Cryogenics 41 (2001) 149155

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Cryogenic treatment to augment wear resistance of tool and die steels

D. Mohan Lal *, S. Renganarayanan, A. Kalanidhi
Department of Mechanical Engineering, Anna University, Chennai 600 025, India
Received 1 May 2000; accepted 28 March 2001

Abstract
Cryogenic treatment is a supplementary process to conventional heat treatment process in steels. It is an inexpensive one time
permanent treatment aecting the entire section of the component unlike coatings. Though the benets have been reported widely,
there are issues debated upon, in respect of the treatment parameters, extent of benets experienced in dierent materials, underlying
mechanism and pretreatment conditions. A study on the improvement in wear resistance and the signicance of treatment pa-
rameters in dierent materials has been made. It is found that cryogenic treatment imparts nearly 110% improvement in tool life. It
is even superior to TiN coatings. The underlying mechanism is essentially an isothermal process. 2001 Elsevier Science Ltd. All
rights reserved.

Keywords: Cryotreatment; Wear resistance; Tool steels; Die steels

1. Introduction it is likely to transform into martensite under certain

The freezing of metals has been acknowledged for
many decades as an eective method for increasing
``wear life'' and decreasing residual stress in tool steels
[1]. It is believed that the life of cutting tools get ex-
tended substantially due to cryogenic treatment. Cryo-
genic treatment is an inexpensive one time permanent
treatment aecting the entire section of the component
unlike coatings. The treatment is an add-on process over
conventional heat treatment in which the samples are
cooled down to prescribed cryogenic temperature level
around (93 K) at a slow rate, maintained at this tem-
perature for a long time and then heated back to room
temperature. Researchers have been skeptical about the
process because it imparts no apparent visible change in
the material and the mechanism is also unpredicted.
However a number of aerospace, automotive and elec-
tronic industries in USA, China and other developed
countries have adopted this process in their regular
treatment/production line to improve wear resistance
and dimensional stability of components [2].
In the heat treatment of tool steels the problem of
retained austenite after heat treatment has prevailed
since the development of tool steels. This retained
austenite is soft and unstable at lower temperatures that
*
Corresponding author.
0011-2275/01/$ - see front matter 2001 Elsevier Science Ltd. All rights reserved.
PII: S 0 0 1 1 - 2 2 7 5 ( 0 1 ) 0 0 0 6 5 - 0
conducive conditions. It should be noted that freshly
formed martensite is also brittle and only tempered
martensite is acceptable. To further aggravate this
problem the transformation of austenite to martensite
yields a 4% volume expansion [3] causing distortion
which cannot be ignored. Thus retained austenite should
be alleviated to the maximum possible before any
component or tool is put into service. The degree of
undercooling decides the potential to transform retained
austenite to martensite completely [4]. In this context
cryogenic treatment is handy. It also causes the precip-
itation of nely dispersed carbides in the martensite. It
would be the interest of researchers to quantify the
benets and also know the conditions at which the
treatment derives maximum benets.
This cryogenic treatment being an add-on process to
conventional heat treatment is recommended by many
researchers [46] to be done before high temperature
tempering. However Popandopulo and Zhukova [7]
have recommended high temperature tempering to pre-
cede cryogenic treatment. The treatment temperature is
also debated upon.
The present work is a comparative study on the wear
resistance improvement of cryogenically treated samples
with standard heat treated samples through: (1) Flank
wear test and (2) Sliding wear test. A proprietary cryo-
genic treatment cycle shown in Fig. 1 has been consid-
ered as the reference. The need for lowering down the
150 D. Mohan Lal et al. / Cryogenics 41 (2001) 149155

with TiN and then cryogenically treated. The various

Fig. 1. Cryogenic treatment cycle.
temperature to very low levels has been debated in the
previous literature and hence two more intermediate
temperature levels and soaking times were considered
for the study. Since coatings are sought after nowadays
to improve tribological properties it was found reason-
able to compare the eects of cryogenic treatment with
those of PVD (TiN) coatings also.
2. Experimentation
Standard bar/rod stock available in the market was
procured and samples of the required size were made.
Initially the composition of the samples was conrmed.
The samples were heat treated as per prescribed ASM
standards [8,9]. After conventional quenching some
samples were tempered, some were directly subjected to
cryogenic treatment. After tempering some of the sam-
ples were cryogenically treated while some were left as
such and some were coated with TiN through physical
vapour deposition technique. Some samples were coated
cases considered are listed in Table 1.
Cryotreatment was made immediately after quench-
ing without tempering except in cases 7 and 8. However
always cryotreatment was followed by low temperature
tempering at 423 K. All tempered and cryotreated
samples (cases 7 and 8) were cryotreated after conven-
tional tempering.
Since it was observed from the earlier literature that
cryogenic treatment augments the wear resistance and
life of materials other than steel also, transformation of
retained austenite to martensite cannot be the main
underlying mechanism. Hence it was part of the objec-
tive to study the eect of cryogenic treatment on tool
steel when there is no retained austenite. To avoid re-
tained austenite in the samples, during heat treatment
the lower austenitizing temperature range was selected
for samples to be cryogenically treated [5]. The absence
of retained austenite above 0.1% level after conventional
heat treatment was ascertained through X-ray dirac-
tion pattern studies.
2.1. Flank wear test
The materials considered for this study were M2 and
T1 steels which are normally used for single point cut-
ting tools. D3 steel was also considered to check the
inuence of cryogenic treatment with respect to the
carbon percentage. The tool steel samples were made
into a single point cutting tool with standard tool sig-
nature as given in Table 2 which is the prescribed one to

Table 1
List of treatment conditions considered for wear resistance study
Cases Purpose Nomenclature
followed
1. Hardened and tempered Standard tool for comparing the tool life of cryotreated tools SHT (standard
heat treated)
2. Cryotreated at 93 K for 24 h Cryogenic treatment for tool steels CT (93/24)
3. Cryotreated at 133 K for 24 h To check the eect of lowering the temperature deep below cold CT (133/24)
treatment levels
4. Cryotreated at 163 K for 24 h To check the eect of lowering the temperature deep below cold CT (163/24)
treatment levels
5. Cryotreated at 93 K for 6 h To check the signicance of isothermal holding time at the CT (93/6)
treatment temperature
6. Cryotreated at 93 K for 6 h and quenched in To check the eects of reducing the temperature below 93 K CT (93/6) + LN2 /2
LN2 for 2 h
7. Tempered and cryotreated at 133 K for 24 h To conrm whether tempering is to be done before cryogenic TCT (133/24)
treatment
8. Tempered and cryotreated at 93 K for 24 h To conrm whether tempering is to be done before cryogenic TCT (93/24)
treatment
9. Titanium nitride coated To compare the benets of cryogenic treatment with that of surface TiN
coatings
10. Cryotreated (CT (93/24)) and then coated To compare the benets of cryogenic treatment with that of surface CT + TiN
with Titanium coatings
11. Titanium nitride coated and then cryo- To compare the benets of cryogenic treatment with that of surface TiN + CT
treated (CT (93/24)) coatings
 D. Mohan Lal et al. / Cryogenics 41 (2001) 149155 151

Table 2 30 min in every given condition. After making the set-

Tool signature for ank wear test ting, the wheel-setting was checked for atness using a
Back rake angle 0 vernier dial gauge of 0.01 mm accuracy. The samples
Side clearance angle 6 were randomly selected to avoid any biased conditions
Top rake angle 8
End clearance angle 6
and the test was conducted totally for 10 number of M2
Cutting edge angle 90 samples and 15 number of D3 samples. The samples
Nose radius 0 mm were more in number for D3 as much variation was
observed. The average of all the samples was taken as
avoid built-up edge. This was subjected to turning op- the observed value in each case.
eration in a high speed lathe following the machining The observations of the above tests are discussed in
specications given in Table 3. In all test cases a mini- the following paragraphs. A test of statistical signi-
mum of three identically treated samples were consid- cance for the observations in sliding wear test was also
ered to check the repeatability and the average is taken conducted.
as the observed value.
As soon as the lathe was started a stop watch was
switched on to note down the machining time. At the 3. Results and discussion
end of every run before new depth of cut was set the
ank wear was measured in a toolmaker's microscope. All attempts made in this research were towards in-
The above procedure was repeated until the ank wear vestigation of the eects of cryogenic treatment to aug-
exceeded 0.4 mm. The total machining time before ment wear resistance. The observations and ndings are
reaching 0.4 mm ank wear was considered to be the discussed here.
tool life of the sample. The ank wear was normally
observed at every 10 min interval and in some cases at 3.1. Flank wear test
lesser time interval also depending upon the wear rate
experienced. Fig. 2 shows the ank wear observed in M2, D3 steels
subjected to dierent cases of cryogenic treatment in a
2.2. Sliding wear test ank wear test. Fig. 3 shows the ank wear experienced
by cryogenically treated samples as compared to TiN-
The materials considered for this test are D3 and M2 coated tools. However the dierent cryogenic treatment
samples which are used for dies and punches, respec- cases were restricted to M2 and D3 steel samples only. It
tively. A pin on disk wear test was conducted as per could be seen that cryotreatment (CT (93/24)) yields
ASTM guidelines [10]. The sample was made as the pin 110.2% improvement in T1 steels as compared to SHT
(with 5 mm diameter and 25 mm length) and a grinding tool samples. The life of the tool was found to increase
wheel of 50 mm diameter was chosen as the disk. The due to cryogenic treatment [CT (93/24)] irrespective of
test setup can cause either the disk or the pin to revolve the material. It has imparted 86.6% and 48% improve-
about the disk centre. The pin can be loaded at the top
to press against the disk. The speed of revolution also
can be varied and thus the test can be conducted with
the following parameters:
1. load;
2. speed;
3. sliding distance.
Three tracks viz. at 45, 35 and 25 mm PCD were set on
the grinding wheel and three loads viz. 20, 30, 50 N were
considered with each one corresponding to a particular
track. Three specic linear sliding speeds were also
considered for each load condition. The sliding distance
was also varied by continuously running for 10, 20 and

Table 3
Machining specications for ank wear test
Cutting velocity 30 m/min
Feed 0.13 mm/rev
Depth of cut 0.50 mm
Cutting method Dry (without coolant)
Fig. 2. Flank wear versus machining time for dierent cases of cryo-
Work piece material Mild steel rod
genic treatment.
152 D. Mohan Lal et al. / Cryogenics 41 (2001) 149155
Fig. 3. Flank wear versus machining time for dierent cases.
ment in M2 and D3 steels, respectively, as compared to
SHT tool samples. However the improvement was
maximum in T1 type which may be attributed to the
tungsten alloying carbides present in the material which
is exclusively meant for single point cutting tools.
3.2. Comparison of dierent cryotreatments considered
As discussed earlier whether a tempered tool when
cryogenically treated can yield positive results is an
interesting aspect. It could be seen from Fig. 2 that
TCT (93/24) has imparted 69% and 33.9% improvement
whereas CT (93/24) has imparted 86.6% and 48% im-
provement on M2 and D3 steels, respectively. Hence
tempering before cryotreatment is not desirable as
compared to cryotreatment directly after conventional
quenching. This can be attributed to the stabilization of
carbides and microstructural phases during tempering
process which inhibits further transformation during
cryogenic treatment. However it is apparent that this
could be overcome by higher degree of undercooling as
explained below. The tempered M2 samples subjected
to CT (133/24) have only 13.3% improvement whereas
those tempered and subjected to CT (93/24) have 69%
improvement which may improve further if cooled be-
low 93 K. Although M2 samples subjected to CT (133/
24) after tempering have 13.3% improvement, D3
samples suer from a loss in tool life of 19.6% which
may be due to the higher percentage of carbon that
requires higher degree of undercooling to overcome any
stabilization eects. Thus from the present study it is
inferred that it is desirable to avoid tempering before
cryotreatment. Since the cryogenic treatment itself is
done at a very slow rate (cooling and heating) it itself
relieves the brittleness and stresses accumulated. How-
ever low temperature tempering at 423 K after cryo-
genic treatment is done to relieve any brittleness
remaining.
3.3. Cryogenic treatment and TiN coating compared
The eects of TiN coating on cryotreated tools and
cryotreatment on TiN-coated tools are also presented in
Fig. 3. TiN coating imparts 48.4%, 42% and 41% im-
provement while cryogenic treatment imparts 110.2%,
86.6% and 48% in T1, M2 and D3 steels, respectively.
Thus it is observed that cryotreated tools outperform
TiN-coated tools, while the cost of TiN coating and
cryogenic treatment are 25% and 10% of the tool cost,
respectively.
In T1, M2 and D3 samples CT + TiN yields a life
improvement of 205.3%, 153% and 146% for T1, M2
and D3 steels, respectively, while TiN coating followed
by CT yielded an improvement of only 104% and 109%
in M2 and D3 steels, respectively. Hence the eect of
cryotreatment on TiN coating is not favourable as it has
resulted in shorter tool life. This may be because of the
uneven contraction during cryotreatment of the coating
material and the substrate leading to incipient cracks at
the interface. Hence cryogenic treatment should not be
done after TiN coating.
Cryotreatment in combination with TiN coating
works extremely well with multiplied tool life before
regrinding. However after rst regrinding the tool will
perform as a cryotreated tool, as the coating will be lost
while regrinding. In this context since cryogenic treat-
ment aects uniformly the entire cross-section of the
tool the same wear life can be expected even after any
number of regrinding. It is evident that cryogenic
treatment imparts better wear resistance throughout the
section and hence it is superior to any coating as coat-
ings are made for few microns only.
3.4. Sliding wear test
The wear of any tool is a complex function of load
and speed. Hence these two variables were considered
for the study and the wear resistance has been calculated
as a non-dimensional parameter incorporating the load,
the velocity of slide, the volume loss/s and the Vickers
hardness [11] as follows:
WR FV =WHv ;
 D. Mohan Lal et al. / Cryogenics 41 (2001) 149155
where, `WR' is the wear resistance, F is the load in
Newtons, V is the linear velocity in m/s, W is the volume
loss of material in m3 =s due to wear, and Hv is the
Vickers hardness in N=m2 .
In this, the other cases of cryogenic treatment are also
included for discussion.
Figs. 4 and 5 show the comparison of wear resistance
improvement observed in M2 and D3 steels, respec-
tively, for dierent cryogenic treatment conditions.
The percentage change in wear resistance imparted
by various treatment conditions with respect to SHT
sample has been studied and in general, it is seen that
the wear resistance improvement through cryogenic
treatment is phenomenal at higher speeds in almost all
cases. The wear resistance of the various cases con-
sidered by and large falls in the following decreasing
order:
1. CT (93/24);
2. TCT (93/24);
3. CT (133/24);
4. CT (163/24);
5. CT (93/6 + LN2 /2);
6. SHT;
Fig. 4. Variation of wear resistance with velocity for dierent cases
(D3 steels).
153
7. CT (93/6);
8. TCT (133/24).
The samples treated at 93 K for 6 h and subsequently
dipped in liquid nitrogen have wear resistance almost
closer to those treated at 163 K for 24 h. It is also ob-
served that treatment at 163 K for 24 h has reasonably
comparable results at lower load (20 N). As the load
increases in M2 steel the improvement in wear resistance
due to cryotreatment [CT (163/24)] also increases and it
is observed to be phenomenal in the case of 50 N load at
higher velocities.
In the case of CT (133/24) the eects are marginal for
D3 steel at 20 and 30 N load condition whereas at 50 N
load the eects are reasonably good. However the im-
provement in M2 steel is good by and large for all
conditions. Hence from the stand point of economy the
above treatments CT (163/24), CT (133/24) can be
considered for D3 steel at higher loading conditions and
in all conditions for M2 steels.
Other cases considered, namely cryotreatment [CT
(93/6)] and [CT (93/6 and LN2 /2)] do have a very mar-
ginal drop (or) increase in life when compared with SHT
samples. Hence it could be inferred that such treatments
Fig. 5. Variation of wear resistance with velocity for dierent cases
(M2 steels).
154 D. Mohan Lal et al. / Cryogenics 41 (2001) 149155

are of no use for these steels. Making a cross-reference
to the ank wear test it can be understood that 6 h of
soaking is insucient for cooling at 93 K as experienced
in cold treatment at 213, 203 and 193 K (which required
a minimum of 0.5, 1 and 2 h of soaking time, respec-
tively, for positive results).
It is also inferred that cryogenic treatment in LN2 (77
K) for 2 h following CT (93/6) has also imparted some
improvement which indicates that lowering down the
temperature below 93 K also has an eect which may
continue even below 77 K. However, the source of re-
frigeration will be a problem. It could be also inferred
that the wear resistance improvement process whatever
may be the mechanism is an isothermal process which
requires long periods such as 24 h or more which de-
pends on the soaking temperature. Samples treated at
163 K for 24 h showed marginal improvement in the
wear resistance but were better than samples treated at
93 K for 6 h. This suggests that soaking time is more
important than the lowering of temperature. This rein-
forces the idea that the improvement is predominantly
based on some isothermal process which may be mar-
tensitic transformation or precipitation of ne alloying
carbides.
TCT (133/24) did not yield favourable results while
TCT (93/24) yielded comparable results though not
equal as the CT (93/24) case. This shows that the sta-
bilization of phases that would take place during tem-
pering requires a sucient degree of undercooling and
time to get transformed to stable harder/tougher phases
that oer better wear resistance.
To check the statistical signicance of the im-
provement in cryogenic treatment a test for signi-
cance was made on the wear resistance calculated
from the observations. The calculated values and
levels of signicance are tabulated in Table 4. It could
be seen that the improvement in CT (93/24) is statis-
tically signicant at 95.5% level for both M2 and D3
steels.
4. Conclusions
This work was carried out with the background of
diverse claims and reports in terms of property im-
provement towards enhanced tool life and possible
reasons suggested for the same by previous researchers.
Based on the investigations the following conclusions
are drawn:
1. Untempered samples when cryogenically treated
yield 3%, 10% and 10.6% extra life over tempered
and cryogenically treated T1, M2 and D3 samples,
respectively. Hence it is desirable to cryogenically
treat without tempering.
2. Tempered samples when cryotreated at 133 K for
24 h yielded negative results, but when cryotreated
at 93 K for 24 h the results were favourable. Hence
tempered samples if treated at still lower tempera-
tures may yield still better results on par with un-
tempered cryotreated samples. This also suggests
to conclude that the stabilization of phases that
would take place during tempering requires su-
cient degree of undercooling and time to get trans-
formed to stable harder/tougher phases that oer
better wear resistance.
3. Cryogenic treatment done at 93 K as per the pre-
scribed cycle yields 20% extra life as compared to
the maximum life achieved through cold treatment.

Table 4
Results of statistical test for signicance
Specimen Testing condition, load/velocity Standard heat treated (SHT) Cryogenically treated [CT (93/24)]
Average wear resistance [X ] X 2r Average wear resistance
D3 20 N/0.32 m/s 172.6082 187.2383 211.6253
20 N/0.49 m/s 182.93 206.7252 223.2101
20 N/0.66 m/s 215.8256 267.2452 293.0401
30 N/0.25 m/s 160.8256 172.209 188.5049
30 N/0.381 m/s 207.5232 232.2132 262.485
30 N/0.513 m/s 236.0576 265.9599 276.2411
50 N/0.18 m/s 75.46281 85.3695 163.339
50 N/0.272 m/s 77.08347 79.238 211.8152
50 N/0.366 m/s 91.88877 97.018 209.3221

M2 20 N/0.32 m/s 3624.565 4580.606 5047.305

20 N/0.49 m/s 3629.82 4891.659 4953.365
20 N/0.66 m/s 3065.886 3415.341 5023.397
30 N/0.25 m/s 1787.374 2366.939 4193.299
30 N/0.381 m/s 2398.99 2699.17 3616.413
30 N/0.512 m/s 3097.166 3444.804 4937.116
50 N/0.18 m/s 3686.359 5006.21 5249.851
50 N/0.272 m/s 4175.855 4896.093 4952.512
50 N/0.366 m/s 4371.603 4738.78 5313.115
 D. Mohan Lal et al. / Cryogenics 41 (2001) 149155
4. Cryogenic treatment [CT (93/24)] is superior to TiN
coatings also.
5. The eect of cryotreatment on TiN coating is not fa-
vourable which may be because of uneven contrac-
tion of the coating material and the substrate
leading to incipient cracks at the interface. Hence
cryotreatment should not follow TiN coating.
6. TiN coating in combination with cryotreatment pro-
vides 45% extended tool life than cryotreatment
alone. However after rst regrinding the tool will be-
have like a cryogenically treated tool only.
7. Comparing the results of CT (93/6) and CT (93/24) it
could be concluded that the mechanism causing im-
provement in wear resistance/tool life is essentially
an isothermal process.
8. Samples treated at 163 K for 24 h [CT (163/24)] were
better than samples treated at 93 K for 6 h [CT (93/
6)]. Hence soaking time is more important than low-
ering the temperature. The above two conclusions
reinforce the idea that the improvement is predomi-
nantly based on some isothermal process.
9. With reference to the sliding wear test it is observed
that cryogenic treatment imparts better red hardness
for D3 steel than for M2 steel.
10. A statistical test of signicance on the levels of im-
provement in wear resistance shows that the improve-
ments experienced in CT (93/24) and TCT (93/24)
are signicant at 95.5% level, as shown in Table 4.
155
Acknowledgements
The authors acknowledge the help rendered by M/S
Tribiology India Limited, Chennai in carrying out the
cryogenic treatment for the samples.
References
[1] Pete P. Frozen gears. Gear Technol 1993;(March/April):269.
[2] Pillai RM, Pai BC, Satyanarayana KG. Deep cryogenic treatment
of metals. Tools Alloy Steels 1986;(June):2058.
[3] Avner SH. Introduction to physical metallurgy. New York:
McGraw-Hill; 1982.
[4] Moore K, Collins DN. Cryogenic treatment of three heat treated
tool steels. Key Eng Mater 1993;86&87:4754.
[5] Bayer HE. Can I benet from the use of low temperature
treatment?. Steel Process 1953:5028.
[6] Vaccari JA. Deep freeze improves products. Amer Machinist
Automated Manuf 1986;(March):901.
[7] Popandopulo AN, Zhukova LT. Transformation in high speed
steels during cold treatment. Metal Sci Heat Treatment
1980;22:70812.
[8] ASM, Principles and practices for iron and steel, heat treaters
guide. 2nd ed., 1995.
[9] ASM, Tool steels properties and selection, metals hand book,
vol. 3, 1990, pp. 42147.
[10] ASTM, Standard test method for wear testing with a pin-on disk
apparatus, G99-95, vol. 14-02, 1995, pp. 3869.
[11] Barron RF. Do treatments at temperature below 120 F help
increase the wear resistance of tool steels? Here are some research
ndings that they do. Heat Treating 1974;(June):147.