Metallogr. Microstruct. Anal.
DOI 10.1007/s13632-015-0206-4
TECHNICAL ARTICLE
Effect of Deep Cryogenic Treatment on the Microstructure
and Mechanical Properties of HY-TUF Steel
Ahmad Zare1 • H. Mansouri1 • S. R. Hosseini1
Received: 26 November 2014 / Revised: 8 January 2015 / Accepted: 17 April 2015
 Springer Science+Business Media New York and ASM International 2015
Abstract This paper analyzes how a deep cryogenic
process changes the microstructure and mechanical prop-
erties of a medium-carbon low-alloy steel. The light
microscopy, microhardness testing, and transmission elec-
tron microscopy reveal that g-carbide and martensite are
constituent phases of deep cryogenic treated (DCT) steel,
while the microstructure of conventional heat-treated
(CHT) steel consists of cementite, martensite, and retained
austenite. Transmission electron microscopy also shows
that the particles of g-carbide have the shape of ultra-fine
globules in DCT martensite. The g-carbides grow in a
Hirotsu and Nagakura orientation relationship to the
martensitic matrix that enables highly coherent interphase
boundaries. The results of the mechanical tests, including
tensile and Charpy impact tests, show that the deep cryo-
genic process can improve toughness in terms of elonga-
tion (*12.81%), tensile fracture energy (*266 MPa), and
the ductile–brittle transition temperature (*-17.2 C).
The results of fractography are also consistent with the
improvement in toughness. It is also found that the strength
and macrohardness values are increased. Unlike CHT steel,
discontinuous yielding is observed in DCT steel. Moreover,
there is no change in Young’s modulus due to the deep
cryogenic treatment.
Keywords Mechanical properties  Deep cryogenic
treatment  Conventional heat treatment  Martensite 
g-Carbide
& Ahmad Zare
ahmad273273@gmail.com
1 resulted in an improvement in the mechanical behavior of
Department of Materials Engineering, Maleke-ashtar
University of Technology, 83145-115 Isfahan,
Islamic Republic of Iran
Introduction
Cryogenics can be specified as the application of extreme
low temperatures and its effects on the properties of
engineering materials. In physical metallurgy, cryogenic
processes can be utilized as a complementary process to
improve the mechanical properties of bulk metals [1].
Medium-carbon low-alloy HY-TUF steel is a structural
steel that possesses high resistance to crack propagation
and high strength after conventional quenching and tem-
pering heat treatments. This steel, in the heat-treated con-
dition, is often used for aerospace and aircraft components,
such as ultra-sensitive screws and landing gears. In these
applications, resistance to crack propagation is an impor-
tant factor because crack propagation could lead to catas-
trophic failure. In recent decades, significant attempts have
been made to enhance this property by adjusting the che-
mical composition, optimizing the steel-making process,
and tuning heat treatment parameters. For example,
vacuum arc remelting (VAR) is used to produce HY-TUF
steel to remove non-metallic inclusions, which decrease
toughness [2]. However, the effect of deep cryogenic
treatments on the toughness of HY-TUF steel has not been
investigated to date.
The phase transition of retained austenite to martensite
is usually completed for most steels in the temperature
range of -60 to -110 C, resulting in an increase in
strength, wear resistance, and dimensional stability, and a
decrease in toughness [3, 4]. Studies show that cooling of
martensite below the martensite finish temperature (usually
temperatures below -120 C), a process referred to as a
deep cryogenic treatment, and subsequent tempering
steels [5–9]. The advantage of utilizing a deep cryogenic
process is that it enhances the formation of g-carbides,
123

resulting in an enhancement in toughness, wear resistance,
and tensile and fatigue strengths due to fine size of these
precipitates with a homogenous distribution and spherical
morphology. Formation of g-carbides is reported to be a
result of stress-assisted low-temperature diffusion of car-
bon atoms. The stresses are mainly supplied from thermal
stresses during cooling and phase transformation stresses of
austenite to martensite [10, 11].
According to many studies [10, 12–15], deep cryogenic
processing at liquid nitrogen temperature enhances the
mechanical properties of many tool and die steels. How-
ever, there are only a few researchers and commercial heat
treaters who perform heat treatment process of medium-
carbon low-alloy steels with deep cryogenic process. Pre-
vious works on HY-TUF steel showed superior mechanical
properties of deep cryogenic treated (DCT) steel for
holding time of 48 h at liquid nitrogen in comparison to
other holding times (12, 24 and 72 h) [16]. To our
knowledge, no research has been done on the effect of deep
cryogenic process on the microstructural changes of
medium-carbon low-alloy steels and its simultaneous cor-
relation to mechanical micromechanisms. This study aims
to investigate the effect of deep cryogenic treatment on
microstructural aspects such as volume fraction, mor-
phology, and type of constituent phases (martensite, car-
bide, and retained austenite). Moreover, mechanical
properties such as Young’s modulus, yielding behavior,
micromechanisms of strengthening, increasing toughness,
and mode of fracture are intended to be correlated to
microstructural aspects.
Experimental Method
HY-TUF steel bars with chemical composition given in
Table 1 were used in this study. The steel was received in
the form of 100-mm-diameter forged bars. They were
austenitized under argon protective atmosphere, DCT at
liquid nitrogen temperature (-196 C) and tempered
according to heat treatment schedules listed in Table 2. As
shown in this table and recommended by [2], oil quenching
was used for hardening machined components made from
HY-TUF steel. Oil is an ideal quenchant for achieving the
required hardness and strength while keeping residual
stresses and distortion, in comparison to water quenching.
No cracking was experimentally observed after oil
quenching.
Table 1 Chemical composition of HY-TUF steel (wt%)
Ni Mn Si Mo Cr C Fe
1.80 1.40 1.60 0.45 0.30 0.25 Balance
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Metallogr. Microstruct. Anal.
Metallographic studies were carried out on specimens
prepared and etched with two etchants. Vilella’s reagent (1 g
picric acid, 5 ml HCl, and 100 ml ethanol) was used to
reveal retained austenite in martensitic matrix; a mixture of
100 ml H2O, 10 g K3Fe(CN)6, and 10 g NaOH was used to
reveal carbides. Volume fractions of carbides and retained
austenite were measured with image analysis software. The
microhardness of constituent phases was determined using a
load of 300 g force. In order to confirm the presence of
retained austenite in the examined microstructures, the steels
were analyzed by means of x-ray diffraction (XRD). Addi-
tionally, cross-sectional slices (150 lm) were prepared from
the end of deep cryo-treated bars for transmission electron
microscopy studies, by the conventional method of wire
cutting and mechanical grinding to a thickness of about
80 lm. 2.5-mm-disks were prepared from these specimens
and then jet polished with 15% perchloric acid and 85%
acetic acid solution at 25 C until the disks were perforated.
Microstructural characterization of cross-sectional samples
was evaluated using a high-resolution transmission electron
microscope (HRTEM), operating at 300 kV and camera
length of 20 cm. For indexing carbides, three different pat-
terns near major low index zone axis were taken.
Charpy V-notched and tensile samples were wire cut from
the as-received bars and semi-finished by machining, prior to
cryogenic heat treatment. This action was done due to the
high strength ([1200 MPa) of heat-treated steels. After pre-
scribed cryogenic heat treatments, all samples were ground to
final dimensions. For each microstructure, three tensile sam-
ples and four Charpy specimens were also prepared. The
Charpy impact specimens were prepared according to the
ASTM-A370 standard. Ductile-to-brittle transition curves
were obtained using impact tests on Charpy V-notched spe-
cimens at different temperatures between -75 and 95 C.
The specimen temperature was obtained by immersing it in a
mixture of methanol, water, NaCl, and liquid nitrogen for
tests below 25 C and in boiling water for tests above 25 C.
The ductile–brittle transition temperature (DBTT) was de-
fined as the temperature for which the fracture energy is
20.4 J (15 ft-lb) [17]. The tensile samples were prepared
according to ASTM E8M-04 [18] and tested with a cross-
head speed of 2 mm/min (nominal strain rate of 9.3 9 10-4).
The analysis of the failure mechanisms was carried out by
direct topographical observation of fractured tensile samples,
using a scanning electron microscope (SEM).
Results and Discussion
Microstructure
Figure 1 shows the representative microstructures con-
taining carbides (dark regions). A change in the
Metallogr. Microstruct. Anal.
Table 2 The used heat
Specimen Heat cycle and cryogenic process
treatment and supplementary
cryogenic process cycles Austenitizing
CHT 850 C, 1 h ? oil-quenched
DCT 850 C, 1 h ? oil-quenched
Fig. 1 Optical microstructures of (a) CHT and (b) DCT steels
showing carbides
morphology of carbides is observed after performing deep
cryogenic process. In this case, the martensitic matrix is
decorated by a homogeneous distribution of fine spherical
carbides. The volume fractions of carbides are summarized
in Table 3, which shows that the volume fraction of carbide
is higher in DCT steel when compared to that of the con-
ventional heat-treated (CHT) steel. Table 3 also compares
the microhardness of carbides in the studied steels and
clearly shows that the deep cryogenic process produces a
significant increase in microhardness of the carbide phase.
The carbide in DCT steel is g type, and its microhardness
is higher when compared to the carbide in CHT steel (as
discussed later, the presence of g-carbide is confirmed with
Deep cryogenic process Tempering
… 300 C, 1 h ? air cooled
-196 C, 48 h ? Air warmed 300 C, 1 h ? air cooled
diffraction pattern analysis of TEM samples). This indi-
cates that the mechanism of carbide formation has been
changed by the deep cryogenic process. Two different
mechanisms have been suggested for the formation of
g-carbides. Baldissera [19] attributed the abnormally low
tetragonality of martensite to the migration of carbon atoms
at deep cryogenic temperatures. Tyshchenko et al. [10]
proposed the absorption of carbon atoms by gliding dis-
locations during the deep cryogenic treatment and corre-
sponding decrement in the carbon content in martensitic
matrix, which should result in the formation of g-carbides.
It has been reported that during deep cryogenic treatment,
volume dilatation due to the transformation of austenite to
martensite produces noticeable amount of mobile disloca-
tions which are able to glide at the temperature of deep
cryogenic treatment [10].
The effect of g-carbide formation on the carbon content
of martensitic matrix can also be observed in the micro-
hardness values of this phase. As shown in Table 3, the
microhardness of the martensite in CHT microstructure is
higher than that in DCT microstructure. The hardness of
martensite is directly proportional to its carbon content.
Therefore, the martensitic matrix in DCT steel is assumed
to have lower carbon content, confirming the formation of
g-carbides which have higher carbon content (Fe2C)
compared to that of cementite (Fe3C).
Figure 2 shows representative microstructures of the
materials illustrated in Fig. 1, after the removal of all traces
of the earlier etchant and etching with Vilella’s reagent.
Here the microstructure of DCT steel (Fig. 2b) appears to
be fully martensitic, with small amounts of retained
austenite (0.69%), confirming the results of XRD in Fig. 3,
which show no austenite peaks. Table 3 shows the micro-
hardness of the retained austenite phase. It is observed that
the microhardness is essentially the same for the DCT and
CHT samples, considering the standard deviation for this
data. In contrast, the CHT specimen (Fig. 2a), for which
the mean microhardness magnitude is 361, shows a non-
uniform distribution of retained austenite, with a higher
volume fraction (16.58%). This is due to the fact that the
austenite phase is forced to undergo a martensitic trans-
formation when the deep cryogenic process is applied. It is
worth mentioning, as Yu and Yang [20] have reported, that
austenite can be retained even below the martensite start
temperature (Ms), because this phase can be constrained by
martensite laths. Hence, the thermal stresses of CHT
123
 Metallogr. Microstruct. Anal.

Table 3 The resultant microstructure constituents with their microhardness values

Specimen Microstructure constituents
Carbide Retained austenite Martensite
vol.% Microhardness (HV) vol.% Microhardness (HV) vol.% (balance) Microhardness (HV)

CHT 4.41 ± 0.32 900 ± 14.4 16.58 ± 0.50 361 ± 9.7 79.01 ± 0.45 918 ± 17.2
DCT 8.87 ± 0.72 2023 ± 15.6 0.69 ± 0.33 365 ± 11.2 90.44 ± 0.71 753 ± 9.1

Fig. 3 XRD results of (a) CHT and (b) DCT steels

shows that the lattice layers of g-carbide have been

Fig. 2 Optical microstructures of (a) CHT and (b) DCT steels
showing retained austenite
quenching cannot supply sufficient activation energy (shear
stresses) for completing martensitic transformation in some
instances.
The microstructure of the DCT steel as observed in the
TEM is shown in Fig. 4(a). In most regions of the
martensitic matrix, ultra-fine spherical particles of g-car-
bide developed within boundaries of mechanical twins.
According to Fig. 4(a), g-carbide particles vary in size
from *200 to 300 nm. Figure 4(b) is a higher magnifica-
tion view of the rectangular region of the
g-carbide/martensite boundary in Fig. 4(a). This figure
nucleated and grown coherently with the martensitic matrix.
Moreover, the interphase boundaries between g-carbide and
martensite phases are found to be continuous. Fig-
ure 4(c) shows a selected area diffraction pattern and its
indexing. To obtain this diffraction pattern, the incident
electron beam was selected to be parallel to the [131] and
[121] directions of martensite and g-carbide, respectively.
The resultant diffraction pattern (Fig. 4c) is conformed
with that which was obtained by Hirotsu and Nagakura (H–
N). Their TEM studies on martensite and g-carbide phases
show that the [001] direction of g-carbide is parallel to the
[100] direction of martensite; also the (110) plane of g-
carbide is parallel to the (010) plane of the martensite
phase. The H–N orientation relationship between marten-
site (M) and g-carbide (g) phases can be summarized as
below:
ð110Þg jjf010gM ; ½001g jjh100iM ; ð1Þ

123
Metallogr. Microstruct. Anal.
Fig. 4 (a) TEM micrograph of g-carbide precipitation in DCT steel,
(b) HRTEM image of g-carbide/martensite boundary, and (c) indexed
diffraction pattern illustrating martensitic matrix and g-carbide
Fig. 5 Representative engineering stress–strain curves of (a) CHT
and (b) DCT steels
This orientation relationship could also confirm that
g-carbides are coherent with martensitic matrix in DCT
steel.
Mechanical Properties
Figure 5 illustrates typical engineering tension stress–strain
curves of the investigated steels at room temperature. As
shown in this figure, the stress–strain curves of both steels
exhibit the same Young’s modulus (E = 206 GPa), which
has been interpreted to correspond to the independency of
Young’s modulus to microstructure. It should be men-
tioned that Young’s modulus only depends on the com-
position and temperature [21]. Figure 5 also compares
yielding behaviors of CHT and DCT steels. The CHT steel
exhibits a continuous yielding behavior, as opposed to the
discontinuous yielding of the DCT steel, which can be
explained as follows. Sakaki et al. [22] calculated the
distribution of the internal stresses in the tough phase
(austenite) adjacent to martensitic matrix due to the volume
dilatation of martensitic transition based on the continuum
mechanics. They found that there are many preferential
yielding regions within the tough phase (austenite), and
initial yielding begins simultaneously from these regions
under a very low applied force, compared to the typical
yield strength of the austenite, because the internal stresses
decrease the initial yielding strength. Thus the CHT steel,
with 16.58% austenite, yields continuously. The DCT steel
exhibits discontinuous yielding because this mechanism is
strongly dependent on the simultaneous presence of a
deformable soft phase (austenite) and a deformable hard
phase (martensite) in microstructure; with only 0.69%
austenite, this mechanism is not possible in the DCT steel.
The mechanism of discontinuous yielding can be related to
123

Table 4 Mechanical properties of studied steels
Mechanical property Specimen
CHT DCT
Macrohardness (HV) 498 ± 35.8 536 ± 43.6
Yield strength (MPa) 1441 ± 12.3 1584 ± 17.5
Ultimate tensile strength (MPa) 1531 ± 19.2 1697 ± 25.7
Percent elongation 9.94 ± 1.1 12.81 ± 0.6
Tensile fracture energy (MPa) 95 ± 8.9 266 ± 11.4
Strength difference (MPa) 90 ± 11.2 113 ± 4.8
the decrease in carbon content of DCT martensite, which
was investigated by Tyshchenko et al. [10] with TEM
observation, Mössbauer spectroscopy, and internal friction
studies. They reported retained austenite is capable of time-
dependent transformation into martensite with holding at
the temperatures of deep cryogenic processing. This phe-
nomenon, which is known as isothermal martensitic
transformation, can produce mobile dislocations in DCT
martensite due to the volume expansion of c ? M. Carbon
atoms are captured by the mobile dislocations. This will
result in dislocation pinning, which leads to the discon-
tinuous yielding behavior of DCT steel.
The results of macrohardness and tensile tests are given
in Table 4. In this table, the tensile fracture energies as a
criterion of fracture toughness were digitally determined by
calculating the areas under curves of Fig. 5. Variations of
Charpy impact energy with temperature for the studied
CHT and DCT steels are shown in Fig. 6. The determined
ductile-to-brittle transition temperatures (DBTT) are
approximately -12.2 C for the CHT steel and -29.4 C
for the DCT steel. DBTT is referenced as a temperature for
transition of fracture mode from ductile to brittle. As the
CHT steel has a higher DBTT, it is more prone to fracture
at a given temperature in comparison with the DCT steel
which has a lower DBTT. It can be seen from Table 4 and
Fig. 6 that DCT steel has greater toughness in terms of
elongation (*12.81%), tensile fracture energy
(*266 MPa), and DBTT (*-29.4 C). The increase of
toughness observed here is in agreement with the previous
works, which were conducted on medium-carbon low-alloy
steels [23, 24]. It is reported that DCT martensite is tougher
than CHT martensite in medium-carbon low-alloy steels as
explained in ‘‘Microstructure’’ section. The observed im-
provement in toughness of the DCT steel in comparison to
the CHT steel can be related to the fact that DCT
martensite has lower concentration of carbon, and conse-
quently higher ductility in comparison to CHT martensite.
The DCT martensite retards propagation of microcracks,
which consequently increases resistance to brittle fracture
[25]. In addition, in the CHT steel, cementite/martensite
boundaries and regions within them are high-energy sites
123
Metallogr. Microstruct. Anal.
Fig. 6 Absorbed Charpy impact energy vs. testing temperature
curves of (a) CHT and (b) DCT steels
which have a low activation energy for nucleation of
microcracks [26]. This is due to the crystallographic mis-
match between the structure of large-sized cementite and
high-carbon martensite [27]. On the contrary, in DCT steel
as given in Eq. (1) and also reported by Jack and Jack [28],
there is a crystallographic correlation between crystals of
g-carbides and low-carbon martensite, which causes the
formation of coherent boundaries. It should be mentioned
that nucleation of microcracks is retarded at coherent
boundaries (as shown in Fig. 4b) and within regions adja-
cent to boundaries.
From Table 4, it can be seen that the DCT steel has
higher macrohardness, yield strength, and ultimate tensile
strength in comparison to the CHT steel, which can be due
to the presence of g-carbides in the vicinity of martensite.
The parameters which cause lower strength and macro-
hardness of CHT steel are (1) lower volume fraction of
martensite; (2) lower microhardness (or strength) of
cementite in comparison to g-carbides. g-Carbides are
stronger than cementite, due to the orthorhombic structure
of g-carbides, which have stronger atomic bonds and are
coherent with martensitic matrix [28]; (3) lower volume
fraction of carbides (Table 3); and (4) higher volume
fraction of retained austenite.
The difference between the ultimate tensile strength and
yield strength can be considered as a measure of the work
hardening occurring in the sample [29]. Table 4 also gives
the difference between ultimate tensile and yield strengths
of the studied steels. From this it can be concluded that the
clustering of carbon atoms in the vicinity of dislocations
(formation of g-carbides) during the deep cryogenic pro-
cess causes a noticeable decrease in the carbon
Metallogr. Microstruct. Anal.

concentration of the martensitic matrix and consequently

an increase in the work hardening of DCT steel.

Fractography of Tensile-Tested Specimens

Microscopic observations were carried out on the fracture

surfaces of tensile-tested specimens to understand the effect of
the deep cryogenic process on the fracture mode of HY-TUF
steel. For the DCT specimens, observation of the fracture
surface indicates that necking has occurred during tensile
testing. The fracture surface exhibits typical ‘cup-cone’ mode
of fracture, which includes the fiber pattern in the central zone,
the shear lip pattern in outside zone, and the radial pattern. An
example of these patterns is shown in Fig. 7, which corre-
sponds to that for the samples deep cryo-treated at -196 C.
The fracture surface of CHT sample is shown in
Fig. 7(a). There are two parts which can be distinctly
observed from the fracture feature: (1) central zone where
the material fractured through cleavage, and (2) an outer
zone where fracture occurred through growth of dimples
and their subsequent coalescence. Comparison of the ap-
pearance of the fractographs in Fig. 7 shows that the area
of brittle fracture (central zone) for the CHT steel is larger
than that in the DCT steel, while the area of shear lip zone
(outside zone) for the DCT steel is larger than that in the
CHT steel; there is no sign of radial marks for the CHT
steel. This evidence indicates a lower ductility of the CHT
steel compared to that of the DCT steel [30], which
matches the data in Table 4.
SEM micrographs of the central area of fracture surfaces
are shown in Fig. 8. In this figure, mean values of dimple
sizes are also shown on the lower right corners. The frac-
ture surface of the DCT steel (Fig. 8b) exhibits a distri-
bution of dimples with varying sizes, showing a general
ductile fracture mode. There is a direct correlation between
microvoid (dimple) coalescence and fracture strain. Since
larger and deeper dimples are joined together at greater
strains, they are representative of larger fracture strains. On
the contrary, smaller and shallower dimples indicate less
fracture toughness in steels [31]. The mean value of dimple
size at fracture surface of the DCT steel (Fig. 8b) is greater Fig. 7 Stereographs captured from tensile-tested fracture surfaces of
(a) CHT and (b) DCT steels
than that of the CHT steel (Fig. 8a), indicating an
enhancement in ductility (*2.87%). In the CHT steel
(Fig. 8a), a mixture of bright facets and dimples with dominant coherent boundaries of g-carbide/martensite (as
smaller size are observed; these are distinguished as fea- shown in Fig. 4b) limit the nucleation of microcracks as a
tures of semi-cleavage fracture. The reason for the semi- toughening mechanism. On the other hand, the g-carbide
cleavage mode of fracture is related to the formation of prevents crack propagation in the DCT martensitic matrix
large-sized cementite in the high-carbon martensitic by bridging the crack forming ligaments behind the
matrix. Since crack nucleation can easily occur in the high- microcrack tip, or by creating a stress field in front of the
energy boundaries of large cementite/martensite, and crack microcrack tip [33]. This causes higher elongation in
propagation is relatively easy at the high-carbon marten- necking stage for the DCT steel. Hence, with the formation
sitic islands, these result in a decrease in ductility of the of g-carbides, the semi-cleavage mode of fracture is
CHT steel compared to that of DCT steel [32]. The replaced with the dimpled mode.

123

4.
5.
6.
7.
Fig. 8 SEM micrographs captured from central part of tensile-tested
fracture surfaces of (a) CHT and (b) DCT steels (numbers on the
lower right corners are average dimple size)
Conclusion
8.
The CHT and DCT steels with different microstructural
constituents were produced through conventional heat
treatment and supplementary deep cryogenic process at
liquid nitrogen temperature. The mutual relationship
between the microstructure and mechanical behavior can
be summarized as below:
1. Formation of fine homogenized g-carbides, disappear-
ance of retained austenite, and decrease in carbon
content of martensite take place during the deep
cryogenic treatment at -196 C.
References
2. TEM studies show the existence of ultra-fine g-carbide
globules which are coherent with the DCT martensite.
The diffraction pattern of the DCT steel validates the
H–N orientation relationship between martensite and
g-carbide phases.
3. Microhardness values of carbides show cementite and
g-carbides form in CHT and DCT steels, respectively.
Moreover, lower microhardness value of martensitic
matrix in DCT steel confirms its lower carbon content.
This is attributed to the formation of g-carbide during
the deep cryogenic process, which absorbs the carbon
atoms of martensite.
123
Metallogr. Microstruct. Anal.
The resultant engineering stress–strain curves show
that the Young’s modulus (*206 GPa) is not affected
by the performance of deep cryogenic treatment.
Continuous yielding is observed in the CHT steel. This
behavior can be attributed to dislocations which are
unlocked and generated during low-temperature
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DCT steel has greater macrohardness, yield strength,
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is attributed to the lower martensite volume fraction in
the CHT steel, the lower strength of cementite in
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