Materials Science & Engineering A 571 (2013) 193–198

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Effect of cerium and lanthanum on the microstructure and mechanical

properties of AISI D2 tool steel
Mohammad Ali Hamidzadeh n, Mahmood Meratian, Ahmad Saatchi
Department of Materials Engineering, Isfahan University of Technology, Isfahan 84156-83111, Iran

a r t i c l e i n f o abstract

Article history: AISI D2 tool steel has excellent wear resistance with high dimensional stability. This type of steel is
Received 20 November 2012 suitable for making molds. This paper describes investigations into the effect of adding Ce/La on
Received in revised form microstructure of AISI D2 type cold work tool steels obtained by means of optical microscopy, scanning
29 January 2013
electron microscopy, X-ray diffraction, energy dispersive X-ray spectrometry (EDS) and image analyzer.
Accepted 31 January 2013
Available online 14 February 2013
The results showed that after modification with Ce/La, the morphology, size and distribution of M7C3
carbides change greatly. The carbide network tends to break, and all carbides are refined and
Keywords: distributed homogeneously in the matrix, and also reduce the size of chromium carbides and increase
Cold work tool steel the dissolution of carbides during heat treatment. The results of mechanical tests show that the
Grain refinement
toughness of the alloy increased about 75% without reducing the hardness of the alloy.
Mechanical characterization
& 2013 Elsevier B.V. All rights reserved.
Fracture

1. Introduction volume ingots and technical restrictions in ingot casting of these

AISI D2 steel is in group of cold work tool steels. There are high
chromium carbides in the microstructure of these alloys due to
the presence of high chromium ( 12 wt%) and high carbon (1.5–
2.35 wt%) contents that cause excellent wear resistance and high
strength properties. Due to their high abrasion resistance proper-
ties, they are used in the molds [1–4].
Alloy elements such as chromium and carbon segregate
seriously during solidification of this alloy. So, eutectic carbides
often form a network along dendrite boundaries in as-cast
microstructure, which reduce fracture toughness greatly. These
continuous networks of chromium carbide cause deep cracks in
large ingots during hot deformation, that sometimes lead to
the collapse of large ingots [5,6]. To solve this problem in the
production process of high-alloy tool steels, today’s modern
manufacturing techniques such as powder metallurgy and spray
forming are alternative methods to replace conventional ingot
casting. In these methods, due to rapid solidification of molten
steel, an alloy is produced in which very fine and uniform
dispersion of carbides occurs in comparison to conventional ingot
casting [7,8]. But, conventional ingot casting is still used for lower
production costs, due to the high cost of production equipments
and their high technology. Thus, ingot casting modification is a
basic option in producing high-alloy tool steels. Because of high
n
Corresponding author. Tel.: þ98 9126526950; fax: þ98 01213230583.
E-mail addresses: mahamidzadeh@yahoo.com,
ma.hamidzade@ma.iut.ac.ir (M.A. Hamidzadeh).
alloys, there is no possibility of increasing the cooling rate in
order to reduce cell size, dendrite arm or fragmentize of second-
ary phases. In other words, for technological reasons, thermal
modification cannot be effectively used to improve the casting
properties. In such cases, it is necessary to use chemical mod-
ification by adding small quantities of some chemical elements.
Recently, adding niobium and titanium has been investigated
for refining the eutectic chromium carbides in high chromium
cast iron (HCCI) and high alloy tool steels. Presence of these
elements can lead to the formation of ‘‘TiC’’ and ‘‘NbC’’ carbides at
a higher temperature than the eutectic carbides, reducing the
carbon content in the melt and thereby the volume fraction of the
eutectic carbides. Continuity of net-like eutectic carbides greatly
decreases by adding titanium and niobium, and toughness of
ingots cast increases. Replacing eutectic carbides with titanium
and niobium carbides (with high hardness) causes an increase in
abrasion resistance of the alloy [8–13]. But conditions of heat
treatment of these alloys changed because heat stability of
austenite and ferrite phases areas change. So, heat treatments
of these alloys need more investigations after adding elements of
niobium and titanium. On the other hand, by adding Ti and Nb
into D2 tool steel, chemical composition and heat treatment of
the new steel is not according to standard of D2 tool steel.
Formation of TiC or NbC carbides decreases the amount of
chromium eutectic carbides. The dissolved chromium content
increases in the matrix and amount of carbon reduces in the
matrix. The hardenability of new alloy changes due to quantities
of dissolved carbon and chromium as well as, ‘‘martensite start’’
(MS) and ‘‘martensite finish’’ (MF) temperatures change.

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http://dx.doi.org/10.1016/j.msea.2013.01.074
194 M.A. Hamidzadeh et al. / Materials Science & Engineering A 571 (2013) 193–198

Recently, in many investigations rare elements have been used

in order to improve high alloy tool steels. These elements change
the morphology of eutectic carbides and are better distributed in
the matrix of alloy. For example, Wang et al. [14] found that
addition of a desirable amount of boron could alter the carbide
morphology of high chromium ledeburite steel from strip eutectic
and rosette eutectic into divorced eutectic. Moreover, they stu-
died the effect of trace additions of RE–Te–B multiple modifier in
the microstructure of CD-2 steel and concluded that with com-
bined addition of trace amounts of these elements, the carbide
morphology changed from net-like to granular form [15]. It was
also pointed out that CD-2 steel with granular carbide possesses
higher toughness and resistance to crack propagation than con-
ventional CD-2 steel with net-like carbides as well.
It is reported that by adding small amounts of some modifying
agents to high carbon, high alloy steels, the eutectic solidification
progress of austenite/carbides can be modified, and therefore, the
grain size, shape and distribution of carbides in the matrix can be
improved [14–16]. Pan et al. [16] have shown that by adding K/Na
modifier to high speed steels, the continuous carbide network
along dendrite boundaries could be broken up and that carbides
are distributed homogeneously in the microstructure.
Previous studies used very small molds (e.g, using impact
sample size, ‘‘10  10  55 mm3’’) in their experiments and rapid
solidification of molten alloy happened [14–17]. Due to differ-
ences in experimental conditions (rapid freezing) and in ingot
casting of tool steel (slow freezing), the authors can not rely on
the results of their researches. In this study, the addition of trace
elements was studied for improving the structure of D2 tool steel.
But the extent of possible experimental conditions was similar to
ingot casting, and the cooling rate of molten alloy was slow.
Fig. 1. Schematic design of the casting (unit: millimeters). The samples for
metallographic examinations as well as impact test samples were taken from
the A-part of the cast block.
2. Experimental procedure
Table 1
2.1. Materials and casting Chemical composition of steel used in this investigation, the remaining is Fe.

The alloy used in the present study conforms to AISI D2 tool
steel, the chemical composition (in wt%) of which is: 1.5% C, 11.5%
Cr, 0.85% V, 0.6% Mo, 0.37% Mn, 0.2% Si, and Fe in balance. Firstly,
the alloy was melted in a 25 kg capacity medium frequency
induction furnace by using non-oxidation process. Once the alloy
was melted in a furnace under argon gas atmosphere, about 0.1%
pure aluminum was added to deoxidize the melt.
After dross and slag removal, the melt was cast into a dry CO2-
silicate mold at a pouring temperature of about 1600 1C. The mold
was formed in a Y-shaped geometry corresponding to ASTM
standard A571M [18] as shown in Fig. 1.
The melt was being cast at 1600 1C in two molds without
adding a reformer (No. 1) and by adding a modifier (No. 2). The
modifier included 65% Ce and 30% La, and was added about
‘‘0.03% wt’’ to the melt in the runner during pouring process. The
analyzed chemical compositions of set of samples produced for
this investigation are shown in Table 1.
The heat treatment of the specimens consisted of austenitizing
at 1130 1C for 3 h with subsequent slow cooling in the furnace to
700 1C and holding at this temperature for 2 h [19]. Afterward, the
samples were slowly cooled in the furnace to room temperature.
This heat treatment schedule was chosen in order to simulate the
cooling condition of steel ingots in industrial scale.
Samples for microstructural examination and mechanical testing
were taken from the same locations of castings, pointed by arrows in
the scheme shown in Fig. 1, in order to guarantee exactly the same
cooling condition for samples during solidification. Because it was
necessary to make sure, the obtained microstructures were controlled
only by the modifying element but not by the cooling rate.
Element C Cr Mo V Mn Si S P
(wt%) 1.45 11.45 0.58 0.88 0.37 0.18 0.01 0.025
2.2. Microstructural analysis
The microstructures of samples were characterized via optical
microscopy, scanning electron microscopy (SEM), energy dispersive
spectrometry (EDS), and X-ray diffraction (XRD). For metallographic
examinations, the samples were prepared by grinding and polishing,
and were etched electrochemically in a solution of 1 gr CrO3 þ
100 ml pure water with a power supply set to 10 V for about 60 s
[20]. With this arrangement, the eutectic carbide volume fraction as
well as the size of grains was measured by using image analysis
software (Clemex Vision PE). The reported values for each sample
were taken from at least 10 measurements in different fields with a
magnification of 200 times. The existing phases in the structure
were determined through XRD analysis using a diffractometer
(X’Pert Philips) operated at 30 kV and 25 mA with Cu Ka radiation
(l Cu Ka ¼1.5405 Å). The local chemical microanalysis was also
carried out an EDS system (IFIABT-SR50 Eds) attached on SEM.
The mechanical properties reported for experimental specimens
are Charpy impact toughness and hardness. Room temperature
impact tests were performed by using an Amsler Charpy impact
testing device. The size of specimens was 10  10  55 mm3 without
a notch according to ISO 5754 [21]. The reported impact toughness
value for each sample is the average of three test results. The bulk
hardness measurements were carried out using Rockwell ‘‘C’’ scale
with a load of 150 kgf applied for 30 s.
 M.A. Hamidzadeh et al. / Materials Science & Engineering A 571 (2013) 193–198
Fig. 2. Optical micrographs show the effects of modifier on the morphology and distribution of eutectic carbides: (a) No. 1, unmodified steel and (b) No. 2, modified steel.
‘‘A’’ indicates the eutectic carbides and ‘‘B’’ indicates the matrix of alloy.
3. Results and discussion
3.1. Solidification structure of the D2 steel
As observed in Fig. 2a, the microstructures of D2 steel in a state
of cast decomposes to austenite and continuous net-like eutectic
carbides. Three main solid–liquid reactions proceed during soli-
dification of the melts [1,22,23]:
(i) Austenite precipitates from the melts:
L-Lþ g
The volume fraction of austenite phase increases by decreas-
ing the melt temperature and, simultaneously the remaining
liquid is saturated by carbon and alloy elements. Residual
melts and austenite form chromium carbides during the
reaction of eutectic.
(ii) Eutectic transformation (from  1289 1C):
L-M7 C3 þ g
A eutectic reaction occurs between carbon and alloying
agents such as Mo, V, Cr in the retained melts, and ledeburite
comes into being. The ledeburite is composed of eutectic
carbides and austenite.
(iii) Finally, the M3C phase is formed as part of the peritectic
reaction (from  1183 1C):
Lþ M7 C3 -g þ M3 C
This reaction completes the solidification process. Since the
former reaction involves solid-state diffusion, it is relatively
slow and rarely completed. Therefore, the M3C content in the
final microstructure can be ignored. As observed in Fig. 2a,
austenitic is fully developed. Because of the high speed of
solidification, equilibrium phases can not form, which could
be due to the possibility that some high cooling rate is
converted from austenite to martensite.
3.2. Effect of Ce–La on the microstructure
Fig. 2b shows the effect of Ce/La addition on the microstructure
of AISI D2 after heat treatment. As seen in the figure, the eutectic
microstructure is dark. Generally, both samples showed a micro-
structure comprising dendrites of austenite separated by interden-
drite eutectic carbides. As seen in Fig. 2a, the microstructure of steel
includes coarse austenite dendrites together with eutectic carbides.
195
Table 2
The quantitative analysis of metallographic samples.
Sample Dendrite Eutectic carbide Volume fraction of
Number Arm diameter (lm) eutectic carbide
Spacing (lm)
As-cast As-cast Heat As-cast Heat
treated treated
NO. 1 70.2 36 32 18.2 14.8
NO. 2 42 27 23.2 12.8 10.2
The reported values for each sample were taken from at least 10 measurements in
ð1Þ different fields with a magnification of 200 times.
These carbides form as net-like chromium carbide at dendrite
boundaries. But in Fig. 2b, the eutectic structure is finer and the
network chromium carbides are approximately broken. As indicated
in this figure, the morphology of some eutectic carbides become
isotropic as cerium and lanthanum are added.
Table 2 shows the results of quantitative metallography samples.
ð2Þ As seen, dendrite arm spacing (DAS) decreases in modified samples
and diameter of the eutectic chromium carbides decreases in
modified samples, too. The percentage of eutectic carbide phases is
low after improvement. Diameter and percentage of eutectic carbide
phase decrease in all samples after heat treatment due to partial
dissolution of eutectic chromium carbide. It should be noted that the
change in size and morphology of the eutectic structure is important
since it has a direct influence on the mechanical properties. On the
other hand, adding modifier elements of Ce/La to the alloy caused a
ð3Þ decrement in the eutectic carbide volume fraction from 14.8 vol% in
sample No. 1 to 10.2 in sample No. 2.
Fig. 3a shows the backscattered electron (BSE) micrographs of
sample No. 1 without improvement. The eutectic chromium
carbides are as a black phase, and also there are very fine iron
carbides as spherical or blade shapes. The iron carbides are
uniformly distributed in the matrix. In Fig. 3b, (BSE) micrographs
of the improved sample No. 2 can be seen. The chromium carbides
are in the form of hexagonal blocks. The carbide particles are
observed in the matrix of this alloy. The white particles are
observed in the center of some eutectic chromium carbides. Like
the previous sample, there are very fine iron carbides.
The quantitative EDS analysis of the areas specified is con-
ducted, and the results are reported in Table 3 and Fig. 4. From
comparison of data in Table 3, it can be noticed that by adding
Ce/La, the percentage of chromium, vanadium and molybdenum is
increased in the matrix. On the other hand, the atomic percentage
of chromium, vanadium and molybdenum has decreased in the
eutectic carbide.
XRD was performed on the samples, and the results are shown in
Fig. 5. According to the results of XRD analysis in Fig. 5, there are high
196 M.A. Hamidzadeh et al. / Materials Science & Engineering A 571 (2013) 193–198

Fig. 3. Enlarged backscattered electron images of eutectic carbides in (a) sample No. 1 and (b) sample No. 2 steel. Circles indicate needle-like and spot-like secondary
carbides.

Table 3 Also, after hot working, dissolving of large amounts of ele-

Quantitative EDS analysis results of the microstructural constituents in micro-
graph of SEM.
Phase Sample Secpt Metallic element (at%)
type Number type
V Mo Cr Fe
Matrix NO. 1 ED 0.30 0.67 8.14 89.01 Gray region
NO. 2 ED 0.45 0.8 8.73 88.35
M7C3 NO. 1 ED 7.49 2.80 45.00 36.83 Black region
NO. 2 ED 7.05 1.10 44.89 38.64
The values are based on an average of 3 different points per sample.
intensity peaks of ferrite in the results. The low intensity peaks of
residual austenite and carbide phase (M7C3) can be seen. According to
XRD results, by adding modifier elements to the alloy, ferrite and
austenite and eutectic carbide phase values do not change appreci-
ably; therefore it is concluded that the ferrite phase is the dominant
phase in samples, and that there are small amounts of residual
austenite in the alloys.
With regard to the fact that the alloying elements of vanadium,
molybdenum and chromium are present in the alloy and that the
XRD results clearly show the formation of ferrite and austenite, the
amount of alloying elements is present in ferrite and austenite
phases as solid solution in the crystal structure. During the cooling
of steel from high temperature, austenite is decomposed to ferrite
and cementite phases. Due to the presence of alloying elements in
austenite, the eutectoid transformation can be very slow and so
some of these phases are metastable at room temperature because
there is plenty of carbon in the cold-work tool steel.
These data show that the gray region (matrix) in the Fig. 3(a
and b) is composed mainly of iron with small amounts of
chromium, vanadium and molybdenum. Therefore, combined
with XRD results (Fig. 5), it can be concluded that the matrix of
samples is a solid solution of chromium, vanadium and molybde-
num in a-Fe (ferrite). The carbide forming elements of M7C3
carbides are mainly chromium, a small quantity of vanadium and
molybdenum.
Due to reduction in size of eutectic carbides, the interface
between matrix and carbide particles increases. Thus, the amount
of eutectic carbides dissolved, increases during annealing. The
amount of alloying elements (such as Cr, Mo, V and C) increases in
the austenite during annealing. By decreasing the temperature,
the solubility of alloying elements reduces in the austenite phase.
Then, austenite phase decomposes to ferrite phase and fine
carbides. These fine carbides are consisted mainly of elements
of Fe, Cr and Mo. Uniform distribution of fine carbides in the
matrix causes to hardness uniformity in the alloy. In addition,
these fine carbides dissolve quickly in austenite before hot
deformation which leads to improvement in hot workability of
the alloy and short time preheating.
ments (Cr, C, Mo and V) in austenite increases the hardenability of
alloy. Consequently, reduction in size of eutectic carbides leads to
shorter austenitizing time and increase hardenability. Increase in
the interface between carbide and austenite causes to increase in
diffusion rate for the alloying elements and shorter dissolution
time of carbides in austenite.
According to the analysis of the results of EDS (see Fig. 4), the
white particles are composed of cerium, lanthanum and impurity
elements such as sulfur, phosphorus and oxygen. It appears that
these white particles are oxi-sulfide cerium on which chromium
carbides nucleated non-homogeneously. It indicates that the
white particle in Fig. 3b is CexOyS such as Ce2O2S acting as the
heterogeneous nucleus of the eutectic carbide.
These inclusions must have two conditions to become effective
heterogeneous nuclei [24–26]:
First, the melting point of these inclusions is higher than the
eutectic temperature. Secondly, the lattice misfit between the
inclusions and the eutectic carbide is less than 6%.
According to the formula in Ref. [26,27], the DG of Ce2O2S at
the temperature of 1500 1C is  576,367 J/mol, which indicates
that Ce2O2S can be formed at the temperature of 1500 1C, and can
exist in the melt when cerium is added.
Ce2O2S and M7C3 carbide have a close-packed hexagonal
structure with the lattice arameters: a ¼0.4008 nm, c¼ 0.6833 nm
and a ¼0.688 nm, c ¼0.454 nm, respectively [27–29]. The lattice
misfits between (1010) Ce2O2S and (1010) M7C3, and (1010)
Ce2O2S and (1010) M7C3 are 1.60% and 0.69%, respectively, which
are less than 6%. Therefore, Ce2O2S can act as heterogeneous
nuclei of the eutectic M7C3 carbide and refine eutectic carbides.
The relationship between crystallizing planes of Ce2O2S and M7C3
is shown in Fig. 6 [27,30].
On the other hand, cerium and lanthanum are combined
strongly with sulfur and oxygen and drive them out of the melt.
As Fe–C metallurgy and crystallization theory indicate, surface
tension of the melts will increase if [S] and [O] are removed, and
the melts are purified. In addition, this will lead to an increase in
the nucleation free energy of the crystalline phase so that it may
need more energy to form crystal nucleus [16]. As a result, crystal
nucleation occurs at lower temperature, liquid line during solidi-
fication falls down, and the degree of super cooling of eutectic
reaction is enhanced. All the above have resulted in the modifica-
tion of the microstructures of high alloy tool steels. All carbides
are refined and distributed homogeneously in the microstructure,
and carbide network along dendrite boundaries breaks up
completely.
3.3. Effect of Ce–La on the mechanical properties
Table 4 shows the mechanical properties of the steels studied
in this investigation, which include hardness, and Charpy impact
 M.A. Hamidzadeh et al. / Materials Science & Engineering A 571 (2013) 193–198
Fig. 4. Representative EDS spectrum and quantitative composition analysis of cerium and lanthanum-contained precipitate in Fig. 3.
Fig. 5. X-ray diffraction pattern of (blue line) steel No. 1, (red line) steel No. 2, in
annealed condition. (For interpretation of the references to color in this figure
legend, the reader is referred to the web version of this article.)
toughness. Result of hardness shows that heat treated samples
hardness are less than as-cast samples. This case can be due to
transformation residual austenite and martensite to ferrite and
partially dissolution of eutectic chromium carbides during heat
treatment. Generally, matrix hardness as well as the type and
volume fraction of eutectic carbides are the main factors affecting
the overall bulk hardness. As the results show that hardness of
samples in both as-cast and heat treated samples has not been a
significant change after modification of alloy.
It is obvious that the steel No. 1 represents the lowest impact
toughness of 8 70.5 J/cm2, and the modification can increase the
impact toughness value by 75%, to 14 70.7 J/cm2 for steel No. 2.
Generally, the impact toughness is affected by the combined
action of interdendrite carbides characteristics and grains sub-
structure. The poor impact properties of steel No. 1 can be simply
attributed to the presence of continuous network of eutectic
carbides in its microstructure (see Fig. 2a). The major reason for
improvement in toughness is refining and uniform distribution of
eutectic carbides (M7C3) after adding modifier elements.
Fractography observation was also conducted to clarify the effect
of modification on the impact toughness. The typical fractographs of
197
No. 1 and No. 2 steels (without modification and modifier added
steels) in impact tests are shown in Fig. 7. As shown in Fig. 7a, the
fracture surface of steel No. 1 is predominantly cleavage faceted, and
the cleavage facets can be seen to be very broad. However, the
fracture surface of steel No. 2 (Fig. 7b) shows a mixed fracture mode
of ductile fracture along the matrix and cleavage fracture of
interdendrite M7C3 carbides. Fracture happens by a process invol-
ving crack initiation, and crack propagation and sometimes fast
fracture.
The very low impact toughness values of steels No. 1 appear to
be due primarily to their large volume fraction of hard and fragile
M7C3 carbides with net-like distribution. It is obvious that the
M7C3 carbide phase is much harder than the ferritic matrix;
therefore, the cracks initiation and propagation readily occur
either at the weak eutectic carbide/matrix interfaces or by the
eutectic carbides themselves fracturing at relatively low stress
levels [31,32]. Therefore, less energy is absorbed for specimens’
failure which results in a decrease in impact toughness in steels
No. 1.
Accordingly, in steels No. 2 impact toughness can be enhanced.
Steel No. 2 shows the highest impact toughness value because of
better distributed carbides.
4. Conclusions
This study was carried out to investigate the effects of cerium
and lanthanum on the morphology of M7C3 eutectic carbides in
AISI D2 alloy. The results obtained are summarized as follows:
(1) In the microstructure of unmodified AISI D2 alloy, massive
M7C3 eutectic carbides are connected to each other to form a
network along dendrite boundaries.
(2) After Ce/La modification, the morphology, size and distribution
of eutectic carbides change greatly. M7C3 eutectic carbides are
refined and distributed homogeneously in the microstructure,
and carbide network breaks up approximately.
(3) Cerium oxy-sulfide inclusions can act as the heterogeneous
nuclei of M7C3 eutectic carbides to enhance nucleation and
improve the refinement of eutectic carbides.
(4) After Ce/La modification, AISI D2 steel with refined carbide
possessed higher impact toughness, without decreasing in
bulk hardness.
198 M.A. Hamidzadeh et al. / Materials Science & Engineering A 571 (2013) 193–198

Fig. 6. Relationship of crystallizing planes of Ce2O2S and M7C3: (a) (1010)Ce2O2S//(1010)M7C3; and (b) (1010)Ce2O2S//(1010)M7C3. The hollow circle represents the atoms
in Ce2O2S, the solid circle and solid square represent the octahedron and tetrahedron in the M7C3 carbides, respectively [29].

Table 4
Mechanical properties of steels utilized in this study. The numbers after ‘‘ 7 ’’ indicate the standard deviation from the mean value.

Sample numberer As cast hardness Heat treated hardness Impact energy

(HRC) (HRC) (j)

NO. 1 unmodified 437 1 21 7 1 8 70.5

NO. 2 modified 207 1 207 1 14 70.7

For each alloy, the reported values are average of minimum 3 tests.

Fig. 7. Typical SEM fractographs showing the fracture surface of impact sample for (a) unmodified steel, No. 1 and (b) modified steel, No. 2.

Acknowledgment
The authors would like to thank Isfahan University of Technology
for financial support of this research.
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