Review article

Proc IMechE Part E:

J Process Mechanical Engineering
Effect of cryogenic treatment on properties 2022, Vol. 236(4) 1758–1773
© IMechE 2022
of materials: A review Article reuse guidelines:
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DOI: 10.1177/09544089221090189
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Gurkirat Singh1 and K.N. Pandey1

Abstract
The objective of this review paper is to introduce Cryogenic temperature effect on different properties of materials.
Results showed that cryogenic operation improves properties like hardness, fatigue strength, tensile strength, toughness
and resistance to wear in comparison to conventional operations. The improvement is a result of microstructural changes
at cryogenic temperature which helps in conversion of austenite to martensite and carbide nucleation. The results also
showed that doing tempering before or after cryogenic operation has significant influence on material properties which
helps to achieve better carbide distribution. Different heat treatment sequences which involve tempering before or after
Deep Cryogenic Treatment (DCT), provides varied results. Soaking time at cryogenic temperature also has an important
role in refinement of microstructure and affect material properties.

Keywords
Deep Cryogenic Treatment (DCT), Shallow Cryogenic Treatment (SCT), Conventional Heat Treatment (CHT), retained
austenite, martensite

Date received: 30 September 2021; accepted: 5 March 2022

Introduction
The research on cryogenic treatment had started from the
very beginning of 1930’s in Germany. German companies
were trying its application in aircraft engines. The founda-
tion of cryogenics in US came in 1940. In the starting
period till 1960s, the components were experiencing
crack due to uncontrolled temperature variation during
immersion of component into Liquid Nitrogen but later
on as the research progressed in this field, the finer
results started coming into picture with computerized
temperature-controlled system. Deep Cryogenic
Treatment finds its application in the field of advanced
material properties in mechanical Engineering. Results
obtained from Deep Cryogenic Treatment (DCT) showed
improvement in material properties and were better than
conventional Heat Treatment (CHT).1–3 With continuous
research in cryogenic treatment, it can be implemented
on nonferrous and non-metallic materials as well.4–6
Cryogenic treatment took advantage over conventional
heat treatment by improving some of the core properties
of material such as longer service life of the component,
dimensional stability, better wear resistance and reduction
in residual stresses.7–11 Cryogenic treatment is a better
way for the refinement of microstructure. In deep cryogenic
treatment material is processed to a very low temperature up
to −196⁰C.12 Collins and Dormer found that in DCT, mar-
tensite is obtained from the conversion of retained austenite
and promotes carbide formation.13–16 In DCT, η carbides
helps in making the matrix tough.2,17,18
Mechanism
Transformation of retained austenite to martensite is one
of the keys for the improvement of material properties
after cryogenic treatment. Retained austenite has FCC
(Face Centered Cubic) crystal structure as shown in
Figure 1(a). During phase change in cryogenic treatment,
austenite tries to reject 0.8 wt% carbon and transfoms to
BCC structure because BCC structure can only handle
0.01 wt% carbon. But because of very high cooling rate
carbon does not get enough time to escape austenite
(FCC) structure and still remains trapped in austenite
(FCC) and makes diffusionless transformation. This diffu-
sionless transformation results into shear strained BCT
(Body Centered Tetragonal) structure which is martensite
as shown in Figure 1(b).
In BCT ‘b3’ axis is not equal to ‘b1’ and ‘b2’ axis but in
FCC structure all the three axis ‘a1’, ‘a2’ and ‘a3’ are
equal.20 The other key that may be responsible for the
1
Department of Mechanical Engineering, MNNIT-Allahabad, Prayagraj,
India
Corresponding authors:
Gurkirat Singh, Department of Mechanical Engineering, MNNIT-
Allahabad, Prayagraj, India.
Email: gurkiratlpu@gmail.com
K.N. Pandey, Department of Mechanical Engineering, MNNIT-Allahabad,
Prayagraj, India.
Email: knpandey@gmail.com
Singh and Pandey
Figure 1. (a) FCC (face centered cubic) structure (b) BCT (body centered tetragonal) structure.19
improvement of properties of materials after cryogenic
treatment is Ostwald ripening. Precipitation of carbides
appear in the microstructure when material is under hold
at cryogenic temperature. As the holding time increases,
the carbides get coarsen up into bigger size. The mechan-
ism behind coarsening of carbides is Ostwald ripening as
shown in Figure 2. In Ostwald ripening smaller particles
get dissolve into bigger particles. The reason behind that
is smaller particles has large surface area to volume
ratio than the large particles as a result smaller particles
has high surface energy which make them more unstable
than larger particles. This results coarsening of carbide
particles with time which may improve properties of
materials after cryogenic treatment21
Carbide nucleation and retained austenite conversion
are responsible for improvement in material properties
in DCT. Carbide nucleation acts as a barrier for crack
propagation and improves material’s strength.22
Cryogenic treatment helps in getting uniform distribution
of carbides in the microstructure which results improve-
ment in material properties.23–27 DCT also reduces
retained austenite in material and thus increases hardness,
resistance to wear and tensile strength of materials.12,28 In
conventional heat treatment, retained austenite left in the
materials which degrades material properties.
As the temperature lowers the potential of conversion
to other phases decreases. Researchers had developed
various setups for deep and shallow cryogenic setup for
various heat treatment sequences.29–46 A typical cryo-
genic setup is shown in Figure 3(b).
Tempering associated with the cryogenic treatment
plays an important role in altering the properties of mate-
rials. The properties gets affected by partial or complete
transformation of carbides which precipitate during cryo-
genic treatment to new carbides after tempering as shown
in Figure 4.24
At cryogenic temperature volume of metal shrinks with
shrinking of the lattice. G.R.LiT et al. studied material
behavior at cryo temperature.47The volume shrinkage of
an alloy is given by Equation (1)
α(∂V |∂T )p (1)
where α is coefficient of linear expansion and T, V and P
are temperature, volume and pressure respectively. If To
and Vo are initial temperature and volume then the final
1759
volume VT when the temperature shifted to T1 is given
by equation (2)
VT = Vo eα(T1 −T0 ) (2)
Volume shrinkage rate is governed by Equation (3)
[ϕ = [eα(T1 −T0 ) − 1] (3)
As the volume of material shrinks, there is shrinkage in
lattice. The lattice resistance to slipping dislocations is
governed by Equation (4)


2π
σ p = 2 Ep (4)
l
where l is the atomic distance and Ep is the P-N barrier.
Because of volume contraction, the pressure stress will
set up in material. The average pressure stress is governed
by equation (5)
σ = K[eα(T1 −T0 ) − 1] (5)
where K is elastic modulus.
There are number of cryogenic treatment sequences
followed by various researchers which are tempering
prior to or after cryogenic treatment depending upon the
kind of properties to be built in the materials. It is better
to include tempering after cryogenic operation which
results in fine and homogenous distribution of car-
bides.48–64
A Typical Cryo-treatment cycle has ramp down,
soaking period, ramp up and tempering as shown in
Figure 5. and explained below:
• Ramp Down-It is a process in which sample is cooled
from room temperature to cryogenic temperature. The
cooling rate is kept low so that magnitude of thermal
stress can be reduced.
• Soaking- It comes after ramp down where sample is
hold at cryogenic temperature for hours. Soaking of
samples at cryogenic temperature allows the precipita-
tion of carbides. Size and density of carbides greatly
affected by soaking period66–76 as shown in Figure 6.
• Ramp Up-Sample which is soaked at cryogenic tem-
perature for hours is then warmed to room temperature.
• Tempering- It is a process in which material is heated
below recrystallization temperature. From cryo- litera-
ture it is found that better results are obtained when
1760
Figure 2. Schematic representation of Ostwald ripening.21
tempering is performed after cryogenic operation in
cycle.77–81
Materials
Materials on which cryogenic treatment has been
attempted, can be broadly categorized into ferrous and
nonferrous alloys. Depending upon the properties found
after cryogenic temperature, there are few materials that
are suitable for cryogenic treatment. These include
copper, brass, tool steels, monel, aluminium and its
alloys, invar, teflon, Kapton and mylar. Among metallic
materials, ceramics and polymers, the metallic materials
has better combination of strength and plasticity after
cryogenic treatment and therefore contribution of metallic
materials is almost 80% in the field of cryogenic treat-
ment.82 In order to select materials for cryogenic applica-
tions, the physical properties like specific heat, coefficient
of thermal expansion, density, thermal conductivity and
Ductile to Brittle Transition Temperature (DBTT) are
important to be considered.83 For cryogenic applications,
the selection of materials highly depends on their ductile
to brittle transition temperature (DBTT). Ordinary struc-
tural steel will fail in DCT as it’s DBTT is higher than
application temperature. To meet this requirement, steels
with DBTT lower than service temperature are required.
For various materials applications, the cryogenic tempera-
ture may range from 300 K to 4 K depending upon what
type of material we are using.84–107 Applications where
specific strength is the primary need for material selection,
nonferrous metals & their alloys and reinforced plastics
are used but for applications that requires temperature
less than 77 K, steel dominates.
For applications under low temperature, steels are
divided into two parts which are austenitic and ferritic
steels. As Ferritic steels have BCC structure so their
Proc IMechE Part E: J Process Mechanical Engineering 236(4)
applications become limited. Nickel is added in ferritic
steel in order to stabilize the austenite phase and reduce
the brittleness. Ferritic steels include Cr which lies in
10.5–30 wt. %. and microalloying elements like Al, Nb,
Cu, Mo and Ti. Austenitic steels, because of FCC struc-
ture, shows much lower DBTT which makes them
much suitable at very low temperature up to 4 K than fer-
ritic steels.83
Other steels referred for cryogenic applications is mar-
tensitic steel and precipitation hardened stainless steel.
Martensitic steel is an alloy of iron, chromium and
carbon having Cr 10.5–18.0 wt %, higher than ferritic
steels. A small amount of micro alloying element is
added to improve toughness of the steel.83,108
Applications where high strength and high stress corro-
sion cracking resistance is required, the duplex steel
comes into application. Duplex steel belongs to a class
of stainless steel. Mostly used Martensite steel grades
for cryogenic applications have 20–29% chromium.
Because of the presence of ferrite phase, duplex steel
shows DBT which tries to restricts the lowest temperature
applications.109–112
Precipitation hardened stainless steels are formed by
precipitation of intermetallic precipitates and retained aus-
tenite. Because of intermetallic precipitates, precipitation
hardened stainless steels have high strength. Austenitic
steel has FCC structure so its always a good choice for
cryogenic application but having low yield strength is a
major problem when we need high strength and stiffness
applications. For such applications precipitation hardened
stainless steels are considered because of both martensite
and austenitic phases in the matrix.86–88
Bearings used in cryogenic applications like pumping
cryogens and cryogenic engines are highly different
than bearing used in other applications. For such applica-
tions, rolling element bearings are used.113 Need for
Singh and Pandey
Figure 3. (a) Schematic representation of cryogenic setup (b) Experimental setup.46
Figure 4. Schematic representation of carbides conversion during tempering operation.24
corrosion resistance against aerospace applications devel-
oped AISI 440C martensitic stainless steel. This steel
grade provides high strength and resistance to corrosion
but has less fatigue strength. To overcome this problem
440CM and 440N-DUR variant of 440C were devel-
oped.114 Table 1. and Table 2. showing the ferrous and
non ferrous alloys with deep cryogenic treatment for dif-
ferent material properties. Table 3. showing various stages
of heat treatments which were used during the process.
Techniques in material investigation
The property of a material depends on how the material
behaves at particular temperature i.e., what change is
taking place in microstructure and at what rate.
Therefore, material investigation requires techniques to
measure temperature and analysis of microstructure.
Temperature measurement techniques
The microstructure or phase transformation depends on
temperature and time. Therefore, it is very important to
get precise temperature reading. Mohan et al. in their
study on effect of cryogenic treatment on mechanical
1761
properties of Alloy steel 16MnCr5 measured DCT tem-
perature of −186⁰C using R type thermocouple which
had working range of −200⁰C to 200⁰C.148 Zare et al. in
their research on DCT of HY-TUF steel monitored the
samples temperature using K-type thermocouple.129
Koneshlou et al. in their research on DCT of AISI H13
tool steel monitored the specimen temperature using K
type thermocouple. The specimen was lowered down in
cryo container with cooling rate of 0.5⁰C/min using a
step motor.149 Chaanthini et al. in their research on deter-
mining cryogenic effect on aluminium alloy AA2014
used K type thermocouple to measure SCT temperature
of −50⁰C. One end of the thermocouple was connected
to sample and the other end was connected to
Temperature controller unit to display reading.136
Material characterization techniques
Different material characterization techniques have been
used by researchers to characterize material after cryo-
genic treatment, such as optical microscope,50,130,148,149
Scaning Electron Microscopy (SEM),116,135,136,147
Secondary Electron Detector (SED),2,4,14,15 Back
Scattered Electron Detector (BSED)15,24,72,150 and
1762
Figure 5. Cryo-treatment cycle.65
Figure 6. Microstructure of samples (a) CHT (b) DCT-2hrs (c) DCT-24hrs (d) DCT-72hrs.66
Energy Dispersive Spectroscopy (EDS).73,143,151,152
Optical microscope is used as a primary device to get
the brief idea about the material before using some
more sophisticated devices.153 SED is for topographical
details while BSED provides both topographical and com-
position details but exact detection of composition is not
possible with BSED. For this EDS is implemented.
Effect of deep cryogenic treatment on
properties
Hardness
Hardness is the material resistance to indentation or
scratch on its surface. Hardness is used in numerous
engineering design applications. This property is essential
as it directly correlates to the material’s performance and
suitability. Researchers has studied various heat treatment
effects on hardness. Deep cryogenic treatment is one of
Proc IMechE Part E: J Process Mechanical Engineering 236(4)
them. Chaudhary et al. in her investigation on cryogeni-
cally treated coated carbide (KC-9225) concluded that
presence of η carbides improves performance of tool
and showed that hardness of treated samples increased
by 21.75% over untreated samples.134 Zhang et al. did
their experimentation on WC- Co cemented carbide and
found that low cobalt cemented carbide has larger
increase in volume fraction of ϵ-Co (Hexagonal Closed
Packed) than high cobalt cemented carbide.133 ϵ-Co has
higher strength and hardness than α-Co (Face Centered
Cubic). Senthilkumar in his research on EN31 steel
under DCT showed that DCT samples had higher hard-
ness value than conventionally treated samples by
4HRC because of conversion of retained austenite to mar-
tensite and carbide nucleation.125 Li et al. obtained
optimal parameters for improved tool life of WC-Co
cemented carbide inserts with cryogenic temperature
−190⁰C, cooling rate 8⁰C/min, soaking time 90 min and
tempering temperature 60⁰C.154
Singh and Pandey 1763

Table 1. Ferrous Alloys and purpose of cryo-treatment. Table 2. Non-Ferrous Alloys and purpose of cryo-treatment.

S. No. Material Purpose Ref. No. Ref.

115
S. No. Material Purpose No.
1 AISI H13 Wear Resistance
116 5
2 Wear resistance 1 AZ91 Hardness and wear
117
3 Fatigue Resistance resistance
118 131
4 Fracture Toughness 2 Hardness
119 132
5 Hardness and 3 WC-Co cemented Hardness
Toughness carbide
120 133
6 AISI D2 Hardness 4 Strength and
121
7 Hardness hardness
134
5 KC-9225 Hardness
66 135
8 AISI D6 Impact toughness 6 Al6082 Ductility
122 136
9 AISI H21 Hardness and 7 Al AA2014 Tensile strength and
Fatigue resistance fracture toughness
123 137
10 AISI 4340 Impact energy 8 AA7075 UTS
124 138
11 Fatigue strength 9 AA2024 Hardness
125 139
12 EN31 Hardness 10 Monel K-500 Hardness, wear
126
13 EN353 Residual Stress resistance and UTS
127 140
14 Cr-Mo-V-Ni High Impact toughness 11 Hastelloy Hardness and
strength steel toughness
128 141
15 40CrMoV5 tool steel Hardness 12 Mg-1.5Zn-0.15Gd Wear resistance
129
16 HY-TUF steel UTS, Yield Strength Magnesium Alloy
130 142
17 30CrMnSi structural Impact toughness 13 Inconel 718 Wear resistance
143
steel 14 Fatigue strength
144
15 Machinability
145
16 Inconel 625 Wear rate
146
17 Nimonic 90 Wear resistance and
Thakurai et al. performed cryogenic treatment on AISI tool life
H13 tool steel with different soaking time 12hrs, 24hrs, 147
18 Nimonic C-263 Wear resistance
36hrs and 48hrs and found highest hardness for 36hrs
sample time.128 Microstructure of different heat-treated
samples are shown in Figure 7. Up to soaking period of soaking period increased, the grains become finer.140
24hrs not much variation in microstructure detected Oteyaka et al. in their research showed that the hardness
although there was de-carburization which is not evident of AZ91 under DCT increased from 63HV to 75HV. The
in microstructure but as the soaking time increased to hardness was higher in DCT with 6 h than 4 h and 5hrs.131
36hrs or above fine carbides phase detected in micro- Vigneshwaran et al. in their research on drilling of
graphs which resulted from retained austenite conversion Nimonic-80 workpiece samples with cryogenically treated
to martensite. Beyond soaking period of 24hrs, these car- and untreated drill bits found that the treated tool has
bides started becoming coarser due to Ostwald ripening higher hardness than untreated one. They also confirmed
which resulted in increase in carbide density and micro- that surface roughness values (Ra) obtained with cryogeni-
hardness as shown in Figure 8. cally treated is smaller than untreated tool.155 Paydar et al. in
Karthikeyan et al. did their research on WC- Co inserts their investigation on deep cryogenic treatment of 100Cr6
at DCT under different soaking time of 24hrs, 48hrs and alloy steel confirmed that DCT completely eliminated
72hrs. Highest hardness came under 24 h soaking time retained austenite.156 Deshpande et al. in their study on
due to high η-phase carbide density. Beyond 24hrs the comparison of Inconel-718 machinability by using cryo-
hardness decreased due to decrement in η-phase carbide genically treated inserts with MQL (Minimum Quality
density.132 It appeared that DCT suppressed the precipita- Lubricant), dry and Liquid nitrogen environment concluded
tion of η-phase carbides. At DCT(24) + T(Tempering) that Inconel-718 machinability improvement was highest
sample, there was highest η-phase carbide density which for cryogenically treated inserts with MQL than other
filled the voids of tungsten carbide matrix and gave rigid- modes (dry and liquid nitrogen environment).144
ity to the matrix and increased the hardness but as the Mohan et al. investigated the effect of Shallow
soaking period was increased, the η-phase carbide Cryogenic Treatment on AL7075-T6. The results
density decreased which didn’t fill all the voids and showed improvement of hardness after the treatment
resulted decrement in hardness after 24hrs soaking period. due to precipitation, higher dislocation density and
Pandey et al. in their research on DCT of Monel K-500 second phase particles distribution observed by EBSD
found increase in hardness of 10.73% in DCT samples as supplementary Figure 9.157 It was highlighted that the
compared to SCT samples.139 In Hastelloy, Ekambaram hardness and stiffness improvements are the consequence
applied cryogenic treatment at −196⁰C and found that at of precipitation hardening and high dislocation density.
low temperature recrystallization occurs which produced Chetan et al. in their research on machining of Nimonic
coarse grains that resulted in decrease in hardness. As the 90 with carbide inserts concluded formation of dense
1764 Proc IMechE Part E: J Process Mechanical Engineering 236(4)

Table 3. Main processes in cryogenic treatment.

Ramp Down Soaking Ramp Up Tempering

Material Ref. No.
Cooling Soaking Warming
Rate, Tmin, Time, rate, Temperature, Time, Number of Time,
[°C/min] [°C] [hr] [°C/min] [°C] [hr] Tempering, [n] [hr]

EN19 - −80 8 - - - 1 22

07X16H6 Stainless steel 0.85 −175 24 0.39 400 1 1 44

AISI D6 - −180 2 & 24 - 500 & 250 4&2 1&3 66

AA2014 1.77 −50 3, 6,9, 12, 2.28 160 18 1 136

15, 18 &24
HY-TUF steel 0.0036 −196 6, 12, 24, 48 - 300 1 1 129

& 72
30CrMnSi Structural 2 −196 12 - 560 2 1 130

steel
Al6082 0.95 −183 0.17, 0.5, 1 0.95 - - 0 135

& 24
Nimonic C-263 2 −100, 2, 18 & 24 2 200 2 1 147

−140, &
−180
KC-9225 0.00527 −173 11.83 0.00732 199.85 2.5 1 134

EN31 - −196 24 - 150 1 1 125

40CrMoV5 tool steel - −196 12, 24, 36 & - - - 0 128

48
Monel K-500 - −196 24 - - - 0 139

Cr-Mo-V-Ni High - −196 8 - 230 2 1 127

strength steel
Nimonic 90 1.88 −196 8 0.941 - - 0 146

AA2024 - −196 2, 9 & 64 - - - 0 138

3 −185 8, 12, 16, 20, - 100 & 520 1&2 3 145

24 & 32
AISI H13 - −145 24 - 540, 600 & 3, 2 & 3 116

565 2
2 −196 12 - 560 2 1 117

AISI D2 - −185 36 3–4 210 2 1, 2, 3 & 4 120

2.19 & −100, 0.0027, 0.63 & - - 0 121

10.98 −150 0.083 & 1 1.098

AISI 4340 - −196 24 - 300 - 1 123

Mg-1.5Zn-0.15Gd - −196 2 & 24 - - - 0 141

Magnesium Alloy
AA7075 - −196 1 - - - 0 137

Inconel 625 - −196 - - - - - 145

- −196 24, 36 - 200 2 1 142

Inconel 718 2.2 −135 4 2.5 - - 0 143

EN353 1.31 −196 24 0.65 149.85 1.5 1 126

η-phase particles in the microstructure of cryo-treated
carbide inserts were responsible for reduction in forces
during machining. The reduction in cutting forces at dif-
ferent cutting speed at 40 m/min and 80 m/min found to
be 4.5% in comparison to dry machining.146 Padmini
et al. in their research on cryogenic operated Aluminium
test sample 2024 found that hardness of cryo treated
sample is better than non-cryo sample by 3.7% due to
finer grain formation.138 Korade et al. did research on
AISI D2 tool steel having different heat treatment
sequence among Hardening (H), Tempering (T),
Cryogenic (C) and Soft Tempering (S) and found that
hardness became highest for HCT heat treatment
sequence and there is decrement in hardness if the
tempering operations occurred more than once.120 Hadi
et al. analyzed tempering temperature effect on AISI D2
tool steel and found that when sample was tempered at
473 K then hardness value is decreased by 40 HV due
to formation of transition carbides and when tempered
at 773 K then this decrement became 200 HV due to
transformation of transition carbides to cementite and
recovery of martensite.121
Tensile strength
Tensile strength refers to the maximum load that a mater-
ial can handle while it is stretched without getting frac-
tured. Attempts have been made to study the effect of
Singh and Pandey
Figure 7. Micrograph for varous heat treated samples of AISI H13 tool steel.128(a) Untreated; (b) HT + DCT (12 h); (c) HT + DCT
(24 h); (d) HT + DCT (36 h) (e) HT + DCT (48 h).
cryogenic treatment of different materials on tensile
strength.
Koneshlouet worked on AISI H13 for cryogenic treat-
ment and observed that as the cryogenic temperature
decreased the difference in tensile strength also decreased.
The change in tensile strength decreases because most of
the austenite transformed to martensite.149 In non-
cryogenically treated sample, martensite needles, carbides
and retained austenite identified in the microstructure as
shown in supplementary Figure 10. As the temperature
lowered martensite needles became smaller and distribu-
ted more uniformly in the matrix and it was also noticed
that as the cryogenic temperature lowered with an
increase in holding time, more finer carbides with signifi-
cant increase in their density detected as shown in
supplementary Figure 11. which was responsible for
increase in ultimate tensile strength as shown in
supplementary Figure 12. The percentage increase in car-
bides was due to retained austenite transformation to mar-
tensite. The retained austenite percentage decreased from
8.1% to 3.8%. The percentage increase in carbides were
found more in the case of tempering after DCT.
Li et al. in their research concluded that the perform-
ance of steel samples under the cryogenic treatment at
−60⁰C is not as good as cryogenic treatment at
−110⁰C.50 Jamali et al. stated that due to increased
1765
martensite quantity after cryogenic processing, tensile
strength of AISI4340 and AISI4140 steel was higher
than oil quenched samples.123
Chaanthani in his research on cryogenic treatment of
AA2014 alloy noticed precipitation of CuAl2 as shown
in supplementary Figure 13. After SCT for 18 h, these
particles enlarged, refined and more uniformly distributed
along the grain boundaries in the matrix resulting in
increased tensile strength.136
Ramesh et al. studied the effect of DCT on an alloy
having chemical composition of Carbon-0.24%, Manganese-
0.62%, Silicon-0.16%, Sulphur-0.049%, Nickel-0.09%,
Chromium-0.059%, Molybdenum-0.030%, Iron- 98.703%.1
There were signified increase in martensite peaks and carbides
in DCT and DCT + LT(Low Temperature Tempering) as
compared to untreated sample found in XRD test The con-
version of retained austenite to martensite and uniform
homogenous secondary carbides precipitation found more
in DCT sample than DCT + LT sample which was respon-
sible for highest tensile strength in DCT sample among
all samples.158–160 The results showed that there were
percentage increase in tensile strength and elongation
when alloy experienced DCT and DCT + LT. The
tensile strength of DCT + LT is less than DCT because
tempering disturbed the carbide nucleation. With
increase in cryogenic soaking time, the ultimate tensile
1766
strength of Al alloy increase and this increase was
recorded 29% in comparison to solution treatment with
soaking time of 24 hs.135 Effect of rolling with cryogenic
treatment of AA7075 was studied by Prabhakaran et al.
An increase in the Ultimate Tensile Strength in cryo
rolling by 30% over base metal alloy was found.
Decrement in elongation from 6.40% to 1.20% over
base metal alloy was attributed to precipitation of alloy-
ing elements in the matrix.137
Wear resistance
Study of wear of materials is an important aspect espe-
cially if the material has to behave as wear resistant.
Wear resistance can be achieved by Deep Cryogenic
Treatment and is studied vehemently by the researchers.
The cryogenic treatment provides significant change
in the microstructure and wear resistance.137,154
Padmakumar et al. in their investigation on tungsten
carbide milling cutters under cryogenic treatment men-
tioned that tempering after cryogenic treatment causes
little decrement in the resistance of flank and nose wear
and stated that it could be due to less cobalt percentage.122
Das in his research observed that decrease in retained aus-
tenite and change of secondary carbides helped in
improvement of wear resistance of steel.9 For H21 tool
steel Korade et al. found that in DCT samples there
were decrease in carbide size and increase in carbide
density and most of the retained austenite transformed
to martensite as a result there was improvement in hard-
ness and wear resistance.122
Shinde did his research on AISI H13 steel and showed
that carbide density increased upto cryo soaking time of
16hrs after that it decreased and also correlated carbide
particle size with wear rate. It was stated that minimum
wear rate occurs at minimum carbide particles size.115
Mani in his research on turning of Inconel 625 observed
that cryogenic treatment helped in increasing tool life by
lowering the heat generation which helped in reducing
tool wear. The results of cryogenic turning showed
improvement of surface roughness which was found to
be 50.52% as compared to dry turning.145 Bilal et al.
studied the effect of deep cryogenic treatment effect on
milling of Inconel-718 with carbide tool at −196⁰C and
observed that cutting force decreased with deep cryogenic
treatment of carbide tool in comparison to milling of
Inconel-718 with untreated carbide tool. The reason
behind that was increased wear resistance of carbide
tool.161 Tripathy et al. did their investigation on micro
milling of Inconel-718 and found better tool wear resist-
ance with cryogenic treatment than untreated tool. They
recorded 53.6% increment in tool life with cryogenic
treatment.142 Jadhav et al. in their research on machining
of Nimonic C-263 found increase in nose and flank wear
which was attributed to high temperature at the machining
zone while machining done with liquid nitrogen recorded
less wear.147
Cicek et al. in their investigation found that the average
resistance to wear of DCT and DCTT (Deep Cryogenic
Proc IMechE Part E: J Process Mechanical Engineering 236(4)
Treatment with Tempering) samples were better than
CHT samples by 12% and 24% respectively as shown
in supplementary Figure 17.116 Finer carbides brought
higher wear resistance which formed in DCTT
sample.33 From supplementary Figure 14, it was observed
that CHT sample has roughest surface with highest wear.
Supplementary Figure 15. showing CHT, DCT and
DCTT samples with coarse, medium and fine carbides
respectively. Cryogenic treatment results in precipitation
of small size carbides.142,162–164 Li et al. observed that
there was decrease in carbon content when DCT per-
formed between Quenching and tempering due to large
soaking time. Highest decrease in carbon content came
by repeating DCT multiple times.165 Upon warming up
to room temperature, the alloying elements finds it diffi-
cult to dissolve due to insufficient energy thus forms
fine carbides once again.166
Doing tempering after DCT resulted in secondary
chromium cabides precipitation which distributed uni-
formly and homogenously in the microstructure as
shown in supplementary Figure 16. DCTT sample had
minimum weight loss due to smallest precipitate size
resulted after tempering while highest weight loss
occured in untreated sample because of large precipitate
size which produced large trace over the surface when
precipitate removed during wear test In untreated
sample, carbide precipitate size found to be 1-2.5 µm
but in cryo treated samples the carbide size significantly
decreased to 0.1 µm.
The interparticle spacing among carbides in cryo
treated samples were less than untreated samples. The car-
bides in untreated sample were distributed randomly but
in cryo treated samples, the ultra-fine carbides distributed
uniformly.
On Mg- 1.5Zn-0.15Gd alloy Yung Liu et al. found that
as the cryogenic cooling time increases, then not only
volume fraction of secondary phase particle increased
but also refinement of particles took place which resulted
in decrease in wear rate.141
Fatigue strength
Fatigue failures are very dangerous, therefore numerous
research are there to increase the fatigue resistance of
the materials. Cryogenic treatment was also attempted
by various researchers to increase the fatigue resistance
of the materials. Zhirafar et al. in their research on cryo-
genic treatment of AISI 4340 steel found increase in
fatigue limit of material due to increase in strength and
hardness.124 Ono et al. conducted research on cryogenic
operation on Inconel-718 and concluded that coarse
nobium enriched carbides were the root cause for initi-
ation of the fatigue crack. Cryogenic treatment helped in
increasing the fatigue strength of the material.143
Presence of intergranular cracks were observed by
Senthilkumar in cryogenic operation on EN31 steel in
conventional and deep cryogenic treatment with temper-
ing. The crack transmitted around the grains surface and
around the carbide particles.125 Yan et al. in their research
Singh and Pandey
on DCT of Cr-Mo-V-Ni steel shown ductile trans-
granualar fracture in the samples subjected to DCT with
tempering at 230⁰C and brittle intergranular fracture on
samples subjected to DCT with tempering at 380⁰C
which was attributed to the combination of large size of
γ grain and cracks. The numbers of dimples decreased sig-
nificantly when tempering was done at 380⁰C.127 Korade
et al. concluded that fine carbides try to locate themselves
in a gap between large carbides and acts as crack resistant
in AISI steel and thus improved fatigue resistance.122
Baldissera et al. concluded that due to nucleation of fine
carbide and conversion of residual stresses there is an
improvement in fatigue resistance.167 Bhavar et al. in
their research on Deep Cryogenic Treatment of
AISIH13 steel found maximum fatigue life for cryogeni-
cally treated sample with soaking time of 32hrs under
−185⁰C and it decreased a little for soaking time of
48hrs. The improvement in fatigue strength was due to
uniform distribution of martensite needles at cryogenic
temperature.117
Weng et al. in their research shown that cryogenically
treated WC-Co (-196⁰C) cemented carbide samples had
higher fracture toughness KIC value as a result there
were a formation of twists and turns during crack propa-
gation as shown in supplementary Figure 18(b). which
directly indicated higher energy consumption in cryogeni-
cally treated WC-20Co cemented carbide samples168 that
made more difficult for crack to propagate in DCT sample
than untreated sample.
Ono et al. studied effect of cryogenic temperature
(4 K) effect on fatigue property of Inconel-718.143 From
results it was concluded that at high stress amplitude
fecets which were acting as crack initiation sites were
enriched with nobium as shown in supplementary
Figure 19(a), (b), (c) and (d) but at low stress amplitude,
no area was detected which was enriched with nobium as
shown in supplementary Figure 19(e). and supplementary
Figure 19(f). but the facet size at low stress amplitude was
larger than high stress amplitude.
It was also found that at low stress amplitude, the facets
were formed through transgranular crack as shown in
supplementary Figure 20(a). From supplementary
Figure 20(b). it was found that crack tear up nobium
enriched carbide which indicated that nobium enriched
carbides are responsible for fatigue failure.
Bensely et al.in their cryogenic treatment on EN353
steel found better improvement in fatigue strength by pre-
cipitating finer carbides rather than coarser carbides.126
Table 4. Carbide content and fracture toughness of different
heat treated AISI H13 steel samples.119
Carbide Content, Fracture Toughness
Heat Treatment Vc (%) MPa√m
HT1 11.2 54.8(±1.7)
HT2 13.7 67.1(±5.7)
HT3 13.4 62.3(±1.5)
HT4 14.5 77.4(±6.6)
1767
Smith in his cryogenic treatment on chrome silicon steel
compression springs noticed higher compressive residual
stresses on spring’s surfaces than untreated spring which
increased the fatigue life.169
Toughness
Toughness is the capacity of material to observe energy
during impact loading and deform plastically without
fracture. Researchers are continuously contributing their
effort to enhance the toughness of materials so that mate-
rials can work effectively in the area of shock and vibra-
tional applications. Bal and Maity studied the effect of
cryogenic cooling on carbide inserts. At 1⁰C/min they
found increase in hardness in inserts but showed decrease
in toughness. Inserts that were cooled at a cooling rate of
0.5⁰C/min showed increase in hardness and toughness.170
Karthikeyan et al.stated that there were formation of
coarse η-phase carbides which were responsible for
decrease in ductility of the tool.132
Effect of tempering on 30CrMnSi steel was studied by
Amini et al. and it was noticed that if tempering is done
between 250⁰C and 500⁰C then the impact strength of
the steel decreases and steel started to become brittle.171
Pacyan. et al. collected results from cold working deform-
ation after hot rolling of structural steel and noticed that
doing cold working after hot rolling causes increase in
strength and decrease in elongation and impact
strength.172 Mukhopadhyay et al. and Sarkar et al. did
their research on toughness on tool steel and found decre-
ment in toughness was a result of carbide cluster distribu-
tion and it also helped in propagating crack.173,174 Ozer
et al. found that with tempering of AISI H13 steel hard-
ness and toughness values decreases.118 Cardoso et al.
observed that during martensite transformation in DCT
there happened increase in volume which affected stress
concentration as a result DCT Samples have higher tough-
ness than CHT samples in AISI D6 tool steel.66
Perez et al. studied four heat treatments on AISI H13
steel with HT1(Air Quenching with tripple tempering),
HT2(Cryogenic treatment at −196⁰C with air quench
and tripple tempering), HT3 (Oil Quenching with tripple
tempering), HT4(Cryogenic treatment at −196⁰C with
oil quench and tripple tempering).119 The carbide
content and fracture toughness results obtained in all the
treatments shown in Table 4. A graph between heat treat-
ment and fracture toughness is plotted as shown in
supplementary Figure 21.
The increase in fracture toughness of HT2 and HT4
found to be 22.5% and 24% in comparison to their
respective treatment without cryogenic cooling HT1 and
HT3. The cooling rate due to different cooling medium
air and oil also played an important role in creating a dif-
fernce in fracture toughness. The fracture toughness for
oil quench sample came higher in comparison to air
quench. The reason behind that is cryogenic treatment
in HT2 and HT4 resulted finer and homogenous distribu-
tion of carbides with an increase in carbide volume frac-
tion which resulted higher fracture toughness than HT1
1768
and HT3 samples. Meanwhile, both HT2 and HT3
(supplementary Figure 22 (b) and supplementary
Figure 22(c) led to intermediate carbide distributions
compared to HT1 and HT4 (supplementary Figure 22(a)
and supplementary Figure 22(d)).
Advantages and disadvantages
Following are the advantages and disadvantages that have
been noticed in Cryogenic treatment of the materials in
comparison to the conventional heat treatment:
Fine and homogenous distribution of carbides due to
cryogenic treatment led to improvement in:
• Wear resistance
• Hardness
• Tensile strength
• Fatigue resistance
• Toughness
Properties obtained at cryogenic temperature were
retained even after bringing back the samples to room
temperature. Although the response that is obtained in
the material’s performance in deep cryogenic treatment
is better than conventional heat treatment but still there
are some issues that a researcher or user may go across.
These are presented below:
• Large operational cost
• Difficult to maintain different cryogenic temperature.
• Difficulty in fabrication of the setup.
Future scope
Due to different composition from one material to
another, it is difficult to find the optimum soaking time
at which maximum improvement in properties can be
obtained. With the development of computational simula-
tion, density functional theory or molecular dynamics will
be an perfect approach to get precise soaking and
warming time in future so that one may get better hardness
without compromising to the ductility and the toughness
of the material. The computational simulation will help
in making the entire treatment economical as it will help
in finding the liquid nitrogen consumption for treatment.
The simulation will also help in determining the time
which a molecule requires to reach the most stable state.
Controlling cooling rate is also one of the major chal-
lenges in the cryogenic field. From literature, the relation-
ship between sample cracking and cooling rate was not
clear. This problem is expected to get solved in future
by more experimental and computational research.
Future prospects
Ni based super alloys are suitable for applications where a
component has to perform under high pressure and tem-
perature. Such applications include blades of the turbine
and nozzles at the jet exhaust. It has been seen from the
Proc IMechE Part E: J Process Mechanical Engineering 236(4)
literature that most of the research on Ni based alloys
has contributed to improve its machinability but a very
less research is available where the cryogenic cooling
effect on other properties of Ni based alloy like hardness,
toughness, fatigue strength and tensile strength are con-
ducted. Combination of cryogenic cooling with number
of tempering cycles may lead to permanent change in
the microstructure which will affect the properties of Ni
based alloy. Doing so may increase life of the component
and increase the performance in the environment where it
is working like in jet engines and turbine blades.
Conclusion
Deep Cryogenic Treatment (DCT) helps in getting mar-
tensite phase from retained austenite and also helps in
making carbon to move out of the lattice. The carbides
that nucleate with DCT are secondary carbides that are
different in size than primary carbides. The secondary car-
bides are smaller in size than primary carbides. When
tempering is done after DCT, these secondary carbides
become much finer and helps in increasing the wear resist-
ance. Fine and homogenous distribution of carbides
makes the material tough and increase the tensile strength.
Wear resistance depends on carbide particles size. Smaller
the particles size higher the wear resistance. For steels, by
increasing the tempering cycles, the hardness decreases.
Soaking time at DCT affects tensile strength and hardness
by conversion of austenite to fine shape martensite lath. In
case of high temperature alloys which were difficult to
machine, after DCT, their machinability improved and
the life of the tool which were used to machine these
alloys increased due to cryogenic cooling of the tool
chip interface. It is also found that in case of cemented
carbide inserts, creation of η-phase carbides during deep
cryogenic treatment, there is significant increase in the
hardness. Reduction of retained austenite results in
increasing the fatigue strength. Also, the nucleation of
fine carbides during deep cryogenic treatment acts as a
disturbing medium to martensite dislocations and don’t
let the crack to propagate and increase fatigue resistance
of the material.
Declaration of conflicting interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of this
article.
Funding
The author(s) received no financial support for the research,
authorship, and/or publication of this article.
ORCID iD
Gurkirat Singh https://orcid.org/0000-0001-8866-5354
Supplemental material
Supplemental material for this article is available online.
Singh and Pandey
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