Effect of Tempering Temperature On The C-Cr-Mo-V Alloy Year 2022

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journal homepage: www.elsevier.com/locate/jmrt

Original Article

Effect of tempering temperature on the


microstructure, mechanical properties and
abrasive wear behavior of a new CeCreMoeV alloy
steel used in TBM cutter ring

Jinzhe Jiang a,b, Yue Liu b,*, Chunming Liu b,**


a
School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China
b
Key Laboratory for Anisotropy and Texture of Materials (MoE), School of Materials Science and Engineering,
Northeastern University, Shenyang 110819, China

article info abstract

Article history: Tunnel boring machine (TBM) cutter ring material is a type of CeCreMoeV alloy steel
Received 25 April 2022 which possesses high hardness and wear resistance. To systematically study the effect of
Accepted 29 June 2022 tempering temperature on the microstructure, mechanical properties and abrasive wear
Available online 8 July 2022 behavior of TBM cutter ring, a new CeCreMoeV alloy steel (DB3) was subjected to
tempering treatment and abrasive wear test. The results indicate that the tempering
Keywords: temperature controlled the hardness and toughness by adjusting the amount of pre-
TBM cutter ring cipitates and austenite transformation. Outstanding mechanical properties were obtained
Tempering upon tempering at 520  C. The wear resistance of DB3 steel was mainly controlled by
Microstructure hardness under non-impact abrasive wear condition. However, under the condition of
Abrasive wear impact abrasive wear, the wear resistance of DB3 steel was affected by hardness and
toughness, and only in a certain range of toughness, the wear resistance increased with the
increase of hardness. The experimental results can provide some reference for the heat
treatment process of DB3 steel used in TBM cutter ring.
© 2022 The Authors. Published by Elsevier B.V. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

installed on the TBM cutter head rolls continuously on the


1. Introduction rock to break the rock [4]. Fig. 1 shows the picture of TBM and
cutter ring. During the working process, TBM cutter ring is
A tunnel boring machine (TBM) is a large engineering ma- subject to non-impact abrasive wear and impact abrasive
chine for excavating hard rock tunnels, such as highway wear [5,6]. According to statistics, the cost caused by cutter
tunnels [1], railway tunnels [2] and water tunnels [3]. During ring wear accounts for one third of the total construction
the course of hard rock tunnel digging, the cutter ring cost [7,8]. Therefore, it is of great practical significance and

* Corresponding author.
** Corresponding author.
E-mail addresses: liuyue@smm.neu.edu.cn (Y. Liu), cmliu@mail.neu.edu.cn (C. Liu).
https://doi.org/10.1016/j.jmrt.2022.06.156
2238-7854/© 2022 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
196 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9

Fig. 1 e TBM and the cutter ring with diameter of 19 inch.

social value to study the wear resistance of TBM cutter ring The main purpose of quenching is to dissolve the alloy ele-
material. ments into the matrix as much as possible and increase the
In addition to the high wear resistance, the cutter ring hardness of martensitic matrix under the condition that the
material also needs high impact toughness to avoid fracture grain size is not too large [15]. Quenched steel is hard and
during tunnel excavation, which will directly lead to the brittle, and the internal stress is large [16]. Therefore, it is
scrapping of the cutter ring. In the past decades, the TBM necessary to carry out tempering treatment after quenching.
cutter ring is made of H13 steel (4Cr5MoSiV1) which has high Tempering takes a key role in regulating the microstructure
toughness and relatively low wear resistance [5,9e11]. Many and properties of material [17]. At different tempering tem-
valuable studies on the wear resistance of H13 steel cutter ring perature, the amount and type of alloy atoms precipitated
have been conducted by scholars. Tian et al. [9] studied the from martensite are different. In addition, the retained
wear behavior of TBM cutter ring material (H13 steel) sliding austenite could transform to martensite at higher tempering
on rocks with different hardness using pin-on-disc wear tests temperature [18]. For alloy steels containing Cr, Mo and V el-
and found that the wear mechanism and mass loss of H13 ements, secondary hardening can occur during high temper-
steel varied with the hardness of rocks. The mass loss of H13 ature tempering [19], which can be used to produce materials
steel worn against soft stone was the largest and the wear with better strength and toughness. At present, the evolution
mechanism was three-body abrasive wear. Lin et al. [10] found of microstructure, strength and toughness of alloy steel dur-
that the mass loss of H13 steel increased with the increase of ing tempering have been studied by scholars [20e22].
rock hardness, which was contrary to the results of Tian et al. In addition to wear conditions, the microstructure and
[9]. The friction heat and contact stress were also found to be properties of material also have a significant impact on wear
the main causes for the difference in wear weight loss. With resistance. Tempering is a common method to improve the
the increase of rock hardness, the contact stress and friction impact toughness of martensitic steels. Scholars have con-
heat suffered by H13 steel wear surface increased, and the ducted many experiments on the influence of tempering tem-
abrasive particles could pierce into the wear surface and cut perature on the wear resistance of martensitic steel without
away the material easily. The reason for the difference of their primary carbides. Their results consistently show that hard-
wear test results is related to the different wear methods they ness is the main factor determining wear resistance, and
use. Lin et al. [11] and Zhang et al. [5] found that vertical load impact toughness would not effectively improve the wear
and vibration played a major role in the wear resistance by resistance of the steels without a sufficient surface hardness
comparing the wear behavior of H13 steel with different [23e26]. Higher hardness increases the wear resistance of the
properties. When the vibration was small, hardness became material by reducing the cutting depth of abrasive particles on
the main factor affecting wear resistance and the wear the worn surface. However, for the martensitic steels riched in
mechanism changed from plowing to micro-cutting with the primary carbides, the wear resistance is related not only to the
increase of hardness. When the vibration was large, the hardness of martensitic matrix, but also the binding force be-
sample with high hardness may undergo brittle fracture, tween primary carbides and matrix. The selective wear of the
which led to the rapid increase of wear weight loss. The load matrix and the cracking or spalled-off carbides should be
and vibration increased with the increase of rock hardness seriously considered. Kim et al. [27] decreased hardness dif-
[12]. In addition, scholars also studied the effects of tunnel ference between carbides and matrix by heat treatment,
parameters and rock geological conditions on the wear thereby leading to the improvement of the wear resistance of
resistance of the cutter ring [13], and established many life high-chromium white cast irons. Zheng et al. [28] found that
prediction models of the cutter ring [14]. the contribution of the interaction between the cementite and
When the wear condition is determined, the microstruc- pearlite in chromium white cast iron to the wear resistance
ture and properties of material become the main factors decreased with increasing hardness of the pearlite matrix.
affecting the wear resistance. For the cutter ring material, However, there are few literature systematically studying the
quenching and tempering treatment are required before use. effect of tempering on abrasive wear of high carbon martensitic
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9 197

Table 1 e Chemical compositions of DB3 steel (wt.%).


C Si Mn Cr Mo V Ni W Nb P S
0.85 0.90 0.43 6.76 1.82 0.30 0.85 0.35 0.25 0.005 0.02

steel riched in primary carbides and comparing the wear for each sample, and then the average value was taken as the
resistance under impact wear and static wear conditions. final hardness. The impact test was carried out on a standard
In this work, a systematic tempering treatment was pendulum-type impact testing machine at ambient tempera-
adopted on a new CeCreMoeV alloy steel used in TBM cutter ture. The impact specimens were in dimensions of
ring. The static and impact abrasive wear experiments were 10 mm  10 mm  55 mm with a standard Charpy U-notch.
carried out on the tempered specimens at the same time. The
effects of tempering temperature on microstructure and 2.3. Abrasive wear tests
abrasive wear properties of experimental materials were dis-
cussed. The differences of wear resistance and wear mecha- The non-impact abrasive wear test of DB3 steel was con-
nism between static wear and impact wear were compared. ducted on a dry sand rubber wheel abrasive wear test machine
This study provides an important guidance for the formula- (MLG-130, Zhangjiakou, China), as shown in Fig. 2(a). The size
tion of heat treatment process of TBM cutter ring material. of the specimen was 57 mm  25.5 mm  6 mm. Abrasive
particle was quartz sand with the size of 50e70 mesh. During
testing, the flow rate of abrasive particle was 300 g/min, and
2. Materials and methods the rotating speed of the rubber wheel was 200 r/min equiv-
alent to a linear speed of 140 m/min. The load was 100 N. Each
2.1. Material preparation and heat treatment specimen was pretested for 5 min to guarantee the consis-
tency of the wear data.
The experimental material DB3 steel is a novel TBM cutter ring A dynamic abrasive wear testing machine (MLD-10,
steel and its chemical composition is presented in Table 1. Zhangjiakou, China) was employed to impact abrasive wear
The DB3 cutter ring was fabricated by vacuum smelting, tests, as sketched in Fig. 2(b). During the impact wear tests, the
electroslag remelting, multi-directional forging, ring rolling DB3 steel with a size of 10 mm  10 mm  30 mm was fastened
and spheroidization annealing. The specimens used for heat to the hammer head and reciprocated at the frequency of 200
treatment were cut from the 19 inch cutter ring along the beats per minute. The impact energy of 4 J was chosen in this
circumference (Fig. 1b). investigation and the silica sand (8e10 mesh) flowed between
The specimens were austenitized at 1025  C for 90 min the upper specimen and lower specimen at the rate of 300 g/
followed by oil cooling to room temperature, and then min. Before the formal test, each specimen was pretested for
tempered at different temperature for 3 h followed by air 5 min to guarantee the reliability of experimental data.
cooling, as listed in Table 2. Each specimen was repeatedly tested for three times and
the average mass loss was used to evaluate the resistance to
2.2. Microstructure characterization and mechanical abrasive wear for each sample. After testing, the worn surface
property tests and the subsurface morphology were observed using scan-
ning electron microscopy.
For observing the microstructure and worn surface
morphology, the specimens were examined by a field emis-
sion scanning electron microscope (FE-SEM, FEI Quanta 450) Table 2 e Heat-treatment schedules of DB3 cutter ring
equipped with an energy dispersive spectroscopy (EDS). The steel.
volume fraction of the carbides was counted using Image Pro Specimen Details of treatment process
Plus (IPP) software. To measure the change of phase content
DB3 1025 Quenching (1025  C, 90 min)
with tempering temperature, the X-ray diffraction (XRD) was
DB3 460 Quenching (1025  C,
performed with a Cu Ka radiation and a 2q scanning rate of 1 / 90 min) þ tempering (460  C, 3 h)
min from 40 to 95 on the quenched and tempered samples. DB3 480 Quenching (1025  C,
The volume fraction of retained austenite is estimated with 90 min) þ tempering (480  C, 3 h)
the relative intensities of characteristic diffracted peaks, DB3 500 Quenching (1025  C,
considering only the diffraction crystal plane (2 0 0) (2 2 0), (3 1 90 min) þ tempering (500  C, 3 h)
DB3 520 Quenching (1025  C,
1) of austenite and (2 0 0), (2 1 1) of martensite [21]. To identify
90 min) þ tempering (520  C, 3 h)
the carbide crystal structure, the TEM test was conducted
DB3 540 Quenching (1025  C,
using the FEI Tecnai G220 transmission electron microscope. 90 min) þ tempering (540  C, 3 h)
The TEM specimen taken from the tempered DB3 steel was DB3 560 Quenching (1025  C,
mechanically thinned to 0.05 mm followed by electrolytic jet 90 min) þ tempering (560  C, 3 h)
polishing in a solution of 15% perchloric acid and 85% ethanol DB3 580 Quenching (1025  C,
at 25  C [29]. 90 min) þ tempering (580  C, 3 h)
DB3 600 Quenching (1025  C,
The hardness the DB3 steel was measured by a Rockwell
90 min) þ tempering (600  C, 3 h)
hardness tester (HRS-150). Five hardness values were tested
198 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9

Fig. 2 e Schematic illustration of MLG-130 dry sand rubber wheel test equipment (a) and MLD-10 impact-abrasive wear test
equipment (b).

decreases gradually during tempering, so tempered


3. Results martensite is easily etched [32].
The matrix of DB3 steels contains many alloy carbides with
3.1. Microstructure high hardness which plays an important role in improving the
wear resistance. To compare the characteristics of carbides in
Before tempering, the DB3 steel was subjected to quenching quenching and different tempering structure, the size and
at 1025  C. Fig. 3 shows the metallographic morphology of content of primary and secondary carbides in each sample
DB3 steel after quenching. The prior austenite grains of the were statistically measured (Table 3), finding that the prop-
quenched DB3 steel are uniform and fine (Fig. 3(b)). The erties of the primary and secondary carbides hardly change in
secondary carbides are uniformly distributed inside the the quenched and tempered specimens. The size of the pri-
grains and grain boundaries, while the primary carbides are mary and secondary carbides ranges from 3.82 mm to 3.99 mm
mainly distributed on the grain boundaries. Compared with and 0.580.64 mm, respectively. The content of primary and
the traditional TBM cutter ring material of 8Cr steels [31], the secondary carbides ranges from 0.50% to 0.58% and 2.28% to
size of primary carbides is relatively small, and there is no 2.35%, respectively. The average size of primary carbides is
continuous network carbides, which is attributed to the about 6 times that of secondary carbides, but the content is
reasonable addition of carbide-forming elements, electroslag only 1/5 of that of secondary carbides.
remelting, and multi-directional forging process. To identify the crystal type of secondary carbide, TEM
To further observe the characteristics of primary carbides, analysis was carried out on the tempered samples. It is
the as-quenched microstructures of DB3 were examined by confirmed that the secondary carbides belong to M23C6 car-
SEM and element mapping. The primary carbides are mainly bides containing a large amount of Cr element (Fig. 6). These
distributed in chained along grain boundaries (Fig. 4). Large secondary carbides have their origins in annealed micro-
amounts of Mo, W and Cr are detected in the irregular primary structure and are inherited into tempered microstructure
carbides. In addition to Mo and W elements which are because they are not completely dissolved during austenitiz-
enriched in the same position in the primary carbide, the ing. The undissolved secondary carbides have little contribu-
distribution of other carbides (Cr-rich and Nb-rich carbides) is tion on the hardness, because the size of secondary carbides is
adjacent but not coincident. Meanwhile, compared with Cr- larger and they has no pinning effect on dislocation [33].
rich and Mo/W-rich carbides, the size of Nb-rich carbides is However, the secondary carbides are beneficial to wear resis-
smaller (about 200 nm) and most of them distribute at the tance due to their high hardness (higher than 1000 HV) [34].
edge of Cr-rich primary carbides. Retained austenite (RA) and precipitates are the main
Fig. 5 shows the microstructure of quenched and tempered variables during the tempering process, and also the main
DB3 steel. It is found that the quenching and tempering factors affecting the mechanical properties of DB3 steel. In
structure of DB3 steel are composed of martensite and car- order to elucidate the tempering evolution behavior of RA and
bides. The grain boundary is clearly visible in the structure of precipitates, TEM, EBSD, XRD were used to characterize the
quenched DB3 steel (Fig. 5(a)). The martensite is more easily microstructure of tempered DB3 samples.
etched, and the grain boundary become blurred for the DB3 The EBSD phase maps of the DB3 specimens are shown
460  C (Fig. 5(b)). The grain boundary is gradually covered by Fig. 7, in which blue corresponds to BCC lattice (martensite)
the etched martensite matrix with the increase of tempering and red corresponds to FCC lattice (austenite). The irregular
temperature. The quenched martensite with higher solution block RA distributes on boundaries of lath martensite, which
content of alloying elements shows strong corrosion resis- can effectively relax the local stress concentration and
tance. The content of alloy elements in the martensite enhance impact toughness [35]. When the tempering
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9 199

Fig. 3 e Optical micrographs of as-quenched specimen.

temperature is lower than 480  C, there is a lot of RA in DB3 treatment could make the martensite lattice shrink, which
steel. When the tempering temperature exceeds 480  C, the provides more space for RA transformation [37,38]. The vol-
content of RA decreases sharply and disappears completely ume expansion of martensite in DB3 steel mainly caused by C
after tempering temperature beyond 520  C, as shown in (interstitial solid solution) and Cr, Mo, V (substitutional solid
Fig. 7(f). The EBSD mainly detects the phase composition and solution). In order to study the degree of martensite lattice
distribution in the local microscopic region and the accuracy expansion in DB3 steel during tempering, the lattice constant
of statistical results is low. Therefore, XRD analysis was of BCC phase was analyzed, as shown in Fig. 8(b). Compared
employed to measure the volume fraction of the RA phase in a with quenched DB3 steel, the lattice constant of martensite
broad scope for each DB3 sample. increases from 2.8752  A to 2.8759 
A after tempering at 460  C,
Fig. 8(a) and (b) show the XRD diffraction patterns and RA which is due to the precipitation of interstitial solution atom C
content of DB3 samples respectively. According to the analysis from the supersaturated martensite [39]. According to the
results, the variation trend of RA content was consistent with quantitative relationship between martensite lattice constant
that of EBSD result, the volume fraction of RA decreased and carbon content in Eq. (1) [40,41], the lattice constant c
rapidly between 480  C and 520  C. The stability of RA, decreases and a increases with the decrease of carbon content
undercooling and mechanical stress of surrounding phases in martensite.
are the main factors affecting the transformation of austenite
c ¼ a0 þ ap; a ¼ a0 ebp; c=a ¼ 1 þ gp (1)
to martensite [36]. The transformation of retained austenite in
high-carbon and high-alloy steel is mainly controlled by the where p is the carbon content of martensite; a0 is the lattice
compressive stress. Scholars have found that deep cryogenic constant of body-centered cubic a-Fe; a, b and g were

Fig. 4 e The SEM and element mapping of as-quenched specimen.


200 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9

Fig. 5 e SEM images of the specimens quenched at 1025  C (a) and tempered at 460  C (b), 500  C (c), 520  C (d), 560  C (e),
600  C (f).

experimental parameters, which were 0.116 ± 0.002, increases, and the substitutional solid solution atoms (Cr, Mo)
0.013 ± 0.002 and 0.046 ± 0.001, respectively. are precipitated from the martensite matrix gradually, which
When the tempering temperature is higher than 480  C, the reduces the lattice constant of martensite. The change of
driving force for the precipitation of solid solution atoms martensite lattice constant with tempering temperature

Table 3 e Average size and content of the carbides in specimens quenched at 1025  C and tempered at different
temperatures.
specimen Content/% Average size/mm
Primary carbide Secondary carbide Primary carbide Secondary carbide
DB3 1020 0.53 2.28 3.82 0.62
DB3 460 0.55 2.35 3.99 0.60
DB3 480 0.53 2.34 3.85 0.63
DB3 500 0.50 2.30 3.83 0.51
DB3 520 0.51 2.30 3.86 0.58
DB3 540 0.56 2.35 3.90 0.60
DB3 560 0.52 2.31 3.87 0.64
DB3 580 0.58 2.33 3.88 0.62
DB3 600 0.53 2.27 3.98 0.60
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9 201

Fig. 6 e (a) TEM image with indexed selected area electron diffraction (SAED) pattern (inset) of the secondary carbide, (b)
Energy spectrum analysis of the secondary carbide.

provides an explanation for the tempering evolution of RA. thin film respectively. According to the change of martensite
That is, when the tempering temperature is higher than lattice constant mentioned above, the alloy atoms in
480  C, the lattice of martensite shrinks sharply due to the martensite do not precipitate except for carbon atom when
precipitation of substitutional solid solution atom, which al- the tempering temperature is lower than 480  C. As the
leviates the mechanical stress of martensite on RA. Therefore, tempering temperature increases, the alloy atoms acquire
the RA in the DB3 steel transforms into martensite substan- sufficient driving force to undergo short or long range diffu-
tially after cooling. sion, and finally combine with C atom to form alloy carbides.
Although the change of martensite lattice constant with As shown in Fig. 9(b), a large number of fine carbide particles
tempering temperature can be detected by XRD and the pre- precipitate from the martensite matrix when the tempering
cipitation of alloy atoms in martensite can be predicted, the temperature reached 520  C. The dislocation-nucleated car-
type, morphology and distribution of precipitates cannot be bide coarsens gradually as the tempering temperature
identified. Therefore, TEM observation was performed on DB3 increased, as shown in Fig. 9(c) and (d). These carbides that
steels. As shown in Fig. 9(a), the microstructure of DB3 460  C precipitate and grow between the martensitic slabs are iden-
is mainly composed of martensite and remained austenite, tified as orthorhombic M2C carbides on the basis of their
but no precipitates is observed. The RA distributes at the diffraction spot patterns. This is consistent with the results in
boundary and gap of martensite lath in the form of block and the literature [42].

Fig. 7 e EBSD phase maps of DB3 specimens quenched at 1025  C (a) and tempered at 460  C (b), 480  C (c), 500  C (d), 520  C
(e), 540  C (f).
202 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9

Fig. 8 e (a) X-ray diffraction patterns, (b) Volume fraction of RA and lattice constant of BCC phase of DB3 spacimens.

The M2C carbide riched in Mo is dislocation-nucleated, 3.2. Mechanical properties


which is the main strengthening phase in secondary hard-
ening steel [42e44]. Because the radius of Mo atom is larger The high temperature tempering (460e600  C) has a great
than that of Fe atom, they can only move a very short distance regulating effect on the hardness and toughness of DB3
during tempering, so most of them pron to nucleate at dislo- samples (Fig. 10). Before tempering, the hardness of quenched
cation [45]. The fine M2C carbides have a pinning and dragging DB3 steel is the highest, reaching 66.70 HRC, which is associ-
effect on the dislocations. So, they can greatly hinder the ated with the higher hardness of quenching martensite with
movement of dislocations and enhance the hardness of steel higher solution content of alloying elements. Meanwhile, the
[46]. With the increase of tempering temperature, the density impact energy of quenched DB3 steel is the lowest. After
of precipitate decreases, the spacing and size of precipitate tempering, the toughness is improved to some extent. The
increase due to Ostwald ripening [47]. Rockwell hardness of tempered DB3 steels increases steadily

Fig. 9 e TEM images of specimens tempered at 460  C (a), 520  C (b), 540  C (c), 560  C (d).
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9 203

600  C with the lowest hardness has the maximum wear


weight loss of 0.8315 g, which is 6.7 times the mass loss of DB3
1020  C. The specimens with similar hardness, such as DB3
500  C and DB3 540  C, show similar wear weight loss. It seems
that the wear property of DB3 specimens is only related to
hardness, and has nothing to do with impact toughness.
The TBM cutter ring is subjected to not only non-impact
abrasive wear, but also impact abrasive wear in the actual
working condition. To investigate the effect of impact tough-
ness on abrasive wear, impact abrasive wear experiments
were carried out on DB3 specimens.
Fig. 11(b) shows the mass loss of DB3 specimens under
impact abrasive wear conditions. The mass loss of each
sample under impact wear condition is greatly different from
that under non-impact wear condition, and the mass loss of
DB3 specimens has no linear relationship with the overall
hardness or toughness. The DB3 520  C specimen has the best
Fig. 10 e Mechanical properties of DB3 steel under different
wear resistance and the smallest wear loss of 0.0299 g.
heat treatment temperature.
Meanwhile, the DB3 600  C with the lowest hardness has the
worst wear resistance and the maximum wear weight loss of
0.0435 g, which is 1.45 times larger than that of DB3 520  C. In
addition, the specimens with similar hardness and different
with the increase of tempering temperature before 520  C toughness show great difference in mass loss, for example,
followed by a continuously decrease at higher temperature the DB3 500  C with higher toughness shows lower mass loss
(520e600  C). The toughness of tempered specimens increases than DB3 540  C.
in different degrees compared with the quenched specimen. If the experimental results can be divided into three parts
The impact energy decreases gradually between 460  C and according to the difference of toughness, namely, low tough-
560  C, and attains the lowest value of 3.31 J at 560  C. When ness interval of 3.0e4.5 J (as marked with green line in
the tempering temperature exceeds 560  C, the impact energy Fig. 11(b), medium toughness interval of 4.50e7.5 J (blue line),
increases sharply. For CeCreMo alloy steel, the change of high toughness interval of 7.5e10.0 J (red line), the mass loss
tempering hardness within 460e560  C is mainly attributed to decreases with the increase of hardness in each toughness
the precipitates. At a higher temperature, the alloy atoms interval, but the decreasing rate is different. In the medium
have enough energy to precipitate from the quenched toughness interval, the mass loss decreases rapidly with the
martensite in the form of fine dispersion precipitates which increase of hardness. For example, compared with DB3 460  C,
can change the properties of matrix. the hardness of DB3 520  C increases from 62.8 HRC to 64.6
HRC, an increase of 2.87%, while the mass loss decreases by
3.3. Mass loss 23.72%. In the high toughness interval, the mass loss de-
creases slowly with the increase of hardness. For example,
The non-impact mass loss of DB3 specimens has a good linear compared with DB3 600  C, the hardness of DB3 580  C in-
relationship with hardness, as presented in Fig. 11a. The DB3 creases by 7.73%, while the mass loss only decreases by 0.92%.
1025  C with the highest hardness has the best wear resis- Therefore, the sensitivity of mass loss to hardness is lower
tance and the smallest wear loss of 0.1779 g. Meanwhile, DB3 for the DB3 specimens with high toughness. For the DB3

Fig. 11 e Non-impact abrasive wear (a) and Impacteabrasive wear (b) test results plotted on hardness vs mass loss chart.
204 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9

specimens with medium toughness and high hardness, the roundness of carbide is better (Fig. 12(c) and (d)). This is con-
mass loss has the strongest sensitivity to the hardness. cerned with the high matrix hardness of DB3 520  C. The
matrix with higher hardness can not only resist the abrasive
3.4. Worn surface of non-impact abrasive wear cutting effectively, but also plays better support for the
carbides.
Fig. 12 shows the non-impact worn surface morphology of For the DB3 600  C, there are wide and deep furrows on the
DB3 specimens after dry sand rubber wheel test. The wear worn surface, accompanied by obvious wrinkle at the furrow
mechanisms of DB3 specimens under non-impact abrasive edge (Fig. 12(e) and (f)). Coarse wear debris is distributed on
wear mainly involve micro-cutting, plowing and drilling pits, the worn surface. The precipitated phases coarsen and have
but the wear degree of different samples is different. no precipitation strengthening effect on the matrix after
The worn surface of DB3 460  C shows wide and deep tempering at 600  C, leading to a drop of matrix hardness.
grooves caused by granite sliding and rolling, as illustrated in Therefore, the material on the worn surface is easily
Fig. 12(a) and (b). Furthermore, some abrasive particles slid removed by the abrasive particles, resulting in larger mass
into the worn surface directly and chiseled deep pits. The loss.
carbides on the worn surface are distributed in flat and long The worn cross-section of DB3 steels tempered at different
shape along the wear direction after repeated grinding by temperatures is analyzed. It is obvious that the worn cross-
abrasive particles. section of DB3 520  C is relatively flat (Fig. 13(b)), while the
Compared with DB3 460  C, the furrow depth on the worn worn cross-section of DB3 460  C and DB3 600  C has deep
surface of DB3 520  C is significantly shallower, and the cutting grooves (Fig. 13(a) and (c)).

Fig. 12 e The non-impact worn surface morphology of DB3 samples (a, b) DB3 460  C, (c, d) DB3 520  C, (e, f) DB3 600  C.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9 205

The depth and width of cutting grooves are larger than the shallow, and the amount of material removed by abrasive
size of secondary carbides. Therefore, when the matrix is particles is also lower.
softer, the abrasive particles can remove the secondary car- Large cracks appear on the impact worn surface of DB3
bides together with the martensite matrix in the wear process. 560  C as shown in Fig. 14(c). This is attributed to the low
Due to the large interface between primary carbides and impact toughness of DB3 at 560  C. Under the repeated impact
matrix, the primary carbide is not easy to be plowed from the condition, the abrasive particles gradually embed into the
matrix surface by the abrasive particles. Meanwhile, the crack and accelerate the crack expansion, resulting in brittle
hardness of primary carbides is higher than the martensite shedding of the material. Fig. 14(d) shows the impact worn
matrix, it can resist the plowing of matrix surface by abrasive surface morphology of DB3 600  C. There are many abrasive
particles [48]. As presented in Fig. 13(d), the primary carbides particles embedded in the matrix of DB3 at 600  C due to the
protrude on the surface of matrix, and the protruding parts low matrix hardness. In addition, due to the good impact
become flat due to the long-term grinding of abrasive toughness of DB3 at 600  C, the matrix structure chiseled by
particles. the abrasive particles is not easy to fall off from the sample
surface, and these matrix structure cover the abrasive parti-
3.5. Worn surface of impact abrasive wear cles into the worn surface.

The impact worn surface morphology of different tempered


samples is shown in Fig. 14. In general, the wear mechanism is 4. Discussion
mainly furrow removal and micro-cutting. There are lots of
grooves cutting by abrasive particles on the worn surface of 4.1. Influence of tempering temperature on the hardness
DB3 460  C (Fig. 14(a)). A large amount of wear debris with the and toughness of DB3 steel
size of tens of microns accumulate at the edge of the cutting
groove. These wear debris are easy to fall off from the worn The hardness and toughness of DB3 steel are chiefly
surface under the repeated impact of abrasive particles. controlled by tempering temperature. The hardness increased
Compared with DB3 460  C, the depth and width of micro- first and then decreased when DB3 steel was tempered at
cutting grooves on the worn surface of DB3 520  C (Fig. 14(b)) 460e600  C, and reached the maximum value at 520  C. The
are obviously reduced, besides, there are little wear debris on DB3 steel appears obvious secondary hardening phenomenon
the DB3 520  C worn surface. The matrix hardness of DB3 which is related to retained austenite transformation and
520  C is higher than that of DB3 460  C. Under the same carbide precipitation [29]. The change of toughness is opposite
impact conditions, it is hard for the abrasive particles stick to that of hardness. The variation of hardness and toughness
into the worn surface of DB3 520  C, so the depth of cutting of DB3 is consistent with the H13 steel [30]. The hardness and
grooves on the worn surface of DB3 520  C is relatively toughness trends of DB3 steel is coherent with that of H13

Fig. 13 e Worn cross-section morphology of DB3 steels: (a) DB3 460  C, (b,d) DB3 520  C, (c) DB3 600  C.
206 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9

Fig. 14 e Impact worn surface morphology of DB3 samples: (a) DB3 460  C, (b) DB3 520  C, (c) DB3 560  C, (d) DB3 600  C.

steel, but the hardness of DB3 steel with higher carbon con- alloy steel during tempering is related to the fine Mo-rich
tent is higher than that of H13 steel. carbides which precipitate from and cohere with the
Before tempering, the austenitizing process of DB3 steel martensite matrix [32,54,55].
was conducted at 1025  C to make the alloy elements dissolve The secondary hardening mechanism in Fe-based alloy is
into the matrix as much as possible which helps to form similar to that in AleCu alloy [49], which is related to the
martensite with higher hardness. However, the initial tem- interaction between precipitate and dislocation. The
perature of martensite transformation (Ms) diminishes with increased strength/hardness during aging derives from the
the increase of alloying element content in austenite [31], formation of precipitates, which serve as obstacles to moving
which results in much austenite not being able to undergo dislocation during mechanical loading [49,50]. For pre-
martensitic transformation and remaining in the quenched cipitates, not only their microstructure parameters (number
sample (Fig. 7a). The quenched martensite is unstable and the density, volume fraction, and size) but also their interaction
solid solution elements in martensite tend to precipitate and mode with dislocation during deformation affect their
form carbides during tempering, which leads to the decrease strengthening effect [51]. There exist two main types of
of martensite saturation and hardness. Moreover, martensite dislocationeprecipitate interactions: bypassing and shearing,
laths coarsen and dislocation density decreases with and which one works depends on the nature of precipitates,
increasing tempering temperature, which also causes a including their type, size, shape and so on [52]. Precipitates
decrease in martensite hardness [33]. Therefore, the hardness with a smaller radius than the critical value can be sheared,
of quenched DB3 steel decreases in different degrees after while in the case of precipitates larger than the critical size,
tempering (Fig. 10). The transformation of remained austenite dislocation bypassing occurs instead. For the secondary
and precipitation of fine alloy carbides are the main factors hardening FeeMo alloys, M2C precipitates with a size below
causing the change of material properties during tempering 20 nm are usually used as the strengthening phases [50]. As
[22]. As shown in Figs. 8 and 9, the size precipitates gradually shown in Fig. 9(c) and (d), when the tempering temperature
increases, and the diffraction peak intensity of retained exceeds 520  C, the M2C precipitates expands gradually and its
austenite gradually decreases, which changes the properties shape changes from ellipse to strip. As the tempering tem-
of DB3 steel. When the tempering temperature is between perature reaches 560  C, the length of most precipitates has
460  C and 520  C, the hardness increment of DB3 steel caused reached 40 nm, which indicates that the M2Cedislocation
by transformation of austenite and precipitation strength- interaction mode is bypassing. Therefore, the decreased
ening is higher than the hardness reduction induced by hardness of DB3 steel tempered beyond 520  C is related to the
martensite desolvation, which makes the tempering hardness increase in the size of M2C precipitates. At the same time, with
of DB3 steel increase gradually. Many studies have shown that the increase of precipitates, the solid solution hardening is
the main reason for the secondary hardening of CeCreMoeV weakened, which aggravates the decrease of hardness.
j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9 207

4.2. Influence of matrix hardness and toughness on hardness is lower (below 60 HRC), the abrasive particles will
wear resistance press into the matrix deeply under a normal force. Besides, the
abrasive particles will continue to cut into the matrix under
The wear test of DB3 steel tempered at different temperatures the tangential force, resulting in the increase of sliding resis-
was conducted under the condition of non-impact and impact tance of the abrasive particles, and finally the abrasive parti-
abrasive wear, finding that the mass loss of DB3 samples has a cles will be embedded in the matrix, as illustrated in Fig. 14(d).
linear relationship with hardness under non-impact abrasive If DB3 specimen has high toughness, the matrix arched by the
wear condition. However, under the condition of impact wear, embedded abrasive particles will not easily fall off from the
the mass loss is affected by both hardness and toughness. wear surface which will surround the embedded abrasive
The characteristics of matrix structure and carbides have particles and wrap them in the matrix structure. The abrasive
an impact on the wear resistance of steel [60,61]. In this study, particles wrapped by the matrix can also act as wear-resistant
we have confirmed that the primary and secondary carbides phase preventing the subsequent abrasive particles from
do not change greatly during tempering as shown in Table 3, cutting the matrix. Therefore, for the DB3 steel with low
because the tempering temperature is relatively low, which is hardness and good toughness, the change range of wear
not enough to change these carbides. Therefore, the wear resistance is relatively small. For the DB3 steel with higher
resistance of DB3 steels is related with the hardness and matrix hardness, the penetration depth of abrasive particles
toughness of martensite matrix. on the surface of matrix is relatively shallow under a normal
Many scholars have done in-depth research on the rela- force, and the abrasive particles are not easy to embed into the
tionship between hardness and wear resistance of alloy steel matrix. Therefore, micro-cutting is the main wear mecha-
under the non-impact abrasive wear [62e64]. It is generally nism, and with the increase of matrix hardness, the materials
concluded that the higher matrix hardness is helpful to removed from the surface of DB3 steel decrease, resulting in
improve the wear resistance by reducing the cutting depth of lower mass loss. For samples with similar hardness, the
abrasive particles, which is consistent with the research re- penetration depth of abrasive particles on the substrate sur-
sults in this paper, as shown in Fig. 10(a). Among all kinds of face is similar. The difference is that for the samples with
matrix of alloy steel, the martensite has the highest hardness higher hardness but lower toughness, the worn surface is easy
and the best wear resistance. However, the strength and to crack compared with the samples with higher toughness, as
toughness of martensite vary greatly with different solid so- shown in Fig. 14(c). In addition, the debris cut by the abrasive
lution content. In this study, the solid solubility of martensite particles is easy to fall off from the worn surface. Therefore,
was adjusted by tempering at different temperatures to obtain under the same hardness, the material with poor toughness
martensite matrix with different strength and toughness and has higher mass loss.
explored its effect on wear resistance.
In the process of non-impact abrasive wear, the main wear
mechanisms are micro-cutting and plowing. The wear resis- 5. Conclusion
tance of DB3 steel is mainly affected by the indentation depth
of abrasive particles. When the hardness of martensite matrix (1) Higher tempering temperature can promote the pre-
is low, abrasive particles can pierce into the wear surface cipitation of alloy carbides from martensite matrix and
deeply and the material on the wear surface is plowed or the transformation of residual austenite to martensite,
removed more easily, as seen in Fig. 7(a) and (b), which results which is the main reason for the hardness and tough-
in higher mass loss. When the hardness of the martensite ness variation of DB3 steel tempered at 460e600  C. The
matrix increases, it is difficult for the abrasive particles hardness of DB3 steel increases steadily tempered at
piercing into the matrix, and the wear mechanism changes 460e520  C and reaches the maximum value of 64.58
from plowing to micro-cutting. As a result, there are small and HRC at 520  C, which is due to the gradual increase of
shallow cutting grooves on the worn surface (Fig. 7(c) and (d)). fine M2C precipitates that strengthen the matrix. When
Compared with H13 steel [65], the novel TBM cutter ring the tempering temperature exceeds 520  C, the M2C
steel DB3 studied in this paper not only has a certain amount precipitates gradually coarsen and lose the strength-
of carbides protecting the matrix, but also has a higher hard- ening effect on martensite matrix of DB3 steel, which
ness of martensite matrix supporting the carbides, so its wear leads to a drop of tempering hardness. The variation
resistance will be better than H13 steel. Compared with D2 trend of toughness is contrary to that of hardness and
steel containing excessive alloying elements [66],there are reaches the lowest value at 560  C.
no shedding of primary carbides and no micro-crack between (2) The wear resistance of DB3 steel is positively correlated
primary carbides and matrix, an seen in Fig. 12(d), which may with the tempering hardness and has little relationship
be related to the better toughness and hardness of DB3 steel. with the toughness under the non-impact abrasive wear
In addition, the impact toughness of DB3 steel is higher than test. Meanwhile, the wear mechanism is mainly micro-
that of D2, which can better meet the wear condition of TBM cutting and furrow removal. With the increase of hard-
cutter ring. ness, the cutting depth and width decrease. Compared
Under impact wear conditions, the abrasive particles sub- with tempered DB3 steel, the quenched DB3 steel ob-
jected to a large instantaneous impact load are easily pressed tains the best wear resistance because it has the highest
into the worn surface, and then cut or plow the worn surface hardness. Among the tempered specimens, the DB3
under the action of tangential force [67,68]. If the matrix steel tempered at 520  C shows the best wear resistance.
208 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 2 ; 2 0 : 1 9 5 e2 0 9

(3) The wear resistance of DB3 steel is affected by both tunnel boring machine normal disc cutters. J Mech Sci
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