Effect of Spheroidizing Annealing Process on Microstructure and Properties of Quenching and Tempering 60Cr16MoMA Martensitic Stainless Steel

RESEARCH ARTICLE
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Effect of Spheroidizing Annealing Process on

Microstructure and Properties of Quenching and
Tempering 60Cr16MoMA Martensitic Stainless Steel
Huan Teng, Shasha Qian, Jiahao Xie, Hongshan Zhao,* Xicheng Wei,* and Han Dong
necessary to obtain a softened matrix

The effect of spheroidizing annealing on carbide characteristic parameters, before further processing.[9] To achieve
mechanical properties and wear resistance of the quenching and tempering (Q&T) the desired mechanical properties, quench-
high carbon martensitic stainless steel is investigated. The microstructure of the ing after processing and forming is
required so that the microstructure is trans-
steel is characterized and analyzed through various techniques, including scan-
formed into martensite, and tempering
ning electron microscope (SEM), X-ray diffraction (XRD), electron backscattering reduces the internal stress in the martens-
diffraction (EBSD), and transmission electron microscope (TEM). Results show ite and improves the toughness.[10] The
that the microstructure of the annealing steel is mainly composed of ferrite and microstructure of quenching and temper-
M23C6 carbide. With the rise of austenitizing temperature, the average diameter of ing (Q&T) HCMSS is mainly composed
of martensite, retained austenite (RA),
carbide of the annealed steel increases. The average diameter of carbides in the
and different types of carbides.[11,12]
Q&T steel changes in the same way as that observed in the annealed steel. These phases, especially the type, morphol-
The steel has the lowest annealing hardness, highest Q&T toughness, and wear ogy, and distribution of carbide particles,
resistance at an annealed soaking temperature of 860 °C. The influence factor of determine the mechanical properties as well
the toughness and wear resistance can be identified that small-sized carbides and as tribological behavior of HCMSS.[13,14]
low angle grain boundaries exhibit strong interface adhesive strength. This The majority of carbide types in HCMSS
are M23C6 as well as small amounts of
reduces the probability of cracking in the particle or at the interface.
other types of carbides.[15,16] The carbides
exhibit a wide-ranging size distribution,
including size greater than 10 μm coarse
carbide and submicron-level carbide.[10]
1. Introduction Fine and uniformly distributed carbides can enhance the
mechanical properties and wear resistance of the material.[17–19]
High-carbon martensitic stainless steel (HCMSS), due to its high Meanwhile, undissolved fine particles can serve as austenite
hardness, strength, wear resistance, and corrosion resistance, is nucleation sites, preventing excessive growth of grains and
regarded as the ideal functional material for manufacturing bear- enhancing the toughness of the material.[20] On the contrary,
ings, high-pressure vessels, turbine components, and kitchen coarse carbide can deteriorate the mechanical properties and cor-
knives.[1–6] The good hardenability of HCMSS enables the rosion resistance of HCMSS.[21–23] Roscioli et al. showed that car-
martensite transformation under air cooling after the hot bide peeling off from the blade is the main cause of razor failure
deformation.[7,8] Consequently, a spheroidizing annealing is such as chipping.[24] Wang and Li et al. reported that the debond-
ing of large-sized M23C6 carbides from the substrate during the
straining process induced microcracks and reduced the tough-
H. Teng, S. Qian, J. Xie, H. Zhao, X. Wei, H. Dong ness of the material.[25,26] It has been shown that coarser carbides
School of Materials Science and Engineering bond more poorly with the matrix, which can adversely affect the
Shanghai University mechanical properties of the material.[27,28]
Shanghai 200444, P. R. China
E-mail: zhaohs@shu.edu.cn; wxc1028@shu.edu.cn
Numerous investigations have been focused on optimizing
the size, morphology, and distribution of medium/high carbon
H. Zhao, X. Wei, H. Dong
Zhejiang Institute of Advanced Materials, SHU steels through heat treatment, mainly which adjusting heat treat-
Zhejiang 314100, P. R. China ment process. He et al. observed that increasing the austenitizing
H. Zhao temperature during spheroidal annealing resulted in larger car-
State Key Laboratory of Advanced Special Steel bide size and a decrease in the number of carbides per area in
Shanghai Key Laboratory of Advanced Ferrometallurgy 1.12C-8.1Cr steel.[29] Yu et al. investigated the effect of austenitiz-
Shanghai University ing time during spheroidizing annealing on carbides and
Shanghai 200444, P. R. China
mechanical properties. They found that increasing holding time
The ORCID identification number(s) for the author(s) of this article will promote the precipitation of lamellar carbides, leading to
can be found under https://doi.org/10.1002/srin.202300781. enhanced material hardness.[30] Zhu et al. studied the effect of
DOI: 10.1002/srin.202300781 quenching cooling speed on the microstructure of 8Cr13MoV
steel research int. 2024, 2300781 2300781 (1 of 12) © 2024 Wiley-VCH GmbH
1869344x, 0, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/srin.202300781 by Shanghai University, Wiley Online Library on [06/03/2024]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
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steel. Results show that high quenching speed reduces the Cr The specimens were wire cut into 33.0 33.0 6.5 mm.
content in carbides and lowered the martensitic transformation The original microstructure consists of ferrite, carbides with dif-
temperature.[31] Cradoso et al. reported that low temperature ferent morphologies. The Ac1 and Ac3 of the steel were deter-
treatment contributes to the precipitation of fine carbides in mined by DIL 508A dilatometers (TA instruments). Specifically,
AISI D6 tool steel, leading to improved hardness and tough- the Ac1 and Ac3 of the steel is about 840 and 930 °C, respectively.
ness.[32] However, these studies mainly focused on obtaining In order to study the influence of the initial annealed microstruc-
improved microstructural or enhanced properties when ture on the Q&T microstructure, different austenitizing temper-
spheroidizing annealing or Q&T are employed as the final heat atures between the two-phase region is selected, and the variables
treatment. The effect of changes in the initial microstructure on are set in steps of 20 °C. The materials underwent spheroidizing
the final microstructure and properties after quenching remains annealing and Q&T treatments as illustrated Figure 1. The
relatively understudied. Further investigations are needed to quenching process is that specimens were austenitized at
comprehensively understand the influence of the initial micro- 1075 °C for 35 min followed by oil quenching to room tempera-
structure on the final microstructure and properties after the fol- ture and then tempering at 160 °C for 1 h.
lowing Q&T process. The specimens were polished and etched by 5 g
In this study, the influence of the microstructure and mechan- FeCl3 þ 50 mL HCl þ 50 mL ethanol regent. The microstructure
ical properties obtained after different spheroidizing annealing of the specimens in the spheroidal annealed and Q&T state of the
processes on the subsequent Q&T of the material is investigated material observation was performed by using a scanning electron
for 60Cr16MoMA HCMSS. The aim of this work is to study microscope (FEI Apero2, SEM). The size of the carbides and dis-
the effect of initial microstructure on the material properties tribution of which were counted according to ASTM A892-09
Q&T process by adjusting the annealing process parameters. (2020) with the help of IMAGE J image analysis software, using
The study establishes a connection between the carbide param- several random SEM images at the same magnification (the sta-
eters annealed and Q&T, bridges the gap in prior research. The tistics did not include carbides with a diameter of 0.01 μm or
findings presented herein serve as a crucial reference for subse- less). The number of carbides considered for the analysis was
quent material processing and service applications. a minimum of 1800 for each sample, to evaluate the statistical
reliability associated with the measurement. The Q&T samples
for electron backscatter diffraction (EBSD) were vibratory-
2. Experimental Section polished for 4 h to remove the stress layer and then tested using
a Bruker eFlash EBSD detector. The EBSD data were analyzed
Industrial-produced annealed state 60Cr16MoMA martensitic using OxFord AztecCrystal software. Transmission electron
stainless steel was used as the experimental material. The com- microscopy (TEM) samples were firstly polished to 50 μm thick-
position of the studied steel were tested using an arc optical ness, and TEM foils were finally obtained by twin-jet electron-
emission spectrometry analyzer (SPECTRO MAXx), as shown polisher using a solution of 10% perchloric acid and 90% alcohol
in Table 1. at 25 °C. The substructure was examined by TEM (JEM-F200).
The analysis of XRD was accomplished by a Rigaku SmartLab
Table 1. Chemical composition of 60Cr16MoMA steel (mass%). X-ray diffractometer using Cu-Kα radiation. The scanning speed
is 4° min1, and the scanning angle 2θ ranges from 20° to 100°.
C Si Mn P S Cr Mo Ni Nb V Fe The volume fraction of RA can be obtained according to ASTM
0.58 0.26 0.59 0.016 0.001 15.8 0.41 0.45 0.05 0.19 Bal. E97. The following equations were used to calculate the calculate
the volume fraction of RA.
Figure 1. Specimens and heat treatment parameters.
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1.4I γ interspersed with carbide precipitates. Distinctive carbide mor-

Vγ ¼ (1)
I α þ 1.4I γ phologies emerge at different austenitizing temperatures: at
840 °C (Figure 2a), a large number of large-sized carbides
where Vγ represents the volume fraction of residual austenite, appeared, which may be due to the incomplete dissolution of car-
and Iα and Iγ represent the integral strength of the austenitic bides at low temperatures. As the holding temperature increases,
peak and the ferritic peak. the small-sized carbides dissolve and the area of sized carbides
The hardness of the annealed specimens was measured using decreases. Beyond 880 °C (Figure 2c,d), there is a noticeable
a Wilson VH1102 Vickers hardness tester with a test force of increase in coarse pea-shaped carbide, indicating the increase
0.5 kgf and holding for 10 s. Meanwhile, the hardness of Q&T of incomplete spheroidization of carbides.
samples was measured by a Wilson RH2150 Rockwell hardness Figure 3 quantitatively manifests the diameter distribution, box
tester with an applied load of 150 kg. The average value of 10 tests plot, and number of carbides per area of the secondary carbides at
for each specimen was recorded as the standard hardness. four austenitizing temperatures, 840, 860, 880, and 900 °C. It can
The Charpy U-touch sample (10 5 55 mm3) using Q&T be seen that with the austenitizing temperature increasing, the
specimens was performed to measure the impact energy by peak of the carbide counts all appear within the range of
using an INSTRON MPX pendulum-impact tester according 0.4–0.6 μm. However, the proportion of fine carbides (with diam-
to GB/T 229-2020. Three samples were tested at impact testing eter <0.6 μm) has a great difference. For 860A, the fine carbides
for each specimen. accounted for 37.4%, while that only accounted for 31.1% for
Linearly reciprocating ball-on-flat wear tests were carried out 900A. An increase in the austenitizing temperature within the
by RTEC MFT-5000 Multi Function Tribometer with dimensions range of 840–860 °C resulted in slight variations in the first
of 35 20 5 mm3. The grinding body was an Al2O3 ceramic and third quartiles (Q1 and Q3) as well as the average values
ball with a diameter of 6 mm, and the normal load is 10 N with of carbides, as shown in Figure 3b. The average diameter of
30 min, and the frequency is 1 Hz. The samples were wet-sanded the carbides remained constant at 0.80 μm. Nevertheless, a
using silicon carbide papers from 320 grit down to 1000 grit decrease in the carbide number per area was detected, declining
before the test. The depth of the slide was characterized by con- from 0.21 to 0.19 as indicated in Figure 3c. As the austenitizing
tourgraph Senso Neox090 V2. The worn surfaces and the cross- temperature continued to rise, there is a corresponding increase
sectional microstructures parallel to the friction direction were
to 0.90 μm in the average diameter of carbides. Additionally, the
observed by SEM.
values for Q1 (from 0.48 to 0.55 μm) and Q3 (from 1.02 to
1.14 μm) also increase. At the same time, there is a decrease
3. Results and Discussion in the presence of undissolved carbides, leading to a reduction
in the number of carbides per area. This reduction reaches a value
3.1. Microstructure of 0.16 at a temperature of 900 °C.
3.1.1. Microstructure Evolution in Spheroidizing Annealing
3.1.2. Microstructure Evolution in Quenching and Tempering
The microstructure of the specimens at different austenitizing
temperatures is shown in Figure 2. Results indicate that the The microstructure of Q&T specimens are shown in Figure 4.
microstructure of the specimens consists of ferrite matrix The microstructure of all the specimens consists of martensite
Figure 2. SEM images of annealed 60Cr16MoMA with different austenitizing temperatures: a) 840A; b) 860A; c) 880A; and d) 900A.
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Figure 3. Statistical diagrams of relevant parameters of secondary carbide under different austenitizing temperature: a) Carbide size distribution; b) box
plots of different carbide diameter; and c) the number of carbides per area.
and secondary carbides. Compared with the annealed specimens, an increase in the number of carbides within the 0.3–0.7 μm
the number and size of carbides of the material decreased range. However, it is notable that the amount of carbides
after quenching. Significantly, specimens with smaller, more decreases within the 0.1–0.3 μm range. This represents the fact
uniformly distributed carbides in the annealed specimen exhibit that during the austenitizing process, smaller carbides exhibit
correspondingly reduced carbide sizes in the Q&T specimen, as enhanced solubility compared to the larger ones. Remarkably,
shown in Figure 4b. Conversely, larger carbides in the initial the 860AQT stands out with a higher content of fine carbides
microstructure manifest greater resistance to dissolution during in comparison to other processes. Previous studies have shown
the quenching process, as shown in Figure 4c,d. that the refinement of the initial organization facilitates
Figure 5 shows the size distribution and box plots of the size of the refinement of the final organization of the material.[33]
carbides after the Q&T treatment of the material. The carbide Specifically, due to the finer initial carbides of 860AQT steel,
distribution pattern in the Q&T state closely mirrors that these carbides are more easily dissolved during the
observed in the annealed state. Compared to the annealed state, quenching process, culminating in a finely dispersed carbide
the total amount of carbides decreased by about 40% in a single distribution.
picture. Notably, the peak of carbide size distribution occurs The XRD analysis of the specimens subjected to diverse proc-
between the 0.4–0.6 μm range for 840AQT and 860AQT, while essing routes is shown in Figure 6. The 60Cr16MoMA steel
for other processes, the peak tends to progressively shift towards treated through various annealing processes contains carbides
larger sizes. Meanwhile, compared to the annealing process, consisting of M23C6 along with a small amount of MC, martens-
the 1.5 interquartile range (IQR) value declined according to ite, and RA. Different annealing processes do not change the
Figure 5b. The result is explained by the fact that small-sized car- phase of the material after Q&T. The RA content decreases grad-
bides dissolve and the diameter of large-sized carbides reduces. ually with increasing annealing temperature, diminishing from
As a result, there is a concentration in the size distribution and 12.34% to 8.52%. This transition is accompanied by the gradual
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Figure 4. SEM images of Q&T 60Cr16MoMA with the same quenching process: a) 840AQT; b) 860AQT; c) 880AQT; and d) 900AQT.
Figure 5. Statistical diagrams of relevant parameters of secondary carbide under the same Q&T process: a) Carbide size distribution; and b) box plots of
different carbide diameter.
reduction of the γ(200) and γ(220) peaks corresponding to the These results also indicate that the carbides in the initial micro-
austenite phase, and the martensite α(200) and α(211) peaks structure also affect the RA content in the steel.
become more evident.
As pointed out in prior studies,[31] the increase of carbon and 3.2. Mechanical Properties
alloying elements in the austenite prior to quenching leads to a
decline in the Ms of the steel, which increases the RA The evolution of the hardness of annealed state specimens with
content post-quenching. As shown statistically in Figure 6, high- different austenitizing temperatures is shown in Figure 7a. The
temperature quenching is found to preferentially dissolve fine hardness of the annealed state specimens initially decreases and
carbides (with a diameter <0.6 μm). In contrast, the larger-sized subsequently increases. Notably, the lowest hardness is recorded
carbides (with a diameter >1.0 μm) were only reduced in size at an austenitizing temperature of 860 °C. Overall, the change in
without complete dissolution due to the comparatively lower sur- temperature has little effect on the hardness.
face area-to-volume ratio compared with that of the smaller ones, The original microstructure changes into austenite, which has
which reduces the rate of the diffusion process. Earlier findings a higher solubility of the carbon than in ferrite at sufficiently high
have already established a correlation between RA content in temperatures near Ac1, and small-sized carbides are dissolved in
the quenched state and the austenitizing temperature.[15,34] the process. The carbides that remain after austenitizing will
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together or even in direct contact.[35] At different austenitizing

temperatures of 840 °C, 880, and 900 °C, the carbides are signifi-
cantly coarser, thereby reducing carbide spacing. The carbides
will suffer more stress and deformation, consequently enhancing
the hardness of the annealed steel.
As can be seen from Figure 7b,c, 60Cr16MoMA Q&T steel
hardness values of 55-57HRC and impact energy ranging
between 8.3 and 12.6 J. With the rise in austenitizing tempera-
ture, the hardness and impact toughness of the steel exhibit an
initial increase, and maximum values are observed at 860AQT,
followed by a decline. Figure 8 shows the macro morphology of
the impact specimen fracture which can be divided into radial
area and shear lip. These characteristics collectively indicate
the occurrence of brittle fracture. Altering the annealing pro-
cesses does not modify the fracture mode of the quenched
and tempered material. However, it is important to mention that
the 900AQT crack near the notch, which corresponds to the
Figure 6. XRD patterns of 60Cr16MoMA steel treated by various heat
treatments. lower impact energy. The experimental results indicate that
the annealed austenitizing temperature of 860 °C, shows a favor-
able balance between hardness and impact toughness.
grow. Despite the great hardness of the carbide, there is a specific The fracture exhibits a combination of a quasi-cleavage and
spacing because the carbides are distributed uniformly through- dimple, accompanied by the carbides within it. This fracture type
out the ferrite. Under stress and deformation, the ferrite will is classified as a quasi-cleavage fracture, which is further charac-
become the main part of the deformation. Carbides will become terized by microplastic deformation of the matrix. The fractured
the main part of the deformation only when they are very close carbides and the formation of cleavage planes along these coarse
Figure 7. a) Hardness for annealed steel, b) hardness and c) impact energy for Q&T steel with different annealed austenitizing temperature.
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Figure 8. Macro morphology of the impact fracture.
Figure 9. SEM images of the fracture surface of 60Cr16MoMA: a) 840AQT; b) 860 AQT; c) 880 AQT; and d) 900 AQT.
carbides suggest that the fracture behavior is brittleness. shows congruence with the reported fluctuations in hardness
The electron diffraction spectroscopy (EDS) patterns provide evi- during the heat treatment procedures.
dence that the carbide fracture is M23C6, as shown in Figure 9a. The 3D morphology of the wear zone in the material, along
Furthermore, the impact test resulted in the formation of micro with sectional photographs, is comprehensively shown in
voids. Figure 11. It is obvious that wear generally concentrates at the
central region of the wear track, which can be identified by
the existence of noticeable grooves and plastic deformation.
3.3. Wear Properties Interestingly, the wear traces exhibit the least depth when the
annealing procedure is 860AQT. Increasing the holding temper-
Figure 10a shows the variations in the steady-state coefficient of ature significantly deepens (Figure 11c) or widens (Figure 11d)
friction (COF) obtained throughout different heat treatment pro- the wear traces. Notably, the 900AQT shows a wider track com-
cedures. There are clearly noticeable differences in the COF that pared to the other specimens. During the wear process, the
can be observed among various processes. In addition to this, matrix is removed, causing carbides to protrude from the sur-
Figure 10b illustrates the mean COF at steady-state for the mate- face. Besides, not only the Al2O3 ceramic ball grind against car-
rial. It can be seen that as the austenitizing temperature bides, but the carbides also reciprocally grind the ball.
(annealed) increases, the steady-state average COF of the material Remarkably, the 900AQT variant features coarser carbides, inten-
decreases, and approaches to the minimum at 860AQT, after sifying ball wear. Consequently, this results in the transforma-
which there is an increase in the average friction coefficient tion of the spherical surface into a flat one, contributing to a
as the annealed soaking temperature rises. The above trend wider wear track in the sample.
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Figure 10. COF of materials for different heat treatment: a) coefficient of friction; and b) average coefficient of friction.
Figure 11. The 3D morphology of the wear zone: a) 840AQT; b) 860AQT; c) 880AQT; and d) 900AQT.
According to Figure 11, the wear volume of the material is mea- Compared to 860AQT (Figure 12b), the sliding-induced
sured for several heat treatment processes. It is observed that the grooves in the cases of 840AQT (Figure 12a), 880AQT
wear volume for 860AQT is the lowest among the processes exam- (Figure 12c), and 900AQT (Figure 12d) indicate an increase in
ined, indicating superior wear resistance compared to the other both depth and quantity. Significantly, the wear surface of
processes. Meanwhile, the wear volume of 840AQT and 860AQT exhibits a noteworthy decrease in both the quantity
900AQT are similar in volume. Despite the higher hardness of and size of spalled pits. In contrast, for 880AQT and 900AQT,
840AQT, the wear volume remains similar to 900AQT. This a large number of continuous spalled pits appeared, which are
can be attributed to the friction-induced peeling of carbides during accompanied by oxidation in the vicinity of these pits. During
the wear process and the elevated probability of abrasive particle the abrasion process, some of the carbides in the specimen
generation due to lower toughness in both 840AQT and 900AQT. can experience adsorption onto the surface of the Al2O3 ceramic
The wear surfaces found across several heat treatment proce- ball as a result of overheating. During the subsequent frictional
dures are shown in Figure 12. Despite the specific methodology interaction, the adsorbed carbides can play a role in the develop-
applied, the wear failure modes exhibited by the HCMSS are ment of laminar spalled zones or micro-voids.
similar and show a combination of abrasive and adhesive wear Furthermore, as shown in Figure 7c, exhibits diminished
mechanisms. The wear appearance observed in the samples after toughness attributed to larger carbide paricles. This renders
Q&T is significantly affected by the austenitizing temperature the matrix susceptible to cracking under external force ulti-
employed during the annealing process. mately, resulting in surface fatigue wear shown in Figure 12.
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Figure 12. Wear surface of different specimens: a) 840AQT, b) 860AQT, c) 880AQT, and d) 900AQT.
In contrast, 860AQT, characterized by higher toughness, mani- thickness of the plastic deformation layer of sample 860AQT
fests the least occurrence of spalled pits. was the smallest with 3.1 μm, then it had the best wear property,
The cross-sectional microstructure of specimens 840AQT– as shown in Figure 13b.
900AQT after 30 min wear test is shown in Figure 13. After wear Huang et al. have discovered in which the protective role
test, a plastic deformation layer was formed on the subsurface of of micron-sized particles on the surface of the matrix.[36]
the specimen, and the thickness of the plastic deformation layer When the height of these particles is higher than the wear sur-
changed with microstructure after QT treatment. Compared with face, the function of which is to reduce micro-cutting by reducing
the initial microstructure after QT, the martensite matrix in the the contact between the matrix and abrasive particles.
deformation layer had been deformed to a certain extent, and the During the early stages of wear, it is possible for micron-sized
morphology and size of the undissolved carbide had changed M23C6 particles to be present in the martensitic matrix, exhibit-
obviously. As shown in Figure 13a, the thickness of the plastic ing alignment either parallel to or shorter than the height of the
deformation layer of 840AQT was the largest, about 6.3 μm, so worn surface. This will not effectively provide protection for the
the wear property of sample 840AQT was the worst. The matrix. This highlights the fact that a better level of wear
Figure 13. Micrographs of cross sections of samples under different temper processes: a) 840AQT, b) 860AQT, c) 880AQT, and d) 900AQT.
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resistance is directly associated with increased hardness of the Nonetheless, adopting higher austenitizing temperatures neces-
matrix at the early stage of wear. The matrix is exposed and pro- sitates a lengthier cooling period to attain the spheroidizing tem-
tected by the emergence of micron-sized M23C6 precipitates by perature. During both the cooling stage and the initial stage of
continuous sliding. It is important to note that when the matrix is isothermal treatment at 760 °C, the divorced eutectoid transfor-
insufficient to support the micronized particles, the carbide will mation takes place. The interfacial energy decreases and the size
peel off from the surface experiencing wear. These incidents of the carbide and its instantaneous growth rate increases again
significantly diminish wear resistance. Moreover, changes in as the temperature decreases. The following relationship exists
the temperature have the potential to influence the formation between carbide size and austenitizing temperature during
of larger M23C6 particles by precipitation. Consequently, this spheroidizing annealing at varying austenitizing temperatures.
phenomenon can weaken the capacity to support these particles
of the matrix, eventually resulting in the fracture and separation 4.1.1. Stage I (840–860 °C)
of carbides, leading to a subsequent decrease in wear resistance.
At this stage, the primary determinant of carbide size is predom-
inantly the austenitizing temperature. The influence of heat
4. Discussion treatment duration on the carbide size exhibits a relatively milder
impact compared to the potency of the holding temperature. This
4.1. Carbide Ripening During the Annealing Process due to the relatively shorter cooling stage required to attain the
spheroidizing temperature.
According to the LSW theory,[37] there exists the following
(Equation (1)) relationship between the radius of carbides (dr
dt ) 4.1.2. Stage II (860–900 °C)
and the temperature (T ):
At this stage, the size of the carbide is mainly affected by the
dr 2DM C α0 σ s V αm 1 1
¼ (2) cooling time to the spheroidizing temperature. As the cooling
dt r½C β Cαr KT r r
time extended, the size of the carbide increases exponentially,
where DM represents the diffusion coefficient of alloying ele- accompanied by a corresponding surge in the instantaneous
ment in the matrix, r represents the average radius of particles, growth rate according to Equation (1).
Cβ represents the carbides concentration, K is the gas constant. T
is absolute temperature, V αm is partial molar volume of precipi- 4.2. Effect of Phase Interface Bonding Strength between
tates, σ s is interfacial energy of carbides and matrix. Carbide/Matrix on the Toughness and Wear Resistance
During the annealing process, according to Equation (1), this
formula indicates that carbides with radiuses above the average Martensite has a certain level of plasticity, whereas carbide exhib-
radius could increase, whereas carbides with radiuses below the its resistance to plastic deformation.[19] Due to the differences in
average radius would dissolve. As shown in Figure 14, an the mechanical properties of carbide and matrix in steel, coarse
increase in austenitizing temperature promotes the small-sized carbide particles are more likely to cause stress concentration.
carbides dissolution accompanied by the area of large-sized car- M23C6 carbide has an incoherent interface boundary with the
bide decrease. This process, however, encompasses a subsequent matrix, as shown in Figure 15b. The atomic arrangement at
phase wherein carbon atoms within the carbon-rich regions, the interface between M23C6 and martensite exhibits disorder.
formed by the dissolution of smaller carbides, spontaneously dif- Furthermore, there exists a significant difference in the lattice
fuse into the carbon-poor region surrounding larger carbides. parameters between M23C6 (0.58 nm) and martensite
Figure 14. Schematic diagram of carbide growth during the spheroidizing annealing.
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Figure 15. a) TEM image and b) HRTEM of Q&T 60Cr16MoMA steel.
(0.19 nm). It is evident that M23C6 exhibits an incoherent inter- However, for HCMSS, carbide fracture and exfoliation are the
face with martensite. The large-sized M23C6 trends to break up at main mechanisms causing matrix failure.[21] LAGBs exhibit
the boundary easily, thereby promoting crack initiation. With strong interface adhesive strength, which effectively reduces
increased stress concentration, only carbide fracture or cleavage stress concentration effects and hinders the fracture of carbides,
can realize coordinated deformation. such as peeling off from the matrix. Therefore, as the percentage
Figure 16 provides a statistical analysis of the grain boundary of LAGBs decreases, there is a noticeable decline in wear
angles of the steel with different annealing temperatures. It is resistance.
worth mentioning that a rise in the austenitizing temperature
during the process of annealing leads to an obvious change in
the grain boundary angles of the material after the Q&T process. 5. Conclusion
In particular, 860AQT demonstrates a prevalence of 46.4% low
angle grain boundaries (LAGBs, <15°), whereas 880AQT and In this article, the effect of different annealing processes on the
900AQT display lower proportions of LAGBs, measuring at microstructure as well as the properties of HCMSS after Q&T of
29.3% and 25.1%, respectively. Meanwhile, there is a notable rise the material was investigated. The main conclusions are as
observed in the proportion of high angle grain boundaries follows: 1) With increasing annealing temperature, the average
(HAGBs, >15°). carbide size of HCMSS is minimized at 860 °C for 90 min.
The prevailing belief suggests that the HAGBs can hinder Continuing to raise the temperature leads to an increase in
the cracks extension under impact or wear conditions.[38,39] the average carbide size to 0.8 μm; the peak of the carbide size
Figure 16. EBSD analyses of grain boundary angles with different heat treatment processes: a) 860AQT; b) 880AQT; c) 900AQT; and d) statistical
distribution of grain boundary misorientation angles.
l
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Effect of Spheroidizing Annealing Process on Microstructure and Properties of Quenching and Tempering 60Cr16MoMA Martensitic Stainless Steel

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Effect of Spheroidizing Annealing Process on Microstructure and Properties of Quenching and Tempering 60Cr16MoMA Martensitic Stainless Steel

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RESEARCH ARTICLE

Effect of Spheroidizing Annealing Process on

necessary to obtain a softened matrix

Figure 1. Specimens and heat treatment parameters.

1.4I γ interspersed with carbide precipitates. Distinctive carbide mor-

together or even in direct contact.[35] At different austenitizing

Figure 8. Macro morphology of the impact fracture.

Figure 15. a) TEM image and b) HRTEM of Q&T 60Cr16MoMA steel.

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