Wear 302 (2013) 854862

Contents lists available at SciVerse ScienceDirect

Wear
journal homepage: www.elsevier.com/locate/wear

Effects of the sub-zero treatment condition on microstructure, mechanical

behavior and wear resistance of W9Mo3Cr4V high speed steel
X.G. Yan a,b,n, D.Y. Li b
a
b

School of Mechanical Engineering, Taiyuan University of Science and Technology, Taiyuan, Shanxi 030024, China
Department of Chemical and Materials Engineering, University of Alberta, Edmonton, Alberta, Canada T6G 2G6

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 2 September 2012
Received in revised form
12 December 2012
Accepted 14 December 2012
Available online 7 January 2013

The sub-zero treatment can improve mechanical properties and wear resistance of many metallic
materials and the improvement is largely affected by the sub-zero treatment condition. In this study,
samples of W9Mo3Cr4V (W9) high speed steel (HSS) were treated at various sub-zero temperatures
before and after tempering, respectively. The main objective of this work is to investigate the effect of
the sub-zero treatment condition on mechanical properties and wear resistance of the W9 HSS and
correlate it to variations in microstructure. Microstructures of the treated samples were characterized
with electron microscopy (SEM and TEM), and corresponding properties, including hardness, impact
toughness and wear resistance, were evaluated. It was demonstrated that the mechanical properties of
the cryogenically treated samples were superior to those of conventionally treated ones. The
cryogenically treated samples with subsequent tempering performed better than cryogenically treated
samples that experienced prior tempering. The lower temperatures for sub-zero treatment were more
effective in improving the mechanical properties. The life of W9 HSS taps in cutting 30CrMnTi steel was
assessed, which showed a trend similar to that observed during wear testing. Efforts are made to clarify
possible mechanisms responsible for the improvements.
& 2013 Elsevier B.V. All rights reserved.

Keywords:
Sub-zero treatment
W9Mo3Cr4V
Microstructures
Mechanical properties
Heat treatment

1. Introduction
The sub-zero treatment is a well-known and an effective
method to improve dimensional stability [1], fatigue behavior
[2], toughness [37] and wear resistance [829], which is commercially used to improve the performance of many metallic
materials for decades. The sub-zero treatment is the process of
cooling a material to sub-zero temperatures, which are classied
into three different temperature ranges: cold treatment (CT,
Z193 K), shallow cryogenic treatment (SCT, 193113 K) and deep
cryogenic treatment (DCT, 11377 K) [20]. These treatments can
be carried out using cryogenic equipment with liquid nitrogen, or
industry refrigerator, or processes with ice, depending on the
temperature range.
The service life of cutting tools is crucial for increased
productivity and thus an important economic factor. High speed
steel (HSS) is one of important tool materials used in the industry,
which was developed more than a century ago and has been
continuously improved for applications as a wear-resistant material
for drills, taps, milling cutters, broaches, slotting tool and hobs.
n
Corresponding author at: School of Mechanical Engineering, Taiyuan University of
Science and Technology, Taiyuan, Shanxi 030024, China.
Tel.: 86 351 6998483.
E-mail addresses: yan_xg2008@126.com, yanxianguo@hotmail.com (X.G. Yan).

0043-1648/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.wear.2012.12.037

In recent decades, great efforts were made for considerably

improved fatigue behavior, toughness and wear resistance of HSS
using the sub-zero treatment. Leskovsek et al. [11] investigated the
Inuence of deep-cryogenic treatment procedure on the wear
resistance of HSS and showed that different cryogenic treatment
procedures resulted in different combinations of hardness and
fracture toughness, leading to an order-of-magnitude difference in
the wear resistance of samples under study. Extensive studies were
conducted to investigate effects of various sub-zero treat parameters on properties of various steels. Kalin et al. [12] reported that
the subsequent tempering after cryogenic processing did not show
signicant impact on the fracture toughness of M2 high speed steel.
However, Kelkar et al. [13] studied M2 steel samples experienced
various combinations of hardening, cryo-treatment and triple
tempering, and observed that the cryo-treatment followed by
tempering eliminated residual strain to a large degree, which is
benecial to the fracture toughness. By coupling the deep cryogenic
treatment with conventional vacuum heat treatment, Pellizzari
et al. [15] reduced the wear rate of AISI-M2 HSS up to 42%. Dhokey
et al. [28] related hardness, carbide density, impact toughness and
compressive residual stress with wear rates for M35 HSS specimens
which were hardened at 1473 K, triple tempered at 673 K, cryosoaked at 88 K for 448 h and soft tempered (373 K) and revealed
inuences of these factors on wear rates. Their results show that the
wear rate is dramatically reduced by 90% after soaking for 16 h. Gill

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

et al. [29] studied mechanical properties and wear behavior of the

AISI M2 HSS and their dependence on microstructure, which was
changed by cryogenic treatments at two levels,153 K (shallow
treatment) and 77 K (deep treatment), prior to double tempering(423 K).The improvement in wear rate by deep cryogenic treatment is signicantly higher than that achieved by shallow
cryogenic treatment. Many studies have demonstrated that an
appropriate combination of soaking temperatures and tempering
treatment, mechanical and tribological properties of high speed
steels can be signicantly improved [7,8,10,23,26,30,31].
Applications of cryogenic treatment to HSS cutting tools have
been largely increased in recent years due to its effectiveness in
stress relieving and prolonging the tool life. Silva et al. [10]
reported that M2 HSS twist drills life increased from 65% to
343% when used to drill steels, taking the catastrophic failure of
tools as the criterion for determining the tool service life.
Firouzdor et al. [33] reported 77% and 126% improvement in
drilling life of M2 steel by cryogenic treatment and cryogenictempering treatment, respectively. Yan et al. [34] suggest that the
effect of soaking temperature on the properties of drill is the rst
factor, the soaking time is the second factor, and the cooling rate
is the third. Adem et al. [35] studied tool lives of cryogenically
treated M35 HSS drills for drilling AISI 304 SS and AISI 316 SS and
showed 32% and 14% improvements, respectively. One of the
present authors studied tool lives of cryogenically treated W9 HSS
taps and obtained very promising results [36]. All these studies
indicate that the improvement in the performance of HSS is
largely affected by the cryogenic treatment condition. It is clear
that an optimized combination of soaking temperature, soaking
period, cooling rate, and subsequent tempering would maximize
the benet of sub-zero treatment with an appropriate balance
between cost and material performance.
In this study, samples of W9 HSS were treated respectively at
different soaking temperatures (193 K, 153 K, 113 K and 77 K)
before and after tempering. The main objective of this work is to
investigate the combined effects of the soaking temperature and
tempering order on mechanical properties and wear resistance of
the W9 HSS, and to correlate the effects to variations in microstructure of the material.

855

subsequent and prior, respectively. Sub-zero treatment soaking

temperatures were 193 K (CT), 153 K (SCT), 113 K (DCT) and 77 K
(DCT), respectively. The samples were cooled to soaking temperatures
at a cooling rate of 270 K/min and held at the same temperature for
4 h, then allowed to warm at room temperature in ambient air. For
sub-zero treatments with subsequent tempering, heat treatment
procedure was austenitizingquenchingsub-zero treatment,
followed by tempering at 833 K for 1 h. Whereas the sub-zero
treatments with prior tempering, heat treatment procedure was
austenitizingquenchingtriple tempering at 833 Ksub-zero
treatment. Since most of residual austenite had transformed to
martensite in high-speed steel after cryogenic treatment [10,17],
there was rarely residual austenite left in sample, so only one-time
tempering was arranged in the present study, which would help
reduce the cost for treating W9 HSS. The soaking time affects the
consumption of liquid nitrogen for the sub-zero treatment. The longer
soaking time, the higher cost of the sub-zero treatment. Considering
the cost and previous experience [9,14,21,25,37], the soaking time
was set as 4 h. In order to avoid thermal shocks from rapid cooling
and heating, average cooling rate was controlled at 270 K/min and the
samples then were warmed in ambient air to the room temperature.
The sub-zero treatment was carried out in a home-made cryogenic
treatment set-up (Fig. 1). The DCT was performed by direct liquidnitrogen soaking at 77 K. In order to distinguish the samples
experienced different processes, these treatment procedures under
study are listed in Table 2 and denoted differently.
2.2. Hardness and impact toughness measurements
Rockwell-C hardness (HRc) of differently treated samples was
measured using a Rockwell hardness tester. The average hardness
value of each sample was determined by averaging hardness
values measured at ve different points that were evenly distributed along the diagonal of the sample having dimensions of
10  10  5 mm3.
Impact toughness test was performed on a JBN-300B Drop
Weight Impact Tester. The dimensions of specimens were
10  10  55 mm3. Each test was repeated three times. The tests
were carried out at the room temperature.
2.3. Microstructural analysis

2. Materials and methods

2.1. Material and treatments
Commercial W9 HSS (composition is given in Table 1) was used
for the present investigation. W9 HSS samples experienced conventional treatment (CONT), cold treatment (CT), shallow cryogenic
treatment (SCT) and deep cryogenic treatment (DCT) in separate
batches, respectively. The CONT included the following steps. Samples
were rst preheated at 10231073 K for 3 min, followed by second
preheating at 11731223 K for 3 min, austenitized at 1503 K for
1.5 min, and stage cooling at 853893 K for 1.5 min. The samples
were then quenched in gas to room temperature. Final triple
tempering was carried out at 833 K for 1 h, respectively. Gas
quenching and tempering were performed in a vacuum furnace.
Other treatment procedures included sub-zero treatments with

Thin foils for transmission electron microscope (TEM) analysis

were prepared. W9 HSS rods were cut into thin slices with
a diamond saw, and then polished to about 100 mm, followed

Table 1
Chemical composition of W9.
Chemical composition [Wt%]
C

Mo

Cr

Mn

Si

0.81

9.25

3.10

3.92

1.35

0.30

0.35

r0.03

r 0.03

Fig. 1. Cryogenic treatment set-up used for the present study.

856

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

Table 2
Different heat treatments and sample codes.
Sample
code

Various kinds of heat treatment cycle

CONT
CT
SCT
DCT1
DCT2
CT-1

Quenching
Quenching
Quenching
Quenching
Quenching
Quenching
(193 K)
Quenching
(153 K)
Quenching
(113 K)
Quenching

SCT-1
DCT1-1
DCT2-1

(1503 K) triple tempering (833 K)

(1503 K) subzero (193 K) tempering(833 K)
(1503 K) subzero (153 K) tempering(833 K)
(1503 K) subzero (113 K) tempering(833 K)
(1503 K) subzero (77 K) tempering(833 K)
(1503 K) triple tempering (833 K) subzero
(1503 K) triple tempering (833 K) subzero
(1503 K) triple tempering (833 K) subzero
(1503 K) triple tempering (833 K) subzero (77 K)

by nal polishing in an electrolytic jet-polisher. The electrolyte

consisted of perchloric acid (62 mL), ethanol (700 mL), butyl
cellosolve (100 mL), and distilled water (137 mL). The jet polishing was performed at a temperature between  20 and 10 1C at
a voltage of between 20 and 25 V with a current of 10 mA. TEM
observations were carried out in a Hitachi H-800 electron microscope operated at 300 kV.
Samples for scanning electron microscope (SEM) examination
were prepared, which were cut from heat treated W9 HSS taps by
wire-cut electric discharge machining. The specimens were
grounded and polished using SiC abrasive papers of different grit
sizes (80-1200) to make surface free from scratches. Final polishing was done on velvet cloth polishing machine with sporadic
application of ne alumina dust. The surface roughness of all the
samples was about 0.01 mm. Nital with composition of concentrated nitric acid (4 mL) with ethyl alcohol (100 mL) was used for
revealing microstructure of the W9 HSS specimens. SEM observations were carried out in a ZEISS EVO MA15 electron microscope
operated at 20 kV. SEM observations of impact rupture were
carried out in a Hitachi H-4300 electron microscope operated at
15 kV.
The microstructure of HSS generally consists of carbide particles in a matrix of tempered martensite. The carbide particles are
classied as primary carbides (PCs: size45 mm) and secondary
carbides (SCs: size r5 mm), which are further sub-classied as
large secondary carbides (LSCs: 1 mm osizer5 mm) and small
secondary carbides (SSCs: size r1 mm) [22]. In this study, quantitative analysis of the carbides was done using Image-Pro Plus
version 6.0 software.
2.4. Sliding test
Sliding wear tests were performed using a MM200 block-onring wear tester (Wuzhongshi Material Tester Ltd., China). Fig. 2
illustrates the testing system, in which a counter-part wheel
rotates to wear the sample under a xed load. The wheel of
40 mm in diameter was made of GCr15 steel (equivalent to AISI
E52100) with its hardness equal to HRC 64 and roughness
Ra o0.5 mm. The dimensions of samples were 30  7  6 mm3,
which were grounded using a SiC grinding wheel of a surface
grinding machine. The sample surface roughness was about
0.4 mm and all samples were cleaned with acetone and dried
with compressed air before testing. The wear tests were performed under a load of 100 N in dry sliding condition at the room
temperature. During testing, the wheel rotated at a speed of
200 r/min. Each sample was worn for 2 h.The wear rate of each
sample was calculated from the weight loss and the each test
was repeated three times in order to obtain an average wear rate.
The amount of wear loss of a sample was determined by

Fig. 2. Schematic diagram of the block-on-ring sliding wear testing system.

Fig. 3. Schematic diagram of the tapping testing system.

measuring its weight before and after the test using a precision
electronic weighing balance having its accuracy equal to 1 mg.
Relative wear resistance is used to rank samples in terms of the
were behavior (the relative wear resistance is dened as the ratio
of wear loss of a sample experienced a sub-zero treatment to that
experienced conventional heat treatment).
2.5. Tapping test
Tapping tests were performed using a TH6563  63 horizontal
boring and milling machine system. In this apparatus, a tap
rotates and moved inside a xed workpiece as illustrated in
Fig. 3. Taps of W9 HSS were treated respectively using the heat
treatment processes listed in Table 2. Diameter of taps was
24 mm and the dimensions of workpiece were 700  500 
48 mm3 with its hardness equal to HB210. Before testing,
30CrMnTi steel blocks (steel of the workpiece) were ground to
eliminate adverse effects of surface defects on the work piece. An
emulsion of mineral oil at 5% of concentration was used as the

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

cutting uid and applied at a rate of 5 l/min. The cutting speed

was 7.5 m/min. The hole length was 48 mm. Tool wear was
measured using a ZGISS optical microscope at X50 magnication.
The end of tool life criterion was the catastrophic failure or the
maximum ank wear value (VBBmax 1.2 mm) or medium value
(VBB 0.6 mm). VB was the width of ank wear scar at the border
of the ank. Based on the criterion, the tool life was determined
by the number of holes machined before the tool failed. VBBmax
and VBB were frequently measured in order to have continuous
control in order to monitor the wear development. The frequency
of tool wear measurement was determined based on the severity
of the testing condition.

3. Results and discussion

3.1. Microstructure
Fig. 4(a) presents a SEM micrograph of A CONT sample
(conventionally treated). Fig. 4(b), (d), (f) and (h) are SEM
micrographs of samples experienced sub-zero treatment at
193 K,153 K,113 K and 77 K, respectively, with subsequent tempering (at 833 K). Fig. 4(c), (e), (g) and (i) are SEM micrographs of
samples experienced subzero treatment with prior tempering
(833 K) at 193 K,153 K,113 K and 77 K, respectively. These micrographs exhibit non-uniform distribution of primary carbides and
fairly uniform distribution of secondary carbides in a tempered
martensite matrix with resolved prior austenite grain boundaries.
Large, irregular white regions represent primary carbides (marked
by PCs) as shown in Fig. 4. The amount, size and distribution

857

of the primary carbides appear identical irrespective of the type of

heat treatment; this is expected because the characteristics of the
primary carbides are controlled only by the time and temperature
of austenitization [22,28], which were constant for the present
study. SEM micrographs in Fig. 4 show that there are two types of
secondary carbides, tiny white patches (marked by SSCs) and
small white regions (marked by LSCs), which are classied as
large and small secondary carbides based on their sizes [21,22].
Das et al. [32] reported that the sub-zero treatments did not alter
the nature of primary and secondary carbides; thus, the white
carbide particles should be MC and M6C [11,30,38]. The volume
fraction of the secondary carbides, specically small secondary
carbides, is inuenced by the heat treatment condition. It appears
that the volume fraction of secondary carbides increases with
decreasing temperature of sub-zero treatment. Similar observations were reported by Das et al. [22] for D2 steel and Gill et al.
[28] for M2 steel. Besides, the sub-zero treatment with prior
tempering led to less increase in the volume fraction of secondary
carbide particles, compared to the sub-zero treatment with
subsequent tempering. Quantitative information on the volume
fraction of carbides corresponding to different sub-zero treats
obtained from SEM observation is presented in Fig. 5, which gives
the number of carbides per unit area samples experienced
different treatments. Relative to the CONT sample, samples
experienced sub-zero treatments show increased amounts of both
small and large secondary carbides. The deep cryogenic treatment
resulted in larger increase in the amount of secondary carbides
than either the cold treatment or the shallow cryogenic treatment. Furthermore, the sub-zero treatment with subsequent
tempering generated more secondary carbides than that with

Fig. 4. SEM micrographs of samples experienced different heat treatment processes. The microstructure of the W9 HSS samples generally consists of a matrix of tempered
martensite and carbides, including primary carbides (PCs: size 45 mm) and secondary carbides (SCs: sizer 5 mm), which are further sub-classied as large secondary
carbides (LSCs: 1 mm o sizer 5 mm) and small secondary carbides (SSCs: size r 1 mm): (a) SEM micrograph of CONT; (b) SEM micrograph of CT; (c) SEM micrograph of
CT1; (d) SEM micrograph of SCT; (e) SEM micrograph of SCT1; (f) SEM micrograph of DCT1; (g) SEM micrograph of DCT1-1; (h) SEM micrograph of DCT2; (i) SEM
micrograph of DCT2-1.

858

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

Fig. 5. Quantitative information on the volume fractions of carbides in samples experienced different sub-zero treatments. The volume fraction of carbides is represented
by the number of carbides per unit area: (a) sub-zero treatment with subsequent tempering; (b) sub-zero treatment with prior tempering.

Fig. 6. TEM micrographs of the martensite twinning morphologies in two different samples: (a) TEM micrograph of CONT; (b) TEM micrograph of SCT.

prior tempering, particularly the increase in the amount of small

secondary carbides as Fig. 5 illustrates.
Fig. 6(a) is a TEM micrograph of martensite twinning in a
conventionally treated sample, and (b) is a TEM micrograph of a
sample experienced shallow cryogenic treatment with subsequent tempering. Both the samples have twinned martensitic
matrixes. In CONT samples, martensite twinning is less and the
twin width is about 50 nm. While in the sample experienced the
shallow cryogenic treatment, martensite twinning is more and
ner with the twin width in the range of 20 nm. The ner
twinning structure generally elevates the strength of the material.
Fig. 7(a) presents a TEM micrograph of martensite in a
conventionally treated sample, and (b) a TEM micrograph of a
sample experienced shallow cryogenic treatment (153 K) with
subsequent tempering. In the conventionally treated sample, lath
martensite arrays are less ordered and lath is thick. While in the
samples experienced shallow cryogenic treatment, the lath martensite arrays are ordered with ner lath. There are many tiny
black patches (marked as SSCs) in tempered martensite matrix
lath of sample experienced the shallow cryogenic treatment with
subsequent tempering, which are small secondary carbide
precipitates.
These observations clearly reveal that the cryogenic treatment
rened the secondary carbides, increased their amount and
population density, and led to the formation of a more homogeneous and rened microstructure.
3.2. Variation of hardness
Fig. 8 illustrates results of hardness tests (HRC) on samples
experienced different heat treatment. As illustrated, the sub-zero
treatment with subsequent tempering is more effective in

strengthening the material than that with prior tempering.

For sub-zero treatments with subsequent tempering, SCT W9
HSS samples show signicantly higher hardness than CONT
samples. The increase in hardness of DCT1 and DCT2 samples is
trivial when compared with that of the SCT sample. The shallow
cryogenic treatment boosted the sample hardness due to near
complete transition of soft retained austenite to relatively hard
martensite. However, when the sample was subjected to deep
cryogenic treatment, no further marked improvement in hardness
was observed as compared to SCT sample, since the deep
cryogenic temperature produced smaller secondary spherical
carbides, which could be more benecial to the fracture toughness but may not lead to signicant improvement in hardness. For
sub-zero treatments with prior tempering, the improvement in
hardness is slight, compared to that of CONT samples. Thus, it
may be concluded that the increase in hardness of W9 HSS
sample may be primarily attributed to the complete transition
of retained austenite to martensite with little contribution of
precipitation of ne carbides.
3.3. Impact toughness
Results of the impact testing for different cryogenic treatment
processes are shown in Fig. 9 After the sub-zero treatment with
subsequent tempering, W9 HSS shows signicantly higher Impact
toughness, compared to the CONT sample. The lower temperature
of sub-zero treatment resulted in increased impact toughness by
29% (DCT1 sample) relative to that of the CONT sample. As shown,
the impact toughness was also improved when sub-zero treatment with prior tempering was carried out, which is however not
as large as that caused by the sub-zero treatment with subsequent tempering. The increase in impact toughness by cryogenic

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

859

Fig. 7. TEM micrographs of martensite in two different samples: (a) TEM micrograph of CONT; (b) TEM micrograph of SCT.

Fig. 8. Hardness values of samples experienced different heat treatment processes

in different temperature ranges (CONT, CT, SCT, and DCT).

treatment should be attributed to the fact that the lower cryogenic temperature resulted in more uniformly distributed ne
secondary spherical carbides, which may more effectively deect
and block crack propagation, leading to more energy dissipation
during the crack propagation process. Thus, different from the
case of hardness, the improvement in impact toughness of W9
HSS sample caused by the sub-zero treatments may largely be
attributed to the precipitation of ner carbides. Similar observations were reported by Rhyim et al. [3] for D2 steel and Yun et al.
[7] for M2 steel. Das et al. [4] also reported improvement in
fracture toughness for D2 steel by shallow cryogenic treatment.
Fig. 10 illustrates fractographs of a CONT sample (a) and a SCT
sample (b). The former reveals classical cleavage facets in primary
carbides (marked by arrow 1), cracking of primary carbides
(marked by arrow 2) and cracking at the interface between the
primary carbides and the matrix (marked by arrow 3). This is
expected because the primary carbides in W9 HSS are large (see
Fig. 4) and prone to fracture. Fracturing of primary carbides was
observed in D2 steel as well [4]. Cracking along the primary
carbide-matrix interfaces was also observed previously in D2
steel at fractured surfaces [4]. Unlike the primary carbides, the
ner secondary carbides helped accommodate the impact stress
more easily, since the impact energy could be dissipated by the
surrounding soft matrix and cracking propagation could be
deected more frequently, leading to more energy absorption

Fig. 9. Impact toughness values of samples experienced different treatment

processes in different temperature ranges (CONT, CT, SCT, and DCT).

associated with cracking. Fig. 10(b) shows the quasi-cleavage

characteristics with many microvoids in the matrix resulting from
the decohesion of secondary carbides (marked by arrows). No
cracking of secondary carbide particles was observed in the
fracture surfaces, indicating a higher resistance to impact fracture.
3.4. Wear resistance
Sliding wear tests were carried out for the differently treated
samples. Results of the tests are shown in Fig. 11 As shown, the
relative wear resistance of samples by sub-zero treatment with
subsequent tempering is 23 fold higher than that of the CONT
sample. As an example, the CT sample shows a 2-fold increase in
wear resistance, compared to the CONT sample. The largest
increase in wear resistance can reach 3.4 times. It was also
observed that the wear resistance was increased when sub-zero
treatment temperature decreased. Another important observation
is that the extent of improvement in hardness of DCT1 specimens
over SCT specimens is merely about 0.3%, whereas the corresponding improvement in wear resistance is about 17.2%. Apparently, hardness is not the only parameter governing the wear
resistance of the cryogenically treated material. The improved
fracture toughness should also have a considerable contribution
to the wear resistance by providing a higher capability to lower
the probability of fracture. Similar improvements were reported
in the literature [713,15,23,2729]. Such improvement is

860

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

Fig. 10. SEM micrographs of fracture surfaces of samples experienced two different heat treatments: (a) SEM fractograph of CONT sample showed cleavage facets in
primary carbides (marked by arrow 1), cracking of primary carbides (marked by arrow 2) and cracking at the interface between the primary carbides and the matrix
(marked by arrow 3); (b) SEM fractograph of SCT sample showed microvoids (marked by white arrows) formed by decohesion of secondary carbides.

Fig. 11. Relative wear resistances of samples experienced different heat treatment
processes in different temperature ranges (CT, SCT, and DCT).

dependent on the wearing condition, which results in different

degrees of plastic deformation and pull-out of carbides [28] as
well as fracture of carbides and carbide-matrix interfaces.
Although the hardness and sliding wear tests provided the
information on properties of the cryogenically treated W9 HSS,
they may not well represent the performance of W9 HSS tools
under the condition that is closer to realistic situation, e.g.,
cutting processes which may involve high chip-tool interface
temperatures, high tension on the tool surfaces and great interaction between the tool and the work material. In order to further
investigate the performance of the cryogenically treated W9 HSS,
W9 HSS tap service-life test was performed. The taps were treated
under various conditions as listed in Table 2, respectively. The
total number of holes that each tool made before failure was
determined as the tap life. Five taps were tested for each group.
30CrMnTi was cut with untreated and treated taps at different
temperatures with subsequent and prior tempering, respectively.
Results of the tests are presented in Fig. 12. As shown, the lives of
the treated tools were always longer than those of untreated tools
and decreasing the sub-zero treatment temperature considerably
increased the lives of the taps. By the sub-zero treatments with
subsequent tempering, the tap life was increased by 54%, 127%,
140% and 142% for CT, SCT, DCT1 and DCT2, respectively. Whereas

Fig. 12. Cutting hole numbers of taps experienced different heat treatment
processes in different temperature ranges (CONT, CT, SCT, and DCT).

corresponding percent increases in tap life caused by the sub-zero

treatment with prior tempering were only 9%, 18%, 54% and 61%,
respectively. Clearly, the sub-zero treatment with subsequent
tempering is much more effective in improving the material.
The tap life was the longest when cryogenically treated at
temperature in the range of 11377 K with subsequent tempering. There was no catastrophic failure of taps (i.e. tap broken)
experienced sub-zero treatment during the tapping test, implying
that the sub-zero treatments may improve the impact toughness
of the W9 HSS taps. Fig. 13 illustrates worn areas of the ank face
of the taps (after 110 holes were made), which were conventionally treated and those experienced different sub-zero treatments
with subsequent tempering. It appears that the wear width
increased with raising the sub-zero treatment temperature. The
Morphologies of these worn-out surfaces strongly support the
signicant improvement in wear resistance of W9 HSS steel taps
by the sub-zero treaments, compared to that by the conventional
treatment.
The improvement in W9 HSS tap life with respect to the
treatment condition shows a trend similar to that observed
during the sliding wear tests. The increased wear resistance and
prolonged service life of W9 HSS tap are attributed to homogeneously distributed ner carbides and enhanced austenite-tomartensite transition by the sub-zero treatments. All the sub-zero

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

861

Fig. 13. Morphologies of worn areas of the ank face of the taps after completion of tapping 110 holes: (a) ank face of CONT tap; (b) ank face of CT tap;(c) ank face of
SCT tap; (d) ank face of DCT1 tap.

treatments improved the wear resistance of W9 HSS, compared

to that of samples experienced the conventional treatment
(i.e. CONT). The sub-zero treatment with subsequent tempering
is more effective than that with prior tempering.

treated at temperature in the range of 11377 K with subsequent tempering. For treatment effectiveness and cost
efciency, the deep cryogenic treatment at 113 K could be
the optimal choice.

4. Conclusions

Acknowledgments

Based on the results obtained in the present investigation, the

following conclusions are drawn:

Authors would like to thank the Natural Science Foundation

of China (NSFC) for nancial support (No. 51275333).

(1) All types of sub-zero treatments increased the hardness of

W9 HSS, compared to the conventional treatment (CONT).
The main reasons for the increase in hardness are the transition
of retained austenite to martensite and the formation of
homogeneously distributed ner secondary carbides.
(2) All the sub-zero treatments enhanced the wear resistance of
W9 HSS, compared to the conventional treatment (CONT). The
improvement caused by the shallow (SCT) and deep cryogenic
treatment (DCT1,DCT2) was signicantly larger than that
achieved by CT, and the maximum improvement was
obtained by DCT2, which was however only slightly larger
than that achieved by DCT1. The improvement in wear
resistance by sub-zero treatment is attributed to the matrix
strengthening by ner secondary carbides, the formation of
more and ner twinning, in addition to the transformation of
more retained austenite to martensite. Similar trend was
observed during testing the lives of W9 HSS taps experienced
the cryogenic treatment under different conditions.
(3) The wear resistance ability of W9 HSS was maximized by
incorporating processes for the heat treatment procedure in
the following order: austenitizing, quenching, deep cryogenic
treatment, and tempering.
(4) The performance of the W9 HSS samples was not signicantly
affected by the deep cryogenic treatment temperature. It was
shown that the tap life was the longest when cryogenically

References
The effect of some heat treatment
[1] C.H. Surberg, P. Stratton, Klaus Lingenhoe,
parameters on the dimensional stability of AISI D2, Cryogenics 48 (2008)
4247.
[2] Paolo Baldissera, Fatigue scatter reduction through deep cryogenic treatment
on the 18NiCrMo5 carburized steel, Materials and Design 30 (2009)
36363642.
[3] Y.M. Rhyim, S.H. Han, Y.S. Na, J.H. Lee, Effect of deep cryogenic treatment on
carbide precipitation and mechanical properties of tool steel, Solid State
Phenomena 118 (2006) 914.
[4] D. Das, R Sarkar, A.K. Dutta, K.K. Ray, Inuence of sub-zero treatments on
fracture toughness of AISI D2 steel, Materials Science and Engineering A 528
(2010) 589603.
[5] Shaohong Li, Yinzi Xie, Xiaochun Wu, Hardness and toughness investigations
of deep cryogenic treated cold work die steel, Cryogenics 50 (2010) 8992.
[6] F. Meng, K. Tagashira, R. Azuma, H. Sohma, Role of eta-carbide precipitations
in the wear resistance improvements of Fe12CrMoV1.4C tool steel by
cryogenic treatment, ISIJ International 34 (1994) 205210.
[7] D. Yun, L. Xiaoping, X. Hongshen, Deep cryogenic treatment of high-speed
steel and its mechanism, Heat Treatment of Metals 3 (1998) 5559.
[8] R.F. Barron, Cryogenic treatment of metals to improve wear resistance,
Cryogenics 22 (1982) 409413.
[9] D. MohanLal, S. Renganarayanan, A. Kalanidhi, Cryogenic treatment to
augment wear resistance of tool and die steels, Cryogenics 41 (2001)
149155.
[10] F.J. Silva, S.D. Franco, A.R. Machado, E.O Ezugwu, A.M.J. Souza, Performance
of cryogenically treated HSS tools, Wear 261 (2006) 674685.
[11] V. Leskovsek, M. Kalin, Vizintin, Inuence of deep-cryogenic treatment on
wear resistance of vacuum heat treated HSS, Vacuum 80 (2006) 507518.

862

X.G. Yan, D.Y. Li / Wear 302 (2013) 854862

[12] M. Kalin, V. Leskovsek, J. Vizintin, Wear behavior of deep cryogenic treated

high speed steel at different loads, Materials and Manufacturing Processes 21
(2006) 741746.
[13] Kelkar Rajendra, Nash Philip, Zhu Yuntian, Understanding the effects of
cryogenic Treatment on M2 tool steel properties, Heat Treating Progress 7
(2007) 5760.
[14] D. Das, A.K. Dutta, V. Toppo, K.K. Ray, The Effect of cryogenic treatment on the
carbide precipitation and tribological behavior of D2 steel, Materials and
Manufacturing Processes 22 (2007) 474480.
[15] M. Pellizzari, A. Molinari, L. Girardini, L. Maldarelli, Deep cryogenic treatment
of AISI M2 high-speed steel, International Journal of Microstructure and
Materials Properties 3 (2008) 383390.
[16] D. Das, A.K. Dutta, K.K. Ray, On the enhancement of wear resistance of tool
steels by cryogenic treatment, Philosophical Magazine Letters 88 (2008)
801811.
[17] D. Das, A.K. Dutta, K.K. Ray, Inuence of varied cryotreatment on the wear
behavior of AISI D2 steel, Wear 266 (2009) 297309.
[18] D. Das, A.K. Dutta, K.K. Ray, Inconsistent wear behavior of cryotreated tool
steels: role of Mode and mechanism, Materials Science and Technology 25
(2009) 12491257.
[19] D. Das, A.K. Dutta, K.K. Ray, Correlation of microstructure with wear behavior
of deep cryogenically treated AISI D2 steel, Wear 267 (2009) 13711380.
[20] D. Das, A.K. Dutta, K.K. Ray, Inuence of temperature of sub-zero treatments
on the wear behavior of die steel, Wear 267 (2009) 13611370.
[21] D. Das, A.K. Dutta, K.K. Ray, Optimization of the duration of cryogenic
processing to maximize wear resistance of AISI D2 steel, Cryogenics 49
(2009) 176184.
[22] D. Das, A.K. Dutta, K.K. Ray, On the renement of carbide precipitates by
cryotreatment in AISI D2 steel, Philosophical Magazine 89 (2009) 5576.
[23] Franjo Cajner, Vojteh Leskovsek, Darko Landek, Hrvoje Cajner, Effect of deepcryogenic treatment on high speed steel properties, Materials and Manufacturing Processes 24 (2009) 743746.
[24] D. Das, A.K. Dutta, K.K. Ray, Sub-zero treatments of AISI D2 steel: Part II. Wear
behavior, Materials Science and Engineering A 527 (2010) 21942206.
[25] K. Amini, S. Nategh, A. Shafyei, Inuence of different cryotreatments on
tribological behavior of 80CrMo12 5 cold work tool steel, Materials and
Design 31 (2010) 46664675.
[26] B. Podgornik, F. Majdic, V. Leskovsek, J. Vizintin, Improving tribological
properties of tool steels through combination of deep-cryogenic treatment
and plasma nitriding, Wear 288 (2012) 8893.

[27] N.B. Dhokey, J.V. Dandawate, Study of Wear Stabilization in Cryoprocessed

Cobalt-Based High Speed Steel, Transactions of the Indian Institute Of Metals
65 (2012) 405412.
[28] Simranpreet Singh Gill, Jagdev Singh, Rupinder Singh, Harpreet Singh, Effect
of cryogenic treatment on AISI M2 high speed steel: Metallurgical and
mechanical characterization, Journal of Materials Engineering and Performance 21 (2012) 13201326.
[29] N.B. Dhokey, J. Dandawate, H. Gangurde, A. Harle, Metallurgical investigation
of cryogenically cracked M35 tool steel, Engineering Failure Analysis 21
(2012) 5258.
[30] G. Alexandru, C. Ailincai, Baciu, Inuence of heat treatments at low temperature on the length life of very high speed tool steels, Metallurgy Journal.
(1990) 283388.
[31] J.Y. Huang, Y.T. Zhu, X.Z. Liao, I.J. Beyerlein, M.A. Bourke, TE Mitchell,
Microstructure of cryogenic treated M2 tool steel, Materials Science and
Engineering A 399 (2003) 241244.
[32] D. Das, A.K. Dutta, K.K. Ray, Sub-zero treatments of AISI D2 steel: Part I.
Microstructure and hardness, Materials Science and Engineering A 527
(2010) 21822193.
[33] V. Firouzdor, E. Nejati, F. Khomamizadeh, Effect of deep cryogenic treatment
on wear resistance and tool life of M2 HSS drill, Journal of Materials
Processing Technology 206 (2008) 467472.
[34] Hongjuan Yan, Honghai Xu, Ying Liu, The research on process of deep
cryogenic treatment for W4Mo3Cr4VSi HSS drill, Advanced Materials
Research 97-101 (2010) 457460.
Ekici, Yakup Turgut, Performance of
[35] Adem, Turgay Kvak, Ilyas Uygur, Ergun
cryogenically treated M35 HSS drills in drilling of austenitic stainless steels,
International Journal of Advanced Manufacturing Technology 60 (2012) 6573.
[36] X.G. Yan, S.Q. Pang, Y.T. Li, Z.Q. Liu, H. Guo, Study on the life of high speed
steel taps with cryogenic treatment, Advanced Materials Research 426 (2012)
317320.
[37] X Jinyong, L Yanping, W Jianzhong, K Xiaoyun, G Yuan, X. Zhong, A study on
double glow plasma surface metallurgy MoCr high speed steel of carbon
steel, Surface and Coatings Technology 201 (2007) 50935096.
[38] Li Xiong, Li Shiyan, Zhang Hongbing, Ruan Xueyu, Microstructure of 6W
5Mo4Cr2V high speed steel after cryogenic treatment, Journal of Shanghai
Jiaotong University 36 (2002) 905910.