Metallographic Preparation of Cast Iron: Application Notes

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Metallographic

preparation of Cast iron


Application
Iron is one of the most diverse met-
Notes
als and alloyed with carbon and other
elements it offers an enormous variety
of cast iron and steel alloys. Cast iron
has been produced in China as early
as 600BC and in Europe it was first
known in the 14th century. With the
development of coal fired blast fur-
naces the properties of iron improved
and a better castability opened new
fields of applications for products in
every day life. With the industrialisa-
tion cast iron became an important
construction material as buildings from
the 19th century show: the domes of in the automotive and engineering in-
train stations, market halls, and green dustry. In addition, specific cast irons
houses of botanical gardens, bridges are the material of choice for sea water
and the Eiffel Tower still document the pump housings, rolling mill rolls and
substantial application of cast iron dur- parts for earth moving equipment.
ing that time. As the morphology of graphite has
a major influence on the mechanical
The term cast iron refers to those iron- properties of cast iron, metallographic
carbon-silicon alloys which contain quality control of grey iron is an in-
2.5% - 4% carbon and usually 1-3% tegral part of its production process. Austempered ductile
silicon. Cast iron is an important engi- Using standard reference comparison iron, Beraha color etch,
DIC, 500x
neering material with a number of ad- charts and/or image analysis tech-
vantages, mainly good castability and niques, the morphology, size and dis-
machinability and moderate mechani- tribution of the graphite is determined
cal properties. on an unetched, polished sample.
Depending on the specification, the
Because of its economical advantages sample is then etched to check the
cast iron is used for many applications structure of the matrix.

Difficulties during metallographic preparation


Cutting: White cast iron is very hard and size can be difficult. The matrix of
and therefore difficult to cut. ferritic and/or austenitic cast irons is
Grinding and polishing: Graphite is prone to deformation and scratching.
soft and retaining it in its true shape

Solution
- Cubic boron nitride cut-off wheel
- Thorough diamond polishing on hard
polishing cloths and final oxide
polishing.

Fig.1: Grey iron with flake graphite, 200x Fig. 2: Same as Fig.1, showing correct polish 200x
insufficient polish
Production and Fig. 6: Exhaust manifold,
compacted graphite iron

application of
cast irons

Production Austempered ductile iron (ADI) is a ductile


Cast irons are melted in a cupola- or induc- iron austenitized at 840-950°C and then
tion furnace charged generally with pig quenched to 250-400°C where it is held un-
iron, cast iron scrap, steel scrap and vari- til the matrix is changed to ausferrite. This is
ous additions. The alloy composition and a mixture of needle-like ferrite and a carbon
the cooling rate will influence whether the saturated retained austenite, which gives the
iron will solidify grey or white. ADI iron a high strength and ductility. The
A fast cooling rate results in a white solidi- microstructure looks like bainite but has no
fication and the formation of iron carbide carbides.
(Fe3C or cementite). At the eutectoid trans- High-strength ADI irons are mainly used
formation a fast cooling rate promotes the Fig. 4: Grey iron with flake graphite in 200x for wear resistant parts for heavy trucks,
formation of pearlite, whereas a slow cool- pearlitic matrix farm and earth moving equipment. Applica-
ing rate promotes the formation of graphite tions of ductile ADI irons are for parts with
and ferrite. evenly dispersed graphite flakes in a pearl- dynamic stress such as axle journals, gear
The microstructure of grey cast irons can itic matrix (see Figs. 3 and 4). drives, crankshafts, pull hooks and wheel
have either a pearlitic and/or ferritic matrix Grey iron has a high damping capacity, hubs.
with free graphite in the shape of flakes, excellent sliding properties and thermal
nodules or temper carbon respectively. conductivity, which makes it suitable for For making Compacted graphite iron (CG)
Through alloying and heat treatment the machine bases, damping plates for pianos, the same raw material is used as for mak-
properties of cast iron can be adjusted for engine blocks, flywheels, piston rings, ing ductile iron. By carefully controlling the
certain applications, for instance, alloying brake discs and drums. amount of magnesium added to the melt
with molybdenum and nickel improves for nodulizing approx. 80% of graphite is
their heat and corrosion resistance. Ductile iron with spheroidal graphite formed as compacted graphite, the rest as
In the following the individual cast irons (SG), also called nodular or spheroidal nodules.
will be briefly described and their major iron, is made from the same raw material The quality control of compacted iron is
fields of application mentioned. as grey iron but requires higher purity. very important as the formation of graphite
The melt should be free of Pb, As, Sb, Ti, is critical. A slightly higher percentage of
and Al and have very little phosphorus nodules can be tolerated, but the formation
and sulphur. By adding trace amounts of of flakes has to be avoided as they would
magnesium to the melt before casting, the lower or even eliminate the beneficial prop-
graphite forms in a spherical shape instead erties of the compacted iron.
of flakes. Compacted graphite iron has better
Ductile iron has greater strength and duc- strength, ductility, alternating stress fatigue
tility than grey iron of similar composition. strength and higher resistance to oxidation
Ductile iron has good machining qualities than grey iron; and it is better to cast, easier
and is used for heavy duty gears, pistons, to machine, has better damping qualities
Fig. 3: Grey iron with fine flake graphite, 100x
rolls for rolling mills, gear cases (Fig.10),
unetched valves, tubes and door hinges. Pearlitic
ductile iron is the initial material for cam-
Grey iron with flake graphite (FG) has and crankshafts which are surface hard-
between 2.5-4% carbon, 1-3% silicon and ened for wear resistance (Fig. 8).
0.2-1% manganese. Carbon and silicon
promote the formation of graphite flakes
and ferrite. Phosphorus in small amounts
increases the fluidity of grey iron. It also
forms a ternary phosphorus eutectic called
“steadit”, which constitutes a web like
structure increasing the wear resistance.
In the flake form, graphite provides
notches within the metallic matrix and
consequently lowers the tensile strength,
especially when the flakes are very large.
In unalloyed grey iron the best mechanical
properties can be achieved with fine and
Fig. 5: Filter head of ADI cast iron for the Fig.7: Part of a wheel cassette of austempered
hydraulic system of a pressure die casting ductile iron
machine for plastics
Fig. 8:
Crankshaft, ductile iron

Fig. 9: White cast iron, pearlite with ledeburite 200x Austenitic cast iron, etched with 3% Nital 200x
+ modified Beraha’s reagent

and thermal conductivity and retains the good retention of strength and hardness is easier to cast and therefore suitable for
shape better under temperature changes at elevated temperatures. Due to its large precision casting of complicated shaped
than ductile iron. masses of carbides, especially when al- parts with a narrow wall thickness.
Applications: cylinder heads for high turn- loyed, white cast iron has an excellent The main properties of austenitic cast irons
ing diesel motors, axle- and gear cases, resistance against wear and abrasion. It is are: corrosion resistance against sea water
exhaust manifolds (Fig. 6), housings of used for shot-blasting nozzles, rolling mill and alkaline media and high strength and
turbo chargers. rolls, crushers, pulverizers and ball mill scale resistance at high temperatures.
liners. They are used specifically for applications
White cast iron contains 1.8-3.6% carbon, in the maritime environment, for instance
0.5-1.9% silicon and 1-2% manganese. By chilling grey or ductile iron on the out- for large pump housings and other parts of
A fast cooling rate prevents the precipita- side and letting it cool slowly inside, it is desalination plants, or bushings and linings
tion of carbon as graphite. Instead the car- possible to produce parts with a hard sur- in chemical plants, compressors for ag-
bon, which is in solution in the melt, forms face of white cast iron with a ductile core gressive gases, housings for gas turbines
iron carbide (Fe3C, also called cementite). (chilled cast). and turbo chargers.
The structure of white cast iron consists of
pearlite and ledeburite (Fig. 9), a eutectic Malleable iron with tempered
of pearlite, converted from austenite, and graphite (TG)
cementite. Ni-hard alloys (8-9% Cr, 5-6% Malleable iron is made by heat treating
Ni) have a martensitic matrix with chro- white cast iron. Through a two stage, long
mium carbides. time heat treatment (tempering) white cast
iron is converted to ferritic or pearlitic mal-
White cast iron has a high compressive leable iron. The carbon of the iron carbide
strength and alloyed versions have a first goes into solution, and through slow
cooling then precipitates in irregular nod-
ules called temper carbon. Pearlitic malle-
able iron can be hardened.
Increasingly malleable iron is replaced
by nodular iron for economical reasons,
especially since the fields of application are
very similar.

Austenitic cast iron


Cast irons with at least 20% nickel and
1-5.5% chromium have an austenitic
matrix with graphite in form of flakes or
nodules. Austenitic cast iron can be an
economic alternative to stainless steel as it
Ferritic malleable iron 200x Fig.10: Differential housing of ductile iron
Difficulties in the
preparation of
cast iron

Alloyed white cast irons are very hard (HV Time constraints often make it difficult to
600) and can be difficult to cut, especially maintain consistent preparation results
large sections. It is important to point out, using manual methods and often, due to
that despite this hardness diamond cut-off the geometry of the test piece, automatic
wheels are not suitable for cutting white preparation is not a suitable alternative.
cast iron. However, as the design of the test pieces
The main problem when preparing sam- is usually arbitrary, their dimension and
ples of cast iron is to retain the graphite form can be changed in order to fit into an
in its original shape and size. Although in automatic system (Fig.13). This has been
the microscope the image of the graphite successfully carried out by some manu-
Fig.11: Insufficient polish leaves graphite 200x
is viewed as 2-dimensional, it should be nodules covered with smeared metal facturers who where then able to make the
remembered that it is actually 3-dimen- preparation more efficient and improve the
sional. This means that during grinding and evaluation of the graphite.
polishing the appearance of graphite can Most of the standard microscopic checks
slightly change, and that a certain percent- of cast irons are done with a magnification
age of graphite is cut very shallow with of 100x, which makes the graphite appear
only a weak hold in the matrix. Therefore black. Only with higher magnifications can
there is always a possibility that the graph- it be verified if the carbon is completely
ite can not be completely retained. Espe- retained. Well polished graphite is grey
cially very large flakes or agglomerations (Fig.14).
of flakes have the tendency to loose the
graphite. Therefore graphite nodules can Fig.12: Correct polish shows shape and size of 200x Note: cast irons with graphite are not
not always be retained or polished well. graphite nodules suitable for evaluation suitable for electrolytic polishing as the

In malleable cast irons graphite exists in graphite is washed away by the electrolyte.
the form of rosettes or temper carbon. A common preparation error is the insuffi- However, if only a quick identification of
This is a friable form of graphite and can cient removal of smeared matrix metal after the microstructure of the matrix is required
be particularly difficult to retain during the grinding, which can obscure the true shape electrolytic polishing and etching can be
preparation. and size of graphite (compare Figs.11 and used (Fig.15).
12). This is particularly prevalent in ferritic
or austenitic cast irons that are prone to
deformation and scratching. For these ma-
terials a thorough diamond and final polish
is especially important.

The difficulties associated with the prepa-


ration of cast irons with graphite can be
compounded in situations where metallog-
raphy is an integral part of the casting line
quality system.

SEM image of grey iron with flake graphite

Fig.14: Well polished graphite flakes 500x

SEM image of ductile iron with graphite nodules Fig.13: Sample holder for semi-automatic polishing of Fig.15: Ductile iron electrolytical polished and etched
quality control samples in cast line shows the pearlitic matrix and ferrite surrounding
graphite. Graphite is washed away
Grinding Grinding

Step PG FG Step PG FG

Surface MD-Piano 220 MD-Allegro Surface Foil/Paper MD-Largo*

Type Diamond Diamond Type SiC Diamond


Abrasive Abrasive
Size #220 9 μm Size #220 9 μm

Suspension/ Water DiaPro Suspension/ Water DiaPro


Lubricant Allegro/Largo 9 Lubricant Allegro/Largo 9

rpm 300 150 rpm 300 150

Force [N]/ 30 30 Force [N]/ 30 30


specimen specimen

Time (min) Until plane 5 Time (min) Until plane 5

Polishing Polishing

Step DP 1 DP 2 Step PG FG OP**

Surface MD-Dac MD-Nap Surface MD-Dac MD-Nap OP-Chem

Type Diamond Diamond Type Diamond Diamond Collodial Silica


Abrasive Abrasive
Size 3 µm 1 μm Size 3 µm 1 μm 0.04 μm

Suspension/ DiaPro DiaPro Suspension/ DiaPro DiaPro OP-U


Lubricant Dac 3 Nap B 1 Lubricant Dac 3 Nap B 1 NonDry

rpm 150 150 rpm 150 150 150

Force [N]/ 40 30 Force [N]/ 30 20 10


specimen specimen

Time (min) 4 1-2 Time (min) 4 1-2 1

Table 1: Alternatively DiaPro diamond suspension can be Table 2: *In cases where retention of graphite is very difficult, MD-Plan cloth can be tried for
Preparation method replaced by DP-Suspension, P, 9 µm, 3 µm and Preparation method fine grinding.
for white cast irons 1 µm respectively, applied with blue lubricant. for cast irons with **This step is optional
graphite
Alternatively DiaPro diamond suspension can be replaced by DP-Suspension P, 9 µm,
3 µm and 1 µm respectively, applied with blue lubricant

Recommendations for the Grinding and polishing:


preparation of cast iron Traditionally cast irons with graphite have
been ground with silicon carbide Foil/Paper.
Cutting: For sectioning hard, white cast In recent years diamond grinding has
irons a cubic boron nitride wheel is recom- replaced silicon carbide for fine grinding
mended. For large sections automatic cut- most cast irons as it keeps the samples
ting is more efficient than very flat and doesn’t leave the graphite in
manual cutting. For cutting relief (compare Fig.16 and 17).
cast irons with graphite it is Hard white cast irons and ADI irons can
recommended to select an be plane ground with diamond (MD-Piano
aluminium oxide wheel 220) and also fine ground with diamond Fig.16: Grey iron prepared with fine grinding on silicon
carbide Foil/Paper, still shows scratches
according to the hardness (MD-Allegro, see table 1). Soft and medi-
of the cast iron to be cut. um hard cast irons with a ferritic, austenitic
or pearlitic matrix are plane ground with
Mounting: Quality control samples are silicon carbide Foil/Paper and fine ground
usually prepared unmounted. For failure with diamond on MD-Largo, see table 2).
analyses samples it is recommended to For cast irons that tend to corrode dur-
use hot compression mounting. For soft ing polishing it is recommended to use
to medium hard cast irons a phenolic resin water free diamond suspension, A, and
(MulitFast) is recommended, for harder yellow lubricant. The preparation data are
types of cast irons a reinforced resin for 6 samples, 30 mm dia., mounted and
(DuroFast) is more suitable. clamped into a specimen holder.
Fig.17: Same as Fig.16, prepared with fine grinding with
diamond on MD-Largo, showing good edge retention
Struers ApS
Pederstrupvej 84
DK-2750 Ballerup, Denmark
Phone +45 44 600 800
Fax +45 44 600 801
[email protected]
www.struers.com

Cleaning: As many cast irons tend to cor-


rode easily the cleaning of samples has to AUSTRALIA & NEW ZEALAND
Struers Australia
NETHERLANDS
Struers GmbH Nederland
be fast and should always be carried out 27 Mayneview Street
Milton QLD 4064
Zomerdijk 34 A
3143 CT Maassluis
with cold water. Under no circumstances Australia
Phone +61 7 3512 9600
Telefoon +31 (10) 599 7209
Fax +31 (10) 5997201
should the samples be left in contact with Fax +61 7 3369 8200 [email protected]
[email protected]
water. Thorough rinsing with ethanol and NORWAY
BELGIUM (Wallonie) Struers ApS, Norge
fast drying with a strong stream of warm Struers S.A.S. Sjøskogenveien 44C
370, rue du Marché Rollay 1407 Vinterbro
air is recommended. If corrosion still oc- F- 94507 Champigny Telefon +47 970 94 285
curs cleaning and rinsing with water free sur Marne Cedex
Téléphone +33 1 5509 1430
[email protected]

alcohol only is recommended. Austempered ductile iron, etched with 200x


Télécopie +33 1 5509 1449
[email protected]
AUSTRIA
Struers GmbH
Zweigniederlassung Österreich
3% Nital, pol. light
Etching: Initially, the cast iron samples BELGIUM (Flanders)
Struers GmbH Nederland
Betriebsgebiet Puch Nord 8
5412 Puch
are microscopically examined unetched Note: do not use diamond cut-off wheels! Zomerdijk 34 A
3143 CT Maassluis
Telefon +43 6245 70567
Fax +43 6245 70567-78
to evaluate shape, size and distribution of Plane grinding, fine grinding and polishing Telefoon +31 (10) 599 7209 [email protected]
Fax +31 (10) 5997201
graphite and possible cast porosity. After are carried out with diamond. [email protected] POLAND
Struers Sp. z o.o.
this initial evaluation the sample is etched CANADA Oddział w Polsce
Struers Ltd. ul. Jasnogórska 44
for microstructure with 1 - 3% Nital. Integrated into online casting, semi-auto- 7275 West Credit Avenue 31-358 Kraków
The following Beraha reagent can be used matic preparation equipment can achieve Mississauga, Ontario L5N 5M9
Phone +1 905-814-8855
Phone +48 12 661 20 60
Fax +48 12 626 01 46
for colour etching and can be modified better results for a reliable and reprodu- Fax +1 905-814-1440
[email protected]
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according to the alloy: cible graphite evaluation than manual CHINA


ROMANIA
Struers GmbH, Sucursala
1000 ml water preparation. Struers Ltd. Bucuresti
No. 1696 Zhang Heng Road Str. Preciziei nr. 6R
200 ml hydrochloric acid Zhang Jiang Hi-Tech Park
Shanghai 201203, P.R. China
062203 sector 6, Bucuresti
Phone +40 (31) 101 9548
24 g ammonium difluoride Author Phone +86 (21) 6035 3900
Fax +86 (21) 6035 3999
Fax +40 (31) 101 9549
[email protected]
To 100 ml of this stock solution add 1 g Elisabeth Weidmann, Anne Guesnier, [email protected]
Struers A/S, Copenhagen, Denmark SWITZERLAND
potassium metabisulfite. CZECH REPUBLIC & SLOVAKIA Struers GmbH
Struers GmbH Organizační složka Zweigniederlassung Schweiz
Note: When working with chemicals the Acknowledgements vědeckotechnický park Weissenbrunnenstraße 41
We wish to thank CLAAS GUSS GmbH, Bielefeld, Přílepská 1920, CH-8903 Birmensdorf
standard safety precautions have to be CZ-252 63 Roztoky u Prahy Telefon +41 44 777 63 07
Germany, for supplying sample material and giving Phone +420 233 312 625
observed! permission for the reproduction of the foundry photo on Fax +420 233 312 640
Fax +41 44 777 63 09
[email protected]
page 1 and Figs. 5 and 7. Our special thanks go to Dr. [email protected]
[email protected]
Summary Christine Bartels for her generous support and also to SINGAPORE
Struers Singapore
Ute Böhm.
Cast irons are ferrous alloys with mostly GERMANY
Struers GmbH
627A Aljunied Road,
#07-08 BizTech Centre
We thank GF Eisenguss GmbH, Herzogenburg, Austria,
2.5%-4% carbon and 1-3% silicon. The for the permission to reproduce Figs. 6, 8 and 10.
Carl-Friedrich-Benz-Straße 5
D- 47877 Willich
Singapore 389842
Phone +65 6299 2268
carbon is either present as graphite in grey We thank Zentrale für Gussverwendung, Düsseldorf, Telefon +49 (0) 2154 486-0 Fax +65 6299 2661
Fax +49 (0) 2154 486-222 [email protected]
irons or in form of iron carbide and alloy for the permission to reproduce the two SEM photos [email protected]
on page 4. SPAIN
carbides in white cast iron. The difficulty in FRANCE Struers España
Struers S.A.S. Camino Cerro de los Gamos 1
the metallographic preparation is to retain Bibliography 370, rue du Marché Rollay Building 1 - Pozuelo de Alarcón
the true shape and size of the graphite in Literature from Zentrale für Gussverwendung, F-94507 Champigny
sur Marne Cedex
CP 28224 Madrid
Teléfono +34 917 901 204
Düsseldorf
its flake, nodular or tempered form. Dur- Téléphone +33 1 5509 1430
Télécopie +33 1 5509 1449
Fax +34 917 901 112
[email protected]
Vera Knoll, Gusseisen, 2003
ing grinding the matrix is smeared over [email protected]
Metals Handbook, Desk Edition, ASM, Metals Park, FINLAND
the graphite and unless it is followed by a Ohio, 44073, 1997 HUNGARY Struers ApS, Suomi
Struers GmbH Hietalahdenranta 13
very thorough diamond polish, the graphite ASM Handbook Vol. 9, Metallography and Magyarországi Fióktelepe 00180 Helsinki
Microstructures, ASM, 2004 2040 Budaörs Puhelin +358 (0)207 919 430
is not shown in its true form. Especially Szabadság utca 117 Faksi +358 (0)207 919 431
Schumann, VEB Deutscher Verlag für Phone +36 2380 6090 [email protected]
cast irons with a soft ferritic matrix tend Grundstoffindustrie, Leipzig, 1968 Fax +36 2380 6091
to smear and are prone to deformation Werkstoffkunde und Werkstoffprüfung, W. Domke,
Email: [email protected] SWEDEN
Struers Sverige
and scratching. Plane grinding with silicon Verlag W. Giradet, Essen, 1977 IRELAND
Struers Ltd.
Box 20038
161 02 Bromma
carbide Foil/Paper is recommended, fol- Unit 11 Evolution@ AMP Telefon +46 (0)8 447 53 90
Whittle Way, Catcliffe Telefax +46 (0)8 447 53 99
lowed by fine grinding and polishing with Rotherham S60 5BL [email protected]
Tel. +44 0845 604 6664
diamond. A brief final polish with colloidal Fax +44 0845 604 6651 UNITED KINGDOM
[email protected] Struers Ltd.
silica is optional. Unit 11 Evolution @ AMP
ITALY Whittle Way, Catcliffe
Struers Italia Rotherham S60 5BL
White cast irons are very hard and a cubic Via Monte Grappa 80/4 Tel. +44 0845 604 6664
20020 Arese (MI) Fax +44 0845 604 6651
boron nitride cut-off wheel is recommend- Tel. +39-02/38236281 [email protected]
ed for sectioning. Fax +39-02/38236274
[email protected] USA
Struers Inc.
JAPAN 24766 Detroit Road
Marumoto Struers K.K Westlake, OH 44145-1598
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Tokyo
141-0022 Japan
Phone +81 3 5488 6207
Fax +81 3 5488 6237
[email protected] 28.02.2019 R05 / 62140306

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