Bensely CTD Influence Alloy Carbide Aisi m2 PDF

Full version of the abridged article, "Influence of deep cryogenic treatment on alloy carbide precipitations and
mechanical properties of AISI M2 high speed tool steel," published in Cold Facts, Spring 2012, Volume 28, Number 2.
Influence of deep cryogenic treatment on alloy carbide precipitations

and mechanical properties of AISI M2 high speed tool steel
A.Bensely1*, S. Venkateswaran2, Angel D Subisak3, D. Mohan Lal4, A.Rajadurai5,
Gyngyvr B. Lenkey6, Pete Paulin7
1
3012 Shadowood Pkwy, Atlanta, Georgia 30339, USA

Cognizant Technologies Solutions, Tamilnadu, India
3
Department of Biomedical Engineering, The Ohio State University, Columbus, Ohio- 43210, USA
4
Department of Mechanical Engineering, Anna University, Sardar Patel Road, Chennai-600 025, India
5
Department of Production Engineering, Madras Institute of Technology, Chrompet, Anna University,
Chennai-600 044, India
6
Department for Structural Integrity, Bay Zoltn Foundation for Applied Research,
Institute for Logistics and Production Systems, Hungary
7
300 Below Inc., Decatur, Illinois 62526, USA
2
________________________________________________________________________
Abstract
Reckoned on a tonnage basis, tool steel represents only a few percent of the total
quantity of steel produced but its importance to the industry as a whole is immense. New
processing methods such as shallow cryogenic treatment (SCT) and deep cryogenic
treatment (DCT) are being considered as supplementary processes to conventional heat
treatment in order to improve the properties of steel. An improvement in the properties
can be expected from high speed steel (HSS) with a higher amount of primary and
secondary carbides. The present investigation aims to examine the effects of multiple
tempering on deep cryogenically treated AISI M2 tool steel and the resultant mechanical
properties such as hardness and toughness. It has been found that the hardness values of
multiple tempered DCT samples are 30 to 35 VHN higher than the conventionally heat
treated (CHT) samples. The fracture toughness value of CHT, SCT and DCT samples
after third tempering has been determined using Sailor- Corten relation and was found to
be 25.31 MPa (m) , 26.51 MPa (m), and 26.12 MPa (m) respectively. Characterization
analyses have been done on the samples through microstructural and fractography
studies. In order to study the tempering transformation of various heat-treated samples,
Thermo Mechanical Analysis (TMA) has been carried out.
Keywords: AISI M2 Tool Steel, Carbide Precipitations, Deep Cryogenic Treatment,

Fracture Toughness, Fractography.
*
Corresponding author. Tel.: +1-(678)-528-8994 ; E-mail address: bensely@gmail.com
1. Introduction
The need for greater productivity calls for the development of new, higher
performance tools and tool materials capable of higher cutting speeds and feed rates. It is
important to remember that for complex machining jobs that require several tools, floorto-floor time depends on the best performing tool. Generally complex shaped HSS tools
are used, improving their performance brings along higher productivity of the entire
system. Its main applications are for drills, taps, milling cutters, broaches and also bits
where the economical cutting speed is too low to think about carbide tools. In recent
decades interest in low temperature effects have been demonstrated particularly during
heat treating cycles of the tool steels. Research has shown that cryogenic treatment
increases product life, and in most cases provides additional qualities to the products such
as stress reliving, increased service life and increased hardness and toughness
simultaneously [1].
Several papers have been published about the benefits arising from deep
cryogenic treatment (DCT) at 77 K on the properties of tool steels. In particular
depending on the material, wear resistance may increase up to 100 . In this process the
lowest temperature (77 K) can be easily obtained by using liquid nitrogen. Liquid
nitrogen (LN2) is a relatively inexpensive means of cooling. There is some evidence to
indicate that some of the desirable changes are happening very near this temperature
range. However, most researchers believe that cryogenic treatment promotes the
complete transformation of retained austenite into martensite at cryogenic temperature.
Others claim that cryogenic treatment facilitates the formation of fine epsilon carbides in
the martensitic matrix. The extent of benefits of this emerging processing route can only
be suitably exploited, if the underlying mechanism of this process is carefully unfolded in
an organized manner. The main objective of this study is to examine the effect of
cryogenic treatment on AISI M2 high-speed tool steel with respect to microstructural
changes and changes in mechanical properties such as hardness and toughness.
2. Literature survey
Since the late 1930s, low temperature treatment has been adopted by industry
mainly as a part of the heat-treating cycle of tool steel [2]. Cryogenic treatment has been
tried since the early 60s and now draws much attention due to its claimed advantages.
Though many firms and researchers have recorded their experiences regarding the effect
of the treatment, published literature is not unequivocal. Claims are often diverse and the
factors to which they are attributed are varying and sometime contradicting.
Barron [2] investigated the effect of temperature below dry ice temperature on
wear resistance of tool steel material and concluded that the transformation of austenite to
martensite is dependent on temperature and independent of soaking time at that
temperature. Moore [3] conducted research on cold treatment and found the phenomenon
of austenite retention in high- speed steels. It was shown that properties are improved by
cold treatment where more than one temper is involved; at least one temper can be
omitted with cold treatment, which requires one hour, compared with several hours for
tempering. Barron [4] studied the effect of LN2 temperature (77 K) and dry ice
temperature (189 K) treatment on abrasive wear resistance of different metals. It was
concluded that the metal such as tool steel, can exhibit retained austenite at room
temperature can have wear resistance significantly increased by subjecting the metal to a
long soak (longer than 20 hrs) at the temperature of the order of 77 K. The hardness of
the material was not influenced by the cryogenic treatment for any of the samples.
Molinari et al., [5] studied the effect of deep cryogenic treatment on mechanical
properties of tool steels AISI M2 and AISI H13 and concluded that it increases the
hardness and improves the hardness homogeneity, reduces tool consumption and down
time for the equipment setup, thus leading to a cost reduction of about 50%. Flavio et al.,
[6] studied the effect of cryogenic treatment on M2 high speed tool steel. Before the
cryogenic treatment, the tools have previously been subjected to conventional thermal
treatment to obtain the secondary hardness and was concluded that the cryogenic
treatment had favorable influences on the performance of the tools tested. This means
that depending on the application, the cryogenic treatment may be a good alternative for
having productivity enhancement. Yong et al., [7] did a detailed study to analyze the
differences in tool performance between cryogenically treated and untreated tungsten
3
carbide tool inserts during orthogonal turning of steel. By measuring the flank wear, it
was concluded that the tools under mild cutting conditions stand to gain from cryogenic
treatment, but heavy duty cutting operations with long periods of heating of the cutting
tool will not benefit from it.
Meng et al., [8] studied the effect of cryogenic treatment on the wear behavior of
Fe-12Cr-Mo-V-1.4C tool steel. The precipitation of fine carbides instead of the usual
carbides following cryogenic treatment at 77 K and improvements in both wear resistance
and toughness were reported. It was suggested that the lattice parameters of the
martensite formed are different from that formed in conventional treatments, which may
well account for its subsequent lack of response to extended exposure to deep cold
temperatures. At deep cryogenic temperatures there is a time-dependent decomposition of
the primary martensite. This decomposition causes some initial softening but nucleates
numerous coherent nano-carbides. Huang et al., [9] conducted a research on
microstructural changes of cryogenically treated M2 tool steel by soaking the sample in
LN2 for a period of one week. The microstructural images showed precipitation of
homogeneously distributed spheroidized carbide with a face centered cubic structure in
the cryogenically treated samples during subsequent tempering. Also volume fraction of
carbides in the cryogenically treated samples was higher than the non-cryotreated sample,
11% in the former and 5% in latter. Zhirafar et al., [10] compared the results of various
mechanical tests, including rotating fatigue, impact and hardness on AISI 4340 steel after
various heat-treating conditions. It was concluded that hardness and fatigue strength of
the cryogenically treated specimens increased whereas the toughness had decreased
compared to that of the conventionally treated steel. The transformation of retained
austenite to martensite along with possible carbide formation during tempering is a key
factor in improving hardness and fatigue resistance of the cryogenically treated
specimens.
Mohan Lal et al., [11] carried out experiments in T1 HSS tool specimens to study
the hardness improvement, induced residual stresses and microstructural variations due to
DCT. The study concludes that the conversion of austenite to martensite is an isothermal
process and the maximum hardness attained by quenching at 203 K is 67 HRC. As the
quenching temperature is lowered, induced tensile stress become more and quenching at
4
193 K leads to high hardness but induces residual stresses increases which is detrimental
to tool life. Microstructural analysis showed that the larger alloy carbide began to
precipitate into finely dispersed carbides when soaked for two hours and more. Mohan
Lal et al., [12] carried out a study on the improvement in wear resistance and the
significance of treatment parameters in different materials. It was found that cryogenic
treatment imparted nearly 110% improvements in tool life. For the tool samples,
cryogenic treatment should not follow TiN coating and after first regrinding, the tool
behaved like a cryogenically treated tool. It was concluded that soaking time is more
important than lowering the temperature.
Bensely et al., [13] investigated the effect of cryogenic treatment on wear
resistance improvement and microstructural changes in case carburized steel (EN353). It
was concluded that the DCT imparts better wear resistance (372%) compared to
conventionally treated sample and 152% with SCT samples. Bensely et al., [14] has
studied the influence of cryogenic treatment on the tensile behavior of case carburized
steel 815M17. After tensile testing, it was found that there is a reduction in tensile
strength for SCT and DCT samples over CHT by the factor of 1.5% and 9.34%
respectively. The SEM analyses of the fracture surface indicated the occurrence of more
extensive microvoids and microcracks formation for the CHT samples compared to the
SCT and DCT samples.
Leskovsek et al., [15] studied the effect of the wear behavior of vacuum heattreated AISI M2 high-speed steel subjected to vacuum heat treatment in conjunction with
a deep-cryogenic treatment at 77 K. Predetermined combinations of the Rockwell C
hardness and the fracture toughness KIC are obtained by varying the tempering
temperatures. The wear behaviors were compared and discussed in terms of these two
properties and the related microstructures. It is found that the DCT samples have better
wear resistance than vacuum heat-treated samples, which is a result of their fracture
toughness and hardness. The wear mechanisms observed for selected samples were
typically plastic deformation with the formation of surface ridges. Stratton [16] reviewed
current thinking and attempts about cryogenic processing. It was explained that there is
insufficient driving force at liquid nitrogen temperature (77 K) to form the nuclei of the
carbides in the martensite formed at low temperature. If the driving force were increased
5
by cooling to a lower temperature, then it might be possible to form carbides in the

martensite formed at low temperatures, thus maximizing performance with a combination
of high hardness and nano sized carbide dispersion. As part of an optimized heat
treatment cycle, deep cold treatment can dramatically improve measured wear by the
precipitation of nano-sized carbides in the primary martensite.
Based on the above literature survey, it is concluded that cryogenic treatment has
the potential to improve the mechanical properties of steel. In order to study the effect of
cryogenic treatment on mechanical properties and alloy carbide precipitation of AISI M2
tool steel, the present research work has been carried out. The treated samples are
subjected to characterization analyses to study the mechanism behind the varying
behavior of the samples.
3. Material and methodology

3.1 Material
For the experimental work, AISI M2 high speed tool steel (available in annealed
condition) is used. Initially, the chemical composition of the samples is confirmed
through optical emission spectroscopy (OES) and reported in Table 1.
Table 1 Result of chemical analysis of AISI M2 raw material in weight %
Element
Carbon
Chromium
Molybdenum
Tungsten
Vanadium
Iron
1.269
4.288
3.005
5.88
4.56
77.67
Name
%
3.2 Research Methodology

The research methodology has been explained in Figure 1. AISI M2 steel rod of
20 mm diameter is procured and cut into suitable length. Then the samples are divided
into three groups namely Group I (CHT), Group II (SCT) and Group III (DCT). All the
three groups are subjected to same heat treatment parameter until free cooling in air
mentioned in Figure 1 as per the ASM specification [17]. The Group I samples after free
cooling are subjected to single, double tempering at 823 K for the soaking period of 3 hrs
6
Procurement of raw material - AISI M2 Tool steel

Chemical analysis to check composition
Samples preparation
Stress relieving at 923 K for 2hrs
Dry preheating at 873 K for 2hrs
Second pre-Heating at 1173 K for1hr
Austenitizing at 1473 K for 10 minutes
Marquenching at 798 K
Shallow cryogenic treatment
Free Cooling in air
Deep cryogenic treatment
Group I
Group II
Group III
Single Tempering at 823 K for 3hrs
Double tempering at 823 K for 3 hrs
Triple tempering at 833 K for 3hrs
Thermomechanical
analysis
Instrumented
impact strength
test
Vickers
hardness
test
Arriving conclusions
Figure 1 Research methodology

7
Optical/
SEM
analysis
and triple tempering at 833 K for 3 hours. The Group II (SCT) samples after free air
cooling are transferred immediately to a mechanical freezer at 193 K and soaked for
5hours, and is followed by single, double and triple tempering. Meanwhile the Group III
samples after free cooling are immediately cooled in a controlled manner from room
temperature to 77 K in a cryoprocessor at a rate of 1.26 K/min, held at the same
temperature for 24 hours and subsequently brought back to room temperature at 0.63
K/min. Liquid nitrogen is used as working fluid to achieve very low temperature. After
reaching room temperature immediately it is subjected to single, double and triple
tempering. Table 2 shows the treatment conditions and nomenclature followed for the
present research work.
Table 2 List of treatment conditions considered for this study

Nomenclature
Explanations
followed
CHTWOT
Conventionally hardened
CHT-1T
Conventionally hardened and single tempered
CHT-2T
Conventionally hardened and double tempered
CHT-3T
Conventionally hardened and triple tempered
SCTWOT
Conventionally hardened + shallow cryotreated at 193 K
SCT-1T
Conventionally hardened + Shallow cryotreated at 193 K + Single tempered
SCT-2T
Conventionally hardened + Shallow cryotreated at 193 K + Double tempered
SCT-3T
Conventionally hardened + Shallow cryotreated at 193 K + Triple tempered
DCTWOT
Conventionally hardened + Deep cryotreated at 77 K
DCT-1T
Conventionally hardened + Deep cryotreated at 77 K + Single tempered
DCT-2T
Conventionally hardened + Deep cryotreated at 77 K + Double tempered
DCT-3T
Conventionally hardened +Deep cryotreated at 77 K + Triple tempered
4. EXPERIMENTAL PROCEDURE:
4.1 Vickers Hardness Test
Hardness test is carried out on an INDENTEC SKV 5030 model Vickers macro
hardness testing machine as per the ASTM designation E92-82[18]. Three readings are
taken for each of the 9 samples. The average Vickers hardness numbers obtained for the
various samples are represented as a graph in Figure 2.
Vickers hardness number (HV 10)
820
810
800
790
780
770
760
750
740
730
CHT-1T
CHT-2T
CHT-3T
SCT-1T
SCT-2T
SCT-3T
DCT-1T
DCT-2T
DCT-3T
Sample identifications
Figure 2 Hardness test results

4.2 Impact strength test
Toughness, as considered for tooling materials, is the relative resistance of a

material to breakage, chipping, or cracking under impact or stress. It is an important
property in most tool steels, which determines the resistance of steel to cracking and
fracture at dynamic loads. Toughness data is useful to predict which steels may be more
or less prone to chipping or breakage than other steels, but toughness data cannot predict
the performance life of tools.
Instrumented impact tests have been more and more widely used for the
determination of dynamic fracture toughness [19]. The three groups of samples are
subjected to Charpy Instrumented Impact test at 295 K to measure the toughness [19].
For calculating static and dynamic fracture toughness from the observed Charpy impact
energy value, the following standard Sailors-Corten correlation [20] is used.
KIC 2
= 8 (CVN)
E
(1)
KId2 = 15.873(CVN) 3/8
(2)
Where
9
KIC = Fracture toughness for static load condition in psi (in)

KId = Dynamic fracture toughness in Ksi (in)
E = Modulus of elasticity in psi
CVN= Absorbed impact energy value in ft.lbf.
4.3 Characterization analyses of the treated samples

Microstructural characterizations of the treated samples are carried out using
optical microscope (LEICA Q` win with Image Analyzers) and scanning electron
microscope (SEM). For the optical micrographs, the samples are mounted on bakelite
moulds, etched with 3% Nital and dried in air.
4.4 Thermomechanical analysis

Thermomechanical analysis is carried out on untempered CHT, SCT and DCT
samples as per ASTM-E 831[21] in order to study the tempering transformation. The
sample is heated from room temperature to 800 K at a uniform rate of 10 K/min. By this
method, the deformation of a substance under non-oscillatory load is measured as a
function of temperature while the sample is subjected to a controlled temperature
program in a specified atmosphere.
5. Results and discussions
5.1 Hardness
The result of Vickers hardness test is shown in Figure 2. It indicates that there is
no large variation in hardness values among the SCT and DCT samples for different
stages of tempering but significant variation is observed between the CHT-1T, SCT-1T
and DCT-1T samples. However, on comparing the improvement caused by shallow and
deep cryogenic treatment, a marginal increase in the hardness values is noted for all the
stages of tempering in SCT and DCT samples when compared with CHT samples.
Generally the wear resistance improvement can be influenced by hardness values. An
increase in hardness can increases the abrasion resistance and the load bearing capacity of
the material [5].
10
5.2 Toughness
The cutting performance of high speed steel is primarily determined by its
toughness, resistance to both wear and tempering at operating temperatures. The
toughness of high-speed steel is determined by the state of tempering of the matrix and
the spatial and size distribution of the primary carbides. The uniform distribution and
small size carbides in the matrix represents an important toughness advantage. Wear
resistance is generally a function of hardness and of the type, volume, and shape of the
primary carbides present in the materials. Temperature resistance is largely determined
by the composition and growth of secondary hardening carbides [22]. From Table 3, it is
observed that the value of impact energy for DCT-1T and DCT-2T samples have lower
value then all other samples. This is due to the presence of higher martensitic structure.
This can be supported by the higher hardness value reported in Figure 2.
Table 3 Instrumented Impact strength test results
Impact energy
(J)
KIC
MPa (m)
K Id
MPa (m)
CHT-1T
3.6
27.273
5.258
CHT-2T
3.4
26.509
5.202
CHT-3T
3.1
25.313
5.113
SCT-1T
3.1
25.313
5.113
SCT-2T
3.5
26.869
5.230
SCT-3T
3.4
26.509
5.202
DCT-1T
2.83
24.185
5.026
DCT-2T
2.83
24.185
5.026
DCT-3T
3.3
26.117
5.173
Sample ID
5.3 Fractography
The fracture surface micro morphology of the AISI M2 test specimens are
examined by using scanning electron microscope (SEM) in order to relate toughness
behavior to key microstructural features. Figure 3 (a-c) shows the fractured surface of
conventionally
heat
treated
with
single,
11
double
and
triple
tempering.
Dimples
Secondary cracks
Secondary Cracks
Voids
Flat facets
(a) CHT-1T
(b) CHT-2T
(c) CHT-3T
Figure 3 Fractographic image of conventionally heat-treated sample
Voids
Secondary cracks
Shallow Dimples
(a) SCT-1T
(b) SCT-2T
(c) SCT-3T
Figure 4 Fractographic image of Shallow Cryogenically treated sample
12
(a) DCT-1T
(b) DCT-2T
(c) DCT-3T
Figure 5 Fractographic image of Deep Cryogenically treated sample
Primary Alloy Carbides (MC)

Pearlitic
structure
M6 C
M23C
6
Figure 6 Micrograph of AISI M2 Raw material in annealed condition
13
(a) CHTWOT
(b) CHT-1T
(c) CHT-2T
(d) CHT-3T
Figure 7 Optical micrograph of conventionally heat-treated sample
14
Large elongated
primary carbide
Small secondary
carbides
Spheroided carbide
(a) CHT-1T
(b) CHT-2T
Retained austenite
(c) CHT-3T
Figure 8 Scanning electron microscopic image of conventionally heat-treated sample
15
(a) SCTWOT
(b) SCT-1T
(c) SCT-2T
(d) SCT-3T
Figure 9 Optical micrographs of Shallow cryogenically treated samples
16
Clustered Carbides
(a) SCT-1T
(b) SCT-2T
(c) SCT-3T
Figure 10 Scanning electron microscopic image of Shallow Cryogenically treated

samples
17
(a) DCTWOT
(b) DCT-1T
(c) DCT-2T
(d) DCT-3T
Figure 11 Optical micrographs of Deep cryogenically treated samples
18
(a) DCT-1T
(b) DCT-2T
(c) DCT-3T
Figure 12 Scanning electron microscopic images of deep cryogenically treated

samples
Figure 3(a) reveals the presence of uneven array of dimpled facets with a
scattering of large voids. The presences of small cleavage facets many of which are
separated by secondary cracks are also found. The fractured surface is characterized by
quasi cleavage pattern [23]. The Figure 3(c) shows several secondary cracks, which seem
19
to have grown from the primary crack. On the surface, the carbides have been laid bare,
and in several places, dislodged.
Figure 4 (a-c) show the fracture surface of SCT samples with single, double and
triple tempering respectively. The presence of small spherical carbides in the matrix
which is not present in CHT samples is observed. In this case also the fractured feature is
identified as quasi cleavage pattern. Inter granular fracture features are also identified in
few regions.
Figure 5 (a-c) shows the micro morphology of the fractured surface of the DCT
samples. It is observed that there are small and poorly defined quasi-cleavage facets
connected by shallow dimples on the surface. The presence of dimples gets reduced and
more flat facets are seen on comparison with CHT samples. It can be attributed to the
presence of higher martensitic structure with less carbon content.
5.4 Microstructure
Figure 6 shows the microstructure of AISI M2 raw material. The micrograph
reveals the presence of lamellar pearlite with carbides precipitated from austenite.
Pearlite, which forms the base of annealed steel, has a lower hardness value of 24HRC,
which makes the metal capable of being machined or plastic-worked in the cold state.
Due to annealing at high temperature followed by slow cooling, pearlitic structure with
low carbon concentration is formed, and also more carbide is precipitated at the grain
boundaries [23]. The structure of high-speed steel in the annealed condition consists of
M6C, M23C6, MC types of untransformed carbides in the pearlitic matrix.
Figure 7(a) shows the microstructure of CHT untempered sample. The
micrograph of hardened sample reveals the presence of untempered martensite and
undissolved carbides in the martensitic matrix. The large sized elongated carbides found
along the boundaries are identified as primary carbides and the small spherical carbides
present within the martensitic grains are identified as secondary carbides. When steel is
hardened, it acquires the structure of tetragonal martensite and a certain amount of
retained austenite. Steel in this condition is hard, brittle, highly stressed and liable to
develop quench cracks, particularly tool steels. To overcome this, the hardened steel
should have a potential tendency to attain a stable condition. But this equilibrium or
20
stable condition cannot be achieved at room temperature because of the low mobility of
atoms. When the temperature increases, the mobility of atoms increases due to
accelerated diffusion rate and, results in a structural change of the hardened steel to give
rise to a stable state [24]. This in effect is the process of tempering. Usually the structure
of high-speed steel in the hardened condition consists of 70 to 80% tetragonal martensite,
15 to 30% highly alloyed untransformed austenite and 9 to 12 % of undissolved M6C and
MC carbides [24]. Figure 7(b-d) shows the presence of retained austenite along with
carbides of various sizes.
Figure 8 (a) reveals the presence of large elongated primary carbides and small
spherical secondary carbides in a tempered martensitic matrix and freshly formed
martensites in CHT-1T sample. Also, the primary alloy carbides elongated in a rod like
structure of M6C type can be seen. For this type of steel MS temperature is well below the
critical transition temperature and so most of the martensitic structure will be present as
plate martensite often surrounded by large amount of retained austenite. From Figure 8
(b), it is observed that the presence of carbides that are spheroidized and distributed
uniformly through out the structure in CHT-2T sample. It is the very initial stage of
secondary carbide precipitation. In Figure 8 (c), no drastic change in carbide precipitation
is observed after triple tempering of CHT samples.
During quench hardening process of tool steel, high carbon and alloy content
leads to increase in the austenitizing temperature. It will produce the harder martensitic
structure but simultaneously lower the martensitic start temperature (MS) and martensitic
finish temperature (MF) so that after conventional heat treatment there will be chance of
20 to 30% of retained austenite content in the steel [22]. In the hardening treatment,
cooling takes place in two stages. The tool steel is quenched in a molten salt bath kept at
temperature above that of the martensitic start temperature. The steel is held there until
temperature equalization is complete. The tool is then allowed to cool freely in air which
results in the formation of martensite. Due to the temperature difference between the
surface and the center during the process, martensitic formation is much lower. This
results in less residual stress and minimum distortion. But the amount of retained
austenite is generally high.
21
Most of the austenite in the hypereutectoid steel will transform to martensitie

during hardening treatment. The untransformed part is called retained austenite. The
presence of retained austenite is undesirable. It reduces hardness and wear resistance of
tool steels. Conventionally two possible ways are used for eliminating this retained
austenite phases, one is multiple tempering and another method is cryogenic treatment.
Aforesaid one requires controlled temperature range to form complete martensitic
structure otherwise bainitic structure will form. So in this work in order to study the
effect of cryogenic treatment, the conventionally heat-treated samples are subjected to
shallow cryogenic treatment and deep cryogenic treatment.
Multiple tempering has been the traditional approach taken to deal with the
problem of retained austenite. From the Figure 8(b) it is observed that the carbides are
spheroidized and there are newly formed harmful interlath carbides from the
transformation of retained austenite to martensite and also the presence of tempered
martensite due to the transformation of retained austenite during second tempering. This
type of tool steel with carbon content more than 1% and no cobalt content are usually
triple tempered in order to achieve the toughness requirements. From the Figure 7 (d) the
presence of more tempered martensite and uniformly dispersed fine carbides in the
martensitic matrix after triple tempering is observed.
From the Figure 9 (a), it is observed that there is a large precipitation of
untempered martensite in the SCT-untempered sample, and there is more precipitation of
spheroidized secondary carbides in SCT samples compared with CHT samples. From
9(b) it is clear that there is no drastic change in the micro future when compared with
Figure 9(a). Figure 9 (c) shows the micrograph of SCT-2T sample. After double
tempering more precipitation of small secondary carbides in the martensitic matrix is
identified, and the transformation of untempered martensite into tempered martensite is
also observed. After third tempering, there are no large variations in the precipitations of
both primary and secondary carbides as is shown in Figure 9 (d). Figure 10 (a) shows the
micrograph of SCT-1T sample, which reveals that the carbides are clustered and there is
uneven precipitation of more secondary carbides in the double (Figure 10 (b)) and triple
(Figure 10 (c)) tempered samples. In the SCT samples, emerging of secondary carbide
precipitations are not visible during second and triple tempering, which can be attributed
22
to the decrease in hardness values as shown in Figure 2. A close observation of highly

magnified SEM image of SCT samples reveals the presence of a large amount of small
secondary carbides when compared to CHT samples. For the high carbon, high alloyed
M2 tool steel; the martensitic finish temperature is well below the limit of dry ice
temperature so there will be retention of retained austenite in the martensitic matrix.
Figure 11(a-d) shows the micrograph of DCT samples without tempering along
with the micrographs of three stages of tempering. It is observed from the micrograph
there is a fine distribution of small spheriodized carbides in the martensitic matrix. From
the Figure 12(a) it is seen that the carbide precipitation is very minimum i.e., initial stages
of secondary carbide precipitation. Figure 12 (b) shows the micrograph of DCT-2T
sample. After second tempering, a large amount of carbide precipitation is seen and it is
more uniformly distributed throughout the matrix. Due to this DCT samples experience
higher hardness values than CHT and SCT samples. After third tempering (Figure 12 c)
there is further increase in hardness, which is due to further precipitation of fine alloy
carbides precipitation. From these micrographs, it is observed that the sizes of the
secondary carbides are much finer and uniformly distributed throughout the section of the
DCT samples.
The precipitation of more hard carbides in the deep cryogenically treated samples
tends to reduce carbon and alloy contents in the matrix, which improves the toughness of
the matrix. These differences could be due to the formation of the carbides in
cryogenically treated samples instead of carbides in conventionally treated samples.
During the cryogenic treatment the secondary carbides precipitate in the austenite matrix,
promoting the transformation of the retained austenite to martensite. Changes in the
martensitic lattice parameters and a high density of lattice defects have been reported. It
is suggested that the complete transformation of austenite to martensite and prolonged
holding of martensitic matrix at cryogenic temperature leads to these defects and the
defect sites may act as nucleation sites for the precipitation of the fine array of carbides
after tempering treatments [9].
The effect of tempering on CHT, SCT and DCT samples are compared. There is
no large variation in the hardness values between tempering stages for the CHT samples
as is evident from the Figure 7(a-d). In SCT samples the hardness values when compared
23
with CHT samples is more due to the complete elimination of retained austenite but the
carbides are coarsened during tempering periods. In DCT samples during first tempering
it is observed that the secondary carbide precipitations started at lower extent and
coarsening of primary carbides also occurs. In the case of DCT-2T sample the carbide
precipitation is more and the carbides are uniformly distributed and also having
spheroidized shape. This is the main reason for higher values of hardness. In the DCT-3T
sample it is found that the carbide coarsening had occurred and there is no further
precipitation of carbides.
5.5 Thermo mechanical analysis:

The material experiences a sudden contraction and enlargement in the sample
length according to the temperature range. The data are continuously recorded and it is
Expansion Coefficient (10
-6
/ K)
shown in Figure 13.

95
90
85
80
75
70
65
60
55
50
45
40
35
30
25
20
15
10
5
0
CHTWOT
SCTWOT
DCTWOT
323
393
463
533
603
673
743
813
883
953
Temperature( K)
Figure 13.Plot of linear expansion of specimen vs. Temperature (K)
24
1023
It is observed that there is a sudden contraction between the temperature range of

373 K to 423 K which is due to the redistribution of the carbon atoms in the martensite by
segregation of the carbon atoms to lattice defects and a clustering of carbon atoms i.e.,
the precipitation of a carbon rich phase called carbide. As a consequence, the carbon in
the martensite is reduced to approximately 0.3%. From 423 K to 543 K, it is observed
that there is increase in length, which is due to decomposition of the retained austenite to
ferrite and cementite. From the temperature interval of 543 K to 633 K there is a sudden
contraction; this may be attributed to the formation and growth of cementite (Fe3C) at the
expense of carbides. From 623 K to 773 K, the length increased, the main reason for
this being the effect of carbide coarsening. At 823 K, it is observed that the slight
increase in length is due to the decomposition of a minor part of the austenite. At higher
temperatures, precipitation of alloy carbides and breakdown of martensite occur as a
result of which there is a contraction in length [25].
6. Conclusions
The study came out with the following findings
From the hardness test, it is identified that there is a slight increase in the
average hardness value for DCT samples when compared to CHT samples.
SCT samples experienced higher hardness values when compared with CHT
samples and is due to the reduction of retained austenite.
CHT sample shown the presence of large elongated primary carbides and
small spherical secondary carbides in a tempered martensitic matrix along
with newly formed martensite. Whereas the DCT samples show that the sizes
of the secondary carbides are much finer and uniformly distributed through
out the matrix.
The precipitation of more hard carbides in the deep cryogenically treated
samples can reduce the carbon and alloy contents in the matrix which can
improve the toughness of the matrix.
There is no large variation in fracture toughness value between CHT, SCT and
DCT samples.
Fractographic analysis of all the samples shown that the fracture mode is quasi
cleavage.
25
Acknowledgement:
The authors gratefully acknowledge the timely help rendered by the employees of
Chennai Metco, Chennai and Department of Chemistry, A.C College of Technology,
Anna University Chennai for testing.
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Full version of the abridged article, "Influence of deep cryogenic treatment on alloy carbide precipitations and

Influence of deep cryogenic treatment on alloy carbide precipitations

3012 Shadowood Pkwy, Atlanta, Georgia 30339, USA

Keywords: AISI M2 Tool Steel, Carbide Precipitations, Deep Cryogenic Treatment,

Corresponding author. Tel.: +1-(678)-528-8994 ; E-mail address: bensely@gmail.com

by cooling to a lower temperature, then it might be possible to form carbides in the

3. Material and methodology

Table 1 Result of chemical analysis of AISI M2 raw material in weight %

3.2 Research Methodology

Procurement of raw material - AISI M2 Tool steel

Shallow cryogenic treatment

Free Cooling in air

Deep cryogenic treatment

Single Tempering at 823 K for 3hrs

Double tempering at 823 K for 3 hrs

Triple tempering at 833 K for 3hrs

Figure 1 Research methodology

Table 2 List of treatment conditions considered for this study

Conventionally hardened and single tempered

Conventionally hardened and double tempered

Conventionally hardened and triple tempered

Conventionally hardened + shallow cryotreated at 193 K

Conventionally hardened + Shallow cryotreated at 193 K + Single tempered

Conventionally hardened + Shallow cryotreated at 193 K + Double tempered

Conventionally hardened + Shallow cryotreated at 193 K + Triple tempered

Conventionally hardened + Deep cryotreated at 77 K

Conventionally hardened + Deep cryotreated at 77 K + Single tempered

Conventionally hardened + Deep cryotreated at 77 K + Double tempered

Conventionally hardened +Deep cryotreated at 77 K + Triple tempered

Vickers hardness number (HV 10)

Figure 2 Hardness test results

Toughness, as considered for tooling materials, is the relative resistance of a

KId2 = 15.873(CVN) 3/8

KIC = Fracture toughness for static load condition in psi (in)

4.3 Characterization analyses of the treated samples

4.4 Thermomechanical analysis

5. Results and discussions

Primary Alloy Carbides (MC)

Figure 6 Micrograph of AISI M2 Raw material in annealed condition

Figure 7 Optical micrograph of conventionally heat-treated sample

Figure 9 Optical micrographs of Shallow cryogenically treated samples

Figure 10 Scanning electron microscopic image of Shallow Cryogenically treated

Figure 11 Optical micrographs of Deep cryogenically treated samples

Figure 12 Scanning electron microscopic images of deep cryogenically treated

Most of the austenite in the hypereutectoid steel will transform to martensitie

to the decrease in hardness values as shown in Figure 2. A close observation of highly

5.5 Thermo mechanical analysis:

Expansion Coefficient (10

shown in Figure 13.

It is observed that there is a sudden contraction between the temperature range of

Barron .R.F, Do treatment at temperature below -120 F help to increase the

Moore C. Development of the BOC Ellenite process (cold treatment of metals

Barron .R.F, Cryogenic treatment of metals to improve wears resistance

Molinari .A, M.Pellizzari, S.Gialanella, G.Straffelini, K.H.Stiasny, Effect of

Flavio J. da silva, Sinesio D. Franco, Alisson R.Machado,Emmanuel .O . Ezugwu,

Yong A.Y.L, K.H.W. Seah, M.Rahman, Performance evaluation of

Huang J.Y,Y.T.Zhu,X.Z. Liao, I.J.Beyerlein, M.A. Bourke,T.E.Mitchell,

Mohan Lal D. Renganarayanan S. Kalanidhi A. and Murugesan S.N., Effect of

Mohan lal .D, S. Renganarayanan, A.Kalanidhi, cryogenic treatment to augment

Bensely .A, A.Prabhakaran, D.Mohan lal,G. Nagarajan, Enhancing the wear

Bensely.A ,D.Senthilkumar , D.Mohan lal,G.Nagarajan,A.Rajadurai, Effect of

Leskovek .V, M. Kalin and J. Viintin, Influence of deep-cryogenic treatment

P.F. Stratton, Optimising nano-carbide precipitation in tool steels, Materials