Volume 5, Issue 6, June – 2020 International Journal of Innovative Science and Research Technology

ISSN No:-2456-2165

A Review on the Cryogenic Treatment of Stainless

Steels, Tool Steels and Carburized Steels
Savyasachi N Rincy Reji
Department of Metallurgical and Materials Engineering, Department of Metallurgical and Materials Engineering,
Amal Jyothi College of Engineering, Amal Jyothi College of Engineering,
Kanjirappally, India Kanjirappally, India

Jain Anna Sajan Ajmal Mohamed Rafi

Department of Metallurgical and Materials Engineering, Department of Metallurgical and Materials Engineering,
Amal Jyothi College of Engineering, Amal Jyothi College of Engineering,
Kanjirappally, India Kanjirappally, India

Abstract:- Conventional heat treatment of steel involves retained austenite within the martensitic structure cryogenic
heating the material to its austenitizing temperature, treatment is done after quenching and before tempering.
followed by quenching and tempering. Rapid cooling
transforms austenite to martensite which begins and Stainless steels are alloys of iron and carbon and
finishes at the martensite start temperature (MS) and containing a minimum chromium content of 10.5%.
martensite finish temperature (MF) respectively. The Chromium imparts corrosion and heat resistance to the steel.
presence of alloying elements except aluminium and Other elements like nickel, molybdenum, aluminium,
cobalt lowers both the MS and MF temperature which titanium, copper, nitrogen may be added to improve certain
can go down to subzero temperatures. Thus CHT physical characteristics of the steel. Stainless steels have
cannot fully transform the austenite to martensite excellent corrosion resistance and they are 100% recyclable.
resulting in the formation of retained austenite within Due to their excellent physical properties, they find
the martensitic structure. The retained austenite in the applications in cutlery and kitchenware, medical
steel can transform to martensite under working applications, construction, power generation among others
conditions. This newly formed martensite being applications [4]. Tool steels are used for cutting, forming or
untempered is brittle and reduces the product life of the shaping a material [3]. They are carbon-, alloy-, or high-
material. Thus, cryogenic treatment is done prior to speed steels, capable of being hardened or tempered. Tool
tempering and after quenching to convert the retained steels are used in many applications requiring strength,
austenite to martensite. This paper aims to review the toughness, hardness and resistance to wear [5] Carburizing
cryogenic treatments of stainless steels, tool steels and steel is produced when low carbon steel is subjected to a
carburized steels so far and their effect on their carburizing liquid or gas at high temperature. Carburized
properties. steels possess more wear resistance, fatigue strength and
hardness [6].
Keywords:- Retained Austenite; Cryogenic Treatment;
Stainless Steels; Tool Steels; Carburized Steels. The aim of this study is to give a brief introduction on
martensitic transformation, cryogenic treatment and its
I. INTRODUCTION significance, and understanding the effect of cryogenic
treatment on stainless steels, tool steels and carburized
Heat treatments have always been important in steels.
imparting required properties in metals and alloys. This
improvement in properties is achieved by changes in A. Martensitic Transformation
microstructure [1]. Heat treatment of metals is not only In the study of quenching of steels, researchers found
limited to high temperatures, but also to sub-zero the transformation of face centered austenite into lens
temperatures, which is called cryogenic treatment. shaped or plate like regions with body centered tetragonal
Cryogenic treatment involves cooling metals or alloys to (bct) lattices. Crystals formed by such transformations are
sub-zero temperatures to enhance various mechanical called “martensite” and the lattice transformations are called
properties. Liquid nitrogen is commonly used to cool metals “martensitic transformations” [7]. On quenching, the rate of
to temperatures as low as -196⁰ C [1]. .Quenching of steels diffusion is lowered and hence no phase transformations
from austenitizing temperature transforms austenite to dependent on diffusion take place. Thus martensitic
martensite when the cooling rate is higher than the critical transformations are diffusionless transformations. During
cooling rate[2]. Tempering can make this martensite harder the transformation, gamma iron changes to alpha iron. Since
and tougher. Quenching cannot transform all the austenite to no diffusion of carbon and other metallic atoms takes place,
martensite, even at high cooling rates. Hence, the the chemical composition of alpha iron and gamma iron will
martensitic structure will also contain some amount of remain the same. The solubility of carbon is greater in
untransformed austenite called retained austenite which can gamma iron than in alpha iron. Thus the alpha iron
reduce the product life [3]. In order to reduce the amount of (martensite) formed will be supersaturated.

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 MS and MF temperatures  Retained austenite
The formation of martensite begins at the MS From figure 2, it is evident that all alloying elements
temperature. As the temperature decreases, more and more except aluminium and cobalt tend to lower the MS point of
austenite transforms to martensite and at the MF temperature steel. The decrease in MS point is proportional to the amount
the formation of martensite comes to an end. Lowering the of elements dissolved in steel. Of all the alloying elements,
temperature below MF does not result in any further carbon has the greatest effect in reducing the MS
martensitic transformation. The MS temperature is constant temperature. Manganese, chromium and nickel follow this
for particular steel and does not change with varying cooling order [9]. High carbon steels and tool steels have their MS
rates. In contrast, MF temperature can be lowered by temperatures as low as room temperature.
decreasing the cooling rates [1].
Thus, conventional heat treatment (CHT) which
The MS lowers with the addition of all alloying includes heating the material to its austenitizing temperature
elements except aluminium and cobalt [1]. The relation for a particular time, followed by quenching and tempering,
between alloying elements and MS temperature is given by cannot transform all the austenite to martensite resulting in
[8]: the formation of retained austenite within the martensitic
MS (°C) = 561─ 474(%C) ─33(%Mn) ─ 17(%Ni) ─ structure. In other words, retained austenite is the
17(%Cr) ─21(%Mo) (1) untransformed austenite formed during austenite to
martensitic transformation. This retained austenite is
Figure 1 shows the effect of carbon content on MS and detrimental to the life of the product. During the working
MF temperatures of steel. conditions of the material, the retained austenite can
transform to martensite. This newly formed martensite being
untempered is brittle and can reduce the product life [10].

The presence of retained austenite can be reduced or

eliminated by two heat treatment processes. They are:
Cryogenic treatment or sub-zero treatment and Tempering
[1].

II. REVIEW ON CRYOGENIC TREATMENT

Cryogenic treatment (CT), also known as sub-zero

treatment, consists of cooling the steel to sub-zero
temperatures, which is lower than the MS temperature. This
is done after quenching and prior to tempering. Thus, all the
retained austenite gets converted to martensite. In the 1930s,
German companies used cryogenic treatment for
components of aircraft engines [3].
Fig 1:- Effect of carbon content on MS and MF temperatures
of steel [1] A. Types of cryogenic treatment
Depending on the temperature at which the cryogenic
treatment is carried out, it is classified into two types:
 Deep Cryogenic Treatment (DCT), which is carried out
at -196°C using liquid nitrogen and slowly brought to
the room temperature.
 Shallow Cryogenic Treatment (SCT), which is carried
out at -80°C and then soaked in room temperature [3].

Fig 2:- Effect of alloying elements on MS temperature of a

steel containing 1% carbon [1]

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ISSN No:-2456-2165
B. Cryogenic Heat Treatment Process C. Treatment Parameters
The cryogenic heat treatment process for steels The typical process parameters in cryogenic treatment
consists of: are minimum temperature, hold time, cooling and heating
rate [3].

J.D. Darwin et al. [13] used Taguchi method to

optimize the process parameters of DCT for a 18% Cr
martensitic stainless steel. The DCT parameters such as the
cooling rate, the soaking temperature, soaking time,
tempering temperature, and tempering time, were
considered for the optimization study and the optimum
levels were found out. The authors showed that soaking
temperature is the most significant factor and the optimum
soaking temperature for reducing wear resistance is -184°C.
The contribution of soaking temperature on wear resistance
was found to be 72%.

D. Senthilkumar and I. Rajendran et al. [14] have

studied the effect of deep cryogenic treatment parameters of
SS 4140 to reduce wear loss. The four process parameters
Fig 3:- Cryogenic heat treatment process [3] considered for optimization are hardening temperature,
soaking period, tempering temperature, and tempering
The heat treatment process includes heating to period. They concluded that hardening temperature is the
austenitizing temperatures, which will produce a most important factor in the DCT process by ANOVA
microstructure composed of austenitic phase and primary analysis and the optimum hardening temperature is 880°C.
carbides. Austenitizing is followed by rapid cooling, or The contribution of hardening temperature to wear loss is
quenching. This transforms some or most of the austenite 17.34%.
into the higher strength martensitic structure with
supersaturated carbon. Tempering allows the supersaturated M. Arockia Jaswin et al. [15] used Taguchi method
carbon to form carbides, called transition carbides that along with the grey relational analysis to optimize the deep
relieve micro stresses in the martensite matrix and prevent cryogenic treatment parameters for En 52 Steel. The factors
cracking of the part [11]. studied for optimization were cooling rate, soaking
temperature, soaking period, and tempering temperature.
Soaking period was found to be the most significant
parameter with a contribution of 49.8% and the soaking
period was 36 hours.

III. EFFECT OF CRYOGENIC TREATMENT ON

VARIOUS STAINLESS STEELS

Many researchers worked on the cryogenic treatment

of stainless steels to study its effects on their mechanical and
microstructural properties. Some have worked to find out
the optimum parameters for deep and shallow cryogenic
treatment.

R.F. Barron et al. [16] studied various metals to

Fig 4:- Cryogenic thermal cycle for the steel [12]
determine which material responds better to shallow and
deep cryogenic treatment in improving abrasive wear
Various advantages of cryogenic treatment are
resistance. Among those samples were martensitic SS440,
increased hardness, increased wear resistance, reduced
austenitic SS303 and feritic SS430. The difference in wear
residual stresses, fatigue resistance, increased dimensional
resistance between the SCT and DCT samples was found to
stability, increased thermal conductivity and toughness.
be less than 10%. The wear resistance for shallow, deep and
These advantages are the results of transformation of
conventional heat treated specimens is shown in table 1
retained austenite to martensite, the metallurgical aspects of
below.
eta-carbide formation, precipitation of ultra-fine carbides,
and homogeneous crystal structure [11].

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Wear Resistance (Rw) P. Johan Singh et al. [20] compared the fatigue life
Shallow Deep extension of notches in AISI 304L weldments for samples
AISI No Conventional with and without cryogenic treatment. However, it was
cryogenic cryogenic
Heat Treated found that fatigue crack initiation life from notches of
treated treated
SS440 1447 1853 1763 cryogenically treated samples was enhanced.
(Martensitic
SS) Jitendra Upadhyay et al. [21] tested the effect of deep
SS303 14.3 15.06 15.84 cryogenic treatment on the mechanical and metallurgical
(Austenitic properties of SS316. Deep cryogenic treatment was
SS) followed by tempering at two temperatures: 350°C and
SS430 11.14 12.94 13.35 250°C. Results showed that the samples which were
(Ferritic SS) tempered at 250°C possessed greater hardness and tensile
Table 1:- Wear test of various Stainless steels [16] strength. However, the toughness of both the samples
negatively affected. Optical microstructural analysis
A. Martensitic Stainless Steels revealed the refinement of grains which could be
G. Prieto et al. [17] investigated the microstructural contributing factor for the decrease in toughness. Micro
changes and effect of cryogenic treatment of AISI 420 hardness test was also done for the base sample, and the
stainless steel on its hardness and impact energy. X-ray deep cryogenic treated samples which were tempered at two
diffraction (XRD) was used for phase analysis and temperatures.
characterization, while scanning electron microscopy (SEM-
EDX) and Energy Dispersive Spectrometry (EDS) was used C. Ferritic Stainless Steels
for carbide volume fraction, size and composition S. Zirafar et al. [12] investigated the effect of DCT on
evaluation. The fractured surfaces of the charpy impact test the mechanical properties of 4340 ferritic stainless steel.
specimens were analyzed using scanning electron Rotating fatigue test, hardness and impact test was done.
microscopy. Results showed that cryogenic treatment The fatigue strength and hardness of cryogenically treated
produces homogeneous precipitation of small carbides and specimens were higher, while the toughness was lower
also cryogenic treatment can be done on low carbon steels to compared to the conventionally treated specimens. The
improve their microstructural and mechanical properties. reason for improvement in fatigue resistance and hardness
The soaking time for the specimens was 2 hours and they was shown through neutron diffraction in which the
were able to increase the hardness and impact energy by 5% transformation of retained austenite to carbon was found to
and 10% respectively. be the reason

A. Idayan et al. [10] showed the influence of deep and IV. CRYOGENIC TREATMENT OF TOOL STEELS
shallow cryogenic treatment on the mechanical properties of
AISI 440C. The percentage of retained austenite in There are a lot of confusions regarding the various
conventional heat treated, shallow and deep cryogenic parameters used in cryogenic treatment, they are still widely
treated samples were found out using ImageJ software and used in tool steel to improve their product life. An enhanced
they were found to be 29%, 8% and 5.7% respectively. product life will improve productivity, efficiency and
Hardness of DCT and SCT treated samples increased economy.
compared to the conventional heat treated specimens.
Fractography analysis using SEM clearly depicts the D. Mohan et al. [22] showed that cryogenic treatment
formation of flat facets in SCT specimens, while in DCT can impart 110% improvement in the tool life. It was
specimens’ micro cracks were observed. noticed that cryogenically treated T1, M2 and D3 samples
improved its product life by 3%, 10% and 10.6%
B. Austenitic Stainless Steels respectively. The wear tests of these samples were done by
Paolo Baldissera et al. [18] [19] revealed the influence Flank wear test and Sliding wear test. Some samples were
of deep cryogenic treatment on the hardness, tensile TiN coated, but it was found that the cryogenic treated
properties, fatigue and corrosion resistance of AISI 302 specimens were superior to the TiN coated specimens.
stainless steel. In [13], the tensile and hardness tests results
are compared to other martensitic stainless steel literature. R.F. Baron et al. [16] studied about various tool steels
The author has also analyzed the influence of two DCT to find out which material responds better to SCT and DCT
parameters that is soaking time and minimum temperature in improving abrasive wear resistance. The following tool
through a design of experiment (DOE) and by first steels were studied:
approximation model. In [14], the authors have discussed
the effect of AISI 302 SS on fatigue and corrosion
resistance. The test was done for both solubilized and
hardened steel. The fatigue resistance was improved in
solubilized SS302 while there were no significant changes
in the hardened material. However, there was no change in
corrosion resistance of both the materials.

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Wear Resistance (Rw) TEM micrographs were obtained. It was found that carbide
Shallow Deep formation increased and was more homogeneous after the
AISI No Conventional cryogenic treatment. The authors concluded it to be the
cryogenic cryogenic
Heat Treated reason for the improvement in wear resistance.
treated treated
S-7 5.12 12.38 13.38
V. Leskovsek et al. [27] studied the influence of deep
P-20 6.25 7.70 6.08
cryogenic treatment on the wear resistance of vacuum heat-
O-1 514 1140 1399 treated ESR AISI M2 high-speed steel. Cryogenically
A-2 48.8 47.9 54.4 treated steels exhibited superior wear resistance compared to
vacuum heat-treated steel. Wear resistance was found to
A-6 2165 1151 2094 improve with increasing tempering temperature. Samples
A-10 1035 2386 2738 which showed sufficiently high values for both fracture
199 630 1628 toughness and hardness exhibited superior wear resistance
D-2
compared to samples which had extremely high values for
H-13 30.2 49.7 63.3 either fracture toughness or hardness only.
T-1 1613 2287 2843
Aleksander CISKI et al. [28] investigated the effects of
T-2 5751 5338 4142
cryogenic treatment on properties of HS6-5-2 high speed
M-1 776 1129 1748 tool steel. DCT of HS6-5-2 caused a reduction in the
M-2 3900 4388 4698 dimensions of martensite plates, which resulted in the
reduced hardness of the material and improved its impact
Table 2:- Wear test of various tool steels [16] strength. Drills that had been treated to deep cryogenic
treatment demonstrated reduced durability during industrial
It was concluded from the above study that lowering tests, despite showing lower wear intensity during three
the temperature enhances the wear resistance in steels. roller-cone test under 100 MPa load.
M. Villa et al. [23] subjected D2 tool steel to various Zbigniew Zurecki et al. [29] studied the effects of
austenitization treatments, followed by various cryogenic cryogenic quenching on the microstructure and mechanical
and tempering treatments. Microstructure and mechanical properties of A2-grade tool steels. Cryogenic quenching of
properties of these samples were studied by X-Ray A2 steel resulted in hardness and wear resistance, at the
Diffraction (XRD), scanning electron microscopy (SEM), expense of reduced impact strength. Increased holding time
vibrating sample magnetometry, hardness measurement and during cryogenic treatment resulted in higher dark carbide
tribology tests and found that some amount of retained number frequency, increased hardness, increased wear
austenite still remained in the cryogenic treated samples. resistance, and reduced impact strength. The study showed
that cryogenic treatment must be done immediately after
Nandakumar Pillai et al. [24] worked on the effect of quenching from austenitic temperature prior to tempering
cryogenic treatment of AISI D series cold worked tool steel. for the cryogenic treatment to be effective.
D2, D3, D5, D6, and D7 grades of tool steel were selected
for this study. It was observed that retained austenite D. Das et al. [30] studied the effects of cryogenic
reduction in D3 tool steel was greater than D2 and D6. The treatment on the wear behavior of AISI D2 steel. AISI D2
microstructure of conventional heat treated specimens steel subjected to cryogenic treatment at 77K showed
contained retained austenite and martensite, while the superior wear resistance compared steel subjected to
cryogenic treated specimens reduced the amount of retained conventional heat treatment. This improvement in wear
austenite percentage and made the martensite finer. resistance is due to the reduction in retained austenite
content and increased number of finer secondary carbides
Marcos Pérez et al. [25] tested the mechanical distributed homogeneously within the microstructure of the
properties of cryogenically treated AISI H13 tool steel. steel. Wear resistance is shown to improve with increasing
Tensile, hardness and fracture toughness tests were also holding time up to 36 hours at 77 K. Further increase in
done. Better mechanical properties were obtained in holding time results in monotonic decrease in wear
cryogenically treated samples compared to conventionally resistance.
treated samples. SEM and X-ray diffraction analysis were
used to study microstructural evolution. Microstructure V. Firouzdor et al. [31] subjected an M2 HSS drill to
revealed the presence of dispersed network of fine carbides. austenizing temperature of about 1100⁰ C and gradually
It was also concluded that there still exists a small amount of subjected it to deep cryogenic treatment at about -196⁰ C for
retained austenite within the tool steel which cannot be 24 hours, while another drill was subjected to tempering at
reduced by heat treatment.
200⁰C for 1 hour after cryogenic treatment. A reference drill
was also taken which was not subjected to any extra heat
J.Y. Huang et al. [26] performed a microstructure
treatment. Cryogenic treatment was shown to improve the
analysis on cryogenically treated M2 tool steel. Both
wear resistance of the drill by 77%, while drills that were
shallow and deep cryogenic treated samples were tested and
subjected to both cryogenic treatment and tempering
compared the results with conventional heat treated samples.
showed improvements in wear resistance by 126%. The

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Volume 5, Issue 6, June – 2020 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
improvements in wear resistance are due to the precipitation A. Akhbarizadeh et al. [37] studied how deep
of fine carbides during cryogenic treatment. Increase in cryogenic treatment affected the austenite grain size,
hardness values due to the transformation of retained hardness and wear resistance of D6 tool steel. The
austenite to martensite also contributes to the improvements microstructural properties and phases present in the heat
in wear resistance. treated samples were examined using scanning electron
microscopy (SEM) and x-ray diffraction (XRD) method.
H.G Naneesa et al. [32] investigated the martensitic From the results it can be concluded that during the
transformation of the AISI D2 tool steel which was cooled cryogenic treatment the retained austenite is almost
continuously from its austenitizing temperature using 10 Ks- completely transformed to martensite.
1
or 50 Ks-1 cooling rates up to the deep cryogenic
temperature. Dilatometry was used for it. SEM revealed the K. Moore and D.N Collins et al. [38] determined the
presence of lathe and plate martensite and transmission effect of various factors affecting the hardness of steels
electron microscope revealed the presence of nano twined which has undergone three types of cryogenic treatment.
martensite. One of the main observations was better The main observation was the increase in hardness greatly
dimensional stability. dependent on cryogenic temperature and independent of
soaking time. The three materials selected for this study was
D. Das et al. [33] examined the fracture toughness of H13, D2 and D17.
AISI D2 steels using the sub-zero treatments – cold
treatment, shallow cryogenic treatment and deep cryogenic V. CRYOGENIC TREATMENT OF CARBURIZED
treatment comparing with the conventional heat treatment STEELS
process. They also identified the mechanism of initiation of
fracture as cracking of primary carbides and the growth of Paolo Baldissera et al. [39] investigated the effect of
micro voids by de-cohesion of secondary carbides. The deep cryogenic treatment on the static mechanical properties
variations in fracture toughness values have also been noted. of 18NiCrMo5 carburized steel, which is used commercially
for manufacturing gears. Deep cryogenic treatment after
N.W. Khun et al. [34] investigated the effects on tempering showed an increase in hardness without much
mechanical and tribological properties of AISI D3 tool steel change in its ultimate tensile strength. Increase in the
due to deep cryogenic treatment with a consolidated soaking time during deep cryogenic treatment corresponds
connection between their wear resistance and hardness. It to an increase in hardness values. Tempering of steel after
was found that an additional DCT process to the deep cryogenic treatment results in increased hardness as
conventionally heat treated samples increased the hardness well as increased values of ultimate tensile strength by up to
with the elimination of more retained austenite and 11%. Tensile test of cryogenically treated groups shows a
formation of homogeneous carbide formation. significant increase in Young’s modulus of the material.
Fractographic analysis of the steel specimens shows no
R. H. Naravade et al. [35] examined the wear behavior changes in fracture mechanisms for different heat treatment
of D6 tool steel subjected to deep cryogenic treatment for 36 methods.
hours. It was identified that the presence of retained
austenite was decreased after the cryogenic treatment and A. Bensely et al. [40] studied the effects of shallow
hence the wear resistance and hardness is improved cryogenic treatment and deep cryogenic treatment on the
compared to the conventional heat treatment process. The tensile properties of case carburized 815M17 steel. The
authors also investigated the significance of multiple investigation revealed a reduction in tensile strength by a
tempering before and after cryogenic treatment on friction factor of 9.34% for DCT and 1.5% for SCT over
and wear behavior of the samples. A variety of heat conventional heat treatment. Fractograph analysis using
treatments were carried out and finally concluded that SEM revealed presence of dimples and flat fracture regions
cryogenic treatment improved the wear resistance and in SCT samples than for CHT and DCT samples.
hardness the most.
M. Preciado et al. [41] investigated the effects of
N.B. Dhokey and S. Nirbhavane et al. [36] did a test tempering prior to DCT on the hardness and wear resistance
using pin-on-disc machine to find out the role of multiple of carburized steel. Tempering prior to DCT was found to
tempering on D3 tool steel which has undergone cryogenic improve the wear resistance of carburized steel. However,
treatment. Wear rate deteriorates during subsequent only those samples that had been tempered at 200⁰ C
tempering and this process is an influential function of fine showed significant improvements in hardness values, which
carbides and its distribution. The mechanism behind was due to the segregation of alloying elements and carbon
improving wear resistance of the particular material was atoms during the transformation of retained austenite to
identified using the results from SEM analysis, hardness martensite.
data and microstructures of the worn out sample.

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ISSN No:-2456-2165
A. Bensely et al. [42] studied the effects of shallow [7]. Van Humbeeck, J., 2001. 5.3 The Martensitic
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