual grains considered
to be of one, or other, of the phases. Regarding the second phase as the reinforcement
means that selected grains become reinforcing particles and are assigned appropriate
elastic, viscoplastic and hardening properties consistent with the assumed purely elastic
deformation of the SiC particles. Each full grain in the model represents 4% of the total
volume and hence the reinforcement volume fraction, V/, can vary in increments of 4%.
 141

1* · » · ι I
a) b)

Φ · Φ Φ1

• + » » [*· » » |

Fig. 2. Unit cell morphologies: a) 16%a and b) 16%b.

In the finite element implementation a 40 x 56 mesh of initially rectangular "crossed

triangle" elements is used.

RESULTS AND DISCUSSION

Tension simulations of up to 5% and compression simulations of up to 25% engineering

strain in the vertical direction were performed for Vf values of 0, 4, 8, 16 and 20%
for a range of microstructural morphologies and matrix properties. Figure 2 shows
two of the morphologies used for composites with Vf values of 16%, which we refer to
as 16%a and 16%b. A detailed picture of the behaviour of the microstructure during
deformation is provided by computed contour maps of the accumulated slip, j a , which
is a measure of total accumulated plastic deformation. Figure 3 shows such a map for
the case of compression of a composite with a Θ' strengthened matrix and the 16%a
morphology where the overall strain level is 25%. Deformation is nonuniform from the
onset of plastic straining and quickly becomes localized in bands almost parallel to
the oblique facets of the particles showing the flow of the matrix material along these
facets. This is a feature common to almost all of the composites studied. The bands
isolate triangular regions on either side of the particles within which there is a very
low strain level. One important feature of the results which could have implications for
fracture, when compared to the homogeneous polycrystal, is that the local plastic strains
at a given overall strain are much higher in the composite than in the homogeneous
polycrystal. The particles appear to cause straining to become localized at lower overall
strains leading to the more rapid development of a deformation pattern. The lack
of symmetry in the deformation pattern is due, of course, to the fact that the initial
lattice orientation is randomly generated in the matrix grains. The figure shows that
the particles have rotated slightly. Severe distortion of the grains is required to allow
the matrix material to flow past the particles. The deformation pattern around each
of the four particles is similar even though the initial slip directions in these areas are
different. This suggests that at high strains localized deformation is governed more by
particle shape and position than by local lattice slip directions. Comparing such maps
for composites with different Vf values we find that deformation patterns become more
142

Fig. 3. Accumulated slip, 7 α , map for a composite with a θ'

matrix and the 16%a reinforcement morphology. The
overall strain is 25% in compression.

intensely localized with increase in V/, i.e., higher peak ηα for the same overall strain and
larger regions of both very high intensity and very low intensity plastic strain within the
microstructure. The dependence of the deformation pattern on particle position is clear
when one compares deformation patterns corresponding to composites with different
microstructural morphologies but with the same Vf values and matrix properties. If a
morphology is such that particles approach one another during deformation then the
matrix material separating a pair of approaching particles will undergo intense straining
and this will effect the distribution of strain throughout the microstructure and hence
the localization level. This is related to constraint of plastic flow. For example the
composite in Fig. 3 shows intense strain levels in the matrix material separating particles
in the vertical direction. On the other hand a composite with the same matrix properties
and the 16%b morphology exhibits a lower peak j a level and a less intensely localized
deformation pattern at the same overall strain level in compression and this is due
largely to the fact that particles do not approach each other in the vertical direction
and hence plastic flow of the matrix is less constrained. Deformation patterns depend
weakly on matrix properties. In contrast to the S-S and GP-II strengthened alloys, who
 143

exhibit a steady strain hardening rate even to high plastic strains, the Θ1 strengthened
alloy exhibits an initial high hardening rate followed by saturation to a constant strain
hardness. We observe that this has the effect of rendering the deformation patterns of
the composites with θ' strengthened alloy matrices more intensely localized than those
of the other two cases.

5.5
a)
5.0
4.5
4.0
3.5
3.0
2.5
2.0
1.5 Reinforcement Compressed and Quenched
0%
4% Quenched
1.0
16% a Unquenched
0.5 16% b
20%
0.0
0 0 0 0.05 0.10 0.15 0.20 0.25 0.30 0.02 0.03
true strain true strain

Fig. 4. Stress strain curves for a selection of composites with

θ' strengthened alloy matrices: a) compressive stress
strain curves, b) tensile stress strain curves for a com-
posite with the 16%a reinforcement morphology sub-
ject to various degrees of pre-déformât ion processing.
The stresses are normalized by the initial yield stress.

The above mentioned of the concept of plastic constraint leads into the consideration
of strengthening mechanisms. The results have shown that a composite gains strength
from accentuated strain hardening of the matrix material due to localization and more
importantly, from the constraint of plastic flow in the matrix and the related develop-
ment of high hydrostatic stresses. Figure 4a shows a set of computed compressive stress
strain curves for composites with Θ' strengthened alloy matrices and various indicated
Vf values. Before saturation the composite hardening rates increase with increasing
Vf and this can be related to both the above mentioned mechanisms. The behavior
of the composites in the high strain region can be explained almost completely by the
development of constraint since the hardness of the matrix material levels off for high
plastic strain. Indeed if we compare the stress strain curves of Fig. 4a for the 16%a and
16%b cases then we see a marked difference in behavior at high strain with the 16%a
material exhibiting an increasing overall hardening rate. This can be related to the
development of an enhanced constraint in this material due to the approach of particles
in the vertical direction. This is evident when one examines hydrostatic stress maps
for the two composites. The former material exhibits a much greater buildup in hydro-
static stress with overall strain than the latter especially in the material separating the
particles in the vertical direction. In general the results show that particle interaction
and its manifestation in the buildup of hydrostatic stress is a very important feature
144

of composite strengthening. Matrix hardening properties effect strengthening by con-

trolling the degree of strengthening due to the enhancement of strain hardening with
localization.

Intense localization could lead to the development of macroscopic shear banding and
hence could be considered as a prelude to failure. Results have shown high tensile
hydrostatic stress buildup in the matrix material close to certain particle vertices. This
has important implications for void growth and particle-matrix interface decohesion.

Figure 4b shows tensile stress strain curves for a composite with a Θ' strengthened
alloy matrix and the 16%a reinforcement morphology. The different curves correspond
to different degrees of pre-déformât ion thermo-mechanical treatments. We see that
the effect of the processing is greatest at initial yield but tends to lose significance as
straining proceeds as the microstructural strains due to deformation become dominant
over the residual strains due to processing.

ACKNOWLEDGEGMENTS

The authors acknowledge the support of the Ford Motor Company. The computations
in this work were carried out at the San Diego Supercomputer Center, the John von
Neumann National Supercomputer Center and the Brown University Computational
Mechanics of Materials Facility with support of the NSF Division of Advanced Scientific
Computing.

REFERENCES
Asaro, R.J. (1979). Geometrical effects in the inhomogeneous deformation of ductile
single crystals. Ada Metallurgical 27, 445-453.
Asaro, R.J. (1983). Micromechanics of crystals and polycrystals. In: Advances in
Applied Mechanics (J.W. Hutchinson, ed.) 23, pp. 1-115. Academic Press, New
York.
Chang, Y.W. and R.J. Asaro(1981). An experimental study of shear localization in
aluminum copper single crystals. Ada Metallurgical 29, 241-257.
Harren, S.V. H.E. Deve and R.J. Asaro (1988). Shear band formation in plane strain
compression. Ada Metallurgical 36, 2435-2480.
Harren, S.V. and R.J. Asaro (1989). Nonuniform deformations in polycrystals and
aspects of the validity of the Taylor model. J. Mech. Phys. Solids, 37, 191-232.
McHugh, P.E., A.G. Varias, R.J. Asaro and C.F. Shih (1989). Computational modeling
of microstructures. Future Generation Computer Systems, 5, 292-318.
McHugh, P.E., R.J. Asaro, C F . Shih and A.G. Varias (1989). Computational modeling
of metal matrix composite materials. Proceedings of 10th International Symposium
on Metallurgy and Materials Science, RISO National Lab., Denmark.
McHugh, P.E., R.J. Asaro and C.F. Shih (1991). Computational modeling of metal
matrix composites: Parts I-III. Manuscript in preparation.
Pierce, D., R.J. Asaro and A. Needleman (1983). Material rate dependence and localized
deformation in crystalline solids. Ada Metallurgica, 31, 1951-1976.
Taylor, G.I. (1938). Plastic Strain in Metals. J. Inst. Metals., 62, 307-325.
 WS10C3

ELASTIC STRENGTH OF PARTICLE AND FIBER REINFORCED

METAL-MATRIX COMPOSITES

B. GRELSSON and K. SALAMA

Department of Mechanical Engineering, University of Houston

Houston, Texas 77004

ABSTRACT

Conventionally, metal matrix composites (MMC) are reinforced with either particles or fibers.
Recently, a new class of composites where a mixture of particles and fibers is used as
reinforcement has emerged. The particles improve the isotropic mechanical and thermal
properties, whereas the fibers introduce directionally favorable properties for specific
applications of the material. The elastic properties of three different matrix alloys containing 6%
alumina fibers and varying alumina particle volume fractions of 9, 13, and 17% have been
determined using ultrasonic velocity measurements. The results show that the elastic moduli
increase with the particle content and the composites have the highest elastic stiffness in the
directions of the fiber plane. A model is developed to explain the observed elastic moduli of this
type of composites. The model uses results of the theories by Ledbetter and Datta for spherical
inclusions and Hashin and Rosen for aligned fibers. Furthermore, it includes an averaging
procedure suggested by Christensen and Waals. The agreement between measured and
calculated elastic moduli is found to be good. In a second series of measurements, the elastic
moduli in two sets of extruded MMCs and one set of pressed MMCs are determined. These
composites are reinforced with silicon carbide particles. Their elastic moduli as well as their
elastic anisotropies are explained using the theories discussed earlier.

INTRODUCTION

In order to increase structural efficiencies in modern design, materials possessing high stiffness
and high strength are required. One class of engineering materials fulfilling these requirements
are metal-matrix composites (MMCs). In these composites, properties of the material can be
tailored by the appropriate selection of matrix and reinforcement materials and by their mutual
arrangement in order to meet specific needs of the designed component. The matrix and the
reinforcement are to be selected so that they combine their different mechanical and elastic
properties in a synergistic way. Also, microstructures resulting from different fabrication
processes are found to influence properties of these composites and provide valuable
information for their further development.

Many models have been developed to determine the effective elastic moduli of composite
materials. Most of these models deal with reinforcement in the form of spherical particles
(Ledbetter and Datta, 1986, Budiansky, 1965), ellipsoidal inclusions (Eshelby, 1957, Chow,
1977) or infinitely long fibers (Hashin and Rosen, 1964, Hill, 1964). Ledbetter and Datta used

145
146
a multiple scattering theory to predict the elastic behavior of composites with a
nonhomogeneous particle distribution. In the model they assume that the particles together with
the matrix form an enriched "sea" that surrounds "islands" of pure matrix material. These non-
spherical islands are aligned and produce anisotropy. On the other hand, in order to determine
the effective elastic properties of fiber reinforced materials, Hashin and Rosen introduced the
composite cylinders model. In this model, the composite is considered to be comprised of
infinitely long circular cylinders embedded in a continuous matrix phase. Each fiber has a
radius, 0, which is surrounded by an annulus of matrix material of radius b, and the ratio alb is
considered to be constant for all composite cylinders. In order to obtain a volume filling
configuration, the absolute size of the cylinders must vary considerably.
In some industrial applications composites used are of a more complex nature, where a mixture
of particles and fibers is used as a second phase. To our knowledge no models that describe the
elastic properties of these composites are available. The present study is concerned with
composites reinforced with low values of both particles and fibers, and hence, no interaction
between fibers and particles is assumed. In modeling these composites, we first consider the
matrix material and the particles to form an effective matrix. Since the particles are
homogeneously distributed in the metal, the effective matrix is considered to be homogeneous
(Ledbetter and Datta, 1986). The effective matrix is then considered to be reinforced with fibers
which are randomly oriented in one plane. The influence of the fibers on the elastic moduli of
the composites is then determined first by using the composite cylinders model for an aligned
fiber system (Hashin and Rosen, 1964) and second by preforming a geometric average
procedure (Christensen and Waals, 1972) which takes care of the 2-dimensionally random
orientation of the fibers. The results obtained show a good agreement between calculations and
measurements where details are given elsewhere (Grelsson and Salama, 1990).

EXPERIMENTAL
The metal matrix composites used in this investigation consist of aluminum alloys as the matrix
material and either SiC-particles or alumina fibers and particles as the reinforcement. The
composites based on Al 7064 and Al 8091 were obtained as extruded rods of 25 mm in
diameter. The specimens based on Al 6061 were received as pressed plates of the dimension 6 x
25 x 60 mm. The alumina reinforced specimens were manufactured by squeeze casting and
received as bars of the dimension 12 x 12 x 50 mm. The volume percentage of reinforcement in
the different sets of MMCs is shown in Table 1. Specimens are cut from the as-received

Table 1. Manufacturing method, matrix alloy and volume fraction of

reinforcement of the MMCs investigated.

Manufacturing method Matrix alloy and volume fraction

of reinforcement

Extruded rods Al 7064 + 0% SiC

Al 7064 + 15% SiC
A17064 + 2 0 % SiC
A18091 + 0%SiC
Al 8091 + 10% SiC
Al 8091 + 15% SiC

Pressed plates Al 6061 + 0% SiC

A16061 + 2 5 % SiC
A16061 + 4 0 % SiC

Squeeze cast bars A132 + 23 % AI2O3

A13 + 19% AI2O3
A1100 + 15%A1 2 03
 147

Extrusion Compression Compression

3 A Direction 3 A Direction Direction

Extruded Al 7064 and Pressed Al 6061 Squeeze cast

Al 8091 MMC rods MMC plates MMC bars
Fig. 1. Specimen geometry and designated coordinate systems.

composites and the faces of each specimen are machined flat and parallel to within ±25 μιη. The
coordinate systems are chosen such that in extruded samples the Xi- and X2-axes are
perpendicular to the extrusion direction. In the pressed specimens the Xi- and X2-axes are in
the plate perpendicular to each other and the Xß-axis is oriented parallel to the compression
direction. In the squeeze cast samples the Xi- and X2-directions are in the fiber rich plane at
right angles to each other and the ^-direction is normal to the fiber rich plane. Fig. 1 displays
schematically the cut of the specimens, the manufacturing parameters, and the orientation of the
coordinate systems. For all specimens the microstructure is examined in the three orthogonal
planes in terms of particle size distribution and area fraction covered by the reinforcement.
Measurements of ultrasonic velocities were performed using the pulse-echo-overlap method
with is described in details elsewhere (Salama and Ling, 1980). X- and Y-cut transducers of 10
and 2.25 MHz were used for the generation of the longitudinal and transverse waves,
respectively. The elastic constant are calculated using the relationship Qj = p Vjj2 where p is the
mass density.

RESULTS AND DISCUSSIONS

Extruded MMCs

The measured Young's and shear moduli along the three principal axes in the Al 7064 MMCs
are listed in Table 2 as a function of the volume fraction of SiC. The same moduli for the Al
8091 MMCs are shown in Table 3. Also included in these tables are the elastic moduli predicted
using a model in which the composites are assumed to consist of an aluminum matrix and

Table 2. Calculated and measured Young's and shear moduli of the Al 7064
MMC specimens. Moduli are shown in units of [GPa].
MMC Al 7064 + 15% SiC Al 7064 + 15% SiC
Modulus calc. meas. calc. meas.

Ell 90.0 90.3 96.8 99.9

E22 90.0 90.5 96.8 97.2
E33 90.9 91.4 98.1 100.5

G12 34.0 34.9 36.6 38.0

G13 34.1 35.6 36.8 39.6
G23 34.1 35.3 36.8 38.4
148

Table 3. Calculated and measured Young's and shear moduli of the Al 8091
MMC specimens. Moduli are shown in units of [GPa].

MMC Al 8091 + 10% SiC Al 8091 + 15% SiC

Modulus calc. meas. calc. meas.

Ell 92.6 91.3 99.3 96.8

E22 92.6 91.8 99.3 96.7
E33 93.2 92.6 100.2 98.3

G12 35.7 35.8 38.4 38.1

G13 35.8 36.2 38.5 38.7
G23 35.8 36.1 38.5 38.5

homogeneously distributed particles of spherical shape. The particles, however, are arranged so
that they form unidirectional fibers of particle-rich and particle-free aluminum. This arrangement
is chosen to model the microstructure observed in the extruded composites containing spherical
particles where the particles cluster together and form areas with high particle concentration and
islands of pure matrix material. Due to the extrusion, these areas align in a rod-like shape along
the extrusion direction.

From Table 2 and Table 3 one can see that the anisotropy for predicted Young's moduli between
the extrusion direction and the two transverse directions is of the same order (~ 1%) as that of
the measured moduli. The anisotropy predicted for the shear moduli is negligible and the
measured shear moduli is within the experimental error. However, there is a tendency in all
measurements indicating that the shear stiffness is lower in the XiX2-plane than in the other two
planes. This agrees with the difference observed in the calculations of Young's moduli where
the extrusion direction is found to be suffer than the two other directions.

Pressed MMCs

The measured Young's and shear moduli along the principal axes in the Al 6061 MMCs
together with the elastic moduli predicted by the model assuming dilute concentrations of
homogeneously distributed particles of spherical shape are plotted in Figs. 2 and 3 as a function
of the volume fraction of SiC-particles. The plots clearly shows that the model predicts the
overall increase of the elastic moduli relatively well for specimens containing 25% SiC.
However, it fails for the 40% SiC-reinforced specimen. In this specimen, the values predicted
by the model are much smaller than the measured ones. The disagreement between predicted
and measured moduli is due to the fact that the model assumes a dilute concentration of
particles. The plots in Figs. 2 and 3 also indicate that the increase of the moduli deviates from a
linear relationship towards higher values of volume fractions of reinforcement. This behavior
may be attributed to particle interactions when the mean-free-pathlength between them is
reduced as their volume fraction is increased.

The measured elastic anisotropies found between the directions in the plate and that normal to
the plate can be explained by the metallurgical investigations where it is observed that the area of
the particles in the compression direction is slightly larger in the compression direction than that
in the plane of the plate. This suggests that the particles have the shape of spheroids and that
they tend to align during the compression such that their c-axes coincide with the compression
direction. The alignment of the particles results in a higher elastic stiffness in the plane of the
plate which agrees with the measured elastic properties. The metallurgical investigations also
show that the aspect ratio is only slightly less than one. According to calculations by Ledbetter
and Datta, such a low aspect ratio does not result in elastic anisotropies as large as they are
found in the investigated MMCs which are approximately 5%. Calculations assuming an aspect
ratio of 0.8 predict an anisotropy of the order of 1% for the Al 6061 matrix reinforced with 25%
SiC.
 149

160

α Ε11
♦ Ε22
Δ Ε33
Ε cale.

10 20 30
Volume percentage of SiC

Fig. 2. Measured and calculated Young's moduli in the Al 6061 MMC specimens
as a function of volume percentage SiC.

as
a.
a G12
O
♦ G13
c/>
"O Δ G23
O
G cale.
E
k_
aj
Φ
sz
CO

10 20 30
Volume percentage of SiC

Fig. 3. Measured and calculated shear moduli in the Al 6061 MMC specimens
as a function of volume percentage SiC.
150

Table 4. Calculated and measured Young's and shear moduli of the squeeze cast MMC
specimens. Moduli are shown in units of [GPa].

MMC Al 123 + 23% AbCh Al 13 + 19^Al2Û3 AI 1100 + 1$% AI2Q3

Modulus calc. meas. calc. meas. calc. meas.

Ell 102.2 101.9 94.9 97.1 88.0 86.4

E22 102.2 102.0 94.9 97.2 88.0 88.2
E33 99.6 100.7 92.1 94.3 85.0 83.9

G12 38.8 38.4 35.9 36.9 33.5 32.8

G13 37.4 37.8 34.4 35.2 31.9 31.0
G23 37.4 38.2 34.4 35.8 31.9 31.1

Measurements in the unreinforced material have shown that the texture present influences the
elastic properties significantly. Here, the texture accounts for a 4% higher Young's modulus in
the compression direction. Thus, it seems reasonable to consider that the texture is responsible
for the major part of the anisotropy observed in the reinforced specimens.

Squeeze Cast MMCs

In the squeeze cast specimens, the alumina fibers are randomly oriented in one plane whereas
the alumina particles are also homogeneously distributed. The elastic moduli along the principal
axes of the composites are predicted using a model which assumes the composites to be
comprised of an effective matrix consisting of the pure aluminum and the homogeneously
particles. The effective matrix is then considered to be reinforced with planar-randomly
distributed fibers. The predicted as well as the measured elastic moduli are listed in Table 4. The
results show that the increase in the elastic moduli due to the reinforcement is reasonably well
predicted by the model. A more crucial test of the applicability of this model is its ability to
predict the elastic anisotropy between the directions in the fiber-rich plane and the direction
normal to the plane. Since the fiber content is the same for all three specimens, the anisotropy is
expected to be more pronounced the lower the stiffness of the effective matrix i.e. the lower the
concentration of alumina particles is. This behavior is experimentally observed as shown by the
values of the Young's and shear moduli in Table 4. The difference in the moduli between the in-
plane directions and the normal direction is less pronounced the higher the stiffness of the
effective matrix becomes. Quantitatively, the measured anisotropies are well predicted by the
model.The model, however, assumes that there is no interaction between particles and fibers
and therefore it is more suitable for composites with low particle content.

ACKNOWLEDGEMENT

This work is sponsored by the Army Research Office under contract No. DAAL03-88-K-0096.

REFERENCES

Budiansky, B. (1965), / . Mech. Phys. Solids, 13, 223.

Chow, T.S. (1977), / . Appl. Phys., 48, 4072.
Christensen, R.M. and Waals, F.M. (1972), / . Comp. Mater., 6, 518.
Eshelby, J.D. (1957), Proc. Roy. Soc. (London), 241A. 376.
Grelsson, B. and Salama, K. (1990), Res. Nondestructive Evaluation, 2, 83.
Hashin, Z. and Rosen, B.W., (1964), / . Appl. Mech., 31, 223.
Hill, R. (1964), / . Mech. Phys. Solids, 12, 199.
Ledbetter, H.M. and Datta, S.K. (1986), / . Acoust. Soc. Am., 79, 239.
Salama, K. and Ling, C.K. (1980), / . Appl. Phys., 51, 1505.
 WS10C4

STRAIN RATE EFFECTS ON VOID NUCLEATION BY INCLUSION DEBONDING

A. NEEDLEMAN

Division of Engineering, Brown University, Providence, RI 02912 USA

ABSTRACT

The effect of imposed strain rate on the initiation of debonding is analyzed numerically for
rigid spherical inclusions in an elastic-viscoplastic matrix subject to uniaxial tension with a
superposed hydrostatic stress. The analyses are based on a cohesive zone type model that
permits the prediction of interfacial decohesion without the necessity of introducing some
additional failure criterion. Since the mechanical response of the interface is specified in
terms of both a critical interfacial strength and the work of separation per unit area,
dimensional considerations introduce a characteristic length. For the conditions analyzed, the
strain rate dependence of the debonding initiation strain is found to increase with increasing
inclusion size.

KEYWORDS

Ductility; void nucleation; damage; finite element analysis

INTRODUCTION

Void nucleation from inclusions and second phase particles plays an important role in
limiting ductility and toughness in structural metals. In order to analyze such phenomena, a
theoretical framework is needed that can describe the evolution from initial debonding
through complete separation and subsequent void growth. A finite strain, cohesive zone type
interface model, Needleman (1987), provides one such framework. In this formulation,
constitutive relations are specified independently for the material (or materials) and the
interface. The constitutive equation for the interface is such that, with increasing interfacial
separation, the traction across the interface reaches a maximum, decreases and eventually
vanishes, permitting complete decohesion to occur. Dimensional considerations introduce an
151
152

interface characteristic length into the formulation, so that the predicted behavior depends on
the ratio of the inclusion size to this characteristic length. The boundary value problem
analyzed in this study is the same as in Needleman (1987, 1990a), which simulates a periodic
array of spherical inclusions in an isotropically hardening elastic-viscoplastic matrix.
Attention here is restricted to the initiation of debonding and is focussed on how the strain to
initiate debonding varies with strain rate.

INTERFACE MODEL

An exponential form for normal separation, as suggested by atomistic calculations, Rose et al

(1981), is used in conjunction with a linear shear dependence. The interfacial tractions are
derived from a potential, which is taken to depend only on the displacement difference across
the interface. In two dimensions, the interfacial tractions (force per unit initial area) are
specified by, Needleman (1990b),

T -CT
un 1 (1)
n - maxe z .6 '2

(^)]exp[-z(|)]
T t = - a „max<e · 'ocz
—■-' ' — ' -'—' ' (2)

where z=16e/9=4.83, with e=exp[l].

Here, n and t refer to directions normal and tangential to the interface in the r-z plane of a
polar coordinate system, and u n and u^ are components of the displacement difference across
the interface. The orientation of n is chosen so that positive u n corresponds to increasing
interfacial separation. From (1) and (2), the work of separation is

<t>sep = 9 c T max s / 1 6 (3)

The interface is characterized by three parameters; the strength a m a x , the work of separation
φ δ6 ρ, and the shear parameter a, which gives the ratio of shear stiffness to normal stiffness at
u n = 0. The values of a m a x , <|>sep and a are taken to be constant along the interface,
although in principle they can be functions of position to account for variations in cohesion.
The characteristic length δ, which is not necessarily equal to the physical interface thickness,
is defined from (3) as ö=16<t>sep/(9amax). Larger values of δ give rise to a more ductile
mode of debonding, Needleman (1987).

Figure 1 shows the normal traction, T n , as a function of u n with u t = 0. At u n =5, - T n / a m a x

=0.1. In more general circumstances, where u t is not identically zero, the curve of T n versus
u n depends on u^. However, regardless of the history of u t , the work of separation is given
by (3), since there is an interface potential.
 153
1.5

1.0

0.5
3
I
> 0.0
I
-0.5

-1.0

-1.5
-0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2
Un/<5

Fig. 1 Normal traction across the interface, T n , as a function of

un, with ut=0.

PROBLEM FORMULATION
Numerical, full field solutions to the quasi-static initial/boundary value problem are based on
a Lagrangian formulation of the field equations. The independent variables are taken to be
the particle positions in the initial, stress free configuration and time. Both finite strains and
rotations are accounted for. In the current configuration the material point initially at X is at
x. The displacement vector u and the deformation gradient F are defined by

u = x-X F = | f <4>
aX
The principle of virtual work is written as

/ s:5F dV + / (Tn ôun+Tt ôut) dS = / Τ·διι dS (5)

v
$int $ext

where V, Sext and Si nt are the volume, external surface and internal, interface surface,
respectively, in the reference configuration, s is the unsymmetric nominal stress tensor (force
per unit reference area) and T=ns, with n the surface normal.

An axisymmetric circular cylindrical cell containing a spherical rigid inclusion is analyzed.

The deformations are restricted to be axisymmetric, the circular cylindrical cell is required to
remain a circular cylinder throughout the deformation history and, within each cell, symmetry
154
is assumed about the cell centerline. Using polar coordinates r and z, the boundary conditions
on the region analyzed numerically are

(6)
u z = 0, T r = 0 onz = 0

u
(7)
z = %ve (Lo +uz)» T r = 0 on z = L 0

u
r = v l · T z = 0 onr = R0 (8)

where (') denotes 9( )/dt and Vi is determined from the condition that the average lateral
stress on r=R0, ΣΓ, is equal to ρΣζ, where Σ ζ is the average tensile stress. The triaxiality of
the imposed stress state, the ratio of hydrostatic stress to Mises effective stress, is given by
(l+2p)/3|l-p|. The cell geometry is specified by L 0 = R0, the radius of the rigid spherical
particle is r 0 and ù=0 on v r2+z ^= r o· From (7), eave=ln(l+uz/L0).

Although it is convenient to phrase the principle of virtual work (5) in terms of the nominal
stress tensor s, the plastic flow rule is more conveniently expressed in terms of a measure of
force per unit current area. The flow rule will be written in terms of the Kirchhoff stress τ=
Fs. The rate of deformation tensor, D, is written as De+DP, with

Λ 1+V o V o fQ\
(9)
De = — τ - - ( τ : Ι ) Ι

Here, E is Young's modulus, v is Poisson's ratio, I is the identity tensor and τ is the Jaumann
derivative of Kirchhoff stress.
The flow rule for an isotropically hardening Mises solid is

DP.-?»-,·
2σ6

where τ is the Kirchhoff stress de viator, given by τ^τ-σ^Ι, with σ[1=τ:Ι/3, έ ρ is the effective
plastic strain rate and σ6 =Λ/3τ:τ/2.

The material strain hardening and strain rate hardening behavior is described by

êp=èo(ae/g)1/m g=a0(ep/e0+l)N (11)

Calculations are carried out using Ε/σ0 = 300, v = 0.3, N=0.1, m=0.01, ε 0 = σο/Ε=0.00333,
and prescribed strain rates e a v e in (7) equal to έ0, 10^ έ0, and 10^ έ 0 .
 155
Numerical solutions are obtained using the finite element method described in Needleman
(1987). A 16x24 quadrilateral mesh is used, with each quadrilateral composed of four
triangular linear displacement elements.

RESULTS

Figure 2 shows the results for the four circumstances analyzed. In all calculations here the
interface strength is fixed at c m a x Aj 0 =3 and the interface shear parameter is specified as a
=1. The ratio of inclusion radius to cell radius, TQ/RQ, is 0.25 so that the inclusion volume
fraction is 1.04 per cent. With p=0.4, the ratio of hydrostatic to Mises effective stress is 1.0,
while with p=0.625, this ratio is 2.0. If E is identified as 207 GPa, which is a representative
value for steels, then Ε/σ0 = 300 corresponds to σ 0 = 690 MPa and c m a x =3 σ 0 = 2.07 GPa.
With δ = 5xl0 -1 ^ m, an arbitrary but plausible choice for iron carbide particles, o7r0 = 0.02,
0.005 and 0.002 correspond to inclusion radii of 0.025xl0"6 m, 0.1xl0"6mand 0.25xl0"6
m, respectively, and from (3), φ^ρ = 0.58 J/m^.

0 . 1 5 I ' ■ ii i i M 1111 i i Ί — i i i 1111| · i ·i i i i 1111| ■ i · i i i i i 1111 ■ i · i — i i i i u i| i i I I —i i i i mi

2 2 2 2 2 2
100 loi 102 103 104 105 ιοβ

Normalized Strain Rate

Fig. 2 Debonding strain, ε^η^, versus normalized strain rate,

é a v e / έ 0 , for the four situations analyzed.
The debonding strain, edbn(j, is identified with the value of e a v e at which the maximum
normal displacement around the inclusion reaches the interface characteristic length δ, or the
value of e a v e at which the overall stress-strain curve reaches a maximum, so that further
debonding occurs under decreasing e ave . This latter situation corresponds to a brittle mode
156

of debonding, as discussed in Needleman (1987). Here, the brittle mode of debonding occurs
for the two larger inclusion sizes, 5/r0 = 0.005 and 0.002. With 6/r0 = 0.02, for both p=0.4
and p=0.625, debonding occurs with increasing overall strain, e a v e . The variation with
inclusion size, with the triaxiality parameter p fixed at 0.4, is seen by comparing the results
for 6/r0 equal to 0.02, 0.005 and 0.002. The effect of stress triaxiality, at fixed inclusion size,
is seen by comparing the curves for δ/Γο=0.02 at p=0.4 and p=0.625.

In order to quantify the strain rate sensitivity, the curves in Fig. 2 were fit to a linear log-log
relation of the form log[ed5 n( i(ê ave )/e(jbncj(è0)]=K log[é a v e / έ 0 ]. Since, there are three
points on each curve, each curve consists of two line segments. For the three curves with
p=0.4, the values of K differ by less than 5 per cent between these two segments. For
δ/Γο=0.002, 0.005 and 0.02, the values of K are -0.085, -0.082 and -0.067, respectively.
Although the difference between these three values of K is not large, there is a clear trend for
increased strain rate sensitivity of the debonding strain with increasing inclusion size (i.e.,
with smaller values of δ/Γ0). The linear fit is not quite so good for the case with 6/ro=0.02

and p=0.625. Between e a v e / έ 0 =1 and e a v e / έ 0 = 10^, K=-0.028, while between e a v e / έ 0

1θ3 and e a v e / έ 0 = 10^, K=-0.025. The increased stress triaxiality gives smaller values of
e
dbnd» a s expected. In addition, the strain rate dependence of e ^ n d *s * e s s t n a n f° r a n v °f
the cases with p=0.4.

ACKNOWLEDGEMENT

The support provided by the Brown Materials Research Group on the Micromechanics of
Failure Resistant Materials, funded by the U.S. National Science Foundation, is gratefully ac-
knowledged. The computations reported on here were carried out on a Stardent GS 2000
computer.

REFERENCES

Needleman, A. (1987). A continuum model for void nucleation by inclusion debonding. J.

AppLMech., 54, 525-531.

Needleman, A. (1990a). A numerical study of void nucleation at carbides. In: Innovations in

Ultrahigh-Strength Steel Technology, Proceedings of the 34th Sagamore Army
Materials Research Conference, (ed. by G.B. Olson et al), U.S. Government
Publication, pp. 331-346.

Needleman, A. (1990b). An analysis of decohesion along an imperfect interface. Int. J.

Fract, 42, 21-40.

Rose, J. H., Ferrante, J. and Smith, J.R. (1981). Universal binding energy curves for metals
and bimetallic interfaces. Phys. Rev. Letts., 47 675-678.
WS10d2

CAST 6061 Al-SiCp COMPOSITES :

PREPARATION AND PROPERTIES

M. Vasudevan and M.K. Surappa

Department of Metallurgy,
Indian Institute of Science,
Bangalore 560 0 1 2 , India.

ABSTRACT

Aluminium alloy (6061) - SiC particle composites containing upto

15 w t % SiCp have been prepared by direct casting technique. Pre-
treatment of alloy ingots prior to melting and additions of
small amounts of Magnesium and Zirconium (Mg + Zr < 1 wt%)
found to aid wettability and bonding between the matrix and
reinforcement. Increase in the elastic moduli of composites
compare well with the predicted values using the modified Tsai-
Halpin equation.

KEYWORDS

Metal Matrix Composites; Cast 6061 Al-SiCp; silicon carbide

particulates.

INTRODUCTION

In recent years aluminium alloy composites containing

particulates and whiskers of silicon carbide are the most widely
researched Metal Matrix Composites (MMCs) system. These light
weight composites are potential candidate materials for a wide
variety of applications. They are envisaged for use in
structural,transport (ground and aerospace), antenna, and
leisure applications. Profound importance of these composites
could be traced to their higher stiffness, superior room and
elevated temperature strengths, improved wear resistance and low
co-efficient of thermal expansion (Divecha §_t a l . , 1981; Surappa
and Rohatgi, 1981a; Mi liiere and Suery, 1 9 8 8 ) .

Several processing routes have been reported on the production

of aluminium alloy composites reinforced with silicon carbide

157
158
(both whiskers and particles) (Divecha et. a l . . 1981; Surappa and
Rohatgi,1981a; Fukunaga and Goda, 1985; Mi M e r e and Suery, 1988;
Schuster et. a l , . 1988; Field, 1988; Willis, 1 9 8 8 ) . Of these
methods, most widely employed are powder metallurgy (PM) and
casting routes. Relative merits of these two methods in terms
of achievable properties are being debated (Arsenault and Wu,
1988; Nordone and Prewo, 1 9 8 9 ) . Nonetheless casting route is
cheap and easily adaptable. Several variations of casting
route viz, compo casting, liquid pressure forming, spray casting
and squeeze casting have been tried successfully to synthesise
Al-SiCp and A l - S i C w and Al-SiCf (short fibers) composites.
However, to date not much work has been reported on the
processing of aluminium alloy composites containing large volume
fraction of silicon carbide particles using conventional casting
route, except that of Durail's process(Schuster et^ al. , 1987).
Durai l's is proprietory method and the details are not reported.
Hence the present work details the process for fabrication of
aluminium alloy composites containing upto 15 w t % silicon
carbide particles (av.size 54 *im) and their properties.

EXPERIMENTAL
Material s

Composition of matrix alloy and the reinforcement (α-SiCp) used

in the present study are shown in tables la. and lb.
respectively. -250 and + 350 mesh (av.size 54 jim) oc-SiC
particles were used as reinforcing phase .

Table la. Composition of the matrix alloy

(weight percent)

Al loy Cu Mg Si Cr Mn Al

6061 Al 0.25 1.0 0.6 0.25 0.03 rem.

Fabrication of Composites

Composites were prepared by dispersing pre-treated SiCp in

molten alloy using vortex method (Surappa and Rohatgi, 1981b).
Alloy was melted under a cover of nitrogen atmosphere. Just
prior to melting ingots were treated with warm alkaline solution
and washed with mixture of acids. This treatment is expected to
help in reducing the thickness of oxide film in the melt during
composite processing. SiC particles pre-heated to 900°C were
added into the melt in a stream of N2- Melt was alloyed with
small amounts of magnesium and zirconium (Mg + Zr < 1 w t % ) . Melt
was degassed with nitrogen before and after dispersion of SiCp.
Composite melts were poured into cylindrical cast iron moulds
(75mm dia and 150mm h t ) . In all the cases residence time of SiCp
in the melt was maintained between 10 and 15 minutes. For the
 159
purpose of comparison base alloy was cast after adding similar
amounts of magnesium and zirconium (Mg + Zr < 0.1%) into 6061
alloy melt.

Table lb. Composition of SiC particle

Constituent wt%

SiC 98.8

Si02 0.75

Carbon 0.40

Α12θ3 0.20

Si 0.60

Fe203 0.05

Extrusion

50 mm dia composite castings were homogenized at 540 C for 3

hours and extruded at 500 C into 16mm dia rods. The extrusion
ratio obtained was 10:1.

Modulus Measurement

The elastic moduli of the composites and base alloy were

measured using a resonance technique (Analysing the vibrational
behaviour of the samples following an impulse excitation)
(Chakraborty et a l . , 1989).

RESULTS AND DISCUSSION

Fabr ication of Composites

Generally silicon carbide particles are not wetted by molten

aluminium or aluminium alloys at a temperature of 750 C and as a
result their retention in the melt is not possible with a
mixing time of around 15 minutes. However, in the present study
it was possible to introduce upto 15 w t % SiCp in molten 6O6I
alloy and produce composite castings. This could be attributed
to improved wettability between SiC and molten alloy for the
following reasons : Use of small amounts of alloying elements
(Magnesium + Zirconium < l w t % ) , pre-treatment of ingots prior to
melting, and maintenance of nitrogen atmosphere during
processing of composites.

Additions of small amounts of magnesium and zirconium improve

the wettability between molten Al alloy and S i C p and this is in
agreement with the results of Oh et al. (1989) and Choh et al.
160
(1987). Similarly lower contact angle between graphite substrate
and molten aluminium has been reported when the latter was
pickled with NaOH, prior to contact angle measurements.
Eustathopoulos et al. (1974) attribute this to the formation of
oxide film of decreased thickness in aluminium droplet when
melted. In the present study it is possible that, treatment of
ingots prior to melting has caused reduction in oxide film
formation and concomitant improvement in the wettability.
Thirdly, Oh et al. (1989) report increased wettability between
molten aluminium and particulates of SiC and B4C in argon
atmosphere compared to air atmosphere. Hence, in the present
study use of N2 atmosphere has further aided in the improved
wettability between molten Al alloy and S i C p . Overall, the
processing conditions employed in the present study have
facilitated in the successful fabrication of composites.

Microstructure

Fig.l (a & b) shows the microstructure of aluminium alloy

composites containing 15 w t % S i C p both in as cast and extruded
state.

Fig. la. Micrograph of 6061 w t % S i C p composites

in as cast state 30X.

As cast composites exhibited some degree of porosity and

occasionally particles are clustered (Fig.la). Most of the pores
have been eliminated by extrusion. Appreciable change in the
uniformity of dispersion of SiCp was observed as a result of
extrusion (Fig.lb). SEM photographs of composites (Fig.2) show
good bonding between dispersed SiC particles and the matrix.
Void or other discontinuities were not observed at particle-
matrix interface.

Elastic Modulus

Elastic modulus of composites containing different amounts S i C p

are shown in Fig 3. Calculated modulus values of composites
using the rule of mixture and also the following modified Tsai -
Halpin (1984) equation
 161

Fig. Ib. Micrograph of 6061 Al-15 w t % S i C p

compositses in the extruded condition
30X.

Fig. 2. SEM photograph of 6061 Al-15 w t % S i C p

Ec = Em (1+2 Sq Vp) / (1-q Vp) (1)

are also shown in the same plot. In the equation (1) S refers to
aspect ratio of S i C p and its value is taken to be 2 in the
present study. The value of q is obtained from the expression,

q = (Ep /Em-1) / (Ep/Em+2S) (2)

It is evident that composite modulus predicted by the rule of

mixture overestimates the experimentally observed values.
However, values calculated using modified Tsi-Halpin equation
agree well with the experimental results.
162

110
'a

ê loo

ο
Σ
^! 80
I—
< Rule of mixtures
ω 70 TSi- Halpin eqn.
O Experimental point
60 .
0 A 8 12 16
WEIGHT PERCENT, SiCD
Fig. 3. Variation in elastic modulus of the
composite with w t % S i C p content
CONCLUSIONS

Aluminium alloy containing upto 15 W t % Silicon carbide

particles can be produced by dispersing pre-treated Silicon
carbide particles in molten alloy by Vortex technique.
Additions of Mg and Zr aids the dispersion of S i C p .

Increase in Elastic moduli of composites agree well with the

values predicted using modified Tsai-Halpin equation.

ACKNOWLEDGEMENTS

Authors thank ARDB for providing the financial support.

REFERENCES

Arsenault, R.J. and S.B.Wu (1988). Scripta Met., 22^, 767-772.

Chakraborty,A., S.B.Bhaduri, J.J.Reddy, R.Mohan Rao and
Y.R.Mahajan (1989). Proc. ICF-7, Advances in Fracture research
(eds) K.Salama et a l ; 2705.
Choh T., and T.Oki (1987). Mater.Sei. and Tech.; 3, 378 - 3 8 5 .
Divecha A . P . , S.G.Fishman and S.D.Karmarkar (1981). J.Metals,
33, 12 - 17.
Eustathopoulos N., J.C.Joud, P.Desre and J.A.Hicter (1974). J.
of Mat.Sei; 9, 1233-1242.
Field M. (1988). Foundry Trade Journal, 593-595.
Fukunaga H. and K.Goda (1985). Bulletin of Japan, Society for
Mechanical Engineers, 2 7 , 1245.
Halpin J.C. (1984). Primer on Composite Materials: Analysis,
Tech. Pub Co.
Milliere C M . and M. Suery (1988). Mat. Sei. and Tech; 4, 41-51.
Nardone V.C. and K.M.Prewo (1989). Scripta Met, 2 3 , 291-292.
Oh S.Y., J.A.Cornie and K.C. Rüssel (1989). Met. Transactions,
20A. 5 2 7 - 5 4 1 .
Schuster D.M., M.Skibo and F.Yep (1987). J.Metals,39 60-61.
Surappa M.K. and P.K.Rohatgi (1981). J.Mat Sei., 16 983
Surappa M.K. and P.K.Rohatgi (1981). Metals Tech., 4, 41 - 4 3 .
Willis T.C. (1988). Metals and Materials, Aug, 4, 85-488.
WS10d3

PREPARATION AND PROPERTIES OF INTERMETALLICS DISTRIBUTED

MATRIX COMPOSITES BY REACTION SQUEEZE CASTING

HIDEHARU FUKUNAGA and XIAOGUANG WANG

Department of Mechanical Engineering, Hiroshima University

Kagamiyama 1-4-1, Higashi-Hiroshima, 724 Japan

ABSTRACT

Using Ti02 anatase whiskers as the reinforcement and aluminium as the matrix mater-
ial, the reaction squeeze casting has been carried out to make the intermetallics
distributed matrix composites. Fabricated RSC samples showed α-Α1 2 0 5 4-TiAl or A1 +
a-Al 2 0 3 +TiAl + TiAl 3 +Ti0 2 presented in the microstructure, and their hardnesses
were Hv 1050 to 70. The reactions at the temperature during RSC process were favored
by thermodynamics and were exothermic reaction. The differential scanning calorime-
ter curve showed the reaction initiated explosively, achieved 1100°C, and continued
for several seconds in the first period. At some RSC process conditions, the reac-
tions proceeded uncompleted and the stratified structures were formed, even the
calculation of the complete reactions leads to a Vf of 41% Ti0 2 for a-Al 2 0 ? +TiAl
or of 32% for α-Α1 2 0 3 +Τ1ΑΙ3 formations.

KEYWORDS

Titanium dioxide; MMCs; intermetallic compound; composites; reaction; squeeze cas-

ting.

INTRODUCTION

The reaction squeeze casting (RSC) is a new concept to make use of the reaction
between the matrix and reinforcement for the fabrication of new metal matrix compo-
sites (MMCs) in a converse way to the traditional opinion how the reaction could be
avoided in the fabrication process (Fukunaga et al., 1990, 1991). Using the RSC pro-
cess, the anatase (Ti0 2 ) whiskers were used as the reinforcement and molten pure
aluminium was employed as the matrix because of their reactivity in the present
study. The characteristics of the RSC process, the reaction products and their
properties were investigated. The results should serve as a useful basis for the ef-
fective design and development of the intermetallics distributed matrix composites.

163
164

Ο^Molten AI
O
Preform

Thermocouie

Fig. 1. Outline of reaction squeeze casting apparatus.

EXPERIMENTAL PROCEDURE

The anatase (Ti02) whiskers having diameter of 0.05 to 1.0>um, length of 5 to 10//■,
density of 3.72 Mg/ra3 and hardness about Hv870 were used as the reinforcement mater-
ial, and aluminium of 99.99% purity was used as the matrix material. The whiskers
were previously pressed to the preform in diameter of 43mm, height of 15mm and the
certain volume fractions of fiber(Vf) using a plunger/sleeve die before the RSC pro-
cess. As shown in Fig.l, the preform was set into the preheated metal die, and heat-
ed to a given temperature, the molten pure aluminium was poured into the die cavity
and squeezed into the preform at a low speed by the plunger at a certain pressure.
The full size of the fabricated samples which was 45mm in diameter and 80mm in
length, were cut to required shape and size for the specimens after the RSC process.
The process conditions are listed in Table 1.

The CA thermocouples with a diameter of 0.2mm were embeded in the preform and the
heat characteristics of the RSC process were meassured using a differential scan-
Table 1. Conditions of the RSC process.

No. Vf«) T«,(°C) TD(°C) Tf(°C) v(mm/sec) P(MPa) r(sec)

1 30 800 410 340 10 100 60

2 47 750 350 300 10 100 60
3 15-47 720-890 340-600 5-20 50-150 60-90
4 47 840 340 10 150 90

No.; process condition mark, Vf; volume fraction of fiber, T A 1 ; pouring

temperature of molten aluminium, T D ; die temperature, T f ; preform tem-
perature, v; plunger speed, P; final squeeze pressure, r; chill time
under hydrostatic pressure.
 165

Fig. 2. Microstructure of reaction squeeze casting products,

consisting of four phases, A, B, C and D.

ning calorimeter(DSC). Optical and scanning electron microscopy(SEM), X-ray difrac-

tion analyser(XRD), micro-XRD and electron probe X-ray microanalyser(EPMA) were used
to examine the morphology and structure of the product phases, the indentation hard-
ness was measured with a Vickers microhardness tester.

RESULTS AND DISCUSSION

With the process condition of No.l in Table 1, the microstucture is shown in Fig.2
for the fabricated RSC sample. There are four parts, that can be classified to sec-
tion A, B, C, and D, but the A and B is continued at the optical micrograph. The
microhardness test of loading 500g shows that the hardness Hv is about 1050 on the
section A, 1050 to 300 on the B, about 990 on the C and 430 to 30 on the D. From the
XRD, micro-XRD and EPMA analysis, it was identified where exist almost α-Α1 2 0 3 +
TiAl in the section A, and A1+ a-Al 2 0 3 +TiAl + TiAl5 +small amount of Ti0 2 through
all the area of the section B, C and D. As a comparison, the hardness of some sub-
stances are listed here (Mondolfo, 1976; Richerson, 1982; etç_.), AI: 17 to25, cr-
A1 2 0 3 : 1600 to 2700, TiAl: 180 to 220, TiAl 5 : 400 to 700. It can be regarded as the
formation of reaction products a-Al 2 0 3 + TiAl(TiAl 3 ), that such a high hardness has
been measured.

According to thermodynamics, the following reaction equations can be written, consi-

dering the free energy changes for possible reaction products between reinforcement
Ti0 2 and matrix aluminium and Al-Ti phase equilibrium (Swalin,1962; Broutman et al.,
1974; etc.):

^Al + Ti0 2 = - | A l 2 0 3 + Ti, AG,, ΔΗ, (1)

Ti + Al = TiAl, AG 2 , ΔΗ 2 (2)

TÎ + 3A1 = TiAl 3 , AG 3 , ΔΗ 3 (3)

166

Kiuur

10 20 30 40
Time (sec)

Fig. 3. DSC curve showing the reaction initiated explosively

and continued for several seconds in the first period.

Here A G i , A G 2 and A G 3 are the free energy and Δ Η ι , Δ Η 2 and Δ Η 3 are the enthalpy
of the reactions (1),(2) and (3). At the standard state the values can be determined
quantitatively, for instance A G t = -268.8 + 0.0966T (KJ), where T is the temperature
(°C) of the reaction. The standard free energy and enthalpy for (1) to (3) has nega-
tive value by the calculation at 660°C, for instance AGi = -205.04KJ, Δ Η 2 = -23.82
KJ. The reactions proceed, and they are exothermic reaction at the RSC process tem-
perature. From (1) to (3), the following reaction equations can be written:

^ A l u ) + T i 0 2 < s ) = fAl 2 0 3 , s ) +TiAl ( s ) , AG4, Δ Η 4 (4)

^Al(,,+Ti0 2 ( a , = fAl 2 03(3)+TiAl3(s>, AG5, Δ Η 5 (5)

and they are also favored by thermodynamics and are exothermic reaction at the stan-
dard state.

Figure 3 shows the time-temperature curve of the RSC process from the differential
scanning calorimeter analysis at the process condition No.2 in Table 1. The tempera-
ture of the meassured point in the preform achieved 1100°C from 300°C within one
second while the squeeze pressure was applied, and maintained the high temperatures
for several seconds. From the calculation of the heat conduction in the RSC process
(Fukunaga, 1988), the whiskers achieve the mixing temperature less than 0.01 second
when molten aluminium contact them. It could be confirmed that the reaction initiat-
ed explosively while the molten aluminium was infiltrating into the preform, and
continued in the first period of several seconds. The reactions (1) to (5) proceed
and they are exothermic reaction even at the non-standard state of the RSC process.

The calculation of the complete reactions leads to a Vf of 47% Ti0 2 required and a
volume contracton of 16.9% for equation (4), to a Vf of 32% and a volume contraction
 167

Fig. 4. SEM photograph of the section A in Fig.2.

of 13.8% for equation (5). It has been found that the height of the RSC composites
was decreased remarkably than the prepared preform height, in the case of low Vf at
the condition No.3 in Table 1, and the shell with the thickness of about 2mm whose
microstructure was same as the section A in Fig.2 formed at the area adjacent to the
aluminium. It could be explained that the flow gaps got narrow because the solid
reaction products appeared around the whiskers as the molten aluminium was infil-
trating into the preform, and the preform was compressed by the applied pressure.
The compressed preform had a higher Vf and was favor to the reaction (4). Figure 4
shows the SEM micrograph of the section A of Fig.2, a-Al 2 0 3 + TiAl products have a
fine structure. The reaction achieved so complete that aluminium diffraction X-ray
could not be identified by the micro-XRD as shown in Fig.5. On the other hand, the

20 30 40 50 60
26(deg)

Fig. 5. XRD pattern for the section A in Fig.2.

168

Fig. 6. Stratified structure, formed in high volume fraction

of Ti0 2 , Vf = 47%.

stratified structure was formed as shown in Fig.6 even in the case of 47% Vf at the
condition No.4 in Table 1. It could not be found thatvthe uniform structure of the
a-Al 2 0 3 +TiAl products were formed across the section of the whole sample. The
reaction was not complete in the RSC process and the multi-phase, Al + Ti0 2 + α-Α1 2 (Κ
4-TiAl + TiAlj, was identified by the XRD analysis.

REFERENCES

Broutman, L.J. and R.H.Krock (ed.)(1974). In: Composite Materials, Vol.1, pp.285.
Academic Press, New York.
Fukunaga, H.(1988). In: Cast Reinforced Metal Composites ( S.G. Fishman and A.K.
Dhingra ed.), pp.101-107. Conf. Proce., ASM, Chicago.
Fukunaga, H., X.Wang and Y.Aramaki (1990). In: Spring Conf. Proce. of Jpn Inst.
Met., pp.99. JIM, Tokyo.
Fukunaga, H., X.Wang and Y.Aramaki (1991). Preparation of intermetallic compound
matrix composites by reaction squeeze casting. J. Mater. Sei. Lett., JJi, 23-25.
Mondolfo, L.F.Q976). In: Aluminum Alloys, pp.68, 385. Butterworths, London.
Murray, J.L.(1986). In: Binary Alloy Phase Diagrams (T.B.Massalski, J.L.Murray, L.H.
Bennett and H.Baker ed.), Vol.1, pp.175. Metals Park, ASM, Ohio.
Richerson, D.W.(1982). In: Modern Ceramic Engineering, pp.81. Marcel Dekker, New
York.
Somiya, S.(ed.)(1989). In: Advanced Technical Ceramics, pp.32. Academic Press,Tokyo.
Swalin, R.A.(1962). In: Thermodynamics of Solids, pp.86. John Wiley & Sons,New York.
Wrzesinski, W.R. and J.C.Rawers (1990). Self-propagating high-temperature synthesis
of TiAl-SiC and TiAl-Al20B intermetallic composites. J. Mater. Sei. Lett., j^, 432-
435.
WS10d4

CHARACTERISTICS OF ALUMINA-SILICA SHORT FIBERS REINFORCED

ALUMINUM ALLOY COMPOSITES

Y.C. FANN, CC. YANG, Y.C. CHEN

Material Research Laboratories , ITRI ,

Hsinchu , Taiwan , R.O.C.

ABSTRACT
After solution treatment , Α356/ΑΙ2Ο3 composite exhibits an enhanced
aging response as compared with A356 unreinforced alloy. No inter-
reaction between AI2O3 fibers and Al matrix are observed under TEM in
A356/AI2O3 composites after as cast and T6 heat treatment. On the
contrary, A356/AI2O3-S1O2 composite shows a degraded aging response
as compared with unreinforced alloy and A356/AI2O3 composite. The
matrix microhardness of A356/AI2O3 composite is almost constant
during aging. Reaction products, which are most likely to be MgO, form
at the interface of fibers and Al matrix in A356/AI2O3-S1O2 composite
after T6 treatment.

KEYWORDS
AI2O3-S1O2 fiber ; Aluminum composite; Squeeze infiltration ; Interface
reaction

INTRODUCTION
Metal matrix composites (MMCs) in aluminium alloy containing a variety
of discontinous reinforcing fibers, offer attractive mechanical properties.
Of increasing interest and practical importance is the developement of
matrix and interfacial microstructure in MMCs in response to heat
treatment. Abis (1988) showed the existence of AI2O3-S1O2 reinforcement
could distinctly influence the aging sequence of an Al-Cu alloy. Friend
(1988) pointed out two factors which degraded the age-hardening
169
170

response of MMCs. The first factor is the chemical reaction between

fibers and high- reactive elements during annealing. The second is an
interaction between quenched-in vacancies and the fiber/matrix
interface. Cappleman(1985) reported that an atomic scale reaction
products were formed at the interface of the δ-Αΐ2θ3/Α1. Nieh and
Karlak(1984) demonstrated that aging response in the matrix of whisker-
reinforced composite could be accelerated compared with those of the
unreinforced matrix subjected to same heat treatment. This was assumed
to result from the large difference in the thermal expansion coefficients
between the matrix and reinforcing material.
To optimize the cost and mechanical performance of discontinously
reinforced MMCs, a detailed examination of microstructure evaluation
and its influence on mechanical properties through heat treatment for
various fibers, are necessary. The present study was conducted to
compare the aging responses and mechanical behavior of δ-Αΐ2θ3 fibers
and AI2O3-S1O2 fibers reinforced aluminum composites.

EXPERIMENTAL
The aluminum matrix used for investigation is A356 alloy which contains
6.8%Si, 0.35%Mg , 0.12%Ti, 0.08%Fe in weight, in addition to Al. The
reinforced fibers are δ-Αΐ2θ3 and amorphous Al203-49wt%Si02 (Isolites
product) with minimal non-fibrous material content. The composites
containing 12 vol% of fiber were manufactured by a squeeze infiltration
method. For comparison, the same heat of molten aluminum was used to
form unreinforced alloye through the identical processing conditions. AU
the specimens were solution treated at 520°C for 3h followed by water
quenching. Aging treatments were carried out in an oil bath set at 175 °C
for different period of time.

Matrix microhardness measurements were conducted on A356/AI2O3

composite, A356/AI2O3-S1O2 composite and unreinforced A356 alloy
using an AKASH1 Hardness Tester. A 136° Vickers diamond indenter and
10 g load were employed. After metallurgical^ polishing, these samples
were indented in fiber free regions to measure the microhardness of the
matrix. More than 10 microhardness values were measured for each
specimen.

The mechanical properties of these materials were assessed by three

point bending test as well as wear resistance test. Microstructural studies
focused on examination of interfaces between fibers and aluminium
matrix by using transmission electron microscopy (TEM) and high
resolution TEM (HRTEM). Wear tests were performed on a pin-on-disk
wear machine under dry sliding. Composite specimens against 52100
steel were carried out under a normal load of 49N. An average of three
tests was used for final result .
 171

RESULTS AND DISCUSSION

The typical optical microstructure of as cast A356/AI2O3 composite and
A356/AI2O3-S1O2 composite are shown in Fig. 1(a) and Fig. 1(b). Both
materials present a fairly uniform distribution of the reinforced fibers.
Only a few areas show inhomogeneity in fiber distribution.TEM
observation, as shown in Fig. 2, revealed that no other reaction products
except silicon particles were observed at the interfaces of fibers and
matrix in the as-cast A356/AI2O3-S1O2 composite. High density of
dislocations as well as subgrains are found in the Al matrix adjacent to
the AI2O3-S1O2 fibers. Similar microstructures except images of fibers
were also observed in the as-cast A356/AI2O3 composite. However, there
is a significant difference on interfacial structures of fibers between
these two composites after being subjected to solution treatment and 3-
hour aging treatment. In A356/AI2O3 composites, there seems to be no
inter-reaction between 5-A1203 fibers and Al matrix. Many fine
precipitates assumed to be Mg2Si are present in the Al matrix. In
A356/AI2O3-S1O2 composites after T6 treatment, some reaction products
form and grow into amorphous AI2O3-S1O2 fibers as shown in Fig. 3.
Selected area diffraction (SAD) patterns , as shown in Fig.4, disclose that
this interfacial product is face-centered cubic (FCC) structure with lattice
constants about 8.2A. In considering the point of thermodynamics and
the stronger reflection in <004> diffraction spots than <002> , the most
likely phase is MgO rather than Mg2Si04 or MgAhQ*. In the Al matrix ,
only a few Mg2Si precipitates are observed. HRTEM observations , as
shown in Fig. 5, reveal that MgO phase grows into the AI2O3-S1O2 fiber.
In front of MgO exists a transition zone. Because the solution treatment
temperature is much higher than the aging temperature , formation of
the MgO must occur after solution treatment instead of during aging
process. As why the MgO phase forms at the amorphous AI2O3-S1O2
fiber and does not form at the 5-Ab03 fibers , is not understood yet.

In the as-cast condition, the matrix microhardness in two composites and

the unreinforced A356 alloy are 70, 66 and 65 DPH (Diamond Pyramid
Hardness) respectively. This data shows that all of these materials have
almost identical hardness in the matrix at as-squeezed condition. The
typical scatter in the Vickers DPH microhardness values was ± 9 % for all
the reinforced and unreinforced alloys. Figure 6. shows the age-
hardening response at 175°C for two composites and unreinforced alloy.
All the microhardness were measured for the AI matrix. With the
presence of δ-Αΐ2θ3 fibers, the peak-aging time is reduced to about 3h
and an immediate response of aging is noticeable with matrix
microhardness increasing from 70 to 106 DPH in the first 3h. In
considering the shape of aging curves of A356/AI2O3 composite and
unreinforced A356 alloy ,they are basically similar. However,
A356/AI2O3-S1O2 composite exhibits a very different aging response with
172

the microhardness being almost constant at 48-53 DPH. These values are
apparently lower than that of unreinforced A356 alloy at peak aging
condition. The bending test results of A356/AI2O3 composite,
A356/AI2O3-S1O2 composite and the unreinforced A356 alloy before and
after heat treatment are summerized in Table 1. The results show a
dramatic drop in the maximum load to failure for A356/AI2O3-S1O2
composite subjected to solution treatment compared with the other two
materials. The wear tests for the A356/AI2O3 composite and A356/AI2O3-
S1O2 composite expressed by the length loss v.s. sliding distance are list in
Table 2 . These datas are calculated after the run-in stage. In the T6
treatment of A356/AI2O3-S1O2 composite , because certain amount of Mg
in the matrix are already consumed after solution treatment due to
formation of MgO , precipitation of Mg2Si during aging must be affected
and prohibited. This results in degradation of mechanical properties and
no aging hardening effect in A356/AI2O3-S1O2 composite during T6
treatment unless the solution treatment is avoided.

CONCLUSION
In the as-cast condition, no inter-reaction at the interfaces of fibers and
Al matrix in both A356/AI2O3 and A356/A1203-SÎ02 composites are noted.
However , reaction products proved to be MgO form at the interfaces of
amorphous AI2O3-S1O2 fibers and Al matrix in the A356/AI2O3-S1O2
composite after T6 treatment. The MgO phase particles are found to grow
into AI2O3-S1O2 fibers. After aging, A356/AI2O3 composite exhibits
improvement in hardness and bending strength in comparison with
unreinforced A356 alloy. However, A356/AI2O3-S1O2 composite shows
poor properties in bending strength and wear resistance. Formation of
MgO at the interfaces between fibers and matrix will result in loss of Mg
in the matrix during solution treatment. This seems to be responsible for
the degradation of mechanical properties of A356/AI2O3-S1O2 composite.
It is suggested that A356/AI2O3-S1O2 composite should be used without
solution treatment.

ACKNOWLEDGMENTS
The authors gratefully acknowledge the financial support provided by
the Ministry of Economic Affairs, Republic of China,under contract
number 33A2100 to ITRI.
REFERENCES
Abis , S. and G. Dongelli , J. Mat. Sei. Let. 7, 51(1988)
Cappleman , G. R. , J. F. Watts and T. W. Clyne , J. Mat. Sei. 20,2159(1985)
 173

Christman ,T. and S. Suresh , Acta Metall. Vol.36, No. 7, P. 1691 (1988)
Friend , C. M. , I. Horsfall , S. D. Luxton and R. J. Young ' Proc. of Int
Symp. on Advances in Cast Reinforced Metal Composite, P. 309, published
by ASM INTERNATIONAL (1988)
Nieh , T. G. and R. F. Karlak , Scripta Metall. 18(1984) 25

(a) <b>

Fig.l Optical micrographs of cross section from (a) A356/AI2O3 composite

and (b) A356/AI2O3-S1O2 composite .

Fig.2 TEM microstructure of as-cast A356/AI2O3-S1O2 composite, where

no evidence of reaction at the interface between fiber and matrix is
noted..
174

Fig.3 The interface of A356/ AI2O3-S1O2 composite subjected to solution

treatment and a 3h aging treatment ,where MgO form, (shown by arrow)

Fig.4 SAD pattern from reaction product at the interface between AI2O3-
S1O2 fiber and matrix, where (a) is <110>,(b) is <111. and (c) is <112>Fig.6
Age hardening response for A356/AI2O3 composite,A356/Al203-Si02
composite and unreinforced alloy.

Table 1 Results of Three-Point Bending Test

Maximum Load to Failure (N)

Matrix Condition A356/A1 O A356/A1203 A356

2 3

As-Cast 281 243 230

Solution 275 164 218

Peak-Aged 368 - 287

 175

Table 2 Steady State Wear Rate of Composites

Wear Rate (mm/m)

Matrix Condition A356/A1203 A356/AI O -SiOl
2 3 2|
As-Cast 5.4xl0' 3 6.8xl0"3

Solution 4.4xl0"3 2.3xl0-2 1

Peak-Aged 4.2xl0- 3 1

Fig.5 High resolution TEM image of MgO at the interface of an AI2O3-S1O2

fiber.
150 7 - 1

40 H—«—1—■—ι—'—1—■—1—■—1—«—1—'—1—■—1—'—I
0 2 4 6 8 10 12 14 16 18
AGING TIME (hours)

Fig.6 Age hardening response for A356/AI2O3 composite, A3S6/AI2O3-

S1O2 composite and unreinforced alloy.
WS11a1

MECHANICAL BEHAVIOUR OF MODIFIED

Al3Ti AND Al3Zr INTERMETALLIC ALLOYS
WITH ORDERED FCC STRUCTURE

R.A. VARIN, I. VIRK and M. B. WINNICKA

Department of Mechanical Engineering

University of Waterloo, Waterloo, Ontario
Canada, N2L 3G1

ABSTRACT

This paper is an overview of recently obtained results on the mechanical behaviour of

ternary titanium (Al3Ti-base) and zirconium (Al3Zr-base) trialuminides which were obtained
by alloying with various elements to form Ll 2 structure. Vickers hardness and compression
tests results are presented and discussed.

KEYWORDS

Intermetallic alloys; ternary titanium and zirconium trialuminides; Vickers hardness;

compressive properties.

INTRODUCTION

Ternary titanium and zirconium trialuminides (Al3Ti - and Al3Zr-base) exhibit brittle
behaviour despite having the Ll 2 crystal structure with the requisite number of five
independent slip systems required for a general plastic flow of polycrystal (Von Mises
criterion) (Kumar and Pickens, 1988; Tarnacki and Kim, 1988; Schneibel and Porter, 1989;
Turner et al., 1989; George et al., 1989a, b; Powers and Wert, 1990; Winnicka and Varin,
1990; George et al., 1990). The modified Ll 2 Al3Ti- and Al3Zr-base intermetallics exhibit
moderate yield strengths and relatively low hardness (George et al., 1990).

The aim of the present work is to critically review the state of our knowledge on the
mechanical properties (hardness, strength and ductility) of modified ternary trialuminides.

179
180

310 AI3T1 -bose

300 Fig. 1. Dependence of Vickers
o AS CAST
hardness at 1000g load on
290 • HOMOGENIZED
■ HIPed the macroalloying element
280 in t h e Al3Ti-base
270 intermetallic with Ll 2
260 structure. Numbers
CSi 250 correspond to those in Table
E 1.
E 240
230
220
2 210
I
> 200
190
180
170
160
150
140
Cr Mn Fe Co (Pd) Ni Cu
MACROALLOYING ELEMENT

AI3T1-BASE

Hardness

In general, Vickers microhardness of ternary titanium and zirconium trialuminides depends

on load (Virk et al.. 1990). For this reason the Vickers microhardness results obtained in
the present work on Al5CuTi2 (the mean of 5 indentations measured by the Java image
analysis system) are compared in Table 1 with other modifications of Al3Ti-base alloy at
a constant load of 1000g at which hardness is already independent of load (Virk et al.
1990). For a better clarity the results are also plotted in Fig. 1 vs. the position of the
macroalloying element in the periodic table of the elements (for the sake of clarity Pd is
located beside Ni although it is really located below Ni in the periodic table).

There is a general trend of decreasing hardness with decreasing atomic number of

macroalloying element, particularly pronounced in as-cast material. This effect has been
first reported by Nie et al. (1990) and has been attributed to the decreasing strength of d-d
bonding as elements from Cu to Cr with smaller number of d electrons are substituted (and
vice versa). Also, the hardness data are very sensitive to the processing method (cast
sample vs. homogenized or HIPed) and homogenization time (Al5CuTi2 specimens #1,2,
3 and 4). Al5CuTi2 specimen #5 has even hardness as low as that for the Mn and Cr
modifications (HIPed), probably due to an increased porosity (5.3 ± 1.5%). Similar
behaviour is noticed for the Pd modification #8 (6% porosity).
Table 1. Vickers hardness values of Ll2Al3Ti-base trialuminides at 1000g load

No. Alloy Intermetallic Porosity Second VHN Reference

Ele- (at%)
ment Phase
(%) (%) (kg/mm2)

Cu Al5CuTi2
1 As cast (twice melted) 1.110.3 Negligible 286114 This work
2 Horn. 24h/1050°C 1.710.4 0 252130 This work
3 Horn. 48h/1050°C 2.810.9 0 222113 This work
4 Horn. 72h/1050°C 2.610.5 0 208114 This work
5 Horn. 72h/1085°C 5.311.5 0 165115 Virketal.1990
Ni Al^NigTi^
6 HIPing 175MPa/2h/1200°C None None(?) 220110 Nie et al. 1990
7 Horn. 100h/1050°C Large(?) Small 220 Turner et al. 1989
Pd Al^PdgTi^
8 Horn. 100h/1050°C 6 2 190 Powers and Wert,1990
Co Al^CogTi^
9 HIPing 175 MPa/2h/1200°C None None(?) 209110 Nie etal. 1990
Fe Al22Fe3Ti8
10 HIPing 175 MPa/2h/1200°C None None(?) 17916 Nie etal. 1990
Mn Al^MngTi^
11 Arc-melted Small Small 20519 Zhang etal. 1990
12 HIPing 175 MPa/2h/1200°C None None(?) 14915 Zhang et al. 1990
Cr A^CTgTi^ ·
13 Arc-melted Small Small 19417 Zhang et al. 1990
14 HIPing 175 MPa/4h/1200°C None None(?) 15112 Zhang et al. 1990
A^CTgTi^
15 Arc-melted Small Small 21819 Zhang etal. 1990
16 HIPing 175 MPa/4h/1200°C None None(?) 16613 Zhang etal. 1990
Table 2. Compressive mechanical properties of Ll 2 Al3Ti-base trialuminides at room temperature

Alloy Treatment Porosity Second 0.2% offset Ultimate Permanent Reference

Phase strength deformation
(%) (%) (MPa) (MPa) at ultimate
strength (%)1}

Al5CuTi2(A199.99999)Hom.72h/1085°C 5.3±1.5 0 218±40(4) 420±53(4) 11.611.9(4) This work

Al5CuTi2(A199.99999)Hom.72h/1050°C 2.6+0.5 0 196±14(7) 413±48(3) 9.112.2(4) This work
Al5CuTi2(A199.9) Hom.50h/1050°C Winnicka and
(Vacuum melted) 1.110.8 2.6±0.6 -440 -525 -2.7 Varin (1989,1990)

ΑΙ^Νί,Τ^ Hom.l00h/1050°C Large(?) Small -355 -1000 -14 Turner et al.(1989)

Al^FegTi^ Extruded at 1100°C Small None(?) 270 George et_al.(1990)
Al22Fe3Ti8 Horrul00h/1200°C None ? -370 Kumar and Pickens (1988a,
Al5FeTi2 Spray-deposited None Some -500 -1800 -20 Morris and Lerf (1991)
and HIPed lOOMPa/
3h/1150°C
^l67.5^ e 7.5^- 1 25 Hom.l00h/1100°C Some None -200 - 13.9 Cooper et al. (1991)
Al6eMn9Ti25(A199.5) Hot pressed 65/MPa/
100min/1200°C Large(?) Small 390±15 635140 23142) Mabuchi et al. (1989)
Al67Mn8Ti25(A199.95) Arc-melted Small Small -350 -750 7.5 Zhang et_al. (1990)
Al67Mn8Ti25(A199.95)HIPed 175MPa/4h/
1200°C None None(?) -150 -370 -15 Zhang etal. (1990)
Al67Cr8Ti25(A199.5) Hot pressed 65MPa/
100min/1200°C Large(?) Small -400 - 20132) Mabuchi etal. (1990)
A l ^ C r J i ^ A ^ ^ ) HIPed 175MPa/4h
1200°C None None(?) -250 -800 -16 Zhang etal. (1990)

1) Calculated from the Instron chart by the offset method

2) Reported by the authors at fracture
 183

Compressive Properties

Table 2 shows a comparison of room temperature compressive properties (0.2% offset,

ultimate strength and permanent deformation at ultimate strength) taken from literature with
those measured in the present work for Al5CuTi2 modification (4x4x5mm cuboidal
specimens; strain rate 3x10V 1 ; numbers in parentheses indicate the number of specimens
tested). Since the samples contain porosity and they develop microcracks during testing
(Winnicka and Varin, 1991) besides being plastically deformed, then compressing of pores
and forming microcracks may add a certain amount of deformation to the plastic strain
which is then not really a "plastic" strain. Therefore, instead of "plastic strain" we prefer
term "permanent deformation" (Table 2).

Both yield (0.2% offset) and ultimate strength seem to be highly affected by the processing
method (e.g. varying grain size) and possibly by the purity of Al used to produce an alloy
(compare yield strengths for various purities) and the presence of second phase rather than
by the nature of macroalloying element. Regardless of the macroalloying element the
fracture mode in compression and bending of ternary titanium trialuminides at room
temperature is transgranular cleavage (George et al., 1989a, b, 1990; Turner et al., 1989;
Powers and Wert, 1990; Winnicka and Varin, 1990; Zhang et al., 1990). The Fe
modification of Al3Ti was also found to be brittle in single crystal form (Porter et al.,
1989). Recent studies of microcracking development in Al5CuTi2 alloy deformed up to
-10% of permanent deformation in compression (Winnicka and Varin, 1991) have shown
that in high porosity material (volume fraction of pores 5.3 ± 1.5%) cracks are mainly
formed by the link-up of neighbouring pores. In the low porosity alloy (volume fraction
of pores 2.6 ± 0.5%) at higher deformation there exists a directionality of microcrack
formation at -24°, -70° and -90° with respect to the compression axis. These crack lines
pass through several pores and rarely through the pore-free matrix. No extensive
microcracking due to work hardening has been observed. This is in some contradiction to
Turner et al., (1989) who reported extensive internal and external microcracking in the
specimen strained "plastically" by 2%. It should be mentioned that several models have
been proposed to explain the observed brittleness of Al3Ti-base alloys such as a high
activation barrier to dislocation emission from crack tips resulting in the suppression of
crack blunting (Turner et al., 1989) according to the original model of Rice and Thomson
(1989), the larger Burgers vector of a <110> superdislocations coupled with rapid work
hardening by dipoles which inhibits plastic zone formation at crack tips (Vasudevan et al.,
1989) or the poor intrinsic cleavage strength (George et al., 1990). However, none of the
above models can satisfactorily explain all the experimental observations. High-
temperature, short-term compressive properties of Al22Fe3Ti8 and Al5CuTi2 modifications
were investigated by Kumar and Pickens (1988a,b) and Winnicka and Varin (1989, 1990)
respectively. In both cases a peak of yield strength (0.2% offset) and in Al5CuTi2 also a
peak of ultimate strength were observed around 350-400°C, a typical behaviour of
intermetallics having Ll 2 structure. Recently, a small yield peak at ~400°C has been
observed in Al67Cr8Ti25 alloy by Nie et al. (1991). On the contrary, Cooper et al. (1991) and
Kumar et al. (1991) have not observed a positive temperature dependence of yield strength
in HIPed or homogenized Al^ 5Fe7 5Ti25 and in forged Al^CrgTi^ and Al^Mn/Ti^,
respectively. It may be possible that the appearance of the strength peak vs. temperature
is strongly structure-sensitive depending on such factors as grain size, solid solution
strengthening, etc. This aspect definitely needs further clarification. In Al5CuTi2
compressive permanent deformation increased with increasing temperature. However, even
at elevated temperatures fracture in compression of Al5CuTi2 still occurred by cleavage with
184

4.0 AI3Zr-base A^Zr-base

700
• o-RT
•-PEAK TEMP

3.0l·
_ 600
o o
I- 0L
<
ce
o Ld 500
LL
bJ 2.0
ω
O
O
z
Lu 400
C\J
Ö

cr 1.0
Lu
CL 300h

(b)
200 J_ _L J
Cr Mn Cu Cr Mn Cu

MACROALLOYING ELEMENT MACROALLOYING ELEMENT

900r
AI3Zr-base
o

— 8001-
X
H o-RT
O • -PEAK TEMP Fig. 2. Compressive properties at
Ul 7 0 0 ■ - 9 0 0 ° C three temperatures for Cu,
ce Cr and Mn modifications of
H
c/)
Al3Zr-base intermetallic.
Lü (a) Permanent deformation
> 600 at ultimate strength, (b)
ω 0.2% offset, (c) Ultimate
Lü compressive strength. As-
fr cast material with l-3mm
Û_
Έ 500 grain size.
O
o
LU
5 400

(c)
300 J_ J
Cr Mn Cu
MACROALLOYING ELEMENT
 185

secondary cracking (Winnicka and Varin, 1990).

Al3Zr-BASE

Hardness

At 1000g the values of Vickers hardness (VHN in kg/mm2) of Al5CuZr2, Al^Mr^Zr^ and
Al67CrgZr25 modifications in as-cast condition with stoichiometric matrix, both volume
fraction of porosity and second phase - 2 % (Virk and Varin, 1991a,b), are 342±6.8, 333±2.8
and 345±5.4, respectively. These values are much higher than those for Al3Ti-base alloys
(Table 1) and they do not depend on the atomic number of macroalloying element (Fig. 1).
Surface microcracks start forming at 500g indentation load which is ten times less than that
for Al^MngTi^ and Al^C^Ti^ (Zhang et al. 1990).

Compressive Properties

Compressive tests (4x4x5mm specimen, strain rate SxlO^S"1) were carried out in air from
room temperature (RT) up to 900°C at every 100°C interval. Yield strength (0.2% offset),
ultimate strength and permanent deformation at ultimate strength (measured as the change
in the height of the specimen before and after the test), all exhibited a peak at 500°C for
Al5CuZr2 and Al^Q-gZr^, and at 600°C for Al^MnçZr^. These peak temperatures are much
higher than those for Al3Ti-base alloy (Kumar and Pickens, 1988a,b; Winnicka and Varin,
1989).

Figure 2 shows the results at RT, peak temperature and 900°C (three specimens tested at
each temperature). Permanent deformation is much lower than that for Al3Ti-base (Table
2) even at the peak temperature (Fig. 2a). 0.2% offset room temperature is slightly higher
as compared to Al3Ti-base alloy (Table 2) but significantly higher than that reported by
Schneibel and Porter (1989) for Al-5.5 at.% Fe-25 at%Zr. Also, 0.2% offset is much
higher at peak temperature than any of those reported for Al22Fe3Ti8 (Kumar and Pickens,
1988a,bX Al5CuTi2 (Winnicka and Varin, 1989) and Al-5.5 at.%Fe-25 at.%Zr (Schneibel
and Porter, 1989). Even at 900°C, 0.2% offset is still equal to its room temperature value
(Fig. 2b). Since the measured densities (with - 2 % porosity and - 2 % second phase) of
Al5CuZr2, Al^MriçZr^ and Al^CrgZr^ are 4.6, 4.3 and 4.3 g/cm3, respectively, these alloys
exhibit excellent specific strength at elevated temperatures. From all three Al3Zr
modifications, the one with Mn seems to exhibit the best combination of properties.

ACKNOWLEDGEMENTS

This work has been supported by grants from the Ontario Centre for Materials Research
and the Natural Sciences and Engineering Research Council of Canada which are gratefully
acknowledged.
186

REFERENCES
Cooper, C.V., H.R. Pak and C. M. Wayman (1991). In: High Temperature Ordered
Intermetallics IV (L. Johnson, D.P. Pope and J.O. Stiegler, Eds.) MRS, Pittsburgh,
PA.
George, E.P., W.D. Porter and D. C. Joy (1989a). In: High Temperature Ordered
Intermetallic Alloys ΙΠ (C.T. Liu, A.I. Taub, N. S. Stoloff and C. C. Koch, eds.),
133, 311-315, MRS, Pittsburgh, PA.
George, E.P., W. D. Porter, H.M. Henson, W.C. Oliver and B. F. Oliver (1989b). J. Mater.
Res., 4, 78-84.
George, E.P., J. A. Horton, W. D. Porter and J. H. Schneibel (1990). J. Mater. Res., 5,
1639-1648.
Kumar, K. S. and J. R. Pickens (1988a). In: Dispersion Strengthened Aluminum Alloys
(Y.W. Kim and W.M. Griffith, eds. ), 763-786, TMS, Warrendale, PA.
Kumar, K. S. and J. R. Pickens (1988b). Scripta Metall., 22, 1015-1018.
Kumar, K. S. S. A. Brown and J. D. Whittenberger (1991). In: High Temperature Ordered
Intermetallics IV (L. Johnson, D. P. Pope and J. O. Stiegler, eds.), MRS,
Pittsburgh, PA.
Mabuchi, H., K. Hirukawa and Y. Nakayama (1989). Scripta Metall, 23, 1761-1766.
Mabuchi, H., K. Hirukawa, M. Tsuda and Y. Nakayama (1990). Scripta Metall. Mater.,
24, 505-508.
Morris, D. G. and R. Lerf (1991). In: High Temperature Ordered Intermetallics IV (L.
Johnson, D. P. Pope and J. O. Stiegler, eds.), MRS, Pittsburgh, PA.
Nie, J. P., S. Zhang and D. E. Mikkola (1990). Scripta Metall. Mater., 24, 1099-1104.
Nie, J. P., S. Zhang and D. E. Mikkola (1991). In: High Temperature Ordered
Intermetallics IV (L. Johnson, D. P. Pope and J. O. Stiegler, eds.), MRS.
Pittsburgh, PA.
Porter, W.D., K. Hisatsune, C. J. Sparks, W. C. Oliver and A. Dhere (1989). In: High
Temperature Ordered Intermetallic Alloys HI (C. T. Liu, A. I. Taub, N. S. Stoloff
and C. C. Koch, eds.), B 3 , 657-662, MRS, Pittsburgh, PA.
Powers, W.O. and J. A. Wert (1990). Metall. Trans. A., 21A, 145-151.
Rice, J. R. and R. Thomson (1974). Phil. Mag., 29, 73-97.
Schneibel, J. H. and W. D. Porter (1989). In: High Temperature Ordered Intermetallic
Alloys ΠΙ (C.T. Liu, A. I. Taub, N. S. Stoloff and C. C. Koch, eds.), 133, 335-340,
MRS, Pittsburgh, Pa.
Tarnacki, J. and Y.W. Kim (1988). In: Dispersion Strengthened Aluminum Alloys (Y.W.
Kim and W. M. Griffith, eds.), 741-762, TMS, Warrendale, PA.
Turner, C. D., W. O. Powers and J. A. Wert (1989). Acta Metall., 37, 2635-2643.
Vasudevan, V. K., R. Wheeler and H. L. Fraser (1989). In: High Temperature Ordered
Intermetallic Alloys ΙΠ (C. T. Liu, A. I. Taub, N. S. Stoloff and C. C. Koch, eds.),
133, 705-710, MRS, Pittsburgh, PA.
Virk, I. S., M. B. Winnicka and R. A. Varin (1990). Scripta Metall. Mater., 24, 2181-2185.
Virk, I. S. and R. A. Varin (1991a). Scripta Metall. Mater, in press.
Virk, I. S. and R. A. Varin (1991b). Metall Trans, submitted.
Winnicka, M. B. and R. A. Varin (1989). Scripta Metall., 23, 1199-1202.
Winnicka, M. B. and R. A. Varin (1990). Scripta Metall. Mater., 24, 611-615.
Winnicka, M. B. and R. A. Varin (1991). In: High Temperature Ordered Intermetallics IV
(L. Johnson, D. P. Pope and J. O. Stiegler, eds.), MRS, Pittsburgh, PA.
Zhang, S. J., P. Nie and D. E. Mikkola (1990). Scripta Metall. Mater., 24, 57-62.
WS11a2

Deformation of polysynthetically twinned (PST) crystals

and PST bicrystals of TiAl at room temperature

A. Nakamura, H. Inui, M.H. Oh and M. Yamaguchi

Department of Metal Science and Technology, Kyoto University

Sakyo-ku, Kyoto 606, Japan

ABSTRACT

We have grown TiAl crystals of a nearly stoichiometric composition

composed of a single lamellar grain as well as those composed of two
lamellar grains and studied their deformation behaviour at room tempera-
ture. The deformation behaviour of lamellar grains depends strongly on
the lamellar orientation. Because of such an anisotropy in the deformation
behaviour of lamellar grains with respect to the lamellar orientation, a
large strain discontinuity and therefore crack initiation may occur near
boundaries between coarse lamellar grains. This is suggested to be a
reason for low ductility of TiAl with a structure composed of coarse
lamellar grains.

KEYWORDS

Intermetallic compound; TiAl; Lamellar structure; Bicrystal; Deformation;

Ductility; Brittleness.

INTRODUCTION

Much attention has recently been paid to intermetallic compounds because

of their potentially valuable properties, in particular for high-tempera-
ture structural applications. In the Ti-Al binary system, there are three
intermetallic compounds AI3T1, TiAl and Ti 3 Al, which are all attractive
materials because of their properties such as high melting point, good
oxidation resistance and high strength-to-weight ratio. Recently, we have
succeeded in growing TiAl crystals of a nearly stoichiometric composition
composed of a single lamellar grain as well as those composed of two
lamellar grains.
187
188
The lamellar structure in TiAl of a nearly stoichiometric composition is
composed of lamellae of the major constituent phase, TiAl and those of the
secondary phase, Ti 3 Al. Since the TiAl lamellae contains numbers of thin
twins, we call TiAl crystals with a structure composed of lamellae of
single lamellar orientation only "polysynthetically twinned (PST)
crystals" (Fujiwara et al., 1990). In this paper, we present the results
of some deformation experiments on PST crystals and PST bicrystals of
TiAl.

EXPERIMENTAL

The master ingot of TiAl were produced by first melting high purity
titanium and aluminium in a plasma arc-furnace and then remelting it in a
vacuum arc-furnace. The composition of the master ingot was Ti-49.3at%Al.
Rectangular bars, 10 mm x 10 mm in cross section and 100 mm long, were cut
from the master ingot. From these bars, PST crystals and PST bicrystals
were grown using an ASGAL FZ-SS35W optical floating zone furnace under an
Ar gas flow.

Oriented compression specimens, approximately 3 mm x 3 mm in cross section

and 6 mm long and oriented tensile specimens, approximately 2 mm x 0.5 mm
in cross section and 5 mm in gauge length were cut from PST crsytals and
PST bicrystals of TiAl. Compression and tension tests were conducted at a
strain rate of 2.0 X 10" 4 s"1 at room temperature.

RESULTS AND DISCUSSIONS

Yield stress of PST crystals of TiAl depends strikingly on the angle

between the lamellar boundaries and loading axis. It was high when the
lamellae were parallel or perpendicular to the loading axis and it was
very low for intermediate orientations. When the lamellae were parallel
or perpendicular to the loading axis, shear deformation proceeded across
the lamellar boundaries, while shear deformation occurred parallel to the
lamellar boundaries for intermediate orientations. Then, the former mode
of deformation is seen to be hard and the latter mode of deformation is
easy. Both modes of deformation occur by twinning of the type (111) [112]
which does not disturb the L1 0 symmetry of the lattice or slip of the type
(111) [110] (Hall and Huang, 1989; Inui et al., 1991). Twinning and slip
are complementary to one another (Inui et al., 1991). Since six different
types of ordered domains exist in the TiAl lamellae (Feng et al., 1988;
1989; Yamaguchi and Umakoshi, 1990) and the domains which deform by
twinning in compression deform by slip in tension and vice versa (Inui elt
al., 1991), no tension-compression asymmetry in yield stress exists in PST
crystals of TiAl. Therefore, TiAl PST crystals are expected to show good
ductility not only in compression but also in tension. In fact, the
results of their tensile tests indicate that they can be deformed to the
level of 2 0 % tensile strain.
 189
However, polycrystalline TiAl composed of grains with a lamellar struc-
ture, in particular, of coarse lamellar grains, show poor ductility. Their
tensile ductility is usually 0 ~ 3 % at room temperature. Since the yield
stress and deformation behaviour of lamellar grains is highly anisotropic
with respect to the lamellar orientation, a large strain discontinuity may
arise at grain boundareis between coarse lamellar grains depending on how
the lamellar structure of one of the two adjacent grains is misoriented
with respect to that of the other grain. Such a strain discontinuity
would lead to crack initiation at grain boundaries.

Figure 1 (a) shows schematically the lamellar orientation of a PST bicrys-

tal and Fig. 1(b) shows a microstructure of the grain boundary between the
two lamellar grains composing the PST bicrystal. The upper and the lower
grains are expected to deform in the easy and the hard modes, respective-
ly. Figure 2 shows the tensile stress-strain curve for the PST bicrystal
of Fig. 1. The crystal is seen to be deformed to about k% plastic
strain. However, the plastic deformation occurs mostly in the upper grain
which can deform in the easy mode. Therefore as the plastic deformation
in the upper grain proceeds, strain discontinuity between the upper and
the lower grains becomes larger. Finally crack initiation occurs at a
grain boundary region in the lower grain as shown in Fig. 3. Plastic
deformation occurs also in the region near the grain boundary in the lower
grain. However, the amount of plastic deformation in the upper grain is

w
60

\A
75'

Fig. 1. (a) Lamellar orientation in a PST bicrystal

(schematic) and (b) microstructure in a
boundary region in the PST bicrystal.
190

150

(D 100
o_
ΞΕ
CO Fig. 2.
CO
LU
CT Tensile stress-strain curve
CO 50 for the PST bicrystal of Fig.l
at room temperature.

0
0 5
STRAIN (X)

Fig. 3. Crack observed in the PST bicrystal (Fig.l)

tested in tension at room temperature.
 191
far larger than that in the lower grain. The crack seems to be initiated
by failure of a lamellar boundary, probably an interphase boundary between
TiAl and Ti3Al and to propagate first along the interphase boundary and
then along the boundary between the two lamellar grains. Such crack
initiation at lamellar boundaries has been observed also on rolling of PST
crystals of TiAl (Yamaguchi et al., 1990). This indicates that the
lamellar boundaries are weaker than the boundaries between lamellar
grains. Therefore, if refining of lamellar grains is made, the strain
discontinuity problem would become less acute and then a better ductility
would be obtained in TiAl compounds with a structure composed of lamellar
grains.

REFERENCES

Feng, C.R., D.J. Michel and C.R. Crowe (1988). Scripta Metall., 22, 1481;
(1989). Scripta Metall., 23, 241, 1135.
Fujiwara, T., A. Nakamura, M. Hosomi, S.R. Nishitani, Y. Shirai and M.
Yamaguchi (1990). Phil. Mag. A, 6rt, 591.
Hall, E.L. and S.C. Huang (1989). J. Mater. Res., 4, 595.
Inui, H., A. Nakamura and M. Yamaguchi (1991). High Temperature Ordered
Intermetallics IV, Mater. Res. S o c , Pittsburgh, in press.
Yamaguchi, M., S.R. Nishitani and Y. Shirai (1990). High Temperature
Aluminides and Intermetallics, (S.H. Whang, C.T. Liu, D.P. Pope and J.O.
Stiegler, Ed.), TMS, Warrendale, PA, pp.63-90.
Yamaguchi, M. and Y. Umakoshi (1991). Prog. Mater. Sei., 34, 1.
WS11a3

EFFECTS OF TEMPERATURE ON FRACTURE TOUGHNESS IN TiAl

A.W. JAMES AND P. BOWEN

School of Metallurgy and Materials / IRC In Materials For High Performance Applications,
The University of Birmingham, Edgbaston, Birmingham, B15 2TT, U.K.

ABSTRACT

The effects of oxygen on the fracture toughness of the titanium aluminide intermetallic TÎ-48A1
have been determined at room temperature, 500°C and 800°C. Specimens containing two levels
of oxygen, 1800 and 2300 ppm, have been tested in both three- and four-point bend. Pre-cracks
were introduced either by cycling in reverse bending or by the use of uni-axial compression.
Tests were performed in air at ambient temperature and under vacuum at elevated temperatures.
Detailed fractographic analysis was performed using scanning electron microscopy. The
microstructures and constituent phases have been determined by optical, scanning and
transmission electron microscopy.

The level of oxygen present in the intermetallic compound Ti-48 Al was found to affect markedly
the fracture toughness. The trend observed was one of increasing fracture toughness with
decreasing oxygen content. The fracture surfaces of specimens tested at ambient temperature and
500°C both showed failure to be predominantly by transgranular cleavage. However, at 500°C
there were small regions of intergranular fracture. At 800°C the fracture surface consisted of
features of a more 'rounded' appearance, with limited amounts of transgranular cleavage.

Limited increases in fracture toughness were observed at temperatures of up to 500°C, with

substantial increases observed only at the test temperature of 800°C. At all temperatures the
fracture toughness of the material containing 1800 ppm oxygen was approximately 50% higher
than that of the material containing 2300 ppm oxygen.

KEYWORDS
Titanium aluminide, Fracture toughness, Pre-cracking, Temperature.

EXPERIMENTAL
Experimental binary alloys with the composition TÎ-48A1 (atomic percent) produced by AEA
Technology at Harwell Laboratory have been used throughout this study. Bend specimens
measuring 50mm x 7mm x 4mm were machined from a casting produced from a number of
consolidated arc melted buttons. The weight of each button was approximately 52g. The
commercial titanium powder (IMI 130) used in producing the alloys contained approximately

193
194

2000 ppm oxygen. The aluminium (1050) was of 99.5% purity (the major impurities being iron
and silicon) and contained negligible amounts of oxygen.

Two homogenization heat treatments were performed. These were (i) 24 hours at 1200°C under a
nominal vacuum and (ii) the specimens were wrapped in tantalum foil and homogenized for 10
hours at 1250°C under a vacuum of better than 1(H" mbar. The oxygen contents resulting from
these two heat treatments were 2300 ppm and 1800 ppm respectively .The faces of the specimens
were ground to remove the scale formed during heat treatment and then further polished to Ιμιη,
to facilitate the monitoring of crack initiation and growth during fatigue pre-cracking, by means
of a surface replica technique. The specimens were notched to a depth of approximately 2mm
using a low speed diamond saw with a blade thickness of 150μπι.

Pre-cracking was initially undertaken in four-point reverse bending with the notch loaded in far
field cyclic compression (residual tension) using an Amsler Vibrophore. A frequency of
approximately 40Hz, a fatigue ratio of R = 0.1 and ΔΚ values in the range 25 to 35 MPaVm
were used during cycling. At regular intervals (every 105 cycles) the specimens were reloaded to
a K m a x value of < 5 MPaVm in tension to monitor crack initiation and growth. After failure the
fracture surfaces were removed from the broken specimens and the remaining sections were
notched as described previously to produce half sized (approx. 20mm x 4mm x 7mm)
specimens. These half sized specimens were pre-cracked using uniaxial cyclic compressive
loads. An overload, with values of K m a x up to 120 MPaVm, was applied in the first cycle to
induce plastically a stress field ahead of the notch; the value of the overload was judged by
increasing the load slowly until the first sign of deformation occurred ahead of the notch. The
crack was then grown through this plastically deformed region under the effect of cyclic
compressive loading with values of ΔΚ for the propagation of the crack in the region of 40 to 50
MPaVm. The crack lengths were again measured using surface replicas.

Fracture toughness testing was carried out in both three- and four point -bending (half and full
sized specimens respectively) at ambient temperature, 500°C and 800°C. All fracture toughness
tests were performed on an ESH servo hydraulic machine. The ambient temperature tests were
performed in air, while elevated temperature tests were performed under vacuum. A vacuum of
better than 4.0 x 10"4 mbar at 800°C and better than 2.0 x 10"4 mbar at 500°C was routinely
achieved and maintained throughout testing.

The fracture surfaces of all specimens were examined in the scanning electron microscope
(SEM). Specimens were prepared for optical examination and these specimens were also
examined in the SEM where the determination of phases present was performed using energy
dispersive X-ray analysis (EDX).Grain size was measured using the mean linear intercept
method.

RESULTS

The microstructures resulting from both homogenization heat treatments were similar. The
microstructures consisted of a mixture of allotriomorphic TiAl (γ) grains with lamellar regions of
TiAl and Ti3Al (oc-2). In addition to the presence of T13AI in the fine lamellae, it was also
observed in both 'needle' and 'block' (or 'globular') form within the TiAl grains. The block
Ti3Al was often associated with small regions of coarse lath structure. Ti3Al in 'block' form was
also seen at the grain boundaries. The mean lamellar width of the T13AI was calculated to be
0.29 μπι. The grain size measured using the mean linear intercept method gave a mean grain size
of 80.8 μτη. There was however a large spread of grain sizes, ranging from « 20 μιη to 200 μπι.

Fractography

All specimens tested at room temperature failed by transgranular cleavage, (Fig. 1). The was no
discernible difference in fracture appearance between the fatigue pre-cracked region and the final
fracture.
 195

At 500°C the specimens containing 2300 ppm oxygen failed predominantly by transgranular
cleavage. There were, however, regions of intergranular fracture, together with signs of
secondary intergranular cracking, (Figs 2 and 3). The facet size in the intergranular regions was
of the order of 30 to 70 μιη. The specimens containing 1800 ppm oxygen had far fewer regions
of intergranular fracture. The fracture surface consisted almost entirely of transgranular cleavage.
A moderate amount of secondary cracking had also occurred.

At 800°C the fracture surfaces of specimens from both casts were similar. Unlike the fracture
surfaces resulting from the lower temperature tests, there existed only small regions of
transgranular cleavage. Regions of intergranular fracture were also in evidence. However, the
fracture surface consisted predominantly of features with a more 'rounded' appearance, the
structure appearing less 'crisp', with evidence of limited plastic deformation, (Fig. 4). The
fatigue pre-cracked region could easily be distinguished from the final fracture.

Fracture toughness

The fracture toughness values plotted against temperature are presented in Fig. 5. The 'low'
oxygen data refer to the specimens homogenized for 1250°C for 10 hours, with a post
homogenization oxygen content of the order of 1800 ppm. The 'high' oxygen refer to the
specimens homogenized for 24 hours at 1200°C with a post homogenization oxygen content of
approximately 2300 ppm.

At all test temperatures the 'low' oxygen specimens exhibit a higher fracture toughness than that
of the 'high' oxygen material. At room temperature the fracture toughness of the 'low' oxygen
material was approximately 50% higher than the 'high' oxygen material, with peak values of
13.72 MPaVm and 9.59 MPaVm respectively. At elevated temperatures there are limited data for
the 'low' oxygen material; peak values of 14.16 MPaVm at 500°C and 16.46 MPaVm at 800°C
were achieved. The highest values of fracture toughness obtained at elevated temperatures for the
'high' oxygen material were 10.50 MPaVm and 14.28 MPaVm for the tests performed at 500°C
and 800°C respectively.

The trend is one of increasing fracture toughness with temperature, but, larger increases in
toughness correspond to the change in fracture mechanism from transgranular cleavage to the
more ductile mode observed at 800°C

DISCUSSION

The effect of oxygen on the fracture toughness is clearly evident from the results: as the oxygen
content increases so the fracture toughness decreases. Soboyejo et al performed fracture
toughness tests on a similar Ti -48Al binary alloy containing approximately 1500 ppm oxygen
and reported fracture toughness values of 16.1 and 14.6 MPaVm for specimens tested at room
temperature. These values are slightly higher than those recorded for the alloy containing 1800
ppm oxygen tested in this study. It has been suggested (Kim, 1990) that the maximum amount of
oxygen allowable in the gamma titanium aluminides is of the order 1000 ppm. Oxygen contents
above this level are thought to reduce the already low ductility seriously .

As may be seen from the data presented in Fig. 5, there is a large degree of scatter in the values
of fracture toughness measured for the 'high' oxygen material. The mean fracture toughness
values for room temperature, 500°C and 800°C tests are 8.19, 8.77 and 12.25 MPaVm
respectively. There is very little change in the fracture toughness as the temperature is increased
from room temperature to 500°C. This is consistent with the appearance of the fracture surfaces
which remain predominantly transgranular. All the values obtained from the tests performed on
the 'high' oxygen material at room temperature and at 500°C were found to be within 20% of the
mean values. At 800°C the range of fracture toughness values were found to lie within 15% of
the mean value. The fracture toughness values obtained for the 'low' oxygen material lie within
196

10% of the mean value for all test temperatures. The gamma alloy with 1800 ppm oxygen
showed a mean fracture toughness of around 13 MPaVm at room temperature and increased only
to a mean value of 16.5 MPaVm at 800°C. Even at 800°C there was little evidence of marked
plasticity.

Kim and Froes (1989) reported a strong dependence of fracture toughness on the lamellar
volume fraction. The results of his room temperature tests on a two phase quaternary gamma
alloy gave a value of 12 MPaVm for fine, predominantfy gamma grained structure, while for the
same alloy with a structure consisting predominantly of lamellar grains with strongly interlocking
grain boundaries the value of fracture toughness was reported to be greater than 20 MPaVm. In
Sie current study the lamellar content is in the region of 40 to 45 percent.

The fracture toughness values obtained from tests on specimens with both types of pre-crack,
produced results which were consistent with each other. This is encouraging since it is apparent
that such brittle materials will require cyclic compression to give pre-cracks.

Observations of the fracture appearance made in this study are in good agreement with those
made by other workers (Kim and Froes, 1989; Lipsitt et al, 1975) for specimens fractured at
room temperature. It is widely accepted that the predominant fracture mode at room temperature
is transgranular cleavage. This has been confirmed both in tensile specimens and also in
specimens which have failed in fatigue. Sastry and Lipsitt (1977) observed no significant effect
of stress amplitude or frequency on the fracture topography of specimens fatigued at room
temperature. The transgranular cleavage fractures observed by Sastry and Lipsitt under fatigue
conditions are consistent with the observations made in this study, when no discernible
difference was noted between the pre-cracked region and the final fracture surface of specimens
tested at room temperature. The lack of difference between the two regions, raises the question as
to whether the pre-crack is caused by fatigue or is simple due to static cracking modes.

At 500°C the specimens tested in this study continued to fail predominantly by transgranular
cleavage. Lipsitt et al (1975) also reported that their tensile specimens tested at 600°C had a
fracture appearance nearly identical to those observed on the specimens tested at room
temperature.

At 800°C the fracture appearance of the fracture toughness specimens tested under vacuum noted
in this study differ widely to those observed and reported by other workers. The fracture
surfaces of specimens tested at 800°C in this study consist predominantly of features with a
'rounded' appearance, perhaps indicative of limited plastic deformation. Other workers ( Kim
and Froes, 1989; Lipsitt et al, 1975) have reported extensive intergranular fracture at
temperatures above the brittle-ductile transition. Lipsitt et al (1975) report that at 800°C under
uni-axial tensile conditions the tendency towards intergranular fracture becomes pronounced and
that these regions show considerable evidence of ductility, while regions of transgranular
cleavage are seen only occasionally. Sastry and Lipsitt (1977) report a completely intergranular
fracture surface under fatigue conditions at 700°C when cycling is carried out at low frequencies
and high stress amplitudes. However, they also report mixed intergranular and cleavage fracture
as the stress amplitude is decreased and the frequency increased. This change in the fracture
appearance with fatigue conditions may indicate an environmental effect. Micrographs presented
in the literature clearly show the fracture surfaces of specimens tested in the temperature regime
700° to 800°C to be composed predominantly of 'classical' intergranular features and these have
been suggested as representing upper shelf behaviour. In this study the specimens have been
fractured in bend using pre-cracked testpieces, whereas the other workers have used uni-axial
loading and unnotched tensile specimens. This difference in geometry may help explain the
differences observed in the fracture mode, since the cleavage fracture of aluminides has been
shown to be controlled by a critical value of tensile stress which is independent of test
temperature (Penton,1990). Ahead of a pre-crack, local tensile stresses of up to five times the
yield stress can be produced ( Rice and Johnson, 1970; Tracey, 1976) and therefore such high
tensile stresses can promote cleavage failure to higher temperatures than in an unnotched tensile
test. Therefore in a pre-cracked testpiece the ductile to brittle transition temperature will be higher
and such considerations may help to explain the differences between the fractographic
 197
observations of the present study and those in the literature. This is also consistent with the
modest increases in fracture toughness (of the order of 50%) observed as the temperature is
increased from 500 to 800°C. It is therefore probable that the upper shelf values of toughness
have not yet been attained.

CONCLUSIONS
The level of oxygen present in the intermetallic compound Ti -48 Al has been found to affect the
fracture toughness markedly. Increasing the oxygen content from 1800 ppm to 2300 ppm,
causes a reduction of around 50% in the values of fracture toughness. The fracture toughness of
the alloy containing 2300 ppm oxygen is of the order 8 MPaVm at room temperature and 12 to 13
MPaVm at 800°C. The alloy containing 1800 ppm oxygen has a fracture toughness of
approximately 13 MPaVm and 17 MPaVm at room temperature and 800°C respectively. There is
negligible increase in the value of fracture toughness as the temperature is raised from room
temperature to 500°C. The predominant mode of fracture at temperatures below 500°C is
transgranular cleavage.

It has been demonstrated that despite the brittle nature of the gamma titanium aluminides, the
introduction of a pre-crack into such samples may be undertaken using cyclic loading conditions
with the notch in compression. A comparison of two such techniques, loading in reverse bending
and uni-axial compression, has shown that both these methods produce fracture toughness
values which are closely similar.

ACKNOWLEDGEMENTS

Support for one of the authors (AWJ) from a SERC CASE award with AEA Technology is
gratefully acknowledged, together with useful discussions with Dr M. Strangwood and Dr C.A.
Hippsley.

REFERENCES
Kim, Y-W. (1990). Personal communication
Kim, Y-W and F.H. Froes (1989). Physical metallurgy of titanium aluminides. TMS/ASM Fall
meeting, Indianapolis, Indiana. 1 - 5 October.
Lipsitt, H.A., D. Shechtman and R.E. Schafrik (1975). The deformation and fracture of TiAl at
elevated temperatures. Met. Trans. A, 6A, 1991 -1996.
Penton, R.J.P (1990). The fracture and fatigue of the Ti3Al base alloy super alpha-2. M.Phil
thesis, submitted to the university of Birmingham.
Rice, J.R. and M.A. Johnson (1970). Inelastic behaviour of solids, ed. M.F. Kanninen,
McGraw-Hill, New York.
Sastry, S.M.L. and H.A. Lipsitt (1977). Fatigue deformation of TiAl base alloys. Met. Trans.
A, 8A, 299-308.
Soboyejo, W.O., P.B. Aswath and S. Suresh (1989). Room and elevated temperature fatigue
crack growth and fracture in gamma titanium aluminide. TMS/ASM Fall meeting,
Indianapolis, Indiana. 1 - 5 October.
Tracey, D.M. (1976). J. Eng. Mat. Tech., ASME, 98, 146.
198

Fig. 1 Fracture surface of Ή-48Α1 Fig. 2 Fracture surface of TÎ-48A1

tested at room temperature. tested at 500°C

Fig. 3 Cleavage facets, regions of Fig. 4 Fracture surface of Ή-48Α1

intergranular fracture and secondary tested at 800°C.
cracking in TÎ-48A1 tested at 500°C.

i» -
. D 'low' oxygen D
16- ■ 'high' oxygen D

D ■
14- D ■
c ■
12- B
■
■
1
10" ■
I ■
I 8"
1

■ 1
6" 1 -i 1 ■ ■ 1 i ■ ■

200 400 600 800 1000

Temperature°C

Fig. 5 Plot showing fracture toughness versus temperature for Ti-48A1

alloys containing 1800 (low) and 2300ppm (high) oxygen.
 WS11a4

EFFECTS OF MICROSTRUCTURE ON THE TENSILE AND CREEP PROPERTIES IN TiAl

T.MAEDA, M.OKADA and Y.SHIDA

Advanced Technology Research Labs., Sumitomo Metal Industries, Ltd.

1-8 Fuso-cho, Amagasaki 660, Japan

ABSTRACT

Microstructural influences on a number of mechanical properties have been

investigated in the intermetallic compound TiAl modified by the addition of
molybdenum to Ti-rich TiAl. Three typical microstructures, such as lamellar,
coarse equi-axed and fine equi-axed, were examined and compared on their
tensile properties and creep rupture strength. The results revealed that the
mechanical properties in the TiAl based alloy strongly depended on their
microstructures. The lamellar structure is very brittle at room temperature
but exhibited high strength at the elevated temperature with little
ductility. On the contrary, fine equi-axed grains structure showed high
strength with significant ductility at room temperature, however it showed
lower strength at the high temperature with considerably high elongation.
The coarse equi-axed grains structure exhibited intermediate characteristics
between them in tensile properties, however it showed higher creep rupture
strength than the lamellar structure of as cast materials. Microstructural
dependence in these mechanical behaviors at high temperatures were suggested
to relate to the dynamic recrystallization and the new phase formation
during hot deformation.

KEYWORDS
intermetallic compound ; titanium aluminide ; tensile properties ; strength
; ductility ; creep rupture strength ; microstructure ; hot deformation.

INTRODUCTION
An intermetallic compound TiAl, consisting of equi-atomic titanium and
aluminum, has recently been attracting much attention because of its light
weight with mechanical stability at elevated temperatures, indicating large
potential to be developed as a new light weight and heat resistant
structural materials which can be used for future jet engines and other
applications. However, as general natures in intermetallics, it has been
suffering from a number of essential problems in mechanical properties, such
as poor ductility, low toughness and poor workability even at high
199
200
temperatures. A lot of efforts have recently been made in order to overcome
these problems. The modification of chemistry is one of effective ways to
improve mechanical properties, for example off-stoichiometry in TiAl to
Ti-rich side improves the room temperature ductility (M.Yamaguchi et al.,
1990) and the additions of ternary element such as V, Mn and Cr also result
in the same effect (Y.W.Kim, 1990). The investigation on the Mo modified
TiAl by the authors revealed that Mo has a refining effect on the
microstructure of annealed Ti-rich TiAl, which contributes to the
improvement of room temperature ductility and furthermore Mo can enhance the
creep strength (Maeda et ah, 1991).

Moreover, microstructure in Ti-rich TiAl extensively varies depending on

its chemistry and thermo-mechanical processing applied. It is well known
that Ti-rich TiAl in as cast condition exhibits very unique microstructure
of lamellar morphology consisting of thin twin plates of TiAl(7 ) with thin
layers of Ti3Al(a2) between 7 plates irregularly (M.Yamaguchi et al.,
1990). The lamellar structure is unstable disappears through heat
treatments or hot working at high temperatures, which results in the
formation of equi-axed 7 grains. The influences of microstructure on the
mechanical properties have been limited so far. In the present study, a
comparison of representative microstructures has been made on the tensile
and creep properties in Ti-rich TiAl. The mechanisms in microstructural
effects and designing microstructure in Ti-rich TiAl have been discussed.

EXPERIMENTAL PROCEDURE
The ingots with the nominal composition of TÎ-33.7A1-1.7Mo(wt%) obtained
through arc melting in Ar or vacuum were used. Three types of microstructure
were produced through heat treatments and hot working. The three
microstructures examined, lamellar, coarse equi-axed equi-axed and fine
equi-axed, are shown in Fig.1. Lamellar structure is as cast condition and
consists of very thin 7 plates with thin layers of a 2 forming coarse
grains as 500 to 1000μπι. Equi-axed coarse grains structure is produced by
annealing the ingot at 1473K for 86.4ks result in the disappearance of
lamellar and the formation of fully equi-axed 7 grains up to 200μ m.
Equi-axed fine structure is produced by the isothermal forging at 1223K on
the HIPed ingot with the strain rate of 5x10-4s~1 by 80% in thickness and
followed by annealing at 1273K for 3.6ks and equi-axed and very fine

Fig.1. Microstructures of TiAl examined, (a) Lamellar 100μm

(b) Coarse equi axed, (c) Fine equi-axed —
 201
grains structure smaller than ^0^m was obtained. The tensile test pieces,
4mm diameter and 16mm gage length, and tensile creep rupture test pieces,
6mm diameter were machined from the above materials. Tensile tests were
performed at room temperature and 1073K with a strain rate of 8.3x10- 5 s _1 .
Creep rupture tests were carried out at 1073K in air with the applied stress
between l50-250MPa. The observation of microstructures were carried out by
the optical microscope and TEM. Fracture surfaces were also observed by SEM.

RESULTS AND DISCUSSION

Tensile Properties

Table 1 shows that the tensile properties at room temperature and 1073K on
the three microstructures. At room temperature, the lamellar structure
exhibited no ductility and fracture took place in the elastic region in the
S-S curve so that 0.2% proof srtress was not obtained. On the other hand,
the equi-axed coarse grains structure exhibited 0.2% proof stress with small
elongation, however the fracture strength was lower than lamellar structure.
The equi-axed fine structure exhibited higher 0.2% proof strength and
ultimate tensile strength than coarse structure with higher ductility. This
suggests that equi-axed grain structures are more ductile than lamellar
structures in polycrystalline condition and refining the γ grains results
in the improvement in both strength and ductility at room temperature. And
these results indicate that microstructural modification of lamellar
structure in very coarse grains is necessary for the applications where room
temperature ductility is considered. In addition, refining γ grains is
effective way to improve the room temperature ductility with the increase of
strength. Further refinement to a few microns grains structure by hot
extrusion resulted in the elongation of 2 % with considerable high proof
stress of 608MPa(T.Maeda et al, 1989). The effect refining grain size on the
ductility in an intermetallic compound has been reported in NiAl although at
673K (Schulson and Baker,1983). Generally, TiAl intrinsically has high
modulus with very limited plasticity so that and TiAl based alloys exhibit
very brittle fractures classified cleavage or quasi-cleavage fracture.
Refining grain size should be effective to minimize the local stress
concentration on the grain boundaries or the interfaces between γ and a 2
in the lamellar. However, it must be noted that lamellar structure
mono-directionally controlled to easy mode for deformation can be cold
rolled (Yamaguchi et al. 1990).

Table 1. Tensile properties at room temperature and

1073K in TiAl with varied microstructures.

RT 1073K
Microstructure
0.2XPS UTS El 0.2%PS UTS El
(MPa) (MPa) (%) (MPa) (MPa) (X)

Lamellar — 477 0 448 583 2

Equi-axed (Coarse) 395 414 0.2 302 374 10

Equi-axed (Fine) 459 484 0.5 284 343 81

202

Fig.2. Fractographs of tensile test piece at 1073K.

(a) Lamellar (b) Fine equi-axed

At 1073K, the lamellar structure still exhibited very high strength, where
the fracture strength is even higher than that of room temperature, and the
elongation was obtained but still low as 2%, which is preferable for high
temperature use. In the two equi-axed γ grains structures, the strength is
considerably lower than the lamellar structure with sufficient ductility.
And in the fine equi-axed grains structure, the drop of strength occurred
and extremely high elongation was obtained to be related to superplasticity.
These properties are not preferable as high temperature use but suitable for
hot working with very low strain rate such as isothermal forging. The
fractographs of tensile test pieces of lamellar and equi-axed grains
structure tested at 1073K are shown in Fig.2. In the lamellar structure,
the fracture surface still exhibits very brittle fracture resenting quasi-
cleavage fracture which is almost same fracture surface with that of room
temperature. On the contrary, the fracture surface in the fine equi-axed
structure clearly shows the ductile fracture presenting dimples. It must be
noted that the size of dimples is very fine, suggesting that the small grain
size was maintained during the deformation. This is probably related to the
dynamic recrystallization during hot deformation. These results suggest that
the initial microstructure strongly affect the microstructural change in the
hot deformation, especially on dynamic recrystallization.

Creep Rupture Strength

The creep rupture curves in the three microstructures at 1073K are shown in
Fig.3 presenting that the creep strength is strongly depends on the
microstructure. It must be noted that fine equi-axed grains structure
exhibits considerably low creep strength and the differences with the other
two microstructures become larger at lower stress with longer rupture time.
Minimum creep rate is probably enhanced in fine equi-axed structure,
although there is reportedly no significant difference among the grain sizes
of 25, 42 and 70μ m in single γ phase of Ti-53.4at%Al (Nagai et al.,1990).
This discrepancy probably attribute to two phases structure or to
considerably smaller grain size which is smaller than the previous work. The
difference in the phases and grain size will probably affect the dynamic
recrystallization and grain boundary sliding. Elongation obtained in the
creep tests were 5-6% for lamellar, 13-15% for coarse equi-axed the dynamic
 203
500
450
400
350
«J 300
eu
250
>w
v<^v^
Equi-axed(Coarse)
£ 200 ^•k^

Lamellar
150

Equi-axed(Fine)
100
10 102 io3 10"
Rupture time(ks)
Fig.3. Stress-rupture time curves in TiA1 with three
microstructures.

recrystallization and 70-94% for fine equi-axed, which is close to those in

the tensile test at 1073K as shown in Table 1. TEM micrographs of deformed
microstructure in fine equi-axed structure after creep test at 1073K with
150MPa is shown in Fig.4(a). The deformed structure shows still fine
grains of γ phase where grains of high and very low dislocation density
were observed suggesting dynamic recrystal1ization occurs during creep
deformation. The dislocations piles up at the local grain boundaries and
results in the recrystallization. The repeat of work hardening and dynamic
recrystallization would maintain fine grains structure.

It must be noted that the coarse equi-axed grains exhibit higher creep
strength than lamellar structure, which is inconsistent with the tensile
strength at 1073K. This suggests that the different microstructural change
should have occurred due to the difference in the strain rates, 10- 4 s _ 1 for
tensile tests and approximately 10" 8 s- 1 of creep tests, or in the keep time,

Fig.4. TEM micrographs of creep deformed TiAl.

(a)Fine equi-axed TiAl at 1073K with 150MPa.
(b)Lamellar structure at 1073K with 190MPa.
204
10ks for the tensile tests and 700ks for the creep test with 190MPa. Even
after creep deformation at 1073K, the lamellar morphology was still
maintained after long time holding at 1073K and recrystallization was not
apparent, although lamellar structure transforms to equi-axed grains
structure at 1473K as adopted for the preparation of microstructures in the
present study. However, the detailed observation on the deformed structure
by TEM as shown in Fig.4(b) revealed that very fine particles were formed
along the lamellar plates, which were confirmed to be ß -Ti phase by
electron diffraction. These precipitates result from Mo addition which is
ß stabilizing element in Ti. Similar precipitates were observed in the TiAl
based alloy containing W (Martin et al., 1980) and suggested that the
precipitates of ß phase inhibits the dislocation motion and grain boundary
sliding, which results in the increase the creep strength (Martin et al.,
1983). However, the volume of ß particles observed in the equi-axed
structures were much smaller than in the lamellar structure so that the
precipitates do not contribute the increase of creep strength in the
lamellar structure. Since lamellar morphology in as cast condition was
maintained, the difference of chemistry in a 2 and 7 plates regions in the
lamella still exist, suggesting that the formation of ß -Ti from
nonequilibrium structure was enhanced. It is suggested that the excess
volume of ß -Ti solid solution due to the ternary addition reduces the creep
strength of nonequilibrium 7 +a 2 structure in as cast condition.

CONCLUSION
Tensile properties at room temperature and at 1073K were investigated on the
three typical microstructures, lamellar, coarse equi-axed and fine equi-
axed, in Ti-rich TiAl. And the creep rupture strength at 1073K was also
examined. The results obtained showed that the mechanical properties
strongly depend on the microstructure and implied the difficulty in the
development of superior microstructure for both room temperature ductility
and high temperature strength.

REFERENCES

Kim, Y.W. (1990). Physical metallurgy of titanium aluminides. In: High

Temperature Alumini des and Intermetallies (S.H. Whang, C.T. Liu, D.P. Pope
and J.O. Stiegler, Ed.), TMS, Warrendale, pp. 465-492.
Maeda, T., M. Okada, Y. Shida and M. Nakanishi (1989). Improvement of
ductility through grain refining in TiAl. In: Collected abstracts for the
fall meeting in Japan Institute of Metals, pp. 238-239.
Maeda, T., M. Okada and Y. Shida (1991). Ductility and strength in Mo
modified TiAl, in print In: High Temperature Ordered Intermetallic
Alloys IV ( L. Johnson, J.O. Stiegler and D.P. Pope Ed. ), Mater. Res.
S o c , Pittsburgh.
Martin, P.L., H.A. Lipsitt, N.T. Nuhfer and J.C. Williams (1981). In:
Titanium '80 Science and Technology (H. Kimura and 0. Izumi Ed.), TMS-
AIME, Warrendale, pp. 1245-1254.
Martin, P.L., M.G. Mendiratta and H.A. Lipsitt (1983). Creep deformation of
TiAl and TiAl+W alloys. Metall. Trans., U A , 2170-2174.
Nagai, H., T. Takahashi and H. Oikawa (1990). Effect of grain size on creep
of Ti-53.4mol%Al intermetallics at 1100K. J. Mat.Sei., 25, 629-932.
Shulson, E.M. and D.R. Baker (1983). A brittle to ductile transition in
NiAl. Scripta Met., U , 519-522.
Yamaguchi, M., S.R. Nishitani and Y. Shirai (1990). Plastic deformation of
intermetallic compounds TiAl and TÎ3A1, Ref. of Kim(1990), pp. 63-90.
WS11a5

MICROMECHANISMS OF FRACTURE IN A T13AI BASED ALUMINIDE

R.J.T. Penton*, M.T. Cope* and P. Bowen*

♦School of Metallurgy and Materials/IRC for High Performance Materials, University of
Birmingham, Edgbaston, Birmingham B15 2TT.
tRolls Royce PLC, PO box 31, Derby, DE2 88J.

ABSTRACT

Cleavage fracture in the T13AI based alloy super 012, has been shown to be controlled by a
critical value of tensile stress, which is independent of test temperature. In addition the
temperature dependence of the Fracture Toughness has been measured at temperatures of up
to 750°C, and has been modelled by the use of the concept of critical tensile stress over a
distance.

Fractographic and metallographic observations confirm that at room temperature a

transgranular cleavage fracture mechanism dominates, and as the test temperature increases
then the failure mode changes to microvoid coalescence. At the highest test temperature of
750°C large microvoids are observed to initiate around primary 012 regions. The critical rôle
of primary oc2 regions in promoting cleavage fracture at lower test temperatures is
unconfirmed, but such regions do appear to cleave at higher test temperatures than
transformed ß regions.

KEYWORDS
Super cx2, Fracture Toughness, Elevated Temperatures, Failure Micromechanisms, Critical
tensile stress.

INTRODUCTION
In recent years it has become increasingly clear that the current range of titanium alloys have
reached the limit of their temperature capabilities (Lipsitt, 1985a, 1985b). The search for a
higher temperature alternative has focused on the titanium aluminide intermetalic systems
which combine low density and high stiffness with improved high temperature capabilities
systems. T13AI based on have been the most investigated with a number of alloys under
consideration (Larsen et al, 1990) and a number of test components have also been

205
206
fabricated (Lipsitt, 1985a,1985b; Bampton, 1990; Blackburn and Smith 1982). Confidence
in these alloys is such that some authors (Fleischer et al, 1989) conclude that T13AI base
alloys will be incorporated into all new military engines.

EXPERIMENTAL.

The toughness of the T13AI base alloy Super CC2 ( Ti - 25at% Al - 10at%Nb - 3at% Mo -
lat% V )has been assessed from ambient temperature to 750°C. The material was heat
treated for one hour at 1060°C air cooled to room temperature and followed by ageing at
850°C, and air cooled to room temperature. This heat-treatment schedule produces a
transformed ß grain size of approximately 30μιη, with a volume fraction of primary 012
regions of approximately 20%. The surface was ground away to a depth of 2mm to remove
any oxidation products and other surface layers. Pre- cracking was performed at room
temperature in three point bend under tensile loading, such that a/W » 0.3 - 0.4. SEN
specimens, of dimensions 10mm x 10mm x 70mm long, were loaded to failure on a servo-
hydraulic test machine under vacuum conditions (to prevent oxidation of the fracture
surfaces at higher temperatures). Fracture Toughness values were calculated according to
BS5447: 1977 at room temperature and from P ma x values taken from a load - position
displacement traces at elevated temperatures. Linear load displacement traces were obtained
only to 500°C.

Notched bend specimens were also tested to investigate the importance of the tensile stress
ahead of a notch (Penton, 1990), this is more fully described elsewhere (Griffiths and
Owen, 1971).

Fractography was carried out on two Scanning electron microscopes, an ISI 100A and a
Hitachi S4000 F.E.G., to investigate the failure micromechanims. Fracture surfaces were
carefully sectioned perpendicular to the fracture surfaces and metallographic specimens
prepared.

RESULTS.

Fracture toughness values are shown in Figure 1. At room temperature a valid Kic value is
obtained, and failure occurs by transgranular cleavage, see Figure 2(a). Secondary cracking
is often observed, see Figure 2(b). Primary 012 regions often appear to provide a favourable
crack path but they can also deflect the crack in some cases, Figure 2(b). At test
temperatures of 500°C and above, microvoid coalescence becomes increasingly the
dominant failure mechanism and an increase in toughness, K m a x , is observed, see Figs.
3(a)-(d). Note that regions of isolated cleavage fracture still persist to 700°C, these appear
to coincide with primary oc2 regions, see Fig. 4(a), and some particles have been observed
to fail at sites away from the main crack path in a similar manner to that observed in tensile
tests elsewhere (Ward, 1988). At the highest test temperature of 750°C, the ductile fracture
morphology changes, and much larger microvoids are observed, see Figure 3(d). Optical
sections confirm that the fracture path follows the boundary of the primary oc2 regions Fig.
4(b).

Values of failure load and maximum tensile stress, OF*, obtained from notched bend tests
(using a FEM elastic plastic analysis due to Griffiths and Owen, 1971) are shown in Table
1. It can be seen that the value of σρ* is independent of test temperature (to calculate the
value of O F * , the value of yield stress, a y , must be known.
 207

Table 1 - The Variation of the Critical tensile stress at failure in a blunt notch test with
Temperature

*
Temperature p 0.1% PS p
°C max MPa MPa
kN
20 16.55 910 1590

300 26.11 682 1583

500 28.52 432 1547

DISCUSSION.

Cleavage fracture in super cc2 appears to be controlled by a critical value of tensile stress. In
such cases it is natural to apply a modified Griffith criterion to predict the critical microcrack
nucleus size, and this is estimated as 0.5 μπι (Penton, 1990). Such estimates must be
treated with caution, but clearly regions of primary cc2, of size μηι, would be expected to act
as potent microcrack initiation sites and they do appear to cleave at higher test temperatures
than the transformed β matrix. Their rôle is as yet unconfirmed, however, because they
have also been observed to deflect cracks.

A sharp-crack ductile to brittle transition has been observed in the present study, with
regions of transgranular cleavage persisting to temperatures of 700°C (and identified with
primary oç regions). The trend in toughness with test temperature has been modelled by the
use of the concept of a critical tensile stress over a characteristic distance (Penton,1990) and
it appears to provide a lower bound to the experimental values, see Figure 1.

At the highest test temperature of 750°C, large microvoids initiate around primary oc2
regions, perhaps consistent with a model of comparatively weak interfacial bonding at high
temperatures between primary 012 regions and transformed β regions. At lower test
temperatures microvoids are observed to be much finer, and void initiation sites have not yet
been identified. The extremely clean nature of the material may preclude inclusions as
preferential sites, and if so, then void initiation from triple points in the transformed β matrix
may be suggested.

CONCLUSIONS

1. A temperature independent cleavage fracture stress has been identified as controlling

fracture in Super oc2 at test temperatures of up to 500°C. Together with the assumption of a
characteristic distance, this has been used to predict the temperature dependence of the
fracture toughness.

2. Fracture toughness values increase markedly at temperatures of 500°C and above,

consistent with the appearance of a microvoid coalescence failure mechanism. Regions of
transgranular cleavage still persist to a test temperature of 700°C, and are associated with
primary 012 regions. At the highest test temperature of 750°C, large microvoids are
observed to initiate around primary ot2 regions.
208

ACKNOWLEDGEMENTS.
Support for one of the authors (RJTP) from a SERC CASE award with Rolls Royce, is
gratefully acknowledged together with useful discussions with P.J. Postans.

REFERENCES.

Bampton C.C., "Superplastic Forming and Diffusion Bonding of Titanium

Aluminides", presentation at Aeromat '90, May 1990, Long Beach California
MJ. Blackburn & M.P. Smith, AFWAL Tech. Report No. AFWAL - TR - 82 -
4086, 1982
Fleischer R. L., Dimiduk D.M. & Lipsitt H.A., "Intermetallic Compounds for Strong High
Temperature Materials: Status and Potential", Annu. Rev. Mater. Sei, 19 (1989), pp.
231-263
Griffiths J.R. & Owen D.R.J.,"Plastic Stress Analysis for Notched Bar in Bending"
JMech. Phys. Sol., 19 (1971), p. 395
Larsen J.M., Williams K.A., Balsone SJ. and Stucke M.A., "Titanium Aluminides for
Aerospace Applications", to be publ.
Lipsitt H.A., "Titanium Aluminides - An Overview", Proc. Mat. Res. Soc. Symp. 39
(1985) p 351 - 364
Lipsitt H.A., "Titanium Aluminides - Future Turbine Materials", Proc. of the Nicholas J.
Grant symposium "Processing and Properties of advanced High Temperature Alloys"',
p. 157, 1985
Penton R. J. T., M.Phil Thesis, University of Birmingham, 1990
Ward C.H., Williams J.C., Thompson A.W., Rosenthal D.G. & Froes F.H., "Fracture
Mechanisms in Titanium Aluminide Interme tallies", Proc. Conf., 6th World Conference
on Titanium, paper no. 172, 1988
BS 5447:1977," British Standard Methods of Test for Plane Strain Fracture Toughness
(Kic) of Metallic Materials"

1
-
1 i r | i i i 1 i i 1 i
~1

50 Experimental Fracture Toughness A f -

O Model Prediction

40 -
4 A
A «
":
a
a 30
1
20 A
' A
ô
—^- θ

1 _. . 1 1 . . 1 . . 1i 1 ,

200 400 600

Temperature (°C)
Figl - The Variation of Fracture Toughness with Temperature
as Experimentally measured and as Predicted by the
model.
 209

Fig 2a - Cleavage Fracture after Fig 2b - Section through the

testing at Room Temp. fracture surface at room
temperature.

Fig 3a - Fracture surface after Fig 3b - Fracture Surface after

toughness testing at toughness testing at
600°C. 700°C.
210

Fig 3c - Fracture Surface after Fig 3d - Fracture surface after

Toughness testing at toughness testing at
700°C. Note difference 750°C.
in appearance to fig 3b.

Fig 4a - Section through the fracture Fig 4b - Section through the

surface after testing at Fracture Surface after
500°C, showing ot2 regions toughness testing at
cleaving. Note that one 750°C
region has failed away from
the main fracture path
(arrowed).
WS11a6

RELATIONSHIP BETWEEN STRUCTURAL ORDERING AND STRENGTH IN CASE OF

INTERMETALLIC STRUCTURES OF LI2 TYPE WITH AND WITHOUT ALLOY ADDITIONS

R.Ramesh1, B. Pathiraj1 and B.H. Kolster1'2

1. Foundation for Advanced Metals Science (SGM)

7550 KA Hengelo, The Netherlands.

2. Materials Science Section,

Faculty of Mechanical Engineering
University of Twente, Enschede, The Netherlands.

ABSTRACT

Stoichiometric and off-stoichiometric compositions of NÎ3A1 alloys were

investigated.The long range order parameter 'S' was determined as a function
of temperature using x-rays in order to clarify some of the significant
anomalies noticed in the literature. The Ll2 structure appears to attain a
maximum stability at about 600 C around which temperature its order
parameter was close to its theoretical value. Above 600 C, this structure
becomes less stable and there seems to be a formation of another ordered
structure of lower symmetry. Dilatometry and differential scanning
calorimetry (DSC) measurements substantiated this further. The high
temperature strength dependence was studied for the boron doped
off-stoichiometric N13AI alloy homogenised at different temperatures. The
alloys homogenised at 1000 C exhibited a higher anomalous strengthening
behaviour as compared to the alloys homogenised at 600°C.

KEYWORDS

Long range order parameter; superlattice; thermal expansion coefficient;

intermetallic; flow stress.

INTRODUCTION

Eversince the discovery that small additions of boron to N13AI leads to a

remarkable improvement in room-temperature ductility (Aoki et al., 1979),
there has been an upsurge of interest in its development for high
temperature structural applications. The characteristic anomalous yield
stress behaviour of these alloys has been largely explained on the basis of
a thermally activated dislocation cross-slip from the <111> glide planes to
the <100> sessile planes (Kear et al., 1962).

It is known that N13AI alloys belong to the LI2 kind of ordered structure
(Hansen, 1958). Since XRD (x-ray diffraction) reflections at superlattice
locations have been noticed upto very high temperatures (of the order of
1350 C), it is believed that this ordered structure exists as such upto its
melting point. However, a survey of literature indicates that significant

211
212
anomalies exist on the lattice constant (Noguchi et al., 1981) and order
parameter determination (Corey et ai., 1967, Stoeckinger et al., 1970, Aoki
et al. y 1975) of these alloys. Similar variations were noticed with regard
to thermal expansion coefficients (Stoeckinger et al., 1970) and specific
heat data (Davies et ai., 1965).

To clarify some of these anomalies, a systematic x-ray diffraction study was

undertaken on the stoichiometric and Ni-rich off-stoichiometric compositions
of NÎ3A1 alloys with and without boron additions. The first phase of our
investigation revealed (Ramesh et ai., 1990) that the Ll2 structure in
N13AI attains maximum stability at about 600°C beyond which it becomes
unstable relative to one or more structures. It is possible that the
structural changes we noticed might have some influence on the strengthening
behaviour of these alloys. Hence, the present study was aimed at
investigating the variation of order parameter with temperature and to
correlate the variation in structural ordering to the anomalous
strengthening behaviour of these alloys. Dilatometry and differential
scanning calorimetry (DSC) measurements were also carried out to study
their thermal properties.

EXPERIMENTAL PROCEDURE

Ingots of stoichiometric and off-stoichiometric compositions of Ni3Al alloys

with and without boron additions were made by repeated melting in a vacuum
induction furnace under argon atmosphere and by casting into a split type
copper mould. The ingots were homogenised at 1000°C for 2 days under a
vacuum of 2 x 10" torr followed by furnace cooling. Afew ingots were also
homogenised at 600 C for 3 days and 40 days; the reasons for which will
become apparant later. The values of nominal and analysed compositions are
given in Table 1. An Electron Probe Micro Analysis (EPMA) on all the alloys
revealed the homogenity of the composition. Filings (325 mesh size) produced
from the high temperature (1000 C-2 days) homogenised alloys were subjected
to 2-hour anneals at intervals of 100 C over the temperature range of
200-800°C and at 1000, 1200 and 1300°C in vacuum. For most cases, the high
temperature annealing was followed by furnace cooling to room temperature.
In a few cases, they were quenched in water from high temperature.

TABLE : 1 Alloy Compositions used in this study

Alloy Code Alloy compositions Analysed Nominial

Al (at%) B (wt%)

8B 75 at% Ni-25 at% Al (24.5) -

5B 75 at% Ni-25 at% Al (24.6) 0.1

+0.1 wt% B

2.1.A 76 at% Ni-24 at% Al (23.5) -

7B 76 at% Ni-24 at% Al (23.6) 0.1

+ 0.1 wt% B

X-ray diffractometric recordings of the filings were carried out using

nickel filtered Cu-Κα radiation. The long range order parameter (S) was
estimated based on a comparision of the integrated intensities of
superlattice [(100)&(110)] and fundamental [(200)&(220)] reflections using
 213
the relationship,
_ pif

s2 = li λ^Λ^ά.ΙίίΙΛ^ίίîîil itel£ ÎÉ___2£

(fNi-fAl) (Lp)s (e~ )s

where the symbols have the usual significance.

Dilatometric experiments were performed using a Research Model Dilatronic

(Theta) equipment. Two runs (second run was after quenching) were made for
each sample and the thermal expansion data were obtained over the range
27-1000°C after heating the specimens in vacuum at a slow rate of
3°C/minute. Prior to this, test runs were made with a nickel standard by
means of which suitable corrections were made for system deformation. The
calorimetric data were obtained from a Stanton Redcroft DSC 1500
Differential Scanning Calorimeter over the temperature range of ambient to
1000 C with AI2O3 used as a reference material. From the data obtained only
representative results are discussed here (refer Table II).

TABLE :II Alloys subjected to various experiments which are

discussed in this study.

Alloy code Order Dilatometry DSC Flow stress

parameter

8B X _ - -
5B X - - -
2.1.A X - - -
7B X X X X
X -» refers to results included in this paper.

The flow strength for the boron doped off-stoichiometric alloy homogenised
at 600°C and 1000°C was determined at different temperatures using a
thermo-mechanical simulator (Gleeble 1500) at a strain rate of
2 x 10"4 s"1.

RESULTS AND DISCUSSION

The values of the order parameter obtained for stoichiometric and

off-stoichiometric compositions of N13AI alloys (with and without boron
additions) over the temperature range (300-800 C) for a 2-hour anneal are
shown together with their theoretical values in Fig.1. It is noticed that
the ordering of LI2 structure is near perfect at a temperature of about
600°C in all the cases. The values quoted from the (110)/(220) pair is
slightly higher than that from the (100)/(200) pair owing perhaps to
texture, extinction or other reasons. Such variations are not unusual in
order parameter studies. Beyond 600°C there is a reduction in the order
parameter values especially as noticed from the (110)/(220) pair whose value
now goes below that due to the (100)/(200) pair in contrast to the earlier
situation. The order parameter estimated on the basis of an LI2 structure
for 1000°C gave untenable values like 1.159 for off-stoichiometric
composition (alloy 7B) and 1.25 for stoichiometric composition (alloy 5B).
All these observations indicate that the situation prevailing beyond 600°C
is totally different from the one that exists below this temperature. The
order parameter values for the temperatures above 800 C are not shown as
they were untenable. In general, boron addition appears to aid the ordering
and also the structural change.
214

^Without B-^Without Be- With B -«.With B -«.Theoretical

100-200 110-220 100-200 110-220

(a)

100 200 300 400 500 600 700 800 900

Temperature C

^Without B4.Wit.h0ut Β θ -With B -»--With B -^Theoretical

100-200 110-220 100-200 110-220

(b)

200 300 400 500 600 700 800 900

Temperature C

Fig.l Long range order parameter S as a function of temperature

for (a)stoichiometric N13AI and (b) for off-stoichiometric
NÎ3A1 (with and without boron additions).

Our earlier x-ray diffraction analysis results (Ramesh et al., 1990a, b)

also revealed the instability of the LI2 structure above 600°C and we
believe in the existence of two or more different structures in both
stoichiometric and off-stoichiometric compositions. The existence of these
different structures was confirmed by an experiment in which the samples
were cycled between 600 and 1000°C and held for long durations. The sample
subjected to homogenisation at 1000°C and subsequently water-quenched showed
many overlapping peaks in addition to the satellite peaks at (111) location.
When the same sample is taken to 600°C and held for 2 hours, all the
overlapping peaks vanished at (111) locations. When held for long durations
at 600 C, the reflections at (111), (200) and (220) become very sharp
identical to the earlier situation. When the sample was taken back to
1000 C, all the originally observed anomalies were seen once again. This
provides the evidence for the structural transformation in these alloys at
higher temperatures. Though the exact crystal structure of the new phase(s),
has not been identified it could perhaps be DO22 or DO19 structure referred
to by Noguchi et al .,(1981). It appears that this phase is more stable than
the LI2, not only when there is an increased proportion of the minority
 215
component (like boron) as stated by Noguchi et al., but also when the
temperature approaches about 1000 C.
First Run Δ Second Run

500 600 700

TEMPERATURE ° C

Fig.2 Instantaneous thermal expansion coefficient (a)

values for off-stoichiometric N13AI (alloy 7B).
«H METHODS

No. Start Final Raep/Iso Gas S.Rate

1 25 500 .7 1 30.0
2 500 1000 .7 1 30.0

35 3ö 3ö 3ö sSö äSö 75» Sô Sô Zoöö

TEMPERATURE °C

Fig.3 The DSC data for off-stoichiometric N13AI (alloy 7B).

The thermal expansion coefficient (a) in the range 300-900°C for the
off-stoichiometric composition is shown in Fig.2. In the first run,
decreases were noticed in the alpha values at around 350-450°C and
650-750°C. However, in the second run, the changes noticed were less
pronounced which can be related to an alloy with less or no phase change.
The calorimetric data obtained for the off-stoichiometric composition (alloy
7B) are shown in Fig.3. A distinct slope change can be seen at 350 C and at
630°C. Similar variations in the specific heat values were also noticed
earlier by Davies et ai (1965) at 350°C and 500°C and the reasons for the
changes at around 350°C are not clear. However, the variations noticed at
around 600 C in the thermal properties can be attributed to the instability
of the Ll2 structure.

The flow stress behaviour for the off-stoichiometric boron doped alloy
subjected to three different homogenisation treatments namely, at 1000°C for
2 days, at 600°C for 3 days and 40 days is shown in Fig. 4. The alloys
homogenised at 1000°C exhibited a higher anomalous strengthening behaviour
with temperature as compared to the alloys homogenised at 600 C.
216
— 1 ~ 76N1-24A1-0.1B - - Δ- 76M-24A1-0. IB Q 76W-24A1-0. IB
1000 C-2 days 600 C-3 days 600°C-40 days

1200

1000

i 800

$ 600
PS
(Λ
I 400
200

0
0 200 400 600 800 1000

TEMPERATURE °C

Fig.4 Effect of homogenisation temperatures on the flow

stress of off-stoichiometric Ni3Al (alloy 7B).

Among the two different holding times at 600°C, the alloys homogenised for 3
days exhibited a higher strengthening behaviour as compared to the one
homogenised for 40 days. This difference in the anomalous strengthening
behaviour for the same alloy subjected to different homogenisation
treatments can perhaps be attributed to the structural changes we noticed.
The alloy (homogenised at 600°C) containing predominantly a Ll2 structure
exhibits a lower anomalous strengthening behaviour as compared to that
containing the high temperature ordered structure (homogenised at 1000°C).
Further studies are in progress to understand more about these structural
changes.

REFERENCES

Aoki, K. and 0. Izumi (1975). Defect structures and long range order
parameters in off-stoichiometric N13AI. Phy.Stat.Sol (a), 32, 657-664.
Aoki, K. and 0. Izumi (1979). Improvement in room temperature ductility of
the LI2 type intermetallic compound N13AI by boron addition. J. Jpn. Inst.
Metals, 43, 1190-1195.
Corey C.L. and D.I. Potter (1967). Recovery processes and ordering in N13AI.
J. Appl. Phys. 38, 3894-3900.
Davies, R.G. and N.S. Stoloff (1965). On the yield stress of aged Ni-Al
alloys. Trans.Met. Soc.AIME, 233, 714-719.
Hansen, M.(1958) Constitution of binary alloys, McGraw-Hill, 119.
Kear, B.H. and H.G.F. Wilsdorf (1962). Dislocation configurations in
plastically deformed polycrystalline Cu3Au alloys. Trans.Met.Soc.AIME, 224,
382-386.
Noguchi, 0., Y.Oya and T.Suzuki (1981). The effect of Nonstoichiometry on
the positive temperature dependence of strength of NÎ3A1 and Ni3Ga.
Met.Trans, 12A, 1647-1653.
Ramesh, R., R. Vasudevan, B. Pathiraj and B.H. Kolster(1990). X-ray evidence
for structural transformations in N13AI alloys at higher temperatures.
Naturwissenschaften, 77, 129-130.
Ramesh, R., R. Vasudevan, B. Pathiraj and B.H. Kolster (1990). Ordering and
structural transformations in N13AI alloys.Communicated for publication.
Stoeckinger G.R and J.P. Neumann (1970). Determination of the order in the
intermetallic phase Ni3Al as a function of temperature. J.Appl.Cryst, 3,
32-38.
 WSl1a7

A Pseudo-HIP Process
Applied to the Reaction Synthesis of Intermetallic Compounds

P. H. Shingu, K. N. Ishihara and S. Umeda

Department of Metal Science and Technology,

Kyoto University, Yoshida Sakyoku, Kyoto, 606 Japan

ABSTRACT

A pseudo HIP (PHIP) process has been developed for the purpose of consolidation of
powder compacts to true density. This paper reports the application of this PHIP
process to the reaction synthesis of the NiAl intermetallic compound. Compacts of the
elemental powder mixture of Ni and Al or the powder mixture after subjected to the
mechanical alloying treatment for various length of time are tested as starting
material for PHIP. Significant improvement in mechanical properties of consolidated
NiAl compounds have been noted by the mechanical alloying treatment prior to the
reaction synthesis by PHIP.

KEYWORDS

HIP, Pseudo HIP, Reaction Synthesis, SHS, NiAl, TiAl

THE INTERNALLY HEATED PSEUDO HIP PROCESS

The HIP (Hot Isostatic Pressing) process is widely used for the densification of powder
compacts. The so called pseudo-HIP process has been introduced to substitute the
HIP process as a less costly and safer compaction technique (Ferguson, 1985). In
pseudo-HIP, sand or ceramic powder are used as the pressure transmitting media in
place of an inert gas in the case of HIP. Sand, being a solid, has very small

217
218
compressibility so that quite safe to handle when high pressure is applied by the use of
a common hydraulic press. Charging and discharging of sand can be much quicker in
comparison with gas.

Fig.l. A schematic drawing showing the set-up

for a internally heated Pseudo HIP process.

In the present work, a pseudo-HIP process with a heater embedded in sand around the
sample has been used (Shingu and Ishihara, 1990). A schematic drawing of the set up
is shown in Fig.l. The inner diameter of the stainless vessel was 110mm and the depth
was 140mm. A Kanthal resistance heater in a shape of a coil with 30mm diameter was
set around a sample of about 20mm in diameter. The whole set up can be put into a
vacuum chamber so that the sample can be pressed while the space between sand
grains can be evacuated. The pressure distribution in the sand has been estimated
using a pressure sensitive color paper embedded in various portions in the sand. The
pressure in the horizontal direction was about 50% that of the vertical direction when
the vertical pressure was about 40MPa. When the vertical pressure was increased to
about lOOMPa, the horizontal pressure became about 80% of the vertical pressure.

MECHANICAL ALLOYING OF Ni AND Al

Before compaction of powders, elemental Ni and Al powders were mixed and subjected
to ball-milling up to lOOhrs. Elemental powders of Ni and Al powders were mixed and
 219
put into a stainless steel vial of 120mm ID and 140mm long with 4kg of stainless steel
balls of 9mm diam. The sample powder of 80g was sealed in this vial with Ar gas. 3cc
of methanol was added for the purpose of lubrication. The vial was rotated at a rate
of 90rpm. The powder mixture after the mechanical alloying for a fixed time was
compacted in a die by the pressure of 1500MPa into a cylindrical shape of 15mm
diam. and 10mm high.

REACTION SINTERING BY PSEUDO-HIP

The powder compact samples were set in the pseudo-HIP apparatus, which is shown
in Fig.l, to be reaction sintered to form NiAl intermetallic compound. The heat of
formation of NiAl from the elemental Ni and Al is over 50kJ/mol. When the synthetic
reaction of NiAl starts, the temperature of the compact sample theoretically can reach
by the SHS reaction (Merzhanov and Borovinskaya, 1972, Munir and Anselmi-
Tamburini, 1989) to the melting point of NiAl (1911K). Fig.2 shows the heating
curves of Ni and Al powder compacts subjected to the mechanical alloying (MA) by
ball-milling for various time. Sudden rises in temperature shown in this figure indicate
the occurrence of the synthetic reaction. It is evident that the temperature of start of
the synthetic reaction becomes lower as the MA time increases. Kneading of Ni and
Al metal particles into fine lamination by MA apparently helps the solid state
synthetic reaction to take place at lower temperature.

O
o

f-,
S3
as

Fig.2. Heating curves of samples showing the onset of SHS reaction.

220
All samples were held at 1273K for Ihr under pseudo-HIP condition after the
occurrence of the reaction synthesis. Examination of phases by X-ray diffractometry
after pseudo-HIP revealed the existence of only the NiAl intermetallic compound
phase.

COMPRESSIVE STRENGTH TEST

Samples after pseudo-HIP treatment were cut into rectangular shape of

4mm x4mmX5mm for the compression test. Figure 3 shows the results of compression
tests for samples pseudo-HIP treated at lOOMPa in vacuum condition. Notable plastic
deformability and high fracture strength is seen for a sample MA treated for 50hrs.
Figure 4 shows SEM images of fractured surfaces of the samples shown in Fig.3.
Extreme refinement in grain size due to MA treatment is seen in this figure. The good
mechanical strength and deformability of the sample MA treated for 50hrs, as shown
in Fig.3, is due to the grain refinement by MA. For the lOOhrs MA treated sample, the
grains are still finer than that of 50hrs MA treated sample. However, the density
measurement indicated that the consolidation, by pseudo-HIP at lOOMPa, is better for
the 50hrs MA treated sample than the lOOhrs MA treated one.

Logarithmic strain

Fig.3. Compressive strength test results of samples which were mechanically alloyed
and P-HIP treated in vacuum at 100 MPa. The time of MA processing for each
specimen is indicated in the figure.
 221
CONCLUSION

Reaction synthesis of NiAl intermetallic compound has been performed for the powder
compacts of MA treated Ni and Al powder mixtures. For the pseudo-HIP condition of
lOOMPa in vacuum, the sample which was MA treated for 50hrs showed a compressive
fracture strength of nearly 2000MPa with a plastic strain of nearly 0.3. The marked
increase in mechanical strength can be attributed to the extreme refinement of NiAl
grain size due to MA.

I I
0 μ m 1 0 β m

( 0 , 1 0 , 50h. ) (100h. )

Fig.4. SEM images of fracture surfaces of samples the strength test results which were
shown in Fig.3.
222
REFERENCES

Ferguson B. L. (1985). Int. J. Powder Met. and Powder Tech., *2λ_, 201.
Merzhanov A. G. and Borovinskaya I. P. (1972), Doclady Akademi Nauk SSSR, 204 ,
366.
Munir Z. A. and Anselmi-Tamburini U., 1989, Mat. Sei. Rep.,_3_, (1989) 277.
Shingu P. H. and Ishihara K. N. (1990). J. Japan Soc. Powder and Powder Met., ΎΊ_ ,
670.
 WSl1b1

Shape Memory and Mechanical Properties

in Powder Metallurgy TiNi alloys

Sei Miura, Hiroyuki Kato, Takashi Koyari, Kazuo Isonishi

and Masaharu Tokizane

Department of Engineering Science, Faculty of Engineering, Kyoto

University, Kyoto 606, Japan.
** Faculty of Education, Ibaragi University, Mito, Ibaragi 310, Japan.
*** Department of mechanical Engineering, Faculty of Science and
Engineering, Ritsumeikan University, Kyoto 603, Japan.

ABSTRACT

Using prealloyed powders made by the Plasma rotating Electrode Process (P-
REP) method, a TiNi shape memory alloy was produced by the Hot Isostatic
Pressing (HIP). The obtained compact has a relative density of 99.6Z and
chemical analysis showed no detectable increase in impurity contents.

The results of electrical resistivity measurements and tensile test showed

that the P/M alloy produced by this method exhibits shape memory effect
(SME) and superelasticity due to thermally and/or stress-induced marten-
sitic transformation. An R-phase transformation also occurs, and SME and
superelasticity due to this transformation were observed.

It was found that the transformation and mechanical properties in the P/M
alloy prepared are almost identical to those of the typical alloy grown
from a melt.

KEYWORDS

Powder Metallurgy; Plasma Rotating Electrode Process; Hot Isostatic

Pressing; martensitic transformation; R-phase transformation; shape memory
effect; superelasticity.

INTRODUCTION
In recent years considerable attention has been focused upon "near net
fabrication" of TiNi alloys, which possess excellent properties with
regards to both mechanical strength and shape memory characteristics.
However, until now, TiNi shape memory alloys have not been very success-
fully produced by usual powder metallurgical methods and the stress-strain
characteristics have not been investigated in detail.

Recently the present authors have reported that, by using the prealloyed
powders made by the P-REP method, and consolidating them, the TiNi alloy
produced has shape memory properties almost identical to the typical alloy
grown from a melt (Kato et al.,1990).
The P-REP method, which we used for the production of TiNi powders, is
characterized by uniformity in the shape and size of the powders (Isonishi

223
224
et al.,1989), and by effective suppression of impurity contamination. The
former enables the homogeneous densification in the solidification of
powders to occur. The latter is indispensable in the production of TiNi
shape memory alloys having desired transformation temperature and shape
memory properties, since the nature of the martensitic transformation in
TiNi is strongly sensitive to small amounts of impurities, such as oxygen
and carbon (Wasilewski et al.,1971, Shugo et al.,1985). Therefore P-REP is
a suitable process to prepare powders for TiNi shape memory alloys.

In our previous study only the shape memory effect (SME) was observed,
since the P/M alloy used had a nearly equiatomic composition and had been
heated at 1073K during the HIP treatment. It has been known that an equi-
atomic TiNi alloy also shows superelasticity when it suffers cold work and
subsequent annealing at about 673K (Miyazaki et al., 1982).

To examine both the shape memory and the superelastic properties of the
P/M alloy solidified from P-REP powders, we investigated transformation
and mechanical properties of the alloy in the as-HIP'ed state, and after
the alloy had been cold work and annealed at 673K.

EXPERIMENTAL

Using a prealloyed ingot prepared in a high frequency induction furnace,

TiNi powders were produced by P-REP. The obtained powder had a uniform
size of 150μπι in diameter under the appropriate condition in P-REP; the
anode diameter was 50mm and the rotating velocity was 9X10 3 rpm in a He
atmosphere. The consolidation of these powder by hot isostatic press
(HIP), at 1073K and 180MPa for 2h, achieved a compact, having a relative
density of 99.6%.

Table 1 shows the results of the chemical analysis of the prealloyed ingot
used as the electrode in P-REP, the powder and an as-HIP'ed alloy. It was
found that the weight fractions of Ti, Ni and impurities were not altered
during the P-REP and HIP processes.

TABLE 1. Composition of the P/M TiNi Alloy (at.%)

Ti Ni 0 C

Prealloyed Ingot 50.0 49.7 0.17 0.13

P-REP Powder 50.1 49.6 0.17 0.13
As-HIP'ed Alloy 50.1 49.7 0.14 0.14

These alloys were cut into specimens of rectangular shape with a spark
cutting machine and a slitting wheel. Surfaces of the specimens were
mechanically and electrolytically polished. For surface observation,
boundaries between adjacent powder particles and grain boundaries inside
powder particles were revealed by etching using a solution of HF: HN0 3 :
glycerine (1:1:8). Some of the as-HIP'ed specimens were rolled at R.T. to
67% reduction and annealed at 673K for 24h in a salt bath.

Electrical resistivity measurements were made by the conventional four

point method. Tensile tests were performed with an Instron type testing
machine at a strain rate of 5.6X10"4 /sec. The cold-rolled specimens were
deformed in the rolling direction.
 225

RESULTS and DISCUSSION

Surface Observation of the P/M Alloy

Optical micrography of the etched surface of the P/M alloy, fig.1(a),

shows that boundaries between adjacent powder particles were polygon-shape
on the surface of the specimen, and that grains existed in each particle.
The mean grain size was 63μπι, which was determined by the cross-cut
method. This magnitude is almost identical to the mean grain size of a
TiNi alloy grown from a melt. Figure 1(b) shows a scanning electron
micrograph of the triple point of the particle boundaries. As is expected
in a high density P/M alloy, pores at these points were too small to be
observed.

Fig.1 (a) Optical and (b) SEM micrographs of

the etched surface of an as-HIP'ed P/M alloy.
226
Thermal Transformation Behaviours
The variation of electrical resistance with temperature in an as-HIP'ed
and a cold-rolled specimen is shown in fig.2 and 3, respectively. The
triangular form of the resistivity curve in the cooling run of an as-
HIP'ed specimen is typically observed during martensitic transformation in
a TiNi alloy. The curve for the cold-rolled specimen indicates that an R-
phase transformation (Ling and Kaplow,1981) occurred prior to the
martensitic transformation during cooling.

I.I "As: •HlP'ed

Ms
£ 1.0 -
σ
1
k.
ί 0.9 . Mf / A
>
£ 0.8 - ^ ^
\J^
Q>
k.

n0.7 -
O
k.

t3 0.6 • heating
0)

LU
o cooling
0.5
150 200 250 300 350 400
Temperature / K

Fig.2 Variation of electrical resistivity ratio

with temperature for an as-HIP'ed specimen.

o 1.2 Γ Cold-rolled
o
. .
k.

>» 1.1
'>
tf>
1.0
<>
/
Q>
0.9
σ
υ 0.8
k_
o
(1)
• heating
li 1 0.7 o cooling
_l I l_l L_l I L_l I
200 250 300 350 400
Temperature / K

Fig.3 Variation of electrical resistivity ratio

with temperature for a cold-rolled specimen.
 227

Mechanical Properties; Shape Memory Effect and Superelasticity

The stress-strain curves and the temperature dependence of yield stress
determined from these curves for the as-HIP'ed specimens are shown in
fig.4 and 5, respectively. Before deformation at each temperature the
specimen was heated to 373K and cooled to the testing temperature,
therefore the initial state of a specimen before deformation corresponded
to the electrical resistivity curve of the cooling run. In these stress-
strain curves, the residual strain after deformation was recovered by
heating the specimen to 373K; namely the as-HIP'ed alloy exhibited SME
above and below the transformation temperature.

As-HIP'ed
23IK 290K 311K 326K
£ 200 r

"> 100

ω
0 I
kz
0
Strain (%)

Fig.4 S t r e s s - s t r a i n curves for the as-HIP'ed

specimens.

500 1 ■1 1

Γ A s ^HIP'ed
4 0 0 rΓ Ms -311 K J\
L Mf = 275K J J
σ
Q_ 1 (from E.R. measure- / |
2 300 ment) 4 1
h

t 200
c/>
r* · Mf
Ms/ I
100
•· 1/
• 7

1 1 1 1

250 300 350

Temperature / K

Fig.5 Temperature dependence for yield stress

for the as-HIP'ed specimens.

Different stress-strain behaviour, however, was observed in cold-rolled

specimens, as shown in fig.6. The temperature dependence of the yield
228
stress is shown in fig.7. In correspondence with the electrical
resistivity curve in the cooling run in fig.3, at temperatures between the
Mf and the Rs the martensitic phase coexisted with the R-phase before
deformation and the stress-strain curves showed two-stage yieldings.

Two-stage yielding was also observed at temperatures just above the Ms. In
this case the specimen was the parent phase before deformation and the
first and second yieldings are due to the initiation of stress-induced R-
phase and martensitic transformation, respectively (Miyazaki and Otsuka,
1987). Above the temperature at which the yield stress due to R-phase is
equal to that due to stress induced martensitic transformation, super-
elasticity due to stress induced martensitic transformation occurred.

Cold-rolled
400,
345K

I 2 0 I 20
Strain ( %)

Fig.6 S t r e s s - s t r a i n curves for the cold-

rolled specimens.

500 I 1 1
... r .
I Cold-rolled

400h\ TR-323K
/1
1 Ms*295K
/ 1
σ
f Mf = 246K
5 300 r (from E.R. measure-
l\
ment )

\
t 200 Ms
en Mf 1
- i *.·
looh • · . . ·. ·
o
o
Ί
°oo'
200 250 300i—> i 350
i .. 1 J —

Temperature / K

Fig.7 Temperature dependence of yield

stress for the cold-rolled specimens.
 229
In order to determine the maximum strain recoverable due to SME or super-
elasticity, an as-HIP'ed and a cold-rolled specimens was deformed to
relatively larger strain, as shown in fig.8 and 9, respectively. In the
as-HIP'ed specimen 5.8% of residual strain after deformation at 316K was
recovered due to SME and in the cold-rolled specimen 6.9% strain at 351K
was recovered due to superelasticity.

500

3 4 5 6
Strain (%)

Fig.8 Stress-strain curves for the as-HIP'ed

specimen. Dotted lines show strain recovered
by heating the specimen to 373K.

£ 500 r Cold-rolled Deformed at 35 IK

0 1 2 3 4 5 6 7 8 9 10
Strain (%)

Fig.9 Stress-strain curve for the cold-rolled

specimen.
230
Saburi et al., (1983) showed that a polycrystal1ine TiNi alloy exhibited
small mechanical hysteresis - the difference between the stress required
for the occurence of forward and reverse stress-induced martensitic
transformation, compared with a single crystal. As well recently,
Nakanishi et.al.(1989) found surprisingly large strain recovery due to
superelasticity in the P/M processed Cu-Zn-Al alloy. Their results could
be ascribed to the effect of the refinement of grain size. However the P/M
TiNi alloy used in the present study has the same grain size as the
typical TiNi alloy, shown in fig.1, so the refinement effect would not be
expected in the present case.

The amount of shape recovery due to SME or superelasticity in the P/M

alloy is comparable to that in the usual melted alloy. This indicates that
the particle boundaries existing in the P/M alloy produced by the present
method have strength almost equal to the grain boundaries within a melted
alloy.

ACKNOWLEDGEMENT

We are grateful to The Furukawa Electric Co. Ltd. for the provision of
TiNi prealloyed ingot, and to Mr. H. Esaki of Ritsumeikan University for
his experimental support and valuable discussions.

REFERENCES

Isonishi,K.,Kobayashi,M. and Tokizane,M.(1989). Production of TÎ-6A1-4V

Alloy Powders by Plasma Rotating Electrode Process, Tetsu-to-Hagane,75,
1913-1920.
Kato,H.,Koyari,T.,Miura,S.,Isonishi,K.,and Tokizane, M. (1990). Shape
Memory Characteristics in Powder Metallurgy TiNi Alloys. Script.Met.et
Mater.,24, No.12(in press).
Ling,C.Hung and Kaplow,R.(1981). Stress-Induced Shape Change and Shape
Memory in the R and Martensite Transformations in Equiatomic NiTi,
Met.Trans., ΠΙΑ, 2101-2111.
Miyazaki,S.,0hmi,Y.,0tsuka,K. and Suzuki,Y.(1982). Characteristics of
Deformation and Transformation Pseudoelasticity in TiNi Alloys, J.de
Physique.,C4,255-260.
Miyazaki,S.and Otsuka,K.(1985). Deformation and Transition Behavior
Associated with the R-Phase in TiNi Alloys, Met.Trans., 17Α, 53-63.
Nakanishi,N.,Shigematsu,T.,Inaba,T.,Nagai,S. and lwatsu,0.(1989), Shape
Memory Characters in Powder metallurgical Cu-Zn-Al Alloys, J. of the
Japanese Soc.of Powder and Powder Metallurgy, 36,153-157.
Saburi,T.,Yoshida,M. and Nenno,S.(1984), Deformation Behavior of Shape
Memory Ti-Ni alloy crystals., Script.Met., j^,363-366.
Shugo,Y., Hanada, S. and Honma, T.(1985). Effect of Oxygen content on the
Martensite Transformation and Determination of Defect Structure in TiNi
Alloys, Bulltein of R.I.T.U.(SENKEN IH0),41,23-34.
Wasilewski,R.J., Butler,S.R.,Hanlon,J.E. and Worden,D.(1971). Homogenity
Range and the Martensitic Transformation in TiNi, Met.Trans.,2, 229-238.
WS11b2

STUDY OF PSEUDOELASTIC BEHAVIOUR OF POLYCRISTALLIN SHAPE

MEMORY ALLOYS BY RESISTIVITY MEASUREMENTS
AND ACOUSTIC EMISSION

Pierre VACHER and Christian LEXCELLENT

Laboratoire de Mécanique Appliquée associé au CNRS

Faculté des Sciences et des Techniques
La Bouloie - Route de Gray
25030 BESANCON - FRANCE

ABSTRACT

The determination of the hyperelastic behavior of polycristaLline Cu Zn Al

shape memory alloys is performed using loading-unloading tension and
tension-compression tests with resistivity and acoustic emission
measurements. In the case of uniaxial mechanical· - loading, these
measurements show, on the one hand, that the hyperelastic strain is
proportional to the volume fraction x of martensite, and on the other
hand, that the obtained acoustic emission data allows^ the evolution of x
during the mechanical test, to be followed.

KEYWORDS

Alloys - Shape Memory - Martensitic Transformation - Pseudoelastic -

Resistivity - Acoustic Emission

INTRODUCTION

In the present article, the case concerning pure transformation plasticity

(absence of classical plasticity) will be examined. The elementary
mechanisms are of two types (Patoor et Al. (1987)) :
- (reversible) formation of a variants of martensite from austenite,
- migration of the interfaces between the different variants of
martensite already formed and modification of the corresponding
volume fractions.

During the loading-unloading tension and tension-compression tests on

three polycristalline shape memory alloys Cu Zn Al, the originality of the
present approach resides in the parallel measurement of the :
(i) mechanical parameters (stress curve σ -*■ strain c)
(ii) resistivity used as an indicator of the volume of the transformed
martensite
(iii) accumulated energy E during the acoustic emission (Yamaguchi, 1988)

The equations of pseudo-elastic behavior will be deduced from the

information delivered by these totally independent techniques.
231
232

EXPERIMENTAL PROCEDURE

Choice of the appropriate alloys and mechanical tests

The three shape memory alloys, two of which have transformation

temperatures slightly less than room temperature, have be manufactured by
the company "Trefimetaux". Resistivity measurements have allowed the four
conventional temperatures at 0 % and 100 % of the phase transformation
under zero stress to be obtained.

Alloy Trace metals MF(°C) M

S
A
s A
F
R 232 NO 6 15 17 19,5
R 244 YES 1 5,5 11
R 205 YES -110,5 -98 -94 -91

The trace metals are constituted of a few hundred PPM of Zr, Mg, Fe...

The desired metallurgical state is the monophase ß state and it has been
obtained by a standard open air heat treatment of 10 minutes at 850°C
followed by a water quench.

After treatment, the metallurgical observation shows a single phase

(mother phase or austenitic ß) with an average grain size of S = 300 /im.
The machined samples are rectangular in cross-section for R 205 (gauge
length 75 mm, width 10 mm and thickness 0,6mm) and circular in cross-
section for R 232 and R 244 (gauge length 25 mm, diameter 6 mm).

The mechanical tests performed are primarily loading-unloading tension and

tension-compressions loadings, at temperatures T just over the Ap
transition temperature (analysis of pure transformation plasticity).

The acoustic emission measurements have only been able to be made at room
temperature.

Resistivity measurements

The measurements of resistivity is used as an indicator of the volume of

martensite that has formed. During the mechanical test, a correction has
been made for the effect of the strain on the voltage measured by the four
point method.

In the pure martensite state, (R 205,σ - 0,55 MPa/s,-129°C = T<M f ), the

strain results primarily from the motion of the interfaces which opere
under the effect of the applied external stress. This results in a slight
increase in the resistivity sample with the strain. The variation of this
resistivity pM with the axial strain ε^ has been accounted for. For the
temperature value for which the stress induced martensite no longer forms,
(R 205, σ - 0,55 MPa/s, T « 101°C), the measurements show that even
significant plastic strains (until around 14 %) do not noticeably modify
the resistivity of the austenite (values less than 5 % ) .
 233

Finally, the volume fraction of martensite is given by :

P(x) where the resistivity of the pure austenite is

- 1
(2a)
(1)

l-·1]
and the resistivity of the martensite at a strain of ε 11 is

Ή " 'M(C11> and

'on =
^Μ(ε11 = 0) (2b)

Acoustic emission data

The acoustic emission (A.E.) is due to local microdisplacements which are

produced in the material. Analysis of the generation and character of the
acoustic emission signals yields an insight into the dynamics and kinetics
of the elastic field in the crystal lattice. In this context, in the
absence of external stress by heating and cooling processes, the
characteristics of acoustic emission induced by the thermoelastic phase
transformation have been determined, using single cristal Cu Al Ni, shape
memory alloy (Yoshida and Al. 1988). A.E. is easily detected by suitable
piezoelectric transducers. It is usually analyse by counting the number of
times that the electric signe furnished by the transducer crosses a
prestablished threshold level (ring-down counting technique)
(Scruby, 1987).

In order to quantifiy the martensitic transformation during the mechanical

tests, the accumulated energy E(t) has been calculated at the instant t.

It remains to be seen if this energetic parameter can be related to

the fraction x of transformed martensite.

EXPERIMENTAL RESULTS AND ANALYSIS

Slightly above the transformation temperatures, for these polycristalline

Cu Zn Al alloys, the behavior is purely hyperelastic, that is to say, a
complete reversion of the strain with the discharge for a total strain
et < 2 % (R 205, fig. 1,2).

This 2 % threshold value for polycristal Cu Zn Al alloys seems to be

currently accepted.

For tension-compression tests, the stress response is dissymmetric

((<7max')tension < v(-σ m ι. η Compression)
' Γ
' (figure
>· σ 3 and 4 ) .

This corresponds to a dissymmetric response in the same direction as the

fraction of martensite formed ((x )tension < (x Compression)
r
(figure 7). v
max' '

Moreover, the pseudo-elastic strain is directly proportional to x for

these tests at constant temperature (T slightly higher than A p ) and at
constant strain or stress rates.

(3) in agreement with recent resistivity measure-

Here ment during stress strain tensile curve of 0N0
(1990)
234

Alloy Ms °C A
F Test T a (%)
R 205
-98 -91 t -80 3,2
with trace metals
-70 4,1
ö = 0,55 MPa s"1
R 244 t + 1 % 8,6
1 11 24°C
with trace metals c - 1 % -4,3
t tension
t + 2 % +7,7
I = lu' 4 s"1 24°C c compression
c - 2 % -5
R 232 t + 1 % 8
without trace metals 15 19,5 24°C
I = 10"4 s"1 c - 1 % -3,5

The hyperelastic strain ε is then bounded since the volume fraction x of

martensite varies from 0 to 1. The parameter a represents the maximum
theoretically accessible value of ε . Within experimental error, the
magnitude of this parameter a is two times larger in tension than in
compression. It probably can be related to the calculation made by Patel
and Cohen (1953) for the critical value of the stress σ^$ to initiate the
transformation : σΜ8 = b(T - M s ) with b on the order of 2 MPa/°C for the
alloys in question in tension and b slightly less than (-3 MPa/°C) in
compression. To summarize, figure 3 and 4 shows that the martensite forms
more easily in compression than in tension.

The accumulated energy E which is plotted as a function of the stress has

been obtained in parallel with the acoustic emission.

Refering to a thermodynamic formulation associated to the transformation,

(4) (Ortin and Planes (1988)) the following hypothesis has been made :
Et = Ax (4)
and the parameter A chosen such that : A — (E )max : (x ) (5)
where (E )max : maximum accumulated energy obtained by acoustic emission
at the end of the loading.
( X Q C ) : volume fraction X Q measured by resistivity at the end of the
loading

The results show that the plot of the normalized energy E as a function
of the stress σ, coincides with the evolution of x with σ (figures 3, 4,).

Even if the numerical value of the measured accumulated energy E is not

accurate, its evolution seems to coincide with that of the fraction of
martensite which has formed.

On one part, Patoor and Al. (1988) examine the behaviour of single and
polycristals undergoing a thermoelastic transformation with a "microscopic
=* macroscopic" approach.
 235

On the other part, Leblond and Al. (1986) use the Hill-Mandel
homogeneization method to provide theoritical foundations of behavior laws
during phase transformations. Theses authors obtained the same result
(equation (3)) i.e. :

έ ΡΕ - a( )x (3 bis)

CONCLUSION

A particularly simple relation is apparently obtained between the

hyperelastic strain and the volume fraction x of martensite during
loading-unloading tension or tension-compression tests where resistivity
and acoustic emission measurements have been employed. However, the
proportionality coefficient is already different in compression than in
tension. In addition, if the transformation kinetics of χ(σ,Τ) are
expressed in the exponential form suggested by Koistinen and Marburger
(1959) and revised for the shape memory alloys by Tanaka and Al.(1986),
then discontinuity problems are encountered in the formulation. The
transformation kinetics are much slower under the effect of stress (σ =
cte, cte - T > A F ) than under the effect of temperature alone (σ = 0, T
varying from Ms to M p ) .

In other words, if x is an internal variable necessary for the description

of the hyperelastic behavior, it is not sufficient. An orientation
parameter must be introduced which indicates the nature of the formed
martensite which is essentially different under the effect of a uniaxial
loading applied to the polycristalline sample than under an isotropic
cooling. This is the reason for which certain models are constructed using
a local approach (Leblond and Al. (1956), Patoor and Al. (1988)). Then, an
homogenization method allows more realistic macroscopic behavior laws to
be obtained.

REFERENCES

KOISTINEN D.P. and MARBURGER R.E., Acta. Met.. (1959) 7, 59-70

LEBLOND J.B., MOTTET G. and DEVAUX J.C. (1986), J. Mech. Phvs. Solids. 34.
44, 395-409
ONO N. (1990), Mat. Trans. JIM. 31, 5, 381-385
ORTIN J., PLANES A. (1988), Acta. Met.. 16, 8, 1873-1889
PATEL J.R. and COHEN M. (1953), Acta. Met.. 1, 531-538
PATOOR E., EBERHADT A. and BERVEILLER M. (1987), Acta. Met.. 25, 11, 2779-
2789
SCRUBY C.B. (1987), J. PHYS. E. SCI. INSTRUM.. 20, 946-953
TANAKA K., KOBAYASHI S. and SATO Y. (1986), Int. J. of Plasticity. 2, 59-72
YAMAGUCHI K. (1988), Progress in acoustic emission IV. Proc. 9 — Int. Ac.
Em. Sy. KOBE Japan, November 14,17, (edited by Y. YAMAGUCHI, I. KAMPARA
and Y. HIG0), 1-10
YOSHIDA K., SAKAMAKI K., TAKAGI H., OHASHIK. and YOSHIDA M. (1988),
Progress in acoustic emission IV, Proc. 9 — Int. Ac. Em. Sy. KOBE
Japan November 14-17, (edited by Y. YAMAGUCHI, I. KAMPARA and Y. HIGO)
583-589
236

fig. 1 : Loading-unloading tensile curve

(R 205, ε - 10"4 s"Ί , T - -73°C)

fig. 2 : Proportionality between ε.PE and x

(R 205, σ = 0 , 5 5 MPa s" 1 , T = -80°C)

fig. 3 : P r o p o r t i o n a l i t y between £ P E , x and E t

(R 244, ε - 10"4 s"1, ε - ±1%, T - 24°C)

fig. 4 : Proportionality between ε , x and E.

(R 232, ε = 10"4 s"1, ετ = ±1%, T = 24°C)
WS11b3 DEFORMATION BEHAVIOR OF TiNi SHAPE MEMORY ALLOY UNDER
THERMOMECHANICAL CYCLING
H. TOBUSHI, H. IWANAGA, K. TANAKA, T. HORI and T. SAWADA
H. TOBUSHI and H. IWANAGA
Department of Mechanical Engineering
Aichi I n s t i t u t e of Technology
1247 Yachigusa, Yagusa-cho, Toyota, 470-03 Japan
K. TANAKA
Department of Aerospace Engineering
Tokyo Metropolitan I n s t i t u t e of Technology
6-6 Asahigaoka, Hino, Tokyo, 191
Japan
T. HORI and T. SAWADA
Graduate School
Aichi I n s t i t u t e of Technology

ABSTRACT
The experiments with c y c l i c loading-unloading and the experiments with
heating-cooling under c o n s t a n t s t r e s s of TiNi shape memory a l l o y s were
c a r r i e d o u t . This paper shows t h a t , during the thermomechanical c y c l i n g ,
the transformation s t r e s s e s of the m a r t e n s i t i c transformation and the
r e v e r s e transformation d e c r e a s e , but the transformation temperatures
i n c r e a s e . The c y c l i c recovery s t r a i n is r e p r e s e n t e d by the r e l a t i o n among
the heating temperature, the cooling temperature, the transformation
l i n e s on the s t r e s s - t e m p e r a t u r e plane and the transformation s t r a i n .

INTRODUCTION
In the a p p l i c a t i o n for an a c t u a t o r , a robot and a solid s t a t e heat engine
(Iwanaga, et a l . . 1988, Tobushi, et a l . . 1985, Tobushi, et a l . . 1990b),
the shape memory a l l o y is used as a working element, and the element
performs cyclic motions. In these c a s e s , the decrease in recovery
deformation and recovery force may become important. In oder to evaluate
the r e l i a b i l i t y in the shape memory a l l o y element, the behavior of the
above-mentioned c h a r a c t e r i s t i c values subject to thermomechanical cycling
becomes c r u c i a l .
In the c u r r e n t study, the p r o p e r t i e s of shape memory a l l o y s subject to
the above-mentioned thermomechanical cycling are d i s c u s s e d . That i s , the
c y c l i c p r o p e r t i e s of "yield c o n d i t i o n " in the s t r e s s - i n d u c e d m a r t e n s i t i c
(SIM) transformation and the reverse transformation and recovery
deformation caused by both transformations a r e d i s c u s s e d . Experiments
with cyclic loading-unloading and experiments with thermal cycling under
constant s t r e s s on the TiNi shape memory a l l o y were c a r r i e d o u t .

EXPERIMENTAL PROCEDURES
Material and Experimental Apparatus

The material was a TiNi shape memory a l l o y wire produced by Furukawa

E l e c t r i c Co., Ltd. The specimen was given shape-memory of a s t r a i g h t
l i n e . This was done by keeping the wire s t r a i g h t a t 673K for 20min and
237
238
cooling in the furnace. The reverse-transformation finish temperature At
was about 323K. The outer diameter of the specimen was 0.75mm and the
gauge length 20mm.
The experimental apparatus consisted of a t e n s i l e machine and a heating-
cooling device described in detail in a previous paper (Tobushi, et a l . .
1990a). The axial force, displacement and temperature were measured by a
l o a d c e l l , an extensometer and a thermocouple, r e s p e c t i v e l y . The specimen
was heated or cooled by hot or cold a i r .
Tests with loading-unloading c y c l e s

In the t e s t , the loading and unloading processes were repeated at the

temperature T2 avove A t . The SIM transformation s t a r t s at the s t r e s s <JMS
and completes at σΜ* in the loading process. In the unloading process,
the reverse transformation s t a r t s at s t r e s s σAB and is completed at
σM . The strain rate in the loading and unloading processes was 2%/min.
The values of T2 were 333K, 353K and 373K. The values of maximum strain
ε m were 1, 2, 3, 4, 6 and 8%. The process was repeated 100 times.
Tests with thermal cycling under constant s t r e s s

At f i r s t , the i n i t i a l strain sm with the corresponding s t r e s s am were

given at the temperature Ti. Following this process and keeping the
s t r e s s am constant, the process with heating at T2 followed by cooling
at Ti was repeated 100 times. The values of € m were 1, 2, 4 and 6%. The
value of Ti was 293K and the values of T2 were 333K, 353K and 373K. The
rate of heating and cooling was about 1.5K/s.

EXPERIMENTAL RESULTS AND DISCUSSION

Stress-strain-temperature relation during loading-unloading cycles
Stress-strain curve : The s t r e s s - s t r a i n curves are shown in Fig.l for
T2=373K and €m=8%, at which the SIM transformation is completed. The
curves are parametrized by the number of cycles N.
1200i ,

Fig.l Stress-strain curves in test with loading-unloading cycles

 239
The phenomena observed in each t e s t are summarized as follows. (1) The
s t a r t i n g s t r e s s and completing s t r e s s of the SIM transformation and the
reverse transformation decrease with the increase in N, and the p o s i t i o n
of the s t r e s s - s t r a i n curve becomes lower, i . e . the p s e u d o e l a s t i c
h y s t e r e s i s moves to smaller s t r e s s e s . (2) The decrease in s t r e s s of the
SIM transfomation is l a r g e r than that of the r e v e r s e transformation. (3)
The nonrecoverable s t r a i n € P at an end of each cycle i n c r e a s e s with N,
and the position of s t r e s s - s t r a i n curve moves toward the r i g h t . (4) The
area surrounded by the s t r e s s - s t r a i n curve which r e p r e s e n t s the
d i s s i p a t e d s t r a i n energy density becomes small with N. (5) The phenomena
mentioned in each term vary s i g n i f i c a n t l y in the e a r l y cycles and the
r a t e of these v a r i a t i o n s decreases with N.
S t a r t i n g line and completing line of transformation

The s t a r t i n g condition and the completing condition of the SIM

transformation and r e v e r s e transformation a r e difined by a s t a r t i n g l i n e
and a completing line of each transformation on a s t r e s s - t e m p e r a t u r e
plane (Tanaka, et a l . . 1986, Tanaka et al.» 1988).
The s t a r t i n g s t r e s s and completing s t r e s s of each transformation in
r e l a t i o n to temperature T for N=l and N=100 and for £m=8% are shown in
Fig.2.
As seen in F i g . 2 , on the whole, the position of each transformation line
for N=100 moves downward. This means t h a t , in the case of c y c l i c
deformation under constant temperature, each subsequent transformation
occurs on a lower level of s t r e s s .

Strain behavior subjected to v a r i a b l e temperatures under c o s t a n t s t r e s s

S t r e s s - s t r a i n curve : The s t r e s s - s t r a i n curves obtained by the test with
the thermal cycling under constant s t r e s s a r e shown in F i g . 3 . In F i g . 3 ,
the whole curves for the case of i n i t i a l s t r a i n £ m = l , 2 and 6% a t high
temperature T2=373K are p l o t t e d . In the f i g u r e , the s t r a i n at high
temperature € 2 and the s t r a i n at low temperature f i for N=l and N=100
and € i for N=2 a r e indicated by the several symbols. Also in the f i g u r e ,

1 000 Γ -1
—r i 1 1
N=l N=100
^ 800 L ÖV,= O • ^yyc. -1
öV Φ Φ
^ 6 0 0 L ÖA* Δ ▲
ÖAf A AQ sly i?^
/ ^ ▲
§ 400 •"
s mk. —1

Ç/ y
200 ·"* " " ""''
' >7
y n
A
~ —
■
y

0 1 ·"
2 18 0 3 01 0
\A\
._._.
320
1

34 0
y

360
1

38 0
1

400
ι

Temperature T K

Fig.2 Relation between transformation s t r e s s e s and

temperature for N=l and 100
240

1000
«3 OE2Ü) · ε 2 ( ΐ ο ο )
Δ £ ι ( 1 ) A Ei (100)
(X 800 A Ex (2)

600

n 400
m 200

~0 2 4 6 8
Strain B %
Fig.3 S t r e s s - s t r a i n curves in t e s t with thermal cycles under
constant s t r e s s (T2=373K, e m = l , 2 and 6%)

a s t r e s s - s t r a i n curve obtained by a t e n s i l e t e s t at 373K for maximum

s t r a i n of 8% is shown with a thin curve. As found from the curve in the
i n i t i a l loading process at Ti, the i n i t i a l s t r a i n € m of 1% is near the
s t a r t i n g point of the SIM transformation, s m of 2% in the SIM
transformation region, and c m of 6% in the hardening region of the
m a r t e n s i t i c phase.

It is seen in Fig.3 that the difference of s t r a i n s for high and low

temperature is large for £m=2% while that is small for € m =l and 6%. If
£ m is in the SIM transformation region as it is for € m =2%, t\ for
N=100 is about 5% which is nearly equal to the s t r a i n of the complete SIM
transformation ( H f at Ti.
Strain behavior with heating and cooling

We have p l o t t e d in F i g . 4 , for each i n i t i a l s t r a i n 6 m and high

temperature T 2 , the r e l a t i o n between s t r a i n and temperature as i t
changes with the number of cycles N=l, 2. 5, 20, 50 and 100.
The phenomena observed in each experiment may be summarized as follows.
(1) Although T 2 >Af, if T2 is not higher than a c e r t a i n temperature,
recovery s t r a i n by reverse transformation does not appear. (2) Both
s t a r t i n g temperature and completing temperature of the SIM transformation
and the reverse transformation r i s e with N, and the position of the
h y s t e r e s i s loop of the s t r a i n - t e m p e r a t u r e curve moves toward the r i g h t .
(3) Both s t a r t i n g s t r a i n and completing s t r a i n of the SIM transformation
and the reverse transformation increase with N, and the position of the
h y s t e r e s i s loop of the s t r a i n - t e m p e r a t u r e curve moves upward. (4) In the
case of 2% and 4% for € m which are in the SIM transformation r e g i o n ,
the s t r a i n at low temperature Ti with thermal cycling becomes 5% which i s
equal to the completing s t r a i n of the SIM t r a n s f o r m a t i o n . If T2 is low,
the reverse transformation becomes d i f f i c u l t to appear with thermal
cycling and the h y s t e r e s i s loop diminishes. (5) In the case of € m =l%,
the R-phase transformation occurs s t a b l y for the thermal c y c l e s . In the
case of € m ^ 2 % , the R-phase transformation disappears with the number of
cycles.
 241

8 1 '

T2 = 3 3 3 K * 1% T2=373K
6 -

4
N N
co 2 - 1 , 2 5 , 2 0 . 50 , 1 0 0 6m=jwoJ 1 , 2 , 5 , 20 , 50 , 100
c j - t ( 1
-ra 0
£ B Γ" ' ' 1
in N T2 = 3 3 3 K - I·' ' em=4%
6 Γ 50 , 100 T2=373K -

IT
1 1
4

2
.2,5 20 [ ^SH^^ vKl ]
^ \ ^ _
50 ,N100
5
·20
1
1 y .... \ 1
- ^'^^ 1 ,21
' ' 1 , 1 ., i _ __^ !
0 280 300 320 340 360 380 280 300 320 340 360 380

Temperature T K

Fig.4 Strain-temperature curves in t e s t with thermal c y c l e s

under constant s t r e s s

Conditions for growth of recovery s t r a i n

Based on the c o n s i d e r a t i o n s mentioned above, the behavior of the s t a r t i n g

line and the completing line of the SIM transformation and the reverse
transformation with the thermomechanical cycling is schematically shown
in F i g . 5 .
As seen in F i g . 5 , under the thermomechanical c y c l i n g , the s t a r t i n g l i n e
and the completing line of the SIM transformation and the corresponding
l i n e s of the reverse transformation move downward and to the r i g h t . From
F i g . 5 , the condition for growth of each transformation may be defined as
follows. (1) In the loading process to the point A a t low temperature Ti,
the SIM transformation a p p e a r s . In the case that the temperature i s
raised to T2 keeping the s t r e s s σ α c o n s t a n t , the r e v e r s e
transformation does not appear in a s t a t e a t the point B even if T 2 >Af.
(2) In a s t a t e at the point C, while the r e v e r s e transformation appears
in the e a r l y thermal c y c l i n g , the reverse transformation does not appear,
if a s t a r t i n g line of r e v e r s e transformation σΑβ(Ν) in Nth cycle moves
to the right side of the point C. (3) In the case that the s t r e s s σΛ i s
kept constant during the thermal c y c l i n g , if the completing line of SIM
transformation σΜ-τ(Ν) in Nth cycle moves to the r i g h t side of the point
A, the SIM transformation is completed at Ti in the cooling process and
s t r a i n becomes equal to £ Mf . (4) In the loading process to the point D
a t Ti, the SIM transformation is completed and a s t a t e of the point D i s
in the hardening region of the m a r t e n s i t i c phase. In the case that the
temperature is raised to T 2 , while keeping the s t r e s s a d c o n s t a n t , the
reverse trasformation does not appear in a s t a t e at the point E even if
T 2 >Af.
242

CO
α>
CO

Mr Ms Ti A« Af T 2
Temperature T
Fig.5 Schematic cyclic behavior of each transformation line

CONCLUSIONS
For TiNi shape memory a l l o y , the t e s t with the loading-unloading cycling
and the test with the thermal cycling under constant s t r e s s were c a r r i e d
out. The r e s u l t s are summarized as follows. By the thermomechanical
c y c l i n g , the yield s t r e s s e s of the stress-induced m a r t e n s i t i c
transformation and the reverse transformation decrease and the
transformation temperature r i s e . The conditions for the s t a r t i n g and the
completing of each transformation under cyclic deformation are defined by
the behavior of the transformation l i n e s on the s t r e s s - t e m p e r a t u r e p l a n e .

REFERENCES
Iwanaga, H., H. Tobushi and H. Ito (1988). Basic Research on Output Power
C h a r a c t e r i s t i c s of a Shape Memory Alloy Heat Engine. JSME I n t . J.. Ser.
I. 31. 634-637.
Tanaka, K., S. Kobayashi and Y. Sato (1986). Thermomechanics of
Transformation P s e u d o e l a s t i c i t y and Shape Memory Effect in Alloys.
I n t . J. P l a s t i c i t y . 2. 59-72.
Tanaka, K., H. Tobushi and H. Iwanaga (1988). Continuum Mechanical
Approach to Thermomechanical Behavior of TiNi Alloys. Proc. 31st Jpn
Cng. on Mater. Res.. 51-56.
Tobushi, H. and J. R. Cahoon (1985). Mechanical Analysis of a S o l a r -
Powered Solid State Engine. Trans. CSME. 9. 137-141.
Tobushi, H., H. Iwanaga, Y. Ohashi, A. Inaba, M. Kawaguchi and H. Saida
(1990a). Cyclic C h a r a c t e r i s t i c s of the Shape Memory Effects in TiNi
Alloy Wires and Helical Springs. JSME I n t . J . . Ser. I. 33. 256-262.
Tobushi, H., K. Kimura, H. Iwanaga and J. R. Cahoon (1990b). Basic
Research on Shape Memory Alloy Heat Engine. JSME I n t . J.« Ser. I. 33.
263-268.
 WS11b4

SUFERPLASTIC BEHAVIOR OF Cu-Zn-Al SHAPE MEMORY ALLOTS

Z.Y. ZHENG, R.H. GAN, Z.T. ZHCT, F.Z. LIN, Y.S· CHEN,Z. ΎΕ
2nd Department of Mechanical Engineering,
South China University of Technology,
Guangzhou 510641, P#R. CHINA

ABSTRACT

Cu—Zn-Al shape memory alloys exhibited micrograin superplasticity. Superb-

plastic exxrusion of Cu-Zn-Al shape memory alloys has been conducted. After
superplastic extrusion the miorostructures of the shape memory alloys are
finer and much homogeneous than that of the unextruded specimens of the same
alloys· Measurement of the lifetime of positrons indicated that the total
size of crystal defects in the superplastically extruded specimens of the
Cu-Zn-Al shape memory alloy was near to that of the unextruded speci-
mens» The microstructures of the superplastically extruded Cu-Zn-Al-shape
memory alloys are suitable for the subsequent heat-treatment» After heat-
treatment the shape memory effects of the superplastically extruded specimens
are better than that of the superplastically unextruded specimens·

KEYWORDS

superplasticity; superplastic extrusion; shape memory alloy (SKA).

INTRODUCTION

Cu-Zn-Al SMA has iheif prospect in application· The raw materials for
melting the Cu-Zn-Al shape memory alloys are abundant and accessible. The
production cost of the Cu-Zn-Al shape memory alloys is lower than that of the
Ti-Ni shape memory alloys. The shape memory effect of the Cu-Zn-Al shape
memory alloys was effective,but its resistivity to thermal cycling was lower
than that of the Ti-Ni shape memory alloys. It was found that the Cu-Zn-Al
shape memory alloy with fine grains had the thermal resistivity as that of a
Ti-Ni shape memory alloy (Murakami et al., 1984). It is necessary to re-
fine the grain size of the Cu-Zn-Al shape memory alloys for improving their
characteristic.

The hot workability of the Cu-Zn-Al shape memory alloys was good,but their
cold workability strongly depended on their microstruotures (Yek et al.,1^09).

243
244
The coarse grain size of the Cu-Zn-Al shape memory alloys leaded to their
brittleness (Negishi et al,, 1988)· It is necessary to refine the grain
size of Cu-Zn-Al shape memory alloys for improving the cold workability.

Except the method of adding some elements to the chemical composition of the
Cu-Zn-Al shape memory alloys for refining the grain size,superplastic defor«
mation of Cu-Zn-Al shape memory alloys is probably the way to obtain micro-
structures with fine grains,and eliminating cold: working and intermediate
annealing of these alloys· The micrograin superplastic deformation of the
Cu-Zn-Al shape memory alloys could be realised under certain conditions· The
superplasticity of Cu-Zn-Al shape memory alloys has been investigated· The
superplastic behavior of the Cu-Zn-Al shape alloys and effect of superplas-
tic deformation on their shape memory effect are presented in this paper·

EXPERIMENTAL

In order to study the superplasticity of Cu-Zn-Al shape memory alloys,their

chemical composition and microstructures should satisfy the requirements of
shape memory alloy and superplastic deformation simultaneously· It has been
noted that there are relationships between chemical composition,martensitic
starting temperature Ms and electronic concentration (e/a). The electronic
concentration should be in the range of 1.40-1.50·

To prepare Cu-Zn-Al shape memory alloys electrolytic copper (99·97$Cu),com-

mercially pure, aluminium (97»7%AJ) and mishmetal Al (11> mishmetal) were used
as raw materials. The raw materials for preparing the Cu-Zn-Al shape memory
alloys were melted in a graphite crucible. Castings of the alloys were hor-
mogenized at 850°c for 15 hrs. and then forged into bars with 22 mm and 10 mm
in diameter respectively.

Swerplastic tensile test were conducted with specimens which were made from
bars with 10 mm in diameter,at temperature T* . The Έ* > O.5ŒW1 and Tm is
the melting points of the alloys. Th® bars with 22 mm in diameter were used
to conducted superplastic extrusion at the same temperature and strain rate
used as in the superplastic tensile test,with various degrees of deformation,
which is defined as ]>=s./s—1,where Sp is the initial cross-section area of
the specimens and s is the final cross-sectional area of the extruded specin-
menss. Technology of heat-treating the Cu-Zn-Al shape memory alloys were
investigated.

Measurement of the lifetime of positrons for the specimens superplastically

extruded and unextruded was made with lifetime spectrometer. The specimens
size was 12x20x0.4 mm.

Micrographs and X-ray automatically recorded diffraction patterns were obtain-

ed from the superplastically extruded and unextruded specimens and for the
specimens after heat-treatment.

RESULTS AND DISCUSSION

The Cu-Zn-Al shape memory alloys with 22-28 wt$Zn and 3-4wt^Al exhibited micr
crograin superplasticity (Zheng et al.,1989). The Cu-26.6wt#Zn-4.0wt^Al
shape memory alloy exhibited micrograin superplasticity at 600*c,at a strain
â i
rate è»5x10'* s" and gave an index of strain rate sensitivity m« 0.44· The
bars with 22mm in diameter of the alloy were used to conducted superplastic
extrusion. Micrographs of this alloy superplastically extruded,unextruded
are shown in Pig. 1. The microetructure of superplastically extruded speci-
 245
mens is homogeneous and finer than that of the uneitruded specimen·.

(a) ib)

Pig. 1. Micrographs of the specimens of Cu-26.6wtfZn-

4.0wt^Ai (a) euperplastically extruded and (b)
unextruded·

Crystal defects (dislocations and vacancies') in the specimens of the alloy

were detected with the measurement of the lifetime of positron. The life-
times of positrons in dislocations rt and vacancies z% for superplastically
extruded and unextx^ded specimens are *CÂ =138 ps, ^«291 ps, and' ^ = H 5 P s »
^2«297 ps respectively. This indicates that the lifetime of positrons in
superplastically extruded specimens are nearfethat in the unextruded specimens
The total size of crystal defects is near to that in the unextruded specimens.
The Cu-36wt^Zn-3.5wtfAl shape memory alloy after superplastic extrusion with
different degrees of deformation also gave a homogeneous and finer microstruc-
tures than that of the unextruded specimens (Zheng et al., 199^). The X-
ray diffraction patterns indicated that no ckange of phase constituents oc-
cured,although variation of diffraction intensity was observed.

Some superplastically extruded and unextruded specimens Of Cu-26wt/Zn-3«5*rt%

Al were heated to 790 *c and held at this temperature for 15 minutes, step
quenched in a salt bath at 210Qc for 1 minute and subsequently cooled in wa-
ter at room temperature.
The micrographs of the superplastically extruded and unextruded specimens of
the alloy after heat-treatment show the martensitic state in the specimens
(Pig. 2 ) . The martensite in the grains of superplastically extruded spe-
cimens with different degrees of deformation orients themselves in some pre-
ferred direction,but the martensite in the unextruded specimens orients ran-
domly. The preferred orientation of martensite in the alloy is mainly in-
duced by superplastic extrusion. In this case the formation of martensite in
the superplastically extruded alloy may be linked with the easy formation of
stacking faults and twins. Prom our experimental results there some pheno -
mena involved with texture and transormation texture.

the shape memory effect of the Cu-26wt^Zn-3.|)wt^al alloy is affected by the

superplastic extrusion and the technology of heat-treatment. Curves in Pig. 2
Opshow the shape memory effects of the specimens tiiat underwent the above-,
mentioned heat-treatment. These curves show that the superplastic extrusion
does not deteriorate the shape memory effect of the Cu-Zn-Al shape memory
alloys,but somewhat improve it·
246

Fig. 2 Micrographs and shape memory effects of the super-

plastically extruded and unextruded specimens of
Cu-26wt^Zn-3.5wt$AJ alloy after heat-treatment.

CONCLUSIONS

t. Cu-Zn-Al shape memory alloys with 22-28wt$Zn and 3-4wt%Al exhibit micro-
grain superplasticity;
2. The microstructures of superplastically extruded specimens are homoge-
neous and finer than that of the unextruded specimens of the Cu-Zn-Al shape
memory alloy;
3· Superplastic extrusion does not deteriorate the shape memory effect of
the Gu-Zn-Al shape memory alloys;
4 # Superplastic deformation is not only a forming technology,but also can
improve the microstructures and shape memory effect of the Cu-Zn-Al shape
memory alloys#

REFERENCES

Murakami, K., Y· Murakami, K· Mishima and Y. Ikai (1984). Degradation and

improvement of shape memory effect of Cu-base alloy. J. Japan Inst. me-
 247
tain, 48, 115-121.
îïegishi,A. (1988). Manufacture and technology of ehape memory alloys, Jv
Japan Soo. for technology of plasticity,2$,115-121.
Yeh, C.H.i S. Tong, Y.L. Lin, C.P. Chang and S.E. Hsu (1989)· Study of the
workability of Cu-Zn-Al shape memory alloy. Proc. of MRS Int. Meeting
on Adv. Materials,79, 91-97.
Zheng, Z.Y., Z.W. Xie, S.G. Yuan and Z.P. Chen (1989). Superplasticity of
Cu-Zn-Al shape memory alloys. Proc. of MRS Int. Meeting on Adv. Mate -
rials, 7, 96-102.
Zheng, Z.Y., W.J. Zhong, P.Z. Lin and Y.S. Chen (1990). Behavior of super?-
plastically extruded Cu-26irt$Zn-3.5*~fc^Al shape memory alloy. Proc. of
MRS 1990 Spring Meeting, (being published).
WS11b5

DEFORMATION ANALYSIS OF SHAPE MEMORY ALLOYS

DURING THERMOMECHANICAL PROCESSES

Kikuaki TANAKA* and F.D. FISCHER**

Department of Aerospace Engineering, Tokyo Metropolitan Institute
of Technology, J-191 Hino/Tokyo, JAPAN
5JCJJC
Institut für Mechanik, Montanuniversität Leoben, A-8700 Leoben, AUSTRIA

ABSTRACT

Thermomechanical and transformation behaviors of polycrystalline shape

memory alloys are studied in the process of stress-induced martensitic
transformation from the micromechanical point of view. The microscopic
deformation due to transformation are connected to the macroscopic behavior
of alloys by introducing two different levels of microstructure in alloys;
the microregion and the mesodomain. The thermomechanical constitutive
equation and the micro-fraction defined in the microregion are averaged over
the mesodomain to give a macroscopic constitutive relation.

KEYWORDS

Shape memory alloys, Stress-induced martensitic transformation, Driving

force, Micromechanics, Microstructures, Averaging process, Hysteresis.

INTRODUCTION

Extensive microscopic studies on shape memory alloys have revealed that

their "anomalous" behavior under thermomechanical circumstances is caused by
one or some of the following metallurgical elementary processes (Delaey, e_i
âL·., 1974, Perkins, 1975, Wayman, 1983): The thermoelastic martensitic
transformation and its reverse transformation, the reorientation of the
martensite plates, or in other words, the reversible movement of the twin
boundaries, and the transformation from one martensite variant to the other
which has a different crystallographic structure from the first.

In order to design a shape memory device with a prescribed specification one

has primarily to know the macroscopic behavior of the alloy under the
applied thermomechanical load. A continuum mechanical approach could well
meet these demands by formulating the constitutive relations composed of the
thermomechanical constitutive equations and the transformation kinetics
(Müller, 1980, Bertram, 1982, Falk, 1983, Tanaka, et aK., 1986). The
problem is whether such a continuum approach is compatible with the
microscopic observations. The present paper proposes a theoretical chain

249
250
from the elementary process of "the microregion" which is defined as the
smallest microstructure to the behavior of "the mesodomain" which is a much
larger domain and represents a macroscopic behavior of alloys.

MICROSTRUCTURE IN ALLOYS

Let us introduce a microregion in a polycrystalline shape memory alloy as a

region oriented by a habit plane. Since a habit plane, the x1,x -plane in
Fig.l, characterizes a variant, the microregion, habit plane and the variant
are used synonymously in the present theory. The global coordinate system
o - X . X ^ is attached to the specimen. The local coordinate system o-x^x,.
is so defined that the third axis is taken to be normal to the habit plane.
The directions of the first two axes lying on the habit plane are determined
later. This coordinate system is characterized by the Eulerian angles ω
with respect to the global coordinate.

We then define, as illustrated in Fig.l, a much larger domain in the

specimen, a mesodomain, in such a way that it contains an enough large
number of microregions but is still enough small compared to the size of the
specimen. Metallurgy tells us that a single crystal may have maximum 24
variants. Since a mesodomain naturally contains a sufficient number of
single crystals, their crystallographic orientation may be thought to be
distributed almost randomly in the mesodomain if not a preferred
crystallographic orientation exists. A mesodomain, therefore, contains an
nearly infinite number of habit planes. The averaging over the mesodomain,
the volume average, can be replaced by the ensemble average with respect to
the Eulerian angles ω.

ç ë,

2
/ MESODOMAIN MICROREGION
SPECIMEN

Fig.l Microstructures in shape memory alloys.

MICRODEFORMATION IN ALLOYS DURING TRANSFORMATION

According to the observation of metallurgists, under a critical

thermomechanical condition the martensite/parent interface propagates with
a velocity which is in general very large compared to the speed of variation
of the applied thermomechanical load. We, thus, conclude that only two
states exist in the level of microregion; the non-transformed state and the
transformed state. The intermediate state of transformation, which is not
observed at the level of microregion, is detectable only when the state is
averaged over the mesodomain. When the transformation occurs in a
microregion, it deforms as shown in Fig.l, and a microscopic stress-free
strain tensor
I* = (men + n0m)/2 (1)
 251
is induced (Patoor, ejt al^, 1987), where n and m represent the unit normal
to the habit plane, and the vector of motion, respectively. The first two
axes of the local coordinate system which are yet left undetermined are so
defined that the vector of motion m lies on the χ.,χ^-plane as illustrated
in Fig.l. The microscopic stress-free strain tensor given by Eq.(l) now
reads as
(2)

with respect to the local coordinate system, where ε and r denote the strain
normal to the habit plane, and the shear strain parallel to the habit plane,
respectively. It should be noted that ε and Ϋ are the material parameters.

Thermodynamics of martensitic transformation in alloys have revealed

(Nishiyama, 1978, Patel and Cohen, 1953) that the formation of martensite
starts in the parent phase when a "driving force" defined by
(3)
reaches a threshold value G 0 , where d represents the local stress tensor and

T the temperature. The chemical driving force AG is given as the free

energy difference between the unit volume of martensite and parent phases.
The mechanical driving force U, which represents the contribution of the
applied stress, is given by
(4)
where

Now we introduce the local stress tensor with respect to the global
coordinate system by
(5)
where Q(u>) stands for the transformation materix from the local coordinate
to the global coordinate system. We understand from Eqs.(3) and (5) that
(6)
In order to measure the extent of transformation in a microregion ω which is
subjected to (σ,Τ) let us now introduce the micro-fraction defined by
1 for
0 for (7)

CONSTITUTIVE EQUATION IN A MICROREION

When the material behavior is limited within the elastic range, the
constitutive equation in a microregion can be written in the transformed
state as
(8)
§ means the strain tensor induced in the microregion and
(9)

stands for the thermal expansion term with a thermal expansion tensor a and
the reference temperature TQ. The fourth order tensor I represents the
elastic compliance tensor. Equation(8) can be rewritten as
252
(10)
where the strain tensors with respect to the global coordinate system are
introduced as follows:
(11)

The elastic compliance tensor I evaluated with respect to the global

coordinate system is expressed in the component form as
(12)

AVERAGING PROCESS

Let us define over a mesodomain an average value <f> of an arbitrary

microscopic quantity f(w) evaluated in a microregion ω by the formula
(13)
The weighting function g(u>) represents the distribution density function
characterizing the crystallographic axes. Evaluating <f> for any current
state (d,T) leads to a uniform field <f> in the mesodomain.

In order to measure the extent of transformation in the mesodomain let us

define the macro-fraction ξ as an average value of the micro-fraction € over
the mesodomain;

(14)
From Eqs.(7) and (14) we understand that 0 £ € £ 1. When ξ = 0, the
mesodomain in question is fully in the parent state while for ξ = 1 the
martensitic transformation completes in the domain. In an intermediate
situation the domain is composed of a mixture of the martensite phase with
the volume fraction ξ and the parent phase with the volume fraction l-ξ. In
Fig.l shaded parts in the mesodomain denote the variants where the
transformation has occured. It also illustrates a distribution of the
macro-fraction ξ thus determined along a line in the specimen.

Now by taking an average of Eq.(8) we obtain

(15)

E stands for the macroscopic strain tensor, E for the macroscopic stress-
free strain tensor due to transformation, and Ε~ for the macroscopic strain
tensor due to thermal expansion. When the transformation completes in the
whole mesodomain, E has an extreme value E calculated from

(16)

Following Reuss' assumption (Hashin and Shtrikman, 1962) the macroscopic

stress tensor Σ, which corresponds to E, is assumed to be estimated by
(17)
The effective elastic moduli tensor L is now simply given by
 253
L = <I>. (18)

RATE-TYPE CONSTITUTIVE EQUATION

When the local thermomechanical load changes from (d,T) to (ö+dö,T+dT), some
of the microregions in a mesodomain may newly transform to the martensite
phase as Eq.(7) tells us. As we can calculate the change in macro-fraction
d£ and the increment of dE during this incremental process, a material
tensor £ can be introduced by
dE = Ûd£. (19)
~c
In case Û be a constant tensor S , it follows that Ω = E . Equations(11)~
and (15), lead naturally to the assumption
4
dE T = 9dT, θ = <ά·α·£ Τ >, (20)
with the global thermal expansion tensor Θ.

The incremental form of the thermomechanical constitutive equationdö). in

the mesodomain can now be written as
dE - Ûd£ - 9dT = L:dE, (21)
where the expression in the right-hand side is obtained by assuming that L
remains constant during the incremental process.

KINETICS OF MACRO-FRACTION £

The macro-fraction ξ depends on the global thermomechanical load (E,T)

through the driving force AG and the average process. Under an incremental
loading (dö,dT) which corresponds to the global thermomechanical increment
(dE,dT), the number dN of the microregions transforming to martensite phase
per unit volume of parent phase may be assumed to be
dN = - k<dAG>, dAG £ 0, (22)
with k > 0 as a proportionality constant (Magee, 1968). The change in
macro-fraction d£ is now given by
d€ = [VV(l-C)dN]/V = V(l-£)dN = -kV(l-£XdAG>, (23)
where V and V stand for the average volume of microregion and the volume of
mesodomain, respectively.

Equations(22) and (23) together with Eq.(3) leads a final form of the
kinetics;
<1ξ/(1-ξ) = - b:E + adT, a = - kVOAG/3T>, b = kV<3AG/9ö>. (24)
If the material tensor a and b are constant during the process Eq.(24) gives
a solution
ξ = 1 - exp[a(Mg - T) + b:E]. (25)

NUMERICAL ILLUSTRATION
Numerical simulations are carried out for a Cu-Zn-Sn alloy (Tanaka, e_i a L ,
-3 ~
~
1968). The microscopic deformation is characterized by ε = -4.0x10 and Y
= 0.2, and fis = 246 K and A^s = 248 K.
Figure 2 gives the stress-strain curves at 265 K and 247 K, which clearly
shows the characteristics of the transformation superplasticity and the
254
shape memory effect, respectively. The tensile and compressive behavior are
not the same as illustrated in Fig. 3. Figure 4 shows the hysteresis curves
under temperature cycling at constant applied stress.

Fig. 2 Stress-strain curves.

Compressive

Strain E

Fig. 3 Tensile/compressive Fig.4 Hysteresis under temperature

stress-strain curve. cycling.

REFERENCES

Bertram,A. (1982). NuçIi_Engngi_DesigiK , 74, 173-182.

Delaey,L., Krishnan,R.V., Tas,H. and Warlimont,H., (1974). J^.Maier^„SçL.,
9, 1521-1555.
Falk,F. (1983). Arçh^.Meçh^, 35, 63-84.
Hashin,Z. and Shtrikman,S., (1962). J^.Meçh^Phys^Solids, 10, 344-352.
Magee,C.L. (1968). In: Phase_iransformaiions (Aaronson,H.I., ed.), ASM,
115-156.
Müller,I. (1980). Il_Nuovo_Çimento, 57B, 283-318.
Nishiyama,Z. (1978). Max_tensiiiç_iransformaiion. Academic Press, New York.
Patel,J.R. and Cohen,M. (1953). Açta_Metall^, 1, 531-538.
Perkins,J., ed. (1975). Shape_inemory_effecIs_in_aIIoys, Plenum Press,
New York/London.
Patoor,E., Eberhardt,A. and Bervei1ler,M. (1987). Pr o ç^_^h JRISO J^ni^ J5 ymp ^,
465-470.
Tanaka,K., Kobayashi.S. and Sato,Y. (1986). In±^_J^_Pl_astiçiiy, 2, 59-72.
Wayman,C.M. (1983). In: PhysiçaI_meiaIIurgy (Cahn.R.W. and Haasen.P., eds.),
North-Holland Physics Publishing.
 WS11b6
CYCLIC RECOVERY STRESS OF TiNi SHAPE MEMORY ALLOY
UNDER CONSTANT MAXIMUM STRAIN
H. TOBUSHI and Y. OHASHI
Department of Mechanical Engineering, Aichi Institute of Technology
1247 Yachigusa, Yagusa-cho, Toyota 470-03, Japan
T. HORI and S. KOJIMA
Graduate School, Aichi Institute of Technology

ABSTRACT
The cyclic behavior of recovery stress under constant maximum strain in
TiNi shape memory alloy is investigated experimentally. The influence of
maximum strain and the heating temperature under thermal cycling on
cyclic characteristics of recovery stress is discussed. The main results
are summarized as follows. (1) Both stresses at high temperature and at
low temperature decrease gradually with the number of cycles, but the
recovery stress is almost constant. (2) The recovery stress under thermal
cycling decreases with maximum strain. (3) Both recovery stress and
stress at high temperature increase with the heating temperature, but
stress at low temperature is almost constant. (4) The amount of decrease
in stress at high temperature under thermal cycling is less than that in
yield stress of the stress-induced martensitic transformation in the
pseudoelastic region.

INTRODUCTION
In the application of shape memory alloys, the recovery stress under
constant strain may be employed. In order to evaluate the reliability in
shape memory alloys as the functional material, the behaviors of
transformation temperature, recovery deformation and recovery force under
thermomechanical cycling are very important problems. For these problems,
the authors have studied the basic cyclic properties on the shape memory
effect (Tobushi, et al., 1987), pseudoelasticity (Inaba, et al., 1989,
Kawaguchi, et al., 1991) and the shape memory effect of helical spring
(Tobushi, et al., 1990a) of TiNi shape memory alloy.

In the current paper, following the previous work on the basic mechanical
properties, the cyclic recovery stress under constant maximum strain will
be discussed. The recovery stress under constant maximum strain has been
used in many applications, for example, the tightening force in a pipe
coupling or the driving force in the shape memory alloy heat engine
(Tobushi, et al., 1985, Iwanaga, et al., 1988, Tobushi, et al., 1990b).
The factors which affect the recovery stress are shape memory processing
temperature, maximum strain, heating temperature and cooling temperature.
In the present study, the cyclic behavior of recovery stress under
constant maximum strain in thermal cycling of TiNi shape memory alloy was
discussed experimentally.

EXPERIMENTAL PROCEDURES
Material and Experimental Apparatus

The material was a Ti-55.3wt%Ni alloy wire produced by Furukawa Electric

255
256

Strain ε
F i g . l . I l l u s t r a t i o n of s t r e s s - s t r a i n curve showing t e s t procedure
Co.» Ltd. The specimen was shape-memorized into a s t r a i g h t line from the
wire. In the shape memory p r o c e s s i n g , the wire was kept a t 673K for 20min
and cooled in a furnace. The re ver se-transformat ion finish temperature
Af was about 323K. The o u t e r diameter of the specimen was 0.75mm, the
length between g r i p s was 110mm, and the gauge length 20mm.
An experimental a p p a r a t u s consisted of a t e n s i l e machine and a h e a t i n g -
cooling device and was described in d e t a i l in a previous paper (Tobushi,
1990a). The axial f o r c e , displacement and temperature were measured by a
l o a d c e l l , an extensometer and a thermocouple, r e s p e c t i v e l y . The specimen
was heated or cooled by hot or cold a i r .

Experimental Tests

The schematic s t r e s s - s t r a i n r e l a t i o n in the experiments is shown in

F i g . l . As seen in F i g . l , at f i r s t the maximum s t r a i n € m was given at the
temperature Tt below A f . Following t h i s process and keeping the s t r a i n
€ m c o n s t a n t , the specimen was heated to the temperature T 2 above Af and
then s t r e s s increased to σ 2 . Following t h i s p r o c e s s , if the specimen was
cooled to Tt under constant € m , s t r e s s decreased to <r t . These heating
and cooling processes completed one cycle and were repeated 100 times.
The value of Tt was 293K and the values of T 2 were 333, 353 and 373K. The
values of e m were 1, 2, 4 and 6%. The s t r a i n r a t e t i l l € m was 2%/min.
The r a t e of heating and cooling was about 1.5K/s.

EXPERIMENTAL RESULTS AND DISCUSSION

S t r e s s - S t r a i n . Curve

The s t r e s s - s t r a i n curves obtained by the experiments for maximum s t r a i n

£ m =1, 2, 4 and 6% a r e shown simultaneously for each high temperature T 2
in F i g . 2 . In the f i g u r e , the s t r e s s at high temperature σ 2 and the
s t r e s s at low temperature Ui for N=l and N=100 and j t for N=2 a r e
indicated with the several symbols. Also in the f i g u r e , a s t r e s s - s t r a i n
curve obtained by a t e n s i l e t e s t at T 2 for maximum s t r a i n of 8% i s shown
with a thin c u r v e . As found from the curve in an i n i t i a l loading process
 257

0 2 4 6 8 0 2 4 6 8
Strain B % Strain £ %
F i g . 2 . S t r e s s - s t r a i n c u r v e s in t e s t s with d i f f e r e n t maximum s t r a i n s
a t T t , € m =l% is in the region a f t e r completion of the rhombohedral phase
(R-phase) transformation and i s near the s t a r t i n g point of the s t r e s s -
induced m a r t e n s i t i c (SIM) t r a n s f o r m a t i o n , € m=2% and 4% a r e in the SIM
transformation r e g i o n , and €m=6% i s in the hardening region of the
martensitic phase.
The phenomena observed in each t e s t a r e summarized as follows. (1) The
s t r e s s at high temperature σ 2 i n c r e a s e s as the heating temperature T 2 is
high. The s t r e s s σ 2 takes the almost same value at each T 2 . (2) The
s t r e s s σ 2 which a r i s e s in the f i r s t heating p r o c e s s is lower by about
lOOMPa than the yield s t r e s s of SIM transformation on the s t r e s s - s t r a i n
curve at T 2 . The difference between both s t r e s s e s is large as T2 is high.
(3) The s t r e s s at low temperature σι depends on T 2 s l i g h t l y . (4) The
s t r e s s σ\ which appears in the f i r s t cooling process is lower by about
50MPa than the s t r e s s on the s t r e s s - s t r a i n curve at Ti. (5) Both σ 2 and
(Ji decrease s i g n i f i c a n t l y in the e a r l y cycles and the r a t e of these
v a r i a t i o n s decrease with the increase in N.

S t r e s s Behavior with Heating and Cooling

In o r d e r to i n v e s t i g a t e the s t r e s s behavior with the temperature

v a r i a t i o n in each c y c l e , for maximum s t r a i n £ m =l% and the heating
temperature T2=373K, the r e l a t i o n between s t r e s s and temperature for the
number of cycles N=l and 100 is shown in F i g . 3 . In the f i g u r e , the
s t a r t i n g s t r e s s and the completing s t r e s s of the SIM transformation and
the r e v e r s e transformation σΜ^ , σΜ? , σ Α β and σ^ which were obtained
by the t e n s i l e t e s t under the constant temperature a r e p l o t t e d with the
several symboles, which a r e connected by the dashed c u r v e s . These dashed
c u r v e s r e p r e s e n t a s t a r t i n g line and a completing line of the SIM
transformation and the r e v e r s e transformation (Tanaka, et a l . , 1988). As
258

800
ΓΤ 1 1 1 1 1
ce
N=l
^600 N=100
l_ ' JO tf"" 1
" 2 5 ^^ —J
^400
m
L- '&? *z^~~~ Λ± (JAS Ί
w
^. Ά (TAf Ί
-3200 p==:=©= <><'

0 1'
280
Q
300
^u
320
:x 340 360
X--Ä
|_
380
1

Temperature T K
F i g . 3 . Relation between s t r e s s and temperature for N=l and 100
( € m =l% and T2=373K)

seen in F i g . 3 , in the f i r s t loading process at Ti=293K> the i n i t i a l

s t r e s s σ,π a r i s e s corresponding to the maximum s t r a i n £ m . Following t h i s
p r o c e s s , in the heating process under the constant s t r a i n € m , s t r e s s
v a r i e s s l i g h t l y t i l l about 320K, i n c r e a s e s along the s t a r t i n g line of the
SIM transformation from about 320K to 350K, v a r i e s s l i g h t l y above 350K
and f i n a l l y reaches σ 2 at T 2 . Following t h i s p r o c e s s , in the cooling
process under the constant ε m , s t r e s s decreases along the nearly same
s t r e s s - t e m p e r a t u r e curve in the heating process and f i n a l l y reaches σι
at T t .
The reason why s t r e s s i n c r e a s e s along the s t a r t i n g line of the SIM
transformation from about 320K to 350K in the heating process may be
explained as follows. In the f i r s t loading process to € m at T t , s t r a i n
i s caused by the R-phase transformation. In the heating p r o c e s s , though
the r e v e r s e transformation may occur, the specimen can not recover i t s
o r i g i n a l shape by c o n s t r a i n s on deformation and so the recovery s t r e s s
appears. In t h i s p r o c e s s , the s t r a i n caused by the R-phase transformation
becomes the e l a s t i c s t r a i n of the parent phase at the heating temperature
by the r e v e r s e transformation. The s t r e s s caused by the r e v e r s e
transformation of the R-phase transformation could take the almost same
value as the s t a r t i n g s t r e s s of the SIM transformation σ Μβ . In the range
of t h i s experiment, the r e v e r s e transformation of the SIM transformation
may not occur.
It is seen in Fig.3 that the s t r e s s - t e m p e r a t u r e curves show the long and
thin S-shaped forms. In the case of € m =l%, because am at Ti i s lower
than σΜΒ and s t r e s s approaches σΜ£? with an increase in temperature, the
s t r e s s - t e m p e r a t u r e curve shows the c l e a r S-shaped form. In the case of
€ m =6%, the s t r e s s - t e m p e r a t u r e curve shows n e a r l y the s t r a i g h t l i n e .
The s t r e s s - t e m p e r a t u r e curve for N=100 shows the almost same form as that
for N=l except for the decrease in the s t r e s s l e v e l . On the whole, the
influence of the thermal cycling on the form of the s t r e s s - t e m p e r a t u r e
curve i s l i t t l e .

Behavior of Recovery S t r e s s with Thermal Cycling

 259

01 J I I I I I i I I I
0 20 40 60 80 100
Number of cycles N
F i g . 4 . Changes in s t r e s s e s σ 2 , σ ι and ar as a function of the
repetition c y c l e s ( £m=4% and T2=373K)
As shown schematically in F i g . l , s t r e s s i n c r e a s e s from Ut to σ 2 by
heating from Ti to T 2 . The amount of s t r e s s increment σ =σ2-σι
r e p r e s e n t s the e f f e c t i v e recovery s t r e s s j r caused by h e a t i n g . The
s t r e s s at high temperature σ 2 , the s t r e s s at low temperature σ% and the
recovery s t r e s s ar= σ in r e l a t i o n to the number of cycles N in the
case of 6m=4% for T2=373K a r e shown in F i g . 4 .
It i s seen in Fig.4 that σ 2 and σι decrease rapidly in the e a r l y cycles
and decrease g r a d u a l l y in M 20. The recovery s t r e s s ar takes an almost
constant value in N 10. In the case of another maximum s t r a i n € m and
heating temperature T 2 , the almost same c y c l i c behaviors of σ 2 , σι and
σΓ are observed. It may be said t h a t , in the a p p l i c a t i o n to use σ 2 or
Œr, because these s t r e s s e s decrease rapidly in the e a r l y c y c l e s , the
t r a i n i n g before the p r a c t i c a l use i s e f f e c t i v e .

Cyclic Behavior of S t r e s s at High Temperature

The r e l a t i o n between the s t r e s s at high temperature σ 2 and the number of

cycles N discussed in the preceding section and the r e l a t i o n between the
s t a r t i n g s t r e s s of the SIM transformation (TMS and N obtained in the
c y c l i c deformation t e s t of p s e u d o e l a s t i c i t y a t the constant temperature
T 2 as discussed in the previous paper (Kawaguchi, et a l . , 1991) in the
case of €m=4% a r e shown in F i g . 5 .
It is seen in Fig.5 that both ση^ and σ 2 decrease s i g n i f i c a n t l y in the
e a r l y number of cycles a t every T 2 . While the amounts of decrease in σΜ*
for N=l~100 a r e 100—200MPa, those in σ 2 a r e l e s s than 50MPa.
The reason why t h e r e appears the difference between the amounts of
decrease in σ Μ 3 and σ 2 may be considered as follows. In each cycle of
the cyclic deformation t e s t of p s e u d o e l a s t i c i t y , while the transformation
s t r a i n appears by the SIM transformation in the loading p r o c e s s , the
transformation s t r a i n disappears by the r e v e r s e transformation in the
unloading p r o c e s s . Corresponding to the processes of growth and
disappearance of the m a r t e n s i t i c phase by both t r a n s f o r m a t i o n s , the
i n t e r f a c e between the c r e a t e d phase and the parent phase moves. In the
interface t h e r e may appear the d i s l o c a t i o n s e a s i l y . Because the i n t e r f a c e
moves r e p e a t e d l y with the c y c l i c loading and unloading processes and so
the i n t e r n a l s t r e s s caused by the d i s l o c a t i o n s a c t s r e p e a t e d l y , the yield
260
1 1 1
cd 8 0 0 OöW · ( & (T 2 = 3 3 3 K )
AöW AÖ2 (Τ 2 = 3 5 3 Κ )
S DÖM S ■ (& (Τ 2 = 3 7 3 Κ )
600
Rb^
£ 400

^ 200

0
ο 20 40 60 80 100
Number of cycles N
F i g . 5 . Changes in s t r e s s e s σ 2 and OMS as a function of the
repetition c y c l e s (€ m =4%)
s t r e s s of the SIM transformation UMS decreases s i g n i f i c a n t l y (Kawaguchi,
e t a l . , 1991). On the c o n t r a r y , in the c y c l i c thermal t e s t under the
constant maximum s t r a i n £ m , because € m is kept c o n s t a n t , the i n t e r f a c e
between the m a r t e n s i t i c phase and the parent phase moves s l i g h t l y and
thus cJ2 decreases s l i g h t l y .

CONCLUSIONS
The c y c l i c behavior of recovery s t r e s s under constant maximum s t r a i n of
TiNi shape memory a l l o y was i n v e s t i g a t e d experimentaly. The influence of
maximum s t r a i n and the heating temperature under thermal cycling on
c y c l i c p r o p e r t i e s of recovery s t r e s s was d i s c u s s e d . The main r e s u l t s a r e
summarized as follows. (1) Both s t r e s s e s at high temperature and at low
temperature decrease g r a d u a l l y with the number of c y c l e s , but the
recovery s t r e s s is almost c o n s t a n t . (2) In the heating p r o c e s s , the
s t r e s s i n c r e a s e s along the s t a r t i n g line of the s t r e s s - i n d u c e d
martensitic transformation on the s t r e s s - t e m p e r a t u r e plane by the r e v e r s e
transformation of the R-phase t r an s f o r mat i o n. The s t r e s s - t e m p e r a t u r e
curve moves toward the l o w - s t r e s s d i r e c t i o n keeping the almost same form
with an increase in the number of c y c l e s . (3) The amount of decrease in
the s t r e s s a t high temperature under thermal cycling is l e s s than that in
the s t a r t i n g s t r e s s of the s t r e s s - i n d u c e d m a r t e n s i t i c transformation
under c y c l i c deformation in the p s e u d o e l a s t i c r e g i o n .

REFERENCES

Inaba. A. , Kimura, K. , Iwanaga, H. and Tobushi, H. , Trans. JSME.

55-511, A(1989), 628-633 (in Japanese).
Iwanaga, H. , Tobushi, H. and I t o , H. , JSME Int. J. . S e r . I . 31-3
(1988), 634-637. ~

Kawaguchi, M. , Ohashi, Y. and Tobushi, H. , JSME Int. J. . Ser.I» 34-1

(1991).
Tanaka, K. , Tobushi, H. and Iwanaga, H. , The 31st Jpn Cong. Mat. Res. ,
51-56.
Tobushi, H. and Cahoon, J. R. , Trans. CSME. _9-3 (1985), 137-141.
Tobushi, H. , Iwanaga, H. , Inaba, A. and Kwaguch, M. , Advances in
Plasticity 1989, Pergamon, (1989), 365-368.
Tobushi, H. , Iwanaga, H., Ohashi, Y. , Inaba, A., Kawaguchi, M. and
Saida, H. . JSME Int. J. . Ser.I. 33-2, (1990a), 256-262.
Tobushi, H. , Kimura. K. , Iwanaga,"Tî. and Cahoon, J. R. , JSME Int. J. «
Ser. I. 33-2 (1990b), 263-268.
WS1231

ASPECTS OF MISCIBILITY IN COPOLYMER BLENDS

CHAI Z H I K U A N ; SUN RUONA,* and FRANK E. KARASZ

Department of Polymer Science and Engineering
University of Massachusetts, Amherst, MA 01003, U.S.A.
'Permanent Address: Institute of Chemistry, Academia Sinica, Beijing, China

ABSTRACT

Copolymer blends form an important group in polymer blends, and the study of their miscibility is of
both academic and industrial significance. Several papers (Brannock et al., 1990; Braun et al., 1989;
Cowie et al, 1990a, b; Cruz-Ramos and Paul, 1989; Hellman et ai, 1990; Litauszki et al., 1989;
Shiomi et al., 1990) published in 1989-1990 report recent developments; here, we summarize our own
new results in this active research field.

KEYWORDS

Copolymer miscibility

A-B/C-D AND A-B/A-B BLENDS

Many works describe A-B/C and A-B/A-C blends (where A, B, and C are monomeric units in random
copolymers), but only a few treat A-B/C-D and A-B/A-B (including A/A-B) blends. Usually, the
miscibility-immiseibility boundary on an isothermal composition-composition (c-c) plot accurately
represents the miscibility behavior of blends. From the mean field theory of random copolymer
blends (Kambour et al., 1983; Paul and Barlow, 1984; ten Brinke et ai, 1983), the miscibility
boundary of A-B/C-D blends is determined by
+
WAC v-uyxnc+ x(l~y)xAD + (y-x)V-y)xBD
=
- X(1-*)XAB - yV-y)XcD Xcrit

and

where x and y are volume fractions of A and C in the copolymers; in practice the volume fraction is
replaced by the molar fraction of the units. The parameters rt are the degrees of polymerization of
copolymer i and χϋ is the pair interaction parameter of monomeric units.

263
264
According to the condition

= 0 (3)
> 0

the miscibility boundary can be an ellipse, a parabola, or a pair of hyperbolas.

Our work has focused on CPVC/AN-BT and CPE/AN-BT blends (where CPVC is chlorinated
poly(vinyl chloride), CHClCHCl.CI^CHCl; CPE is chlorinated polyethylene, CHj.CHCl; and AN-BT is
acrylonitrile-butadiene. Two elliptical miscibility boundaries were found for the systems (Figs. 1 and
2). Further resolution of the six pair interaction parameters shows that the repulsion between the
dissimilar units in each copolymer induces the miscibility.

CPVC/AN-BT CPE/AN-BT

+»+o · 8 o é+ + f ·
o o o o oaf;. *
o e +e
Φ *+-P + · o o o > o o o o +4 ·
• · + + + #+ + + # + + + +^ . + ♦ + + + * ' , ' +
+^ · o · +· -*· · ·
+ +++ ++
• · ί-·# + ί" · · ·

CHOCHC! molH

Figure 1. Isothermal phase diagram of Figure 2. Isothermal phase diagram of

CPVC/AN-BT blends at 70°C. O One-phase CPE/AN-BT blends at 70°C. O One-phase
system, · two-phase at 70°C, ® two-phase system, · two-phase at 70°C, Θ two-phase
at 190°C. at 110°C, ® two-phase at 190°C.

Plots of A-B/A-B blends show a miscible boundary consisting of two parallel lines as determined by
the critical condition

XAlfr-yf = Xa (4)

We have found two systems to exhibit parallel miscibility boundaries: CPVC/CPVC blends (Fig. 3)
and MMA-EMA/MMA-EMA blends (Fig. 4, where MMA is methyl methacrylate and EMA is ethyl
methacrylate). Perhaps surprisingly, the pair interaction parameter of CHC1CHC1.CH2CHC1
obtained from the CPVC/AN-BT system predicts well the miscibility boundary of CPVC/CPVC blends.

EFFECT OF SEQUENCE DISTRIBUTION ON MISCIBILITY

Rather than two parallel lines, CPE/CPE blends have as their miscibility boundary one or two bulges
along the diagonal of the c-c plot (Fig. 5). Also shown in this figure are the regions of UCST or LCST
behavior, between 50-190°C. The peculiar miscibility boundary is a result of the effect of sequence
distribution. From previous works (Balazs et al., 1985a, b; Cantow and Schulz, 1986):
 265

CPVC/CPVC MMA-EMA/MMA-EMA

CHCICHCI mol% MMA mol%

0 ΐίΓ^ΪΟ 30 40* 50 60* 70 80 *90 ΐ8θ

CHCICHCI mol% MMA mol%

Figure 3. Isothermal phase diagram of Figure 4. Isothermal phase diagram of

CPVC/CPVC blends at 150°C. Symbols as MMA-EMA/MMA-EMA blends at 70°C.
in Pig. 1. Symbols as in Fig. 1.

CPE(L)/CPE(L)
1. Copolymer A-B is considered to consist of 6
different triads:
· ■ ft-OO
1 BAB 1 4 ABA 1
AAB 2 5 ABB
1 BAA BBA 1
1 AAA 3 6 BBB 1
2. For the 15 triad interaction parameters
it is assumed
= = = = = =
Xl2 5Cl3 *23 X45 *46 *56 ^
=
*36 " *26 *26 Xl6
10 20 30 40 50 60 70 80 90
=
^35 *25 ^25 Xl5
=
CHCI mol%
*34 ~ X24 *24 Xl4
=
(5) Figure 5. Isothermal phasediagram of
^36 ~ X35 X35 " X34 CPE/CPE blends at 70°C. © Regions of
*26 " *25 =
*25 ~ *24 UCST behavior between 50°-70°C, Θ
= regions of LCST behavior at 190°C.
Xl6 ~ ^15 *15 ~ Xl4

3. Introducing Θ to characterize the sequence distribution,

/AB = 2θ//* (6)

where fA and fB are the monomeric unit volume fractions in the copolymer, and fAB is the pair
probability of AB in the copolymer. 0 = 0, 0.5, and 1.0 (fA = fB = 0.5 in the last case) and denotes
block, random, and alternating copolymers, respectively.
266

Adding all the triad interactions we finally obtain the new miscibility boundary as

(x-y)2[A + B(x+y) + C(x+y)2] = χα (7)

Eq. 4 is rewritten as Eq. 7. The last two bracketed terms reflect the effect of sequence distribution.

Eq. 7 describes well the miscibility boundary of CPE/CPE blends. With a known pair interaction
parameter χ^, obtained from the CPE/AN-BT system, one can solve for the remaining 8 parameters.
It is interesting to see that χ14 has the largest attractive energy, in accordance with the maximum
miscibility in some copolymer composition ranges on the c-c plot.

CALORIMETRIC RESULTS OF CPE/CPE BLENDS

Calorimetric studies were carried out with a Setaram C80 microcalorimeter. Heats of mixing were
obtained directly from differential measures in which two component polymers were dissolved into a
solvent in a cell, while at the same time, in another cell, a polymer blend was dissolved into the
solvent. This technique permits higher sensitivity, lower fluctuation, and allows larger samples. The
blends contain a 50/50 weight ratio of two components. AHm is an average of six measurements using
the two solvents dichlorobenzene and dibutyl phthalate. Within experimental error the data show no
solvent dependence; accuracy is estimated at ± 1.0 J/g.

Fig. 6 shows the heats of mixing of CPE/CPE blends, most of which were discovered to be exothermic.
This finding departs from theoretical predictions, as shown in Fig. 7, where all the heats are
endothermic and increase gradually towards the miscibility boundary.

CPE(L)/CPE(L) CPE(L)/CPE(L)

■XHCI mol% _CHC1 mol%

oo
oo o oo o
o oo o
oo oo

10 20 30 40 50 60 70 80 90

CHCI moi%

Figure 6. Heats of mixing (J/g) of Figure 7. Theoretical heats of mixing

CPE/CPE blends at 70°C. (J/g) of CPE/CPE blends at 70°C.

As this disregards differences between small and large molecules, a tentative explanation of
this discrepancy is based on the assumption that in an A-B copolymer, for instance, the effective
volume fractions of A and B are x-a' and l-x-b\ rather than x and 1-x, which are for small molecules.
Using these values we can derive the overall interaction parameter for A-B/A-B blends as
 267

XNend = W ( * - ? ) 2 +
(*-*)(*-y) - *fl (8)

where a and b are the parameters related to the effective volume fractions of the two copolymers.
With Eq. 8 and under certain conditions, a negative heat can then be predicted.

MISCIBILITY IN BRANCHED POLYMER BLENDS

The effect of branching on miscibility was studied using branched chlorinated polyethylenes. Pigs. 8
and 9 show the miscibility boundaries of branched CPE/branched CPE and linear CPE/branched CPE
blends; branching prohibits mixing.

CPE(B)/CPE(B) CPE(U/CPE(B)

CHCI mol% 90
CHCL mol% , (B)
o • • . S3
•
•
·
· ·
·
I/O
if oo
OO
o
80 • · ·
/ oo
[_
•
·
· ·
· ·
· cf o o
· yo o o ooo
oo 70 : t/8°
y
- • • ·······
^o^o oo
'" · ·#/Ο00 Ο o op m 60 0
· · / o o oo
• ^ /' o o o m 50 - • •I oo oo
o o/··
• ••ti8°o 8 • 40 • • ·Χ8 ° o oo o o 81
• · %0 OO O 8 X· . M/O O O O OO O O / * ·
30 - • • βόο _o—·-**-
• ·,ό o · · - · -
a o-^··
• · • ·
• ·
·,· oé · · · • · •• 20 •
o ·'·· · · •
o i# · • 10 • · · • ·
10 20 30 40 50 •60 70· 80 90 0
10 20 30 40 50 60 70 80 90 100

CHCI mol% CHCL mol% . (L)

Figure 8. Isothermal phase diagram of Figure 9. Isothermal phase diagram of

branched CPE/branched CPE blends at linear CPE/branched CPE blends at 70°C.
70°C. Symbols as in Fig. 1. Symbols as in Fig. 1.

The above-described method is also used here to obtain the blend interaction parameter. The entropy
change due to branching is ignored. The branched polymer molecules are regarded as chains
composed of end, linear-middle, and branching-point units, both chlorinated and unchlorinated.

(CH3)6x 1 4 (CHsCl)«,
x)
(CH2)(1 2 5 (CHCl) ( 1 . M X j. x )
-2δ)χ

IjCH),, 3 6 (CCI)«!.«) 1
δ is the volume fraction of branching points, and (1-x) is the volume fraction of chlorinated units in the
chain. The equation for branched CPE/branched CPE blends is

x»w = fr-yftx + (c-i)Ax»] (9)

268
and for linear CPE/branched CPE blends

Xbund = Xi*"?)2 - (c-l)&xt>(x-y)y (10)

where χ is the interaction parameter of linear CPE/linear CPE blends, and (ΰ-Ι)Δχ > 0 indicates that
branching increases the interaction energy in the system and hence is unfavorable for mixing. Eqs. 9
and 10 qualitatively predict the branching effect seen in Figs. 8 and 9.

ACKNOWLEDGEMENT

This work was supported by AFOSR Grant 91-100.

REFERENCES
Balazs, A. C , Karasz, F. E., MacKnight, W. J., Ueda, H., and Sanchez, I. C. (1985).
Copolymer/Copolymer Blends: Effect of Sequence Distribution on Miscibility.
Macromolecules, 18, 2784-2786.
Balazs, A. C , Sanchez, I. C , Epstein, I. R., Karasz, F. E., and MacKnight, W. J. (1985). Effect
of Sequence Distribution on the Miscibility of Polymer/Copolymer Blends.
Macromolecules, 18, 2188-2191.
Brannock, G. R., Barlow, J. W., and Paul, D. R. (1990). Blends of Styrene/Acrylic Acid
Copolymers and Acrylic Polymers. J. Polym. Sei. B, 28, 871-891.
Braun, D., Herth, J., and Hellmann, G. P. (1989). Mutual Miscibility of Chlorinated
Hydrocarbon Polymers Derived from Polyethylene and Polyvinylchloride. Angew.
Makromol. Chem., 171, 53-63.
Cantow, H. J. and Schulz, 0. (1986). Effect of Chemical and Configurational Sequence Distribution on
the Miscibility of Polymer Blends. 1. Blends of Monotactic Homopolymers. Polym. Bull., 15,
449-453.
Cowie, J. M. G., McEwen, I. J., and Nadvornik, L. (1990). A Mean-Field Treatment of the
Interactions in Blends of Poly(vinyl methyl ether) with Poly(styrene-co-nitrostyrene).
Macromolecules, 23, 5106-5108.
Cowie, J. M. G., Reid, V. M. C , and McEwen, I. J. (1990). Prediction of the Miscibility Range in
Blends of Poly(styrene-co-acrylonitrile) and Poly(N-pheny1 itaconi mi de-co-methyl
methacrylate): A Six- Interaction-Parameter System. Polymer, 3J., 486-489.
Cruz-Ramos, C. A. and Paul, D. R. (1989). Evaluation of Interactions in Blends of Ethylene-
Vinyl Acetate Copolymers with Poly(vinyl chloride) Using Model Compounds.
Macromolecules, 22, 1289-1300.
Hellmann, G. P., Kohl, P. R., Herth, J., Neumann, H. J., Andradi, L. N., and Lowenhaupt, B.
(1990). Tailoring of Polymer Blends with Copolymers. Makromol. Chem. Macromol.
Symp., 38, 17-30.
Kambour, R. P., Bendler, J. T, and Bopp, R. C. (1983). Phase Behavior of Polystyrene, Poly(2,6-
dimethyl-l,4-phenylene oxide), and Their Brominated Derivatives. Macromolecules, 16,
753-757.
Litauszki, B., Schmidt-Naake, G., Kressler, J., and Kammer, H. W. (1989). Miscibility of
Poly(methyl methacrylate-co-maleic anhydride) with styrene-acrylonitrile and methyl
methacrylate-styrene copolymers. Polym. Commun., 30, 359-361.
Paul, D. R. and Barlow, J. W. (1984). A Binary Interaction Model for Miscibility of Copolymers in
Blends. Polymer, 25, 487-494..
Shiomi, T., Eguchi, T., Ishimatsu, H., and Imai, K. (1990). Application of Equation-of-State
Theory to Random Copolymer Systems. 2. Copolymer Blends. Macromolecules, 23,
4978-4982.
ten Brinke, G., Karasz, F. E., and MacKnight, W. J. (1983). Phase Behavior in Copolymer
Blends: Poly(2,6-dimethyl-l,4-phenylene oxide) and Halogen-Substituted Styrene
Copolymers. Macromolecules, 16, 1827-1832.
WS12a2

TENSILE STRENGTH OF MISCIBLE BLENDS OF POLY(ACRYLONITRILE-CO-STYRENE)

AND POLY CSTYRENE-CO<-( N-PHENYLMALEIMIDE )]

Y. AOKI

Yokkaichi Research and Development Department,

Mitsubishi Kasei Polytec Company, 1 Toho-cho,
Yokkaichi, Mie 510, Japan

ABSTRACT

The tensile strength of miscible blends of poly(aerylonitrile-co-styrene)

(AS) and poly[styrene-co-(N-phenylmaleimide )J (SMI) exhibited a minimum
value smaller than that of either pure component. This negative deviation
can be explained by the reason that the tensile strength between AS and SMI
is weaker than those of the component copolymers, using a new additivity
rule of tensile strength for miscible blends.

KEYWORDS

Tensile strength; miscible blend; poly(acrylonitrile-co-styrene);

poly[styrene-co-(N-phenylmaleimide )J .

INTRODUCTION

Styrenic polymers have been required to improve various physical properties

, for example, heat resistance, toughness, chemical resistance and etc., to
get wide applications. These improvements can often be performed by blend-
ing other polymers. Recently, we have developed a new high heat resistance
styrenic alloy which contains maleimide copolymers. Glass transition tem-
perature of poly[styrene-co-(N-phenylmaleimide)} (SMI) increases with an
increase in N-phenylmaleimide content.

In a previous paper (Aoki, 1988), we studied miscibility of blends of poly-

(acrylonitrile-co-styrene) (AS) and SMI, and found that ASs are miscible
with SMIs within specific range of copolymer composition. From the binary

269
270
interaction model for copolymer mixture (Kambour et al.. 1983, ten Brinke et
al.. 1983, Paul and Barlow, 1984), segmental interaction parameters between
the different monomer units were estimated and were found to be positive for
all pairs. No attractive interactions were found between the acrylonitrile
and N-phenylmaleimide.

We also studied dynamic viscoelastic properties of miscible blends of AS and

SMI (Aoki, 1990). When the zero-shear viscosities are compared at the same
free volume fractions, they decreased convexly with SMI content. Such com-
positional dependences of the zero-shear viscosities can be interpreted by
the change in the number of entanglement couplings, without any change in
each entanglement molecular weight in the component copolymers.

Mikos and Peppas have proposed a new molecular theory for the molecular wei-
ght dependence of the polymer fracture properties using structural and
entanglement characteristics of the polymers. A chain scission criterion
was invoked for the chain segments being entangled about the fracture plane
and theoretical predictions agreed well with experimental data for the frac-
ture energy and strength of polystyrene and poly(methyl methacrylate) (Mikos
and Peppas, 1988). Therefore, tensile strength of brittle polymers should
relate to entanglement characteristics of the polymers. However, only a few
miscible systems have been studied as far as tensile strength is concerned.
Recently, Sawada and Fujita studied mechanical properties of copolymer
blends of poly[styrene-co-(methyl methacrylate)] with poly[styrene-co-(meth-
acrylic acid)] (Sawada and Fujita, 1989). They reported that tensile
strength of the blends exhibits a maximum value greater than that observed
for either pure component copolymer and this would be the evidence of the
attraction between two copolymer molecules.

In order to make clear the tensile strength of miscible polymer blends

without specific interactions between dissimilar chains, the compositional
dependence of the tensile strength of AS/SMI is studied. A new mixing rule
of tensile strength for miscible blends is proposed. Comparison of the rule
with experimental values is performed.

EXPERIMENTAL

Materials
The AS and SMI were prepared by radical polymerization. The copolymer com-
position was determined by elementary analysis. The AS (AS-26) contained
 271
26.0% acrylonitrile and 74.0% styrène by weight. The SMI (P-30) contained
43.3% N-phenylmaleimide and 56.7% styrene by weight. The molecular weights
of the copolymers were estimated by GPC where the calibration was based on
polystyrene standards. The M of AS-26 is 163 000 and M /M is 1.9. The M
w w
of P-30 is 169 000 and M /M is 2.3. n w
w n
Blend preparation

The polymers were dissolved in selected ratios to a total of 5 wt% in ace-

tone. The polymers were precipitated into methanol and dried in a vacuum
oven at 80 C. Films were pressed between steel sheets in the range 190 C
to 240 °C for 5 min and then quenched to room temperature. Film thickness
of about 1 mm was used for differential scanning calorimeter (DSC) and dy-
namic mechanical measurements. The polymers were molded on the Mini-Max
Injection Molder (Model CS-183, Custom Scientific Instruments, Inc.). In
order to ensure better mixing in the small stator cups, the polymers obtain-
ed in sheet form were cut into smaller chips. The mixed polymers were in-
jected into a mold which had been pre-heated through contact with the hot
stator cup. The mold was then removed and quenched immediately in water.

Measurements

Dynamic mechanical measurements were made to test sample miscibility by us-

ing a viscoelastic spectrometer (Iwamoto Seisakusho Co.) at a heating rate
of 1 °C/min and frequency of 20 Hz. Measurements were begun at 23 °C and
continued until the sample became too soft to be tested. A DSC apparatus
(Seiko Denshi, SSC-560) was also used to determine sample miscibility.
Sampledof about 10 mg were annealed for a few min at 200 C. The samples
then cooled to room temperature and the glass transition temperatures(T )
o
were measured with a heating rate of 20 C/min. Tensile test was made on a
Mini-Max Tensile Tester (Model CS-183TE, CSI, Inc.). This is a horizontal
bench top stress-strain instrument, especially designed to test the dumbbell
specimens produced in the miniature molder. The dumbbell specimen was grip-
ped and clamped in the grip holders. A cross-head speed of 0.571 cm/min was
chosen. Testing was done at a temperature of 23 C.

RESULTS AND DISCUSSION

Miscibility of AS/SMI blends

Figure 1 shows the temperature dispersions of the dynamic storage modulus E f

and'loss modulus E" for pure AS-26, P-30, and their blends. For pure AS-26
272

Fig. 1. Temperature dispersions of the dynamic

storage (EM and loss (E") moduli at 20 Hz
for AS-26, P-30, and their blends.

the maximum at about 112 C on the E" curve arises from the glass transition
of AS-26. In the temperature range of this transition, the E* decreases
markedly. For pure P-30 the transition occuring above 150 °C is the glass
transition. The T occurs at 167 °C on the E" curve. The E" curve of each
blend has only a single peak corresponding to the glass transition temper-
ature. The temperature at which a peak on the E" curve occurs shifts to a
higher temperature with an increase in SMI content, although the peaks are
somewhat broadened.

The DSC thermograms also showed that the blends have one glass transition
temperature which is a function of blend composition and lies between the
values for AS and SMI, although the breadth of the T region are much broad-
o
er, too. These facts are evidence of miscibility of the AS-26/P-30 blends.

Tensile strength of AS/SMI blends

Figure 2 shows plot of the tensile strength of AS-26/P-30 blends as a func-

tion of blend composition. The values for all compositions lie below the
straight line connecting the pure components and there is a large negative
deviation from linearity. The results are contrary to those for the blends
for poly [styrene-co-(methyl methacrylate )} with poly[styrene-co-(methacrylic
acid)J (Sawada and Fujita, 1989). They proposed the following equation for
the compositional dependence of tensile strength of the blends.
 273

800
P-30/AS-26

S 700

if)

600h
\>-σ'

500
0 0.2 Ολ 0.6 0.8 1
Volume Fraction of P-30

Fig. 2. Tensile strength of AS-26/P-30 blends as a

function of volume fraction of P-30.
Experimental data (o) are compared with the
calculated curve (dotted line) of eq. (2).

T.S. = 1T.S.-W- (1)

'blend * , ϋ
Ί Ί T + —T.S.pWp
W + wpw-vu
w
2 2 " P 1 2

where, w. is weight fraction of component i and φ represents the deviation

from the rule of simple additivity. According to Bersted and Anderson, how-
ever, the tensile strength of brittle polymers is proportional to the entan-
glement density (Bersted and Anderson, 1990). Consequently, it should be
considered that the compositional dependence of the tensile strength is ex-
pressed by the same types of equation proposed by Wu for the entanglement
density of miscible polymer blends (Wu, 1987). Then, the tensile strength
of blends is given by
T S = T S
- -blend - -1-1*1 2 + T S
- '2-2*2 2 +
ZxT.S..,^*., (2)
where, φ. is volume fraction of component i and T.S.. . tensile strength due
to i-j type entanglements. When T.S.. p is equal to (T.S..,.. + T.S.p ? )/2,

additivity rule can be satisfied. When T . S . ^ à (T.S.^- + T.S.2_2)/2,

eq. (2) shows positive and negative deviation from linearity, respectively.
As shown in Fig. 2, the tensile strength of AS-