Evaluation of Fracture Toughness of Welded

Evaluation of Fracture Toughness of Welded
High Strength Low Alloy Line-pipe Steel
Banda Venkata Bhargava
Department of Metallurgical and Materials Engineering
National Institute of Technology Rourkela

Evaluation of fracture toughness of welded
high strength low alloy line-pipe steel
Thesis submitted to the
in partial fulfillment of the requirements
of the degree of
Master of technology
in
Metallurgical and Materials Engineering
by
Banda Venkata Bhargava
(Roll Number: 214MM1337)
Under the supervision of
Prof. Krishna Dutta

and
Dr. Shrabani Majumdar
May 2016
Department of Metallurgical and Materials Engineering

i
Dr. Krishna Dutta

Assistant Professor
NIT Rourkela
May 26, 2016
Supervisor's Certificate
This is to certify that the work presented in this thesis entitled ''Evaluation of
Fracture toughness of Welded High Strength Line-pipe Steel'' by ''Banda Venkata
Bhargava'', Roll Number 214MM1337, is a record of original research carried out
by him under my supervision and guidance in partial fulfillment of the
requirements of the degree of Masters in Technology in Metallurgical and
Materials Engineering. Neither this thesis nor any part of it has been submitted for
any degree or diploma to any institute or university in India or abroad.
--------------------------
Krishna Dutta
Principal Supervisor
ii
Material Characterization and Joining Group
R & D, TATA Steel Ltd. Jamshedpur
Dr. Shrabani Majumdar

Principal Scientist
Material Characterization and Joining Group
R & D, TATA Steel Ltd
Jamshedpur
May 26, 2016
Co-Supervisor's Certificate
This is to certify that the work presented in this thesis entitled ''Evaluation of
Fracture Toughness of Welded High Strength Line-pipe Steel'' by ''Banda Venkata
Bhargava'', Roll Number 214MM1337, is a record of original research carried out
by him under our supervision and guidance in partial fulfillment of the
requirements of the degree of Masters of Technology in Metallurgical and
Materials Engineering. Neither this thesis nor any part of it has been submitted for
any degree or diploma to any institute or university in India or abroad.
---------------------------
Shrabani Majumdar
Co-Supervisor
iii
Dedicated
To
My
Parents and Friends
iv
Declaration of Originality
I, Banda Venkata Bhargava, Roll Number 214MM1337 hereby declare that this
thesis entitled ''Evaluation of Fracture Toughness of Welded High Strength Line-
pipe Steel'' represents my original work carried out as a postgraduate student of
NIT Rourkela and, to the best of my knowledge, it contains no material previously
published or written by another person, nor any material presented for the award of
any other degree or diploma of NIT Rourkela or any other institution. Any
contribution made to this research by others, with whom I have worked at NIT
Rourkela or elsewhere, is explicitly acknowledged in the thesis. Works of other
authors cited in this thesis have been duly acknowledged under the section
''Bibliography''. I have also submitted my original research records to the scrutiny
committee for evaluation of my thesis.
I am fully aware that in case of any non-compliance detected in future, the Senate
of NIT Rourkela may withdraw the degree awarded to me on the basis of the
present thesis.
May 26, 2016 Banda Venkata Bhargava

NIT Rourkela
v
Acknowledgment
The satisfaction and euphoria that accompany the successful completion of a task would
be incomplete without the mention of the people who made it possible and whose
constant guidance and encouragement crowned all the efforts with success.
Therefore, I would like to take this opportunity to express my sincere and heartfelt
gratitude to all those who made this report possible.
At first I would like to thank my Guide, Thesis supervisor Prof. Krishna Dutta
Department of Metallurgical & Materials Engineering, National Institute of Technology,
Rourkela who permits me to work at Research and Development, Scientific Services,
Tata Steel, Jamshedpur. Without his support and invaluable guidance, it is impossible for
me to complete this work.
I bow humbly to record my deep sense of gratitude to my Co-Supervisor Dr. Shrabani

Majumdar Principle Scientist, Research and Development, Scientific Services, Tata
Steel Ltd, Jamshedpur, who always motivate me and enlighten me with her valuable
suggestions. With her constant encouragement and able guidance during every stage of
the work that brought the research to a successful completion.
I thank Prof. S. C. Misra Head of the Department Metallurgical and Materials

Engineering, National Institute of Technology, Rourkela, who has encouraged a lot to
carry out this project work at Tata Steel.
I am also grateful to Dr. Kanwer Singh Arora, Tata Steel Ltd, Jamshedpur, for
encouraging, providing research facilities, helping me in analyzing data and supporting
during this investigation.
I thank my beloved friends of various colleges worked along with me in Tata Steel Ltd
Jamshedpur Mr. Govardhan Pujari, Mr. Rajath Rautela, Mr. Pramay Bhatprahari,
Mr. Aditya Arun and Mr. Shaswath Sharma, who made my stay colorful.
At last but not the least I thank my Parents and Family Members without whom support
and motivation I couldn’t complete this work.
May 26, 2016 Banda Venkata Bhargava

NIT Rourkela (Roll Number: 214MM1337)
vi
Abstract
The present investigation revolves around evaluation of fracture toughness of welded API
X65 steel plate. API X65 is a high strength low alloy (HSLA) steel which is used in line-
pipes for transporting oil and natural gas. In the above application, catastrophic failure
due to fatigue is reported to cause sudden damage and loss to human-life as well as
property. Hence, from end application point of view, knowledge on fracture toughness
especially in welded plates is of immense importance. Through the present work, an effort
has been made to add to the limited number of reports on the above subject. In this work,
first, the selected steel was characterized in terms microstructure, hardness and tensile
properties. Thereafter, the welding of steel plates was performed with sub merged arc
welding (SAW) with root pass of shielded metal arc welding (SMAW). The
microhardness profile in base material (BM), heat affected zone (HAZ), weld zone (WZ)
and weld nugget were evaluated along with microstructural characterization of the above
zones using optical and transmission-electron microscopy. The fracture toughness of
various zones of welded plate, was evaluated in terms of J-R curve following the concept
of EPFM. The samples for fracture toughness tests were prepared as per ASTM E1820.
Fractography of the failed specimens were also carried out. The evaluation of fracture
toughness of welded API X65 plates indicates that, JQ value of heat affected zone was
slightly lower than the base material, but for the weld zone it dropped significantly by
53% due to the non-uniform crack front and crack propagation. The phenomenon is
attributed to presence of different defects in the weld region. JQ value for fusion line
samples showed significant scatter with an average reduction of 40% in J Q value as
compared to base material. The scatter in fusion line value can be attributed to error in
precise placement of notch or deviation of crack path during testing. Presence of Nb and
V imparts precipitation hardening effect to the API X65 steel, such that it has a
satisfactory combination of strength and toughness parameters fulfilled by API service
requirements.
Keywords: Sub merged arc welding (SAW); Shielded metal arc welding (SMAW); Base material
(BM); Heat affected zone (HAZ); Weld zone (WZ); Fracture toughness
vii
Contents
Supervisor's Certificate ................................................................................. ii
Co-Supervisor's Certificate ......................................................................... iii
Dedicated ....................................................................................................... iv
Declaration of Originality ............................................................................. v
Acknowledgment .......................................................................................... vi
Abstract ........................................................................................................ vii
List of figures................................................................................................. xi
List of tables ................................................................................................ xiii
Chapter 1
Introduction
1.1 Background and motivation ....................................................................................... 1
1.2 Objectives of the present work .................................................................................. 2
Chapter 2
Literature Review
2.1 Introduction ................................................................................................................ 3
2.2 Classification of HSLA steel...................................................................................... 4
2.3 Effects of alloying elements ....................................................................................... 4
2.4 Processing and manufacturing of line-pipe steels ...................................................... 7
2.5 HSLA steels applications ........................................................................................... 7
viii
2.5.1 HSLA steels in line-pipe applications ................................................................. 8
2.6 Literature on shielded metal arc welding (SMAW) and fracture toughness of HSLA
steels ................................................................................................................................. 9
2.7 Literature on submerged arc welding (SAW) and fracture toughness of HSLA steels
........................................................................................................................................ 10
2.8 Review of fracture toughness testing....................................................................................................

....................... Error! Bookmark not defined. 11
2.8.1 Stress intensity factor K (Equivalent to energy release rate G) ..................................

................. Error! 1112
Bookmark not defined.
2.8.2 J-integral ............................................................ Error! Bookmark not defined. 11

..................................................................................................................................................... 1
2.8.3 Crack tip opening displacement (CTOD).................................................................................11

.......... Error! Bookmark not defined.
2.8.4 Crack tip opening angle (CTOA)1111111111111111111

...................... Error! Bookmark not defined.
2.9 Why CTOD test?..............................................................................................................................................

...................................................... Error! Bookmark not defined. 12
2.9.1 CTOD estimation ...................................................................................................................................

.............................................. Error! Bookmark not defined. 12
2.9.2 Fracture toughness J calculation........................................................................ 12
2.10 J-integral ................................................................................................................ 12
2.11 Re-appraisal of current problem ............................................................................ 14
Chapter 3
Experimental procedures
3.1 Introduction .............................................................................................................. 20
3.2 Material selection and chemical composition .......................................................... 20
3.3 Welding of the material ........................................................................................... 21
3.4 Microscopic examinations and image analysis ........................................................ 22
3.5 TEM analysis ........................................................................................................... 25

ix
3.6 Hardness measurement ............................................................................................ 26
3.7 Tensile test ............................................................................................................... 28
3.8 Fracture toughness testing........................................................................................ 28
3.9 Fractography ............................................................................................................ 30
Chapter 4
Results and Discussion
4.1 Chemical composition ............................................................................................. 31
4.2 Tensile properties ..................................................................................................... 32
4.3 Microstructure and grain size determination ........................................................... 33
4.4 Hardness profiles of API X65 welded sample ......................................................... 37
4.5 J-R curve tests on welded API X65 plates ............................................................... 39
4.6 Fractography of fracture toughness tested broken samples ..................................... 43
Chapter 5
Conclusion and scope for future research
5.1 Conclusions .............................................................................................................. 46
Scope for future research
5.2 Scope for future research ......................................................................................... 47
Bibliography ................................................................................................................. 48
x
List of figures
Figure 2.1: Evolution of line-pipe grade steel .................................................................... 9
Figure 2.2 (a): (a) Load F vs LPD (Load point displacement) for a single specimen
technique ........................................................................................................................... 13
Figure 2.2 (b): J-R curve method used to determine JIC ................................................... 13
Figure 3.1: Cross sectional image of the material after weld ............................................ 21
Figure 3.2: LEICA M165C stereo microscope .................................................................. 21
Figure 3.3: Mecatome T-210 slow speed cutter ................................................................ 22
Figure 3.4: Mecapress II specimen mount press ............................................................... 22
Figure 3.5: Resign powder used in the mounting of the sample ....................................... 23
Figure 3.6: Mechatech Z64 semiautomatic polishing machine ......................................... 23
Figure 3.7: LEICA DM 6000M with image analyzer German made ................................ 24
Figure 3.8: Explain the sequential procedure of electro polishing .................................... 25
Figure 3.9: JEOL-2200FS field emission electron microscope(TEM) .............................. 26
Figure 3.10: Sample holder used for measurement of microhardness ............................. 26
Figure 3.11: The micro-hardness tester used in the present work ............................................ 27
Figure 3.12: Image of sample after hardness indentations ................................................ 27
Figure 3.13: Instron 5582 universal testing machine, made in USA ................................. 28
Figure 3.14: Broken sample after fracture toughness testing ............................................ 29
Figure 3.15: The servo hydraulic test system used for estimation of fracture toughness .......... 29
Figure 3.16: Image of FE-SEM (ZESIS SUPRA 25 German made) ................................ 30
Figure 4.1: Detailed microstructure of API X65 weld ...................................................... 33
Figure 4.2: Representative figure and phase fraction for APIX65 .................................... 34
xi
Figure 4.3: (a)-(c) base material; (d) to (g) weld region; (h) & (I) coarse HAZ and (j)-(l)
fine HAZ ............................................................................................................................ 36
Figure 4.4: Image of the sample after indentations ........................................................... 38
Figure 4.5 (a): Hardness profile vertically top to bottom in weld zone ............................. 38
Figure 4.5 (b): Hardness profiles horizontally across weld zone ...................................... 38
Figure 4.6: Three point bend specimen for J-R curve testing............................................ 40
Figure 4.7 (a): Load vs displacement obtained from the data collected from the equipment
........................................................................................................................................... 40
Figure 4.7 (b): Load vs displacement plot modified to match with standard .................... 41
Figure 4.8: Representative J-R curves for weld and heat affected zone ............................ 42
Figure 4.9: Stereoscopic and SEM micrographs of different regions of tested three point
bend J-R curve sample ....................................................................................................... 44
xii
List of tables
Table 4.1: Chemical composition of API X65 in weight % .............................................. 31
Table 4.2: Mechanical properties of API X65 ................................................................... 32
Table 4.3: JQ value obtained for different regions of welded API X65 ............................. 42
xiii
Chapter 1
Introduction
1.1 Background and motivation

Over the past few years, production of oil and gas increased enormously and due to this,
the transport of such oils and gasses require development of improved line-pipe steels.
The usage of high strength low alloy steels (HSLA) in line-pipe brings in the advantage of
cost reduction by virtue of reduction in wall thickness of pipelines [1]. Manufacturing of
HSLA line-pipe steel for oil and gas transmission follows the API 5L standard [2]. The
desired properties in these steels are high mechanical strength, good weldability, high
fracture toughness, strain tolerance, resistance to environmental degradation such as stress
corrosion cracking. The aim of steel suppliers is to develop all the above properties at a
reasonable price. These steels were first introduced in early 1930`s which was followed
by years of research to achieve optimum structure-property combination. The micro-
alloying elements like niobium, vanadium and titanium were added in certain amounts as
low as 0.005-0.010 percent in early steels. These HSLA steels were firstly used in ship
plates, beams, bridge steels, reinforcing bar and heat treated forgings and was not
introduced into line-pipe steels until 1959 [3]. However due to the predominant changes
in the metallurgical approaches and development of different kinds of rolling techniques
these HSLA steels came into existence with the escalating technological demands of high
pressure line-pipe steel.
In this work, a special grade of HSLA steel developed at TATA steel Ltd., Jamshedpur,
India, was characterised. It was specially aimed to develop a suitable combination of
strength and toughness for the steel owing to different microalloying additions. The study
also compares the properties of the steel and its weldments.
1
Chapter 1 Introduction
1.2 Objectives of the current work

The primary objective of the present investigation is to study and evaluate the fracture
toughness of the welded high strength line-pipe steel. The major scope of the work is
briefly summarised as follows:
(I) To characterize the steel for its chemical composition, its microstructure in base
metal and weld regions and to determine the hardness and tensile properties.
This section consists of (a) chemical composition analysis of the steel specimens (b)
microstructural examination at various zones i.e. parent material, heat affected zone, weld
zone and grain size measurement (c) determination of their hardness and tensile
properties.
(II) To study the facture toughness property of the welded API X65 steel.
The major experiments to fulfil this objective are (a) pre-cracking of the sample under
fatigue (b) examination of the fracture toughness at various zones by J-R curve approach.
(III) Fractographic examinations on the fractured sample using (SEM) scanning

electron microscope.
Fractographic examinations of fractured surface using SEM to study the various features
and understand the type of failure in the fractured sample.
2
Chapter 2
Literature Review
2.1 Introduction
High-strength low-alloy steel (HSLA) were firstly introduced in early 1930`s. The
elements like niobium vanadium and titanium were added independently in amounts of
about 0.005 to 0.010 in early steels, however as strength increased with adding them in
combination and the metallurgical approaches got more refined. The overriding melting
method at early days was Siemens- Martin open hearth process, the steels were ingot
usually semi-killed, and in many cases were normalized. And due to the drastic change in
the manufacturing processes very low carbon fully killed steels, were continuously casted
and brought to the required shape by the use of Thermomechanical controlled process
(TMCP). HSLA steels were firstly used in the ship construction, bridges, reinforced bars
but not introduced into line-pipe application until 1959 [3]. Then after the boom in the
technology has brought to the application into line-pipe steel with rapid evolution of
HSLA technology since then. HSLA is a type of alloy steel that provides very good
mechanical properties and are very highly resistant to corrosion than carbon steel. HSLA
steels are different from other steels that these are not made to meet the specific chemical
composition, however to meet the specific mechanical properties depending on the
application by varying the micro alloying elements accordingly. These steels will have a
very less carbon content varying from 0.05 to 0.025% to respond easily during forming
and welding operations. Other alloying elements are added approximately up to 2.0%
manganese and very little amounts of copper, niobium, nickel, vanadium, titanium,
chromium, nitrogen, molybdenum or zirconium [4, 5]. Cu, Ti, V and Nb are added for
strengthening purposes [5]. These elements are deliberately added to alter
the microstructure of carbon steels, which is generally the amalgamation of
3
Chapter 2 Literature review
ferrite-pearlite, to produce a very fine scattering of alloy carbides in an almost pure ferrite
matrix [6].
Mostly used in cars, cranes, trucks, bridges and other structures where huge amounts of
stress has to be handled and excellent strength to weight ratio is required. However, these
steels are good at strength to weight ratio their cross sections and structures are lighter by
20 to 30% compared to carbon steels with same strength [6].
HSLA steels are more resistant to corrosion than most carbon steels due to lack of pearlite
– and fine layers of ferrite (almost pure iron) and cementite in pearlite. HSLA steels
usually have densities of around 7800 kg/m³ [7].
2.2 Classification of HSLA steel

HSLA steels include many standard grades covered by ASTM standards designed to
provide particular strength, toughness, formability, weldability, and to with stand from
corrosion depending on the application of the material. HSLA steels are not the alloy
steels even though some amount of alloying elements are added to the steels to meet the
requirement. Particularly these are separate steels which are similar to as-rolled carbon
steels with improved mechanical properties by adding the alloying elements, and special
rolling techniques such as controlled rolling and rapid cooling techniques which are
explained briefly later. Because of this they are priced at the base price of carbon steels
not at the base price of the alloy steels which will be a bit expensive compared to the
carbon steels. However these steels are sold with minimum mechanical properties with
the specific alloy content left to the discretion to the steel producers. These steels are
classified into six categories [8, 9] weathering steels, microalloyed steels, rolled pearlitic
steels, acicular ferrite steels, dual phase steels, inclusion-shape-controlled-steels.
2.3 Effects of alloying elements

Manganese is one of the vital element in the line-pipe steels which plays a major role
because it will merges with Sulphur to form MnS. Which will cause hot shortness in
steels. Therefore, the addition of manganese with Sulphur and formation will vulnerable
of a steel to hot shortness [10]. It is added to steels to not only improve the hot working
4
properties of the steel, but it also improves the strength, toughness, hardenability. Iron
sulphide has lower melting point than MnS, which tends to form at the austenite
boundaries in the absence of manganese there are chances of increase in potential crack
growth sites during hot working [11]. With little amount of carbon with high amount of
manganese (Mn 0.8-0.15%) in steel design is depends on manganese leads to solid
solution strengthening [11].Silicon is one of the deoxidizer used in steel making. Silicon
exhibits properties like increase of solid solution hardening effect on ferrite and used to
improve the strength and toughness [10]. The strengthening rate of low carbon steels by
Si was higher in coarse grain region compared to that of the fine grain region. But, silicon
decreases the prior austenite grain size which leads to a fine ferrite grain size [12].
Increasing the amount of silicon will results in decrease in the rate of recrystallization and
increase the strength of austenite due to the solid solution hardening [13].Molybdenum
also has a great effect on increasing the high temperature strength and retarding grain
growth at temperatures just above the critical temperatures of steel [10]. It increases the
steel hardenability and shows very good resistance to hydrogen embrittlement and stress
corrosion cracking in high Sulphur content steels [14]. It has also been reported that
adding molybdenum to Microalloyed steels results in the slowing down of the bainitic
transformation which results in a fine bainitic region [15]. It is the most important
element in the micro alloying elements to stabilize the carbon and has very adverse effect
on austenite recrystallization and hardenability [10]. The rate of initial transformation of
austenite to high ferrite niobium steels is reduced by the solute drag effect of niobium and
pinning effect of the Nb(CN) precipitates [16].Vanadium is used to interfere the austenite
grain growth at peak temperatures results in fine grain therefore achieves good toughness
and strength [10]. But, steels that are hardened by precipitation hardening with vanadium
carbide exhibits poor wear resistance than vanadium free steels. Vanadium and Silicon
has a vital role in the microstructure and hardness. Microalloying with Titanium results in
the deceleration of austenite recrystallization along with precipitation strengthening of
ferrite. Titanium amalgamates with carbon and forms titanium carbides, which are highly
stable and difficult to dissolve in austenite. Titanium subsequently improves the
weldability and resistant to HAZ cold cracking due to TiC precipitate particles which acts
as the effective traps for hydrogen atoms [17].
5
Chromium is added to increase the corrosion resistance of the steels. It also increases the
hardenability and wear resistance of the steels. Chromium amount more than 4 weight %
in steels increases the corrosion resistance. However there will be a subsequent decrease
in the weldability. Chromium can form Cr3C2 by this the wear resistance increases
enormously [10]. Chromium polarizes the cathodic polarization curves of line-pipe steels
which helps in uneven corrosion rate in the line-pipe weldments [18]. Nickle improves
oxidation and corrosion properties of steels along with this it also improves toughness,
impact resistance and solid solution strengthening. Nickle also helps in forming of very
finer pearlite as pearlite is very strong and tougher results in very high toughness and has
no adverse effect on welding [10]. Aluminium is added as a deoxidizer to steels. But
adding this in excessive amount will results in decrease in toughness and the deoxidizing
function ends i.e. at weight% greater than 0.05. Aluminium likely to form aluminium
nitride (AlN) which has a very severe effect on hot ductility of different grades. If weight
% of aluminium increases by 0.02 it promotes precipitation of AlN rather than vanadium
nitride [21]. Copper is regarded as the dangerous element as it causes hot shortness which
reduces ductility of the material at temperatures 1100~1300oC. It also causes surface
defects during hot processing and it has been reported [20]. But, it increases the corrosion
resistance and tensile properties of steels. It is usually the element which causes
embrittlement in low alloy steels. Which promotes grain boundaries to segregate and
reduces the toughness property. It increases the tendency to cracking while welding
because of the embrittlement property present in it so due to this reason the amount of
phosphorous should be low as 0.015 weight% [21]. But when it is present in phosphate
form it reduces the hydrogen uptake. Sulphur is a harmful element in steels which form
sulphide inclusion with manganese and reduces the toughness properties in steels.
Sulphur will separate the grain boundaries which causes intergranular fracture [11].
Nitrogen it has been considered as one of the vital and low cost alloying additions to
steels. Nitrogen will be present in the interstitial atoms as nitrides of iron, titanium,
vanadium, aluminium, niobium and other alloying elements. Depending upon the form it
can be treated a s harmful or beneficial to physical and mechanical properties of the
steels. Because it is a small atom like carbon can easily diffuses in the steels and causes
surface hardening.
6
2.4 Processing and manufacturing of line-pipe steels

An important factor affecting strength and toughness of the material was rolling process
involved in the manufacturing of HSLA steels they are:
1. Thermomechanical Controlled Rolling (TMCR)

2. Thermomechanical controlled process (TMCP)
The TMCR consists in rolling slabs into plates in three main steps.
 First, rolling in temperatures of austenite recrystallization (around 1250oC),

 Second, rolling in austenite non-recrystallization temperatures (around 1050oC),
 Third, finishing rolling in austenite – ferrite Ar3 temperature(910oC) (or even at
lower temperatures depending on the carbon content and on the mechanical
resistance aimed)
 Finally air cooled.
The TMCP is similar to TMCR process for first three steps followed by accelerated
cooling i.e. with water after the third step of the controlled rolling [22, 23].
However, there is a difference between both TMCR and TMCP processes, the final
rolling pass temperature. In the TMCR process this temperature is lower because, as this
process does not have accelerated cooling, the mechanical properties should be
guaranteed during the final rolling pass. Reducing the temperature in this third step of the
process TMCR gives the material micro textures in the steel microstructure. These
textures have different orientations through steel plate’s thicknesses, which causes the
development of residual stresses in the as rolled material and which allows the appearance
of separations.
2.5 HSLA steels applications

HSLA steels are widely used in automotive industry, in oil and gas industry where fluids
or gases with very high pressure has to be transferred for huge distances, in earth movers
7
and heavy off road vehicles, industrial equipment, construction of bridges, trusses, storage
tanks, power transmission lines, in civil constructions etc. these are the additional
applications of this steels.
The choice of particular kind of steel depends on the application in which it is going to be
used depending number of application requirements like thickness, corrosion resistant,
formability, and weldability. Mostly in selection process of steels strength to weight ratio
of HSLA compared with normal low carbon steels. This characteristics of HSLA leads to
the application of line-pipes also [8].
2.5.1 HSLA steels in line-pipe applications

HSLA techniques in line-pipe steels was firstly used in Mannesmann, Europe in
normalized API Grade X-52 vanadium grades around 1952. Then later in 1953and 1962
further extended to API Grade X-56 and X-60 [24, 25].
Then in North America in the year 1959 hot rolled steel utilizing HSLA concepts came up
into existence [3] and this replaced the normalising process completely in Europe by 1972
[24, 25, 26].
HSLA steel was still used in Europe till the mid 1990’s and the applications and research
work on this different kinds on API 5L grades is going on till date.
8
Figure 2.1: Evolution of line-pipe grade steel [26]
2.6 Literature on shielded metal arc welding (SMAW) and

fracture toughness of HSLA steels
HSLA steels are welded because they are used in most practical applications. However
conventional arc welding causes many detrimental effects on the TMCP microstructures
and morphology variations. Changes in microstructure occurs when metal melts and
resolidifies as a coarse grain cast microstructure. These conventional arc welding was
firstly patented in 1892 by C.L Coffin of Detroit [27] for this welding process using a
consumable metal electrode. This was the first recorded process by which metal melts
from an electrode due to presence of arc to retain filler metal which adds alloying
elements to the weld nugget. Due to this filler metal some adverse effects may alleviate in
the weld nugget, however there will be no change in the heat affected zone (HAZ)
because melting and solidification does not happened in this zone. So the only way to
alter the microstructural variation in HAZ is by controlling the thermal cycle during
9
welding. Therefore great amount of research has been carried out in enhancing fracture
toughness of heat affected zone in conventional arc welding process [28]. In literature it
was reported by reducing the grain size of martensite-austenite constituents improve
fracture toughness [29]. Upper bainite has found to have brittle phase with low fracture
toughness. Low fracture toughness was not only because of upper bainite but there was a
partial contribution of lath carbide distribution in microstructure this was reported by
Johnson et al. [30]. The HAZ microstructure and properties can be controlled by varying
heat input, toughness can be increased by the formation of lower bainite at lower heat
inputs [31]. In spite of research efforts, arc welding leads to deterioration in base metal
properties.
2.7 Literature on submerged arc welding (SAW) and

fracture toughness of HSLA steels
Submerged arc welding (SAW) is a very economical process as compared to shielded
metal arc welding (SMAW) process with high deposition rate of four to ten times more
than that of SMAW with high heat inputs. As no visible arc`s and fumes are produced it is
safe for workers in the vicinity of the equipment. Very high currents around 200-400A
can be used without spatter because arc is completely shielded. Operator skill requirement
is very minimal because travel speed and wire feed rate are controlled by the welding
equipment itself. The sub merged arc welding process was first patented by Jones,
Kennedy and Rothermund in the year 1935 [32]. Microstructural and properties of the
weld metal are depended upon the chemical composition and the thermal cycle during
welding. So higher deposition rates requires high heat inputs in SAW. Hence only
chemical composition is available as a means of controlling the characteristics, like
microstructural and toughness of the weld metal. Past studies states that acicular ferrite is
the primary phase which plays vital role in improving the toughness in the weld materials
[33]. These transformed products during welding forms randomly oriented short ferrite
needle like structure with high angled grain boundaries. The fine grained and interlocked
laths of acicular ferrite provides maximum resistance to cleavage fracture, which
improves the notch toughness of the material. Hence it is suggested to increase the
10
acicular ferrite`s volume fraction in the weld metal by controlling the prior austenite grain
size which can be achieved by adjusting alloy content in weld metal. Past investigations
have reported that during transformation from austenite to ferrite, firstly ferrite is formed
along the grain boundaries and thickens in perpendicular direction towards the plane of
the austenite grain boundaries this grain boundary phase is termed as allotriomorph [34,
35]. It has been reported by liu et al. [36] that nucleation of acicular ferrite on oxide
inclusions takes place in weld metals; which further increase the acicular ferrite phase and
reduces the secondary phases which is recommended as acicular ferrite increases fracture
toughness of the weld metal.
Research on fracture toughness of submerged arc welding in HSLA steels is very limited.
Gosh et al. [37] reported variation in weld input parameters effect the tensile properties
fracture and fracture toughness of the material due to the change in the morphology of
weld consists of coarse and fine grains. He also reported that rise in the input energy
declines the ultimate tensile strength, hardness but enhances the ductility of the weld. Lu
et al. [38] reported that fracture toughness in base metal toughness will be always greater
than that of weld region and HAZ because grain coarsening and spherical precipitates
induced by welding heat input in WM and HAZ results a decrease in fracture toughness.
Volume fraction of acicular ferrite increases with increasing titanium content in

submerged arc welded HSLA steels which has been reported by Beidokhti et al. [39] they
have also reported that with increasing titanium content there was a phenomenal decrease
in the MnS inclusions in the weld metal where Ti based inclusion increases impact
toughness of the weld material. In further investigations proposed by Kiran et al. [40]
they have reported that by increasing welding speed tend to degrade weld pool size leads
to higher cooling rate that boost up the volume fraction of acicular ferrite phase and better
weld bead mechanical properties.
11
2.8 Fracture toughness J calculation

The perfect evaluation of ductile fracture behavior is critical task in reliability assessment
in line-pipe steels. An important parameter in the vulnerability of line-pipe steels was
hydrogen embrittlement. Plethora of research investigation were carried out on hydrogen
embrittlement and most of the tests imitate the procedure in the presence of high pressure
hydrogen. However these results are adequate in the safety point of view and directly
fracture toughness properties to be determined instead of assuming with some other
means. Fracture toughness tests are done with large samples in order to maintain the plain
strain condition [41].
2.10 J-integral
J-Integral was firstly proposed by Rice [42] as an energy integral which can be used as
distinct tool to find out the region under the elastic plastic conditions under crack tip
stress and strain. During initial crack extension most of the steels shows considerable
increase in the fracture toughness described by J-integral method commonly crack
propagation was tested by TPB or a compact specimen with deep cracks i.e. pre cracks on
the samples [42, 43].
J-integral method determines the J-integral as a crack extension (Δa). Then the J-integral
was calculated from the area under the load vs displacement curve and the crack
extension was calculated by single specimen (where a single specimen is tested with
loading compliance technique i.e. with loading and unloading sequence applied to a
sample) or multiple specimen technique (by considering many samples and performing
the testes and braking the sample with different loads) shown in the Figure 2.2 (a,b) and
the procedure and the explanation of the J-R curve method was explained by Hejazi et al.
[44].
12
Figure 2.2: (b) Load F vs LPD (Load point displacement) for a single specimen technique [45]
Figure 2.2: (b) J-R curve method used to determine JIC [46]
13
2.11 Re-appraisal of current problem

Now-a-days due to increasing demand of oil and gas industries, transportation of oil and
gas for very long distances through line-pipe became common these days. From the
application point of view HSLA steels are most suitable in which the mechanical
properties can be easily altered by addition of micro alloying in required proportions to
obtain the desired properties to the material based on the application so it is crucial to
study the fracture toughness of the material because it plays a vital role. After a detailed
survey on literature it was found that no report exists, which deals with the fracture
toughness of welded API X65 grade steels. Hence, the current investigation is intended to
study the fracture toughness of welded API X65 steels to fulfil this gap.
14
Chapter 3
Experimental procedures
3.1 Introduction
The aim of the present investigation is to study the facture toughness of welded high
strength line-pipe steel in which the material chosen for investigation was API X65. To
achieve this particular objective various tests were conducted which are discussed in this
chapter. A brief overview of the tests conducted were determination of chemical
composition of the selected steels, measurement of grain size and volume fraction of
phases, determination of mechanical properties of the selected steel, microstructural
characterization using optical and in transmission electron microscope in order to find out
the second phases and precipitates respectively at various zones of the sample i.e. parent
material, heat affected zone and weld zone. Harness profile of the sample was done in all
the regions and in different welds as well which will be explained with the help of a
stereo microscope image for better understanding, experiments related to fracture
toughness, study of fractured surfaces in scanning electron microscope.
3.2 Material selection and chemical composition

Material used in this investigation was 10 mm thick hot rolled plates pertaining to API
X65 grade where API stands for American petroleum institute. Plates of API X65 were
received after rolling at Tata Steel limited. The chemical composition of the received
plates was determined using optical emission spectrometer (ARL 3460).
20
Chapter 3 Experimental procedures
3.3 Welding of the material

Pieces of dimensions 100 x 25 x10 mm were taken for welding. The welding was done
with single bevel groove weld where different types of welds has been planned to be
incorporated in this investigation. SMAW or conventional weld or stick weld fir root run
followed by fill up of the joint by SAW. The cross sectional view of the sample is shown
below in order to get a clear understanding of how the weld has been done Figure 3.1
which has been captured with LEICA M165C stereo microscope ( Figure 3.2). The weld
parameters along with consumables are discussed in the results and discussion. As the
welds were not visible directly, some part of the sample was cut at the weld zone into
25x10 mm sample. The samples were prepared which will be explained briefly later in the
microstructural examination.
Figure 3.1: Cross sectional image of the material after weld
Figure 3.2: LEICA M165C Stereo microscope
21
3.4 Microscopic examinations and image analysis

As mentioned earlier in section 3.3 (Welding of the material) small portion of the welded
sample was cut along the cross section. The sample of size 25x10 mm was cut with the
help of Mecatome T-210 slow speed cutter. The latter is shown in the Figure 3.3.
Figure 3.3: Mecatome T-210 slow speed cutter
The mounting of the sample for microscopic observation was done with the help of
Mecapress II specimen mount press (shown in the Figure 3.4) which is a hot mounting
machine and takes around 20 min to mount the sample. The advantage of mounting the
sample is ease of holding during polishing and handling. The mounting was done using
conducting mounting material to facilitate SEM observation.
Figure 3.4: Mecapress II specimen mount press
22
Generally, two types of resins are used e.g. black coloured conductive resins and red
coloured non-conducting resins. Although red resins (shown in Figure 3.5) are more
economical to use, mounting with black resins is required if SEM examination is planned.
Only samples mounted in black resins are conducting and are suitable for SEM.
Figure 3.5: Red and black resin powder used in the mounting of the sample
The mounted samples were polished using standard metallographic technique. First the
samples were polished using different grades of emery papers (manufactured by Presi,
made in France) with varying grit sizes namely 120, 180, 360, 600, 1000, and 1200. In
order to remove the tapered ness and burr on the sample, grit sizes of 120,180 and 360 are
used for very less time because material removal rate is very high in these papers of high
grit size. Rest of the emery papers were used successively to remove the scratches on the
sample surface. Polishing with emery papers were carried out using Mechatech Z64
semiautomatic polishing machine shown in Figure 3.6.
Figure 3.6: Mechatech Z64 semiautomatic polishing machine
23
In the above machines, there are disks to attach the emery papers and these emery papers
are provided with glue in the back side to easily fix these on the discs. The polishing on
emery papers was followed by polishing with 6µm, 3µm and 0.25 µm diamond slurry
(supplied by FLACON MECAPREX LD 33E) using cloth as polishing surface in the
same machine as mentioned above. The smooth, reflective and scratch-free sample thus
obtained was cleaned with ethyl alcohol and dried with hot air blower. The polished
sample was etched with 2% Nital (a solution of 2ml nitric acid HNO3 in 98 ml ethanol)
and then the sample was cleaned with ethyl alcohol and dried with hot air blower again.
The sample was further etched with 4% picric acid (4gms picric acid ((NO2)3C6H2OH),
100ml ethanol).
The microstructures of the investigated material were examined with optical microscope
shown in Figure 3.7 manufactured by LEICA (model: DM 6000M) with image analyzer
software installed in the attached computer. With the help of image analyzer series of
images were captured at different locations as mentioned earlier i.e. parent material, heat
affected zone and weld zone respectively. The average grain size of the material was
ASTM 10 and approximate phase fraction are shown in Figure 4.1.
Figure 3.7: LEICA DM 6000M with image analyser German made
24
3.5 TEM Analysis

In order to get better understanding of the second phases and precipitates present in the
material TEM analysis has been done for the material. Thin samples of about 0.08 mm or
80 µm have been prepared by mechanical thinning process wherein care was taken not to
introduce any bend in the samples. Thinned samples were etched with Nital in order to
reveal the various zones on the sample. Punching of the sample has been done because
the sample diameter is only 3mm that can be accommodated in sample holder of TEM
equipment. The samples were punched in such a way that in all the different zones at least
two samples can be obtained. After punching, electro polishing of the sample were done
before loading the sample into the TEM. The process of electro-polishing has been
explained briefly with the help of the Figure 3.8. For example, Figure 3.8 (a) shows the
image of the sample after punching; Figure 3.8(b) shows the equipment used for electro-
polishing (Tenopol-5 product of STRUERS) and Figure 3.8(c) shows the image of the
samples after electro-polishing. Different parameters used while electro polishing are as
follows: current: 30-40 milli ampere, voltage: 16V for first cycle for 30 sec followed by
19V for second cycle for 30 sec. Samples were cleaned with methanol before placing into
the solution for electro-polishing i.e. Acitic acid 90% + Percolic acid 10%.
(a) (b) (c)
Figure 3.8: Explain the sequential procedure of electro polishing
The electro polished samples were loaded in the sample holder of TEM shown in Figure
3.9 model JEOL-2200FS Field emission electron microscope.
25
Figure 3.9: JEOL-2200FS Field emission electron microscope (TEM)
3.6 Hardness measurement

The sample was placed in the sample holder (Figure 3.10) securely prior to measurement
of microhardness. Microhardness tester used in the present work (LECO model
LM247AT Michigan, USA) is shown in Figure 3.11. The microhardness profile across
the different zones of the weld region was evaluated.
Figure 3.10: Sample holder used for measurement of microhardness
26
Figure 3.11: The micro-hardness tester used in the present work
The hardness measurement of was made using load of 300 gmf for a dwell time of 10
Sec. The image of the sample after hardness measurement as captured with the help of a
stereo microscope is shown in Figure 3.12. The image is incorporated for better
understanding of the exact location of the sample where the hardness profile was
estimated.
Figure 3.12: Image of sample after hardness indentations
27
3.7 Tensile test

Tensile tests specimen were fabricated according to ASTM- E08 [47] and were loaded to
fracture on universal testing machine, model Instron 5582 shown in the Figure 3.13. The
capacity of machine is 100 kN. Specimen ends were gripped and fixed in machine and its
gauge length was continuously measured by advanced video extensometer (AVE)
attached with the machine, until fracture.
Figure 3.13: Tensile testing machine used in the present work
3.8 Fracture Toughness Testing

Fracture toughness is the property of that describes the ability of a material containing a
crack for resisting fracture. In case of brittle materials, linear elastic fracture mechanics
(LEFM) is applicable and the toughness is usually defined as a value, which is
characterized by the stress intensity factor K. Alternatively, for ductile materials, Elastic
Plastic Fracture Mechanics (EPFM) has been developed. The toughness is defined either
as a point value or as a resistance curve and is usually characterized by the J-integral. A J-
integral based resistance curve i.e. J-R curve shows the resistance of a ductile material
against crack initiation, its stable growth and tearing instability. This is the defined as J-
controlled crack growth regime. To obtain a J-R curve from a single specimen test, an
elastic unloading compliance technique is employed, wherein small elastic un-loadings
28
are applied periodically during the experiment and the change in compliance of these un-
loadings is used to estimate the crack length. This technique utilizes the phenomenon that
as the crack length increases, the specimen compliance also increase i.e. its stiffness is
reduced. Initially the sample was pre-cracked and loaded for fracture toughness test
following ASTM E1820-13 standard [48] using a servo hydraulic test system (Instron
model: 8850 shown in Figure 3.15. A representative sample after fracture toughness
testing is shown in Figure 3.14.
Figure 3.14: Broken sample after fracture toughness testing.
Figure 3.15: The servo hydraulic test system used for estimation of fracture toughness
29
3.9 Fractography
Fractography studies are important to analyze the mechanism of crack growth [49]. This
becomes especially important for welded specimen in order to identify the location of
crack initiation and the subsequent crack growth path. In the present work, failed
specimens after fracture toughness testing were first examined with stereoscope to
examine the macroscopic features of fractured surfaces. Thereafter, micro-fractography
was carried out using a FE-SEM shown in Figure 3.16. The FE-SEM is manufactured by
ZESIS (model supra 25). Before placing the fractured-sample in the FE-SEM, it was
cleaned with ultrasonic cleaner. During fractography, microscopic features associated
with crack-origin as well as crack growth path were documented by capturing relevant
fractographs.
Figure 3.16: Image of FE-SEM (ZESIS SUPRA 25 German made)
30
Chapter 4
Results and Discussion

In this chapter, the obtained results from various characterization techniques are discussed
along with their pertinent analyses.
4.1 Chemical composition

Plates of API X65 material were received from the hot roll mill of Tata Steel Ltd. with
thickness of 10 mm each. The chemical composition was analyzed with optical emission
spectrometer and the results are shown in Table 4.1. The chemical composition of the API
X65 was compared with the API 5L standard [2]. The chemical composition of the
material was in good agreement with the results reported by Hashemi et al. [50].
Table 4.1: Chemical composition of API X65 in weight %
Element Weight % API 5L
C 0.0541 0.430
Mn 1.4980 1.450
S 0.0011 0.015
P 0.0121 0.025
Si 0.2302 0.350
Al 0.0288 0.040
V 0.0355 0.080
Nb 0.0572 0.050
Mo 0.0860 0.250
N 54*
*indicates that it is in terms of ppm (parts per million)
31
Chapter 4 Results and discussion
The nature of the precipitating elements and the micro alloying elements present plays a
major role in the strength and toughness of HSLA steels. For example Nb, V, Ti used for
grain refinement of the HSLA steels: these elements form precipitates and enhances grain
refinement property in the steels [51]. Mo also serves the same purpose but by
amalgamation of some amounts of Nb addition it increases the steel strength [52]. Mn
increases the solid solubility of the steels but if Sulphur is present in steel, it forms MnS
and the effects of MnS and contributes to reduction in ductility of the steels [53].
Therefore, the nature of precipitates and microalloyed elements plays a key role in the
mechanical properties of the steel [54].
4.2 Tensile properties

The tensile tests were carried out on samples fabricated following the ASTM-E08 [47].
The procedure of tensile testing was explained in chapter 3. Specimen ends were gripped
in the machine up to the gauge length marked with two white dots the calibrated distance
between the two white dots was continuously measured by advanced video extensometer
(AVE) attached to the machine till fracture and the readings are obtained in the system
attached to the machine. The obtained tensile properties were summarized in the Table
4.2
Table 4.2: Tensile properties of API X65
Sample Yield Strength Ultimate Tensile Uniform Elongation at

Number (MPa) Strength (MPa) elongation (%) fracture (%)
1 465.53 571.41 11.57 30.23
2 464.00 570.76 12.01 30.65
3 477.84 570.85 11.65 30.01
32
4.3 Microstructure and grain size determination

After welding of the material the sample was prepared as explained earlier and the
microstructural analysis was done with a optical microscope (Model: LEICA DM 6000M
with image analyzer made in Germany).
SAW
(a) (b)
SMAW
CGHAZ
(c) (d)
(e) (f)
Figure 4.1: Detailed microstructure of API X65 weld
33
The detailed microstructure of weld one is shown in Figure. 4.1. Figure. 4.1(a) shows the
parent material microstructure comprising of ferrite and other second phases. As
mentioned earlier, the ratio of ferrite to second phases is approximately 9:1. Figure. 4.1(b)
shows the SAW, SMAW and CGHAZ region (coarse grain heat effected zone) of the
weld. Figure. 4.1(c) and (d) show the CGHAZ and slightly coarsened HAZ region,
wherein prior austenite grain boundaries can be observed. Figure 4.1(e) further away fine
grain HAZ is observed. Figure. 4.1(f) shows acicular ferrite microstructure. In order to
better understand the second phases and precipitates, transmission electron microscopy
was carried out and results are discussed in Figure.4.3.
The average grain size of the base material was found to be 10 µm which also satisfies the
ASTM standard and also reported by Fragiel et al. [55]. By this there was approximately
91% of ferrite and 9% of second phases shown in Figure.4.2
Figure 4.2: Representative Figure and phase fraction for APIX65
As there are some precipitates present in the material it is very difficult to directly know
the second phases present in the material so futher investigation was performed by using
transmission electron microscopy by this the second phases and precipitates were found
out.
34
(a)Bainitic sheave with coarse

(b) Polygonal structure (c) EDX of precipitate – NbC
carbide
(d) Acicular ferrite (e) Inclusion and AF (f) EDX of precipitate – Al2O3
(g) EDX of precipitate-

(h) Bainitic sheaves (i) Coarse Fe3C
complexTiO2
35
(j) Polygonal structure (k) GB decorated with Fe3C (l) EDX of precipitate – NbCN
Figure 4.3: (a)-(c) base material; (d) to (g) weld region; (h) & (I) coarse HAZ and (j)-(l) fine
HAZ
In order to analyze the microstructure in and adjacent to weld zone in APIX65 steel, TEM
analysis was carried out to identify the different microstructural phases (Figure. 4.3).
Bainitic sheaves were observed in parent material, weld zone, grain coarsened and grain
refined region. Acicular ferrite was seen in weld region and it nucleated on inclusion
namely Al2O3 and complex TiO2 types. Coarsened carbides particles (Fe3C) were
observed in parent material and also in heat affected zone. Niobium carbide and niobium
carbonitrides precipitates were observed in parent material and also in grain refined
region but not in grain coarsened region, where it is possible that these precipitates were
dissolved.
Ferrite/ proeutectoid ferrite is formed during the slow cooling from austenite at the
highest transformation temperature. Increasing the cooling rate lead to different kinds of
ferrite phases. At slow cooling, ferrite grains form precipitated at austenite grain
boundaries which leads to polygonal ferrite formation. At higher cooling rates ferrite
loses its polygonal structure and forms elongated crystals termed as Widmanstatten ferrite
(WF). Further increasing the cooling rate will lead to formation of massive ferrite or quasi
polygonal ferrite.
36
Bainite has named after the report submitted by Davenport and Bain in 1930 [56] where
there are six classifications in bainite which was reported by Reynolds in 1991 [57] of this
two were mostly acknowledged they are lower bainite and upper bainite i.e. if the
cementite was formed inside the bainitic ferrite it is termed as lower bainite at lower
temperature and if cementite was present at the grain boundaries of the bainitic ferrite it is
termed as upper bainite at higher temperatures. Acicular ferrite was first reported by
Smith in early 1970`s [58] noted for its high dislocation density and fine grain nature
leads to good mechanical properties like good strength, corrosion resistance and good
toughness at low temperature. Acicular ferrite will have ferrite plates randomly placed
with prior austenite grains [59]. This was formed upon rapid cooling of low carbon steels
where there are ferrite plates with long elongated morphology which is quite different
from that of polygonal ferrite. The formation of acicular ferrite depends on the cooling
rate as mentioned earlier it also depends on the amount of deformation on the rolling
passes tells the volume fraction of acicular ferrite produced, the larger the deformation the
higher the transformation temperature then the higher the amount of acicular ferrite in
microstructure.
4.4 Hardness profiles of API X65 welded sample

Hardness test was carried out for the samples prepared as mentioned in chapter 3. For
better understanding, the stereoscope image of the sample indentation is illustrated in
Figure.4.4. Hardness profiles was done with HV-300 gf and dwell time of 10Sec for
APIX65 base metal and weld joint shown in Figure 4.5 (a) and (b).
37
Weld defect
Indentations
Figure 4.4: Image of the sample after indentations
300
Weld zone hardness (SAW to SMAW bead)
250
Vickers Hardness (HV - 300 gf)
200
150 SMAW root and

SAW fill up bead
back fill pass
100
50
0
0 5 10 15 20 25 30
Indent number
Figure 4.5 (a): Hardness profile vertically top to bottom in weld zone
300
SAW Bead SMAW Root Pass SMAW Back fill Pass
250
Vickers Hardness (HV - 300 gf)
200
150
100
50
0
0 20 40 60 80 100
Indent Number
Figure 4.5 (b): Hardness profiles horizontally across weld zone
38
In Figure 4.5(a), hardness measurements from top to bottom in the weld zone is shown, it
can be seen that despite similar all weld metal strength, the hardness drops by 35 VHN in
SMAW deposit and this can be attributed to tempering effect of the SAW fill up pass.
From microstructural point of view the higher hardness in the weld region is due to the
presence of acicular ferrite in the weld region. Weld hardness across the weld zone along
SAW fill up, SMAW root pass and SMAW back pass are shown in Figure 4.5(b). A dip
in hardness is observed approximately 10 mm away from the weld zone which is HAZ
(heat effected zone). The hardness value of HAZ is slightly lower than that of BM (base
metal) and a bit lesser than that of the weld region, this is due to the presence of bainite,
polygonal ferrite and acicular ferrite in the HAZ region. During welding, these HAZ
region will not experience any melting, but there will be microstructural changes due to
phase transformation shown in the Figure 4.1 (c, d, e). The grain size was varied with the
distance from the fusion line. The coarseness in the microstructure was due to the heat
input of the SAW and SMAW welding processes. From this low hardness value of the
HAZ compared to BM explains slightly softening of HAZ in API X65 weldment reported
by Hashemi et al. [60]. Similarly HAZ softening for this steel was reported by Lee et al.
[61]. It should be noted that tensile properties of the HAZ region was not reported by the
API standard [2]. It is very difficult to determine the strength levels in HAZ which
requires special testing equipment. However Lee et al. reported that some micro-tensile
experiments can determine tensile properties in HAZ [62].
4.5 J-R curve tests on welded API X65 plates

Fracture toughness of API X65 plates were carried out as per ASTM E1820 [48]. Three
point bend specimen geometry was selected and dimensions are shown in Figure. 4.6.
Notch was placed in weld zone, fusion line and heat affected zone beside tests conducted
for parent material. These regions were identified by etching the EDM cut sample and
marking the selected region for notch cutting.
39
Figure 4.6: Three point bend specimen for J-R curve testing
Tests were conducted at a cross head velocity of 0.008 mm/min. Two samples were tested
for each selected zone. J-Integral method determines the J-value as a function of crack
extension (Δa).
The J-value is calculated from the area under the load-displacement curve and crack
extension. This be measured by either multiple specimen technique where different
samples are tested to different loads and break all the samples to measure the crack length
manually. The current investigation is conducted using a single specimen for the J-
integral tests.
Figure 4.7 (a): Load vs displacement obtained from the data collected from the equipment
40
The load applied was in the negative direction as shown in Figure 3.14. The load was
applied from top to bottom by taking the set value as zero before loading the sample so all
the values obtained from the machine are in the negative direction. The results are shown
in Figure 4.7 (a) and by changing the symbol of the obtained results the graph was turned
to the positive planes of the X,Y axis as shown in Figure 4.7 (b).
Figure 4.7 (b): Load vs displacement plot modified to match with standard
Representative J-R curves for weld and heat affected zone, are shown in Figure. 4.8. The
area under the curve represents the energy observed by the specimen before fracture,
which indicates that toughness of heat affected zone is superior to weld zone. Based on
analysis of the obtained curves the JQ values for different regions are listed in Table 4.3.
41
2000
1800
1600
1400
1200
J (N/mm)
1000
800
600
Heat Affect Zone
400
Weld
200
0
0 0.5 1 1.5 2
Δa (mm)
Figure 4.8: Representative J-R curves for weld and heat affected zone
The fracture toughness testing was done for each sample and the obtained results are
tabulated below in Table 4.3 which shows the JQ values in different zones.
Table 4.3: JQ value obtained for different regions of welded API X65
Region JQ value (N/mm)

1960
Base Material
1925
940
Weld zone
890
1425
Fusion line
895
1940
Heat affected zone
1910
From Table 4.3 we can find out the fracture toughness of the material ranging from 890 to
1960 N/mm respectively. There is no significant change in the toughness values in
between base material and heat affected zone. As there is no much variation in
microstructure in base material and in heat affected zone the toughness values are also
almost similar. At room temperature all the values that are required to obtain J Q values
42
have exceeded the API standard 1104 and DNV-OS-F101 standard [62, 63]. The JQ
values of weld zone are about 53% lower than that of base material. The value for fusion
line samples are significantly different i.e. 1425 and 895 N/mm indicating an average
reduction of 40% in JQ value as compared to base material. The scatter in fusion line
value can be attributed to error in precise placement of notch or deviation in crack growth
path during testing. The difference in JQ values in the weld zone may be due to the
presence of defect in the weld nugget as from the stereo microscope image shown in
Figure 4.4. Despite the excellent toughness at various zones, there was a huge difference
between the base metal and weld zone because of the weld defect present in the filled up
weld done with submerged arc welding process and due to this, the criterion of uniform
crack front and uniform crack growth may not be satisfied. The results obtained are used
to determine the crack length and if there is non-uniformity in the crack growth it leads to
less accurate crack estimations. In this study all the samples were tested with constant
thickness so comparison of the samples was valid, as the geometry of all the samples is
same.
4.6 Fractography of fracture toughness tested broken

samples
The fractographic tests of different broken samples after fracture toughness tests are done
in FE-SEM. Typical fractographs are illustrated in Figure 4.9. As one can see from Figure
3.16 the fracture toughness tested samples did not completely break during the test, these
were broke by putting the sample in liquid nitrogen for about 1min followed by
hammering. It is known that introduction of liquid nitrogen makes a steel brittle thereby
makes it easier to break. Figure 4.9 (a) shows the two broken halves of the single edge
notch (bend) specimen. One can clearly note the notch region (represented by ‘N’ in the
figure) fatigue pre-crack region (represented by ‘FP’) crack growth region (represented by
‘CG’) and final failure (represented by ‘FF’). Figure. 4.9(b) shows a magnified view of
sample highlighting the fatigue pre-crack and crack growth region; it also shows the
measurement of fatigue pre-crack front which gives the initial value of crack for the final
J-R curve test. Figure. 4.9(c) mainly shows the crack growth region. Figure. 4.9(d) shows
fatigue striations present in fatigue pre-crack region. In this the presence of secondary
43
micro cracks and slips planes considered as typical fatigue crack surface of API X65
material with fatigue striations present in this region. It is evident from the images that the
fracture occurred shown in Figure 4.9(e) is a higher magnification image of very fine
dimples present in coarse grained heat effected zone indicating ductile fracture with
having very high fracture toughness which is in agreement with Jang et al. [64].
FF
(a) (b)
CG
FP
(c) (d)
(e) (f)
Figure 4.9: Stereoscopic and SEM micrographs of different regions of tested three point bend J-R
curve sample
44
It is reported that the fracture occurred in API 5L series consists a brittle to ductile
transition i.e. the fractures initiates with brittle fracture (trans granular cleavage) and later
is arrested by ductile region [65] . In API series the failure mode for fracture toughness
was ductile fracture due to the ductile behavior of API X65 material. Obviously by the
fractographic study shown in figure 4.9(e) with dimples it is evident supporting for this
conclusion. Figure 4.9(f) shows the final fracture caused by striking the sample with a
hammer after dipping it in liquid nitrogen. The brittle cleavage morphology can be
observed from this fractograph; but this is of no effect in the fracture toughness of the
material as it has been performed for convenience for fractographic study.
Overall, different characterizations were done for API X65 steel. This include chemical
composition, tensile properties, microstructural analysis, TEM analysis, fracture
toughness tests, fractography. The obtained results indicated that the steel is a good
candidate for use in line-pipe steel and its weld.
45
Chapter 5
Conclusion and future scope
5.1 Conclusions
The aim of this investigation was to evaluate the fracture toughness of welded API X65
steel plates keeping in view the limited number of reported works on the subject. The
selected steel was characterized in terms microstructure, hardness and tensile properties.
The welding of steel plates was performed with sub merged arc welding (SAW) with root
pass of shielded metal arc welding (SMAW). The microhardness profile in. base material
(BM), heat affected zone (HAZ), weld zone (WZ) and weld nugget were evaluated. The
microstructural features of the above zones were revealed using optical and transmission
electron microscopy. The fracture toughness of the above zones of welded plate was
evaluated in terms of J-R curve following the concept of EPFM. Major conclusions are:
 The evaluation of fracture toughness of welded API X65 indicates that, JQ value
of heat affected zone was slightly lower than the base material, but for the weld
zone it dropped significantly by 53% due to the non-uniform crack front and crack
propagation. The phenomenon is attributed to presence of different defects in the
weld region.
 JQ value for fusion line samples showed significant scatter with an average
reduction of 40% in JQ value as compared to base material. The scatter in fusion
line value can be attributed to error in precise placement of notch or deviation of
crack path during testing.
 Presence of Nb and V imparts precipitation hardening effect to the API X65 steel,
such that it has a satisfactory combination of strength and toughness parameters
fulfilled by API service requirements.
46
Chapter 5 Conclusion and future scope
Future scope
5.2 Scope for future research

 Study of Fatigue crack growth rate tests (FCGR) can be performed on this
material with same welds.
 Study of fracture toughness with different combinations of conventional welding
techniques can be performed.
 Fracture toughness variations with changing weld parameters like welding speed
and wire feed rate etc. can be performed.
 Study of fracture toughness tests can be performed by welding as spiral
submerged arc welding process with varying thickness by comparing the
toughness values one can recommend the best thickness for practical applications
in oil and gas industry.
47
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Evaluation of Fracture Toughness of Welded

High Strength Low Alloy Line-pipe Steel

Banda Venkata Bhargava

Department of Metallurgical and Materials Engineering

National Institute of Technology Rourkela

Thesis submitted to the

National Institute of Technology Rourkela

in partial fulfillment of the requirements

Metallurgical and Materials Engineering

Banda Venkata Bhargava

(Roll Number: 214MM1337)

Under the supervision of

Prof. Krishna Dutta

Department of Metallurgical and Materials Engineering

Dr. Krishna Dutta

May 26, 2016

R & D, TATA Steel Ltd. Jamshedpur

Dr. Shrabani Majumdar

May 26, 2016

May 26, 2016 Banda Venkata Bhargava

I bow humbly to record my deep sense of gratitude to my Co-Supervisor Dr. Shrabani

I thank Prof. S. C. Misra Head of the Department Metallurgical and Materials

May 26, 2016 Banda Venkata Bhargava

Co-Supervisor's Certificate ......................................................................... iii

Declaration of Originality ............................................................................. v

Abstract ........................................................................................................ vii

List of tables ................................................................................................ xiii

1.1 Background and motivation ....................................................................................... 1

1.2 Objectives of the present work .................................................................................. 2

2.1 Introduction ................................................................................................................ 3

2.2 Classification of HSLA steel...................................................................................... 4

2.3 Effects of alloying elements ....................................................................................... 4

2.4 Processing and manufacturing of line-pipe steels ...................................................... 7

2.5 HSLA steels applications ........................................................................................... 7

2.8 Review of fracture toughness testing....................................................................................................

2.8.1 Stress intensity factor K (Equivalent to energy release rate G) ..................................

Bookmark not defined.

2.8.2 J-integral ............................................................ Error! Bookmark not defined. 11

2.8.3 Crack tip opening displacement (CTOD).................................................................................11

2.8.4 Crack tip opening angle (CTOA)1111111111111111111

2.9 Why CTOD test?..............................................................................................................................................

2.9.1 CTOD estimation ...................................................................................................................................

2.9.2 Fracture toughness J calculation........................................................................ 12

2.10 J-integral ................................................................................................................ 12

2.11 Re-appraisal of current problem ............................................................................ 14

3.1 Introduction .............................................................................................................. 20

3.2 Material selection and chemical composition .......................................................... 20

3.3 Welding of the material ........................................................................................... 21

3.4 Microscopic examinations and image analysis ........................................................ 22

3.5 TEM analysis ........................................................................................................... 25

3.7 Tensile test ............................................................................................................... 28

3.8 Fracture toughness testing........................................................................................ 28

3.9 Fractography ............................................................................................................ 30

Results and Discussion

4.1 Chemical composition ............................................................................................. 31

4.2 Tensile properties ..................................................................................................... 32

4.3 Microstructure and grain size determination ........................................................... 33

4.4 Hardness profiles of API X65 welded sample ......................................................... 37

4.5 J-R curve tests on welded API X65 plates ............................................................... 39