International Journal of Cast Metals Research

ISSN: 1364-0461 (Print) 1743-1336 (Online) Journal homepage: https://www.tandfonline.com/loi/ycmr20

Influence of heat treatment on matrix structures

in cast iron

B.-R. Zhao, S. Ueno, S. Yamada, K. Sugita & H. Nakae

To cite this article: B.-R. Zhao, S. Ueno, S. Yamada, K. Sugita & H. Nakae (2008) Influence of
heat treatment on matrix structures in cast iron, International Journal of Cast Metals Research,
21:1-4, 62-66, DOI: 10.1179/136404608X361675

To link to this article: https://doi.org/10.1179/136404608X361675

Published online: 18 Jul 2013.

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 Influence of heat treatment on matrix
structures in cast iron
B.-R. Zhao*, S. Ueno, S. Yamada1, K. Sugita2 and H. Nakae3
Flake graphite cast iron (FC) samples containing 2%Si, in which the S contents changed from
0?006 to 0?076%, were heated at 1123 to 1323 K and then cooled to determine the pearlite
morphological change, namely lamellar or granular. For the spheroidal graphite cast iron (FCD)
samples, the P contents changed from 0 to 0?2% and those of Sn were from 0 to 0?06% with
0?5%Cu using the 2?5%Si and 0?3%Mn iron.
The pearlite morphology of the FC samples cooled from 1123 K was granular. The pearlite
structure of the Sn–FCD samples was also granular, when cooled from 973 and 1023 K, and that
of P–FCD was granular only in the sample cooled from 1023 K, otherwise the morphology was
lamellar.
The pearlite morphology of FC and FCD samples depends on the solubility of C in the austenite
which can be varied by the heating temperature. This mechanism is identical to that of the lamellar
to rod transition in eutectic alloys.
Keywords: Cast iron, Heat treatment, Matrix structure lamellar and granular, Pearlite morphology

Introduction electrolytic iron, 98% metallic Si, electrode graphite

The objective of this research is to elucidate the influence
of alloying elements and heat treatment on the pearlite
morphology in cast iron. There are two types of
pearlites, namely lamellar and granular, and the
granular one has recently been called spheroidite.1
Nevertheless, the authors use the terminology granular
pearlite for discussing the morphological change from
lamellar to granular. The flake graphite cast iron (FC)
and spheroidal graphite cast iron (FCD) were prepared
for the discussion of the pearlite morphological change
based on their chemical compositions and the heat
treatment. The authors already reported the influence of
sulphur (S) and heating temperature on the pearlite
morphology in FC,2,3 in which S acts as the pearlite
stabiliser. Moreover, if the carbon content in austenite,
which can be controlled by the heating temperature, is
lower than 0?7 mass% (abbreviated per cent), the
granular pearlite precipitates in the high sulphur FC.
The authors then prepared the FCD samples in this
research for the discussion of the influence of the
chemical elements, P and Sn, as surface active elements.4
Experimental
Sample preparation
The FC samples were prepared using a 6 kg Al2O3
lined high frequency induction furnace from 99?9%
1
I Metal Technology Co., Ltd, Japan
2
JFE Steel Corporation. East Japan Works, Chiba, Japan
3
Laboratory for Materials Science and Engineering, Waseda University,
Tokyo, Japan
*Corresponding author, email hakuei_chou@imetal.co.jp
and FeS chemical reagent. The melt, inoculated with
0?3% of the Fe–75%Si–3%Ca alloy, was cast into shell
moulds with a dimension of 30 mm inner diameter and
300 mm length. Their targeted chemical composition
was 3?6%C–2?0 %Si and 0?005, 0?01, 0?02, 0?04 and
0?08%S.
The FCD samples were melted using a 100 kg MgO
lined high frequency induction furnace. The phosphorus
added ones, labelled P–FCD, were prepared from 50%
high purity pig iron, 20% steel scrap and 30% return
scrap. The tin added ones, Sn–FCD, were made of
50%FCD scrap, 50% steel scrap, electrode graphite, Fe–
75%Si, Fe–28%P, pure Sn and pure Cu. The spheroidis-
ing treatment was carried out by the sandwich method
using a 1?4% Fe–45%Si–4?5%Mg–1?1%RE–1?5%Ca
alloy. The targeted composition of the samples was
3?65%C–2?5%Si–0?3%Mn and the P content was chan-
ged from 0?02 to 0?2% for the P–FCD with 0?2%Cu, that
of the Sn–FCD was 0?5%Cu and the Sn content was
changed from 0?01 to 0?06%. All of these melts were cast
into one inch Y block moulds made by an organic
binder and shaken out after a 90 min held. The chemical
compositions of these samples are shown in Table 1.
Heat treatment and matrix observation
The cut FC samples, 30 mm in length, the P–FCD
samples, 25625630 mm, and the Sn–FCD samples,
256256260 mm, used for the heat treatment, were
packed in one stainless container with graphite powder
for preventing their oxidation. The FC samples were at
1123, 1223 and 1323 K for 60 min, and then cooled in
air for normalising within the container. The heating
temperatures of the P–FCD samples were 873, 1023 and
1073 K and held for 60 min, then cooled in air at the

ß 2008 W. S. Maney & Son Ltd.

Received 21 May 2008; accepted 11 July 2008
62 DOI 10.1179/136404608X361675 International Journal of Cast Metals Research 2008 VOL 21 NO 1–4
 Zhao et al. Influence of heat treatment on matrix structures in cast iron

1 Matrix structure of as cast P–FCD and Sn–FCD samples

cooling rate of 18 K min21. Those of the Sn–FCD 2 Matrix structure of FC samples normalised from 1123 K
samples were 973, 1023 and 1073 K and held for
180 min, then cooled in air at the cooling rate of the 4Sn– and 6Sn–FCD is completely pearlite due to the
14?4 K min–1. The heating temperature of the FCD effect of Sn and Cu on the pearlite formation.
samples was set between their Ac1 and Ar1 temperatures,
which were measured using a dilatometer with Matrix structure of normalised samples
w3?0610 mm length samples heated to 1173 K and The matrix structure of the normalised FC samples,
cooled in a vacuum. The heating and cooling rates were cooled from 1123 K, is shown in Fig. 2. As can be
15 K min21. The measured Ac1 and Ar1 temperatures clearly seen, all of the pearlite is granular and the matrix
are shown in Table 2. of the 0S sample is totally ferrite and that of the 1S one
All of the samples were polished and etched with nital is ferrite at the periphery of the sample and granular
for observation of the matrix structure using an optical pearlite at the centre part. This means that the matrix
microscope, while some of the granular FC samples were structure of the 0S and 1S samples is completely
etched by 10%HNO3 nital along with ultrasonics for different from that of the as cast ones, which are nearly
20 s and observed the three-dimensional morphology lamellar pearlite as already shown in Fig. 1. The matrix
observed using an SEM.5,6 Those of the FCD samples, structures of the normalised FC samples, cooled from
etched by 20%HNO3 nital with ultrasonics for 300 s, 1223 K, are shown in Fig. 3.
were used for the SEM observations. As shown, the pearlite is perfectly lamellar. What
happened to produce this difference?
The influence of the heating temperature on matrix
Results structure in the P–FCD samples is shown in Fig. 4 and
Matrix structure of as cast samples that of the Sn–FCD is shown in Fig. 5. The authors can
The matrix structure of the as cast FC samples is totally confirm the formation of granular pearlite in the P–FCD
lamellar pearlite except for the 0S sample, whose matrix samples, cooled from 1023 K, and that of the sample,
consists of a small amount of ferrite beside the flake cooled from 873 K, is lamellar. Nevertheless, the matrix
graphite,2 that of the FCD ones is also totally lamellar structure of the sample, cooled from 1073 K, consists of
pearlite with ferrite, called the bull’s eye structure. The a dual phase, namely fine ferrite and fine pearlite. The
influence of alloying elements, such as P and Sn, on the results of the Sn–FCD ones are similar those of the P–
pearlite stabilising effect can be confirmed in Fig. 1. FCD except for the volume fraction of the pearlite. On
In these cases, the P–FCD samples contain 0?2%Cu the other hand, the pearlite structure of the sample,
and that of the Sn–FCD samples contains 0?5%Cu as cooled from 973 and 1023 K, is granular besides the
already shown in Table 1, therefore, the authors can spheroidal graphite and that of the eutectic cell
confirm the higher pearlite fraction in the 0Sn–FCD boundary is lamellar as shown in Fig. 5.
sample than that in the 0P–FCD sample. The matrix of All of the results are summarised in Table 3. These
results show that the matrix structure is significantly
affected not only by the alloying elements, but also by
Table 1 Chemical compositions of samples, mass%
the thermal hysteresis, such as the heating temperature
Group C Si Mn P S Cu Mg Sn
Table 2 Measured eutectoid temperature of FCD samples
FC 0S 3.56 2.05 0.033 0.005 0.006 – – –
1S 3.58 1.91 0.033 0.005 0.011 – – – Eutectoid temp., K
2S 3.68 1.98 0.033 0.005 0.018 – – –
4S 3.59 1.97 0.033 0.005 0.038 – – – Group Ar1 Ac1
8S 3.37 1.95 0.033 0.005 0.076 – – –
P–FCD 0P 3.59 2.60 0.29 0.017 0.007 0.22 0.037 – P–FCD 0P 946 1052
5P 3.71 2.52 0.25 0.052 0.008 0.24 0.035 – 5P 948 1048
10P 3.69 2.48 0.28 0.098 0.008 0.24 0.037 – 10P 936 1062
20P 3.65 2.38 0.28 0.188 0.008 0.23 0.035 – 20P 944 1048
Sn–FCD 0Sn 3.70 2.44 0.52 0.019 0.007 0.56 0.039 0.010 Sn–FCD 0Sn 950 1051
4Sn 3.68 2.39 0.38 0.017 0.008 0.56 0.042 0.045 4Sn 953 1053
6Sn 3.69 2.41 0.45 0.018 0.007 0.55 0.040 0.056 6Sn 949 1048

International Journal of Cast Metals Research 2008 VOL 21 NO 1–4 63

Zhao et al. Influence of heat treatment on matrix structures in cast iron

4 Matrix structure of P–FCD samples normalised from

3 Matrix structure of FC samples normalised from 1223 K 873 to 1073 K

and as cast. If the heating temperature is between the

Ac1 temperature and the Ar1 temperature, the morphol-
ogy of the pearlite is granular otherwise it is lamellar.
The three-dimensional photo of the granular pearlite is
shown in Fig. 6 for the 6Sn–FCD sample, when cooled
from 1023 K, the morphology is rod like, and that of the
4Sn–FCD sample shown in Fig. 7, has a morphology
that is coral like.
Nevertheless, the pearlite morphology of the as cast
ones is perfectly lamellar as is well known. Of course, the
lamellar pearlite is made by the plate like cementite.
What does this mean?

Discussion
The spheroidising of cementite in steel, namely granular
pearlite, as reported by Sauverur7 adopted the divorcing
mechanism. He showed that if the steel is kept for a
sufficiently long time at a certain temperature, but
slightly below its critical range, preferably between 873
and 973–K, the cementite shows a marked tendency to
collect in the form of rounded particles embedded in a
matrix of ferrite. Moreover, the spheroidising of
5 Matrix structure of Sn–FCD samples normalised from
973 to 1073 K: PL – lamellar pearlite, PG – granular
pearlite and PC – colony like pearlite
cementite is easier in the low carbon steel than that of
the high carbon one. The authors consider that the
critical range should be the eutectoid temperature.
Therefore, he showed that the morphological change is

Table 3 Influence of heating temperature on matrix structure

HT*, K 1123 1223 1323 As cast

CC{ NL{

FC 0S F1 F FzPL PL
1S FzPG PL PL PL
2S PG" PL** PL PL
4S PG PL PL PL
8S PG PL PL PL
HT, K 873 973 1023 1073 As cast
P–FCD 0P FzPL – Fz(PG) FzPL FzPL
5P FzPL – Fz(PG) FzPL FzPL
10P FzPL – Fz(PG) FzPL FzPL
20P FzPL – Fz(PG) FzPL FzPL
Sn–FCD 0Sn – FzPLzPG FzPLzPG FzPLz(PG) FzPL
4Sn – PLzPGzf{{ PLzPGzf FzPLz(PG) PL
6Sn – PLzPGzf PLzPGzf FzPLz(PG) PL
*HT: heating temperature.
{
CC: cooling condition.
{
NL: normalising (cooled in air).
1
F: ferrite.
"
PG: granular pearlite.
""
(PG): granular pearlite ratio ,5%.
**PL: lamellar pearlite.
{{
f: ferrite ratio ,10%.

64 International Journal of Cast Metals Research 2008 VOL 21 NO 1–4


6 Three-dimensional observation of granular pearlite by
SEM: 6Sn–FCD, normalising at 1023 K
the decomposition of the lamellar pearlite to a granular
one. Zener8 also discussed the formation mechanism of
granular pearlite based on the curvature of the cementite
due to the interfacial energy. If the authors consider the
influence of the holding temperature on the pearlite
morphology, they could not agree with these theories.7–9
The authors also consider that these morphological
changes in pearlite are similar to that of the rod to
lamellar transition in eutectic alloys proposed by
Helawell10 and Jackson.11 In this case, the transition is
controlled by the critical volume fraction of the second
phase, namely cementite. The critical fraction is
y30 vol.-%, if the authors consider the carbon content
in the austenite at which the cooling starts based on the
Janowak’s Fe–C–2%Si section phase diagram.12 The
solubility of carbon into the FC austenite can be
calculated as a function of the heating temperature,
then they become as follows, 0?70% at 1123 K, 1?03% at
1223 K and 1?35% at 1323 K. For the as cast samples,
the authors think that the solubility can be calculated at
1423 K, then it is 1?6%. However, these values are for
the carbon contents, then the authors have to convert
these values into the cementite volume fractions assum-
ing that the density of the ferrite is 7?86 Mg m23 and
that of the cementite is 7?66 Mg m23 by Angus.13 These
are as follows, 10?7, 15?7, 20,6 and 25?4 vol.-%
respectively. Therefore, the critical volume fraction
should be between 10?7 and 15?7 vol.-%. If the authors
7 Three-dimensional observation of granular pearlite by
SEM: 4Sn–FCD, normalising at 1073 K
International Journal of Cast Metals Research
Zhao et al. Influence of heat treatment on matrix structures in cast iron
8 Observation of a granular and b lamellar pearlite by
SEM: 6Sn–FCD, normalising at 1023 K
similarly calculate the solubility of carbon into the FCD
austenite using the Fe–C–2?4%Si phase diagramu,14 it is
0?56%C and the volume fraction is 8?6 vol.-%. These
values are far less than 30 vol.-%.
Figure 8 shows the pearlite morphology of the 6Sn–
FCD sample, cooled from 1023 K, in which granular
and lamellar pearlites coexist. These photos show that
the granular one exists near the spheroidal graphite and
the lamellar one is at the eutectic cell boundary.
Figure 9 shows that the pearlite morphology and the
distribution of Si, Cu and Mn were confirmed by the
wavelength dispersive X-ray spectrometry and electron
probe microanalysis (WDX-EPMA). These results show
that the Si and Cu segregate near the spheroidal graphite
and Mn segregates at the cell boundary. This means that
the local eutectoid temperature should be changed with
these segregations. Therefore, not only the solubility of
carbon, but also the contents of the alloying elements
also may affect the pearlite morphology.
Conclusion
The authors have been studying the influence of the
heating conditions and alloying elements on the matrix
structure of flake and spheroidal graphite cast iron, in
particular, the morphological change in pearlite.
The mechanism of the pearlite morphological change
from lamellar to granular is identical for the flake and
spheroidal graphite cast iron, and it is controlled by the
carbon content in the austenite, from which the sample
is cooled. If the heating temperature is between their Ac1
and Ar1 temperatures the morphology is granular,
otherwise is lamellar.
This mechanism differs from the spheroidising
mechanism of pearlite in steel and similar to that of
the eutectic structure, namely a rod to lamellar transi-
tion except for the critical volume fraction. If the volume
fraction of the cementite is less than 10%, the granular
pearlite is formed. There are two types of granular
pearlite, namely, rod like and coral like, confirmed by
the three-dimensional observations by SEM using a
sample deeply etched by nital along with ultrasonic
vibration. The mechanism has not yet been clarified.
2008 VOL 21 NO 1–4 65
Zhao et al. Influence of heat treatment on matrix structures in cast iron
9 Colour mapping of 6Sn–FCD normalising at 1023 K by WDX-EPMA
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