coatings
Article
Very High Cycle Fatigue Properties of 18CrNiMo7-6 Carburized
Steel with Gradient Hardness Distribution
Shaopeng Yang 1,2, *, Peifeng Cheng 1,3 , Fangzhong Hu 2 , Wenchao Yu 1 , Chi Zhang 4 , Kaizhong Wang 2
and Maoqiu Wang 1, *






Citation: Yang, S.; Cheng, P.; Hu, F.;
Yu, W.; Zhang, C.; Wang, K.; Wang, M.
Very High Cycle Fatigue Properties of
18CrNiMo7-6 Carburized Steel with
Gradient Hardness Distribution.
Coatings 2021, 11, 1482. https://
doi.org/10.3390/coatings11121482
Academic Editor: Pier Luigi Bonora
Received: 15 August 2021
Accepted: 23 October 2021
Published: 2 December 2021
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
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iations.
Copyright: © 2021 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Coatings 2021, 11, 1482. https://doi.org/10.3390/coatings11121482
1 Institute of Special Steel, Central Iron and Steel Research Institute (CISRI), Beijing 100081, China;
chengpeifeng_1@163.com (P.C.); yuwenchao@nercast.com (W.Y.)
2 Technical Center, Masteel Co., Ltd., Ma’anshan 243000, China; fangzhonghu@163.com (F.H.);
wkzzkwwkz@sina.com (K.W.)
3 School of Materials Science and Engineering, Kunming University of Science and Technology,
Kunming 650093, China
4 Key Laboratory of Advanced Materials of Ministry of Education, School of Materials Science and Engineering,
Tsinghua University, Beijing 100084, China; chizhang@tsinghua.edu.cn
* Correspondence: yangshaopengpm@foxmail.com (S.Y.); maoqiuwang@hotmail.com (M.W.)
Abstract: As research of the high cycle fatigue of carburized gear steel could not meet the status quo
of longer and longer service lives, research of very high cycle fatigue (VHCF) performance has become
the focus of current research. The VHCF properties of case-hardening steel 18CrNiMo7-6 after being
carburized with gradient hardness distribution were investigated by means of ultrasonic fatigue
tests. The results showed that the carburized specimens with a case hardness of 705 HV and core
hardness of 530 HV showed VHCF phenomenon, and the fatigue lives continuously increased to
even 109 cycles as the stress amplitude decreased to about 500 MPa. Observations of the fracture
surfaces of the fatigue specimens showed that the fatigue crack initiation sites were located in the
transition area with the hardness at about 580 HV. It was found that the transition area had low VHCF
properties, since the core did not show VHCF phenomenon, and the case had a higher hardness.
A fine microstructure was observed in the granular bright facet (GBF) area, and the stress intensity
factor ∆KGBF was measured to be 3.04 MPa·m−1/2 . The 109 cycles fatigue life was predicted based
on the inclusion size, and the 1010 cycles fatigue life was 490 MPa based on the prediction model.
Keywords: carburized gear steel; very high cycle fatigue; stress intensity factor; fatigue prediction
model
1. Introduction
The high-frequency facilities uesd to study the VCHF performance of homogeneous
materials have become a subject of extensive research in recent decades. Researchers found
that when the fatigue life was beyond 109 cycles, fatigue failure could still occur and that the
conventional high cycle fatigue limit could not reflect from the VHCF S-N data [1–3]. The
high cycle fatigue of bearing steel and some high-strength steels had obvious fatigue limits,
but the cycle life of VHCF still increased with the decrease of the stress amplitude [4,5].
Sakai et al. [6] reported ultra-high cycle fatigue properties of SUJ2 steel by rotary bending
fatigue specimens and found a double S-N curve. Under high stress, the crack initiated
on the surface, but under low stress, the failure still occurred, and the crack initiated in
the interior of the sample. A granular bright facet (GBF) region was formed around the
internal nonmetallic inclusion beyond 106 cycles and then extended into the fisheye zone.
Sakai et al. [7] studied the ultra-high cycle fatigue of SUJ steel through axial loading
specimens, and the S-N curve showed a single line tendency. For ultra-high cycle fatigue,
the formation of a GBF region, namely fine granular area (FGA) or optical dark area
(ODA), became a typical feature [8,9], so the regions of GBF were called the crack initiation
characteristic zones of ultra-high cycle fatigue. In addition, many researchers have revealed
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Coatings 2021, 11, 1482 2 of 15

that the GBF region consumed the majority of the total fatigue failure cycle numbers [10–12].
The life consumed by the GBF region was even higher than 99% when the total fatigue life
was beyond 108 cycles [10].
The formation mechanism of the crack initiation characteristic region has become the
focus of research on ultra-high cycle fatigue. Hong et al. [13,14] reported the microstruc-
ture distribution and formation mechanism of a GBF region of high-strength steel under
ultra-high cycle fatigue and proposed the numerous cyclic pressing (NCP) model of the
nanograin layer in the crack initiation region and indicated that repeated cyclic stress was
the main reason for the formation of a nanograin layer in the GBF region. After carburizing,
the surface of carburized gear steel has a hardness gradient, which makes the study of ultra-
high cycle fatigue more complicated [15–17]. Nehila et al. [18,19] indicated the ultra-high
cycle fatigue performance of case-hardened steel with a hardness gradient in the early stage
and found that the failure of the fatigue specimens would still occur beyond 107 cycles,
and the stress amplitude of the surface failure was much higher than that of the internal
failure. Marines Garcia et al. [20] showed the growth mechanism of a short crack to a long
crack in SAE8620 gear steel under ultra-high cycle fatigue failure. Li et al. [21] studied the
crack initiation mechanism of carburized gear steel. The failure process of ultra-high cycle
fatigue was proposed as the inclusion of a fine granular area (FGA)—fisheye (FIE), final
crack growth zone (FCGZ), and material failure zone (MFZ), and the life was predicted.
In a previous work, we investigated the VHCF properties of case-hardening steel
with thorough-carburized specimens for cases with pseudo-carburized specimens for the
core [22]. Some differences were found for the two kinds of specimens, and the carburized
cases should be the weak location, since the pseudo-carburized specimens did not show
the VHCF fatigue phenomenon. It is still unclear whether VHCF failure could occur or
not and where the weak location was for carburized specimens with gradient hardness
distribution. It is also needed to investigate the VHCF behavior of carburized specimens
with gradient hardness distribution for real gears always carburized with a gradient
hardness distribution. As the core component of carburized gear steel 18CrNiMo7-6 used
in heavy-duty locomotive and rail transit, and the demand for the long lives of these
important components, it is particularly important to study the ultra-high cycle fatigue life
performance of carburized gear steel 18CrNiMo7-6 [23,24].

2. Materials and Methods

The experiment materials used in this investigation were low-carbon gear steel, and the
composition is listed in Table 1. All the specimens from 80-mm-diameter hot-rolled bars were
machined hour-glass shapes with finishing margins. Then, the carburizing heat treatment
process was conducted, as shown Figure 1. The specimens were carburized at 930 ◦ C firstly at
a carbon potential of 1.20% for 6.5 h and, then, at a carbon potential of 0.68% for 6 h, followed
by carbon diffusion at 860 ◦ C for 1 h. The gas-quenching specimens were then tempered at
650 ◦ C for 2 h and air-cooled. After being tempered, the specimens were heated at 840 ◦ C
for 2 h and oil-quenched in a furnace (Beijing Research Institute of Mechanical & Electrical
Technology, Beijing, China) with a carbon potential of 0.70% to avoid decarburization. At last,
the twice-low-temperature tempering was conducted at 180 ◦ C for 6 h. After the carburizing
heat treatment, all the specimens were finely ground to the final dimensions of the USF-
2000 ultrasonic fatigue testing machine (Shimadzu, Kyoto, Japan) to ensure surface accuracy
and axiality, as shown in Figure 2.

Table 1. 18CrNiMo7-6 chemical composition (wt.%).

Element C Si Mn P S Cr Ni Mo
18CrNiMo7-6 0.16~0.19 0.15~0.35 0.45~0.65 ≤0.0015 ≤0.0020 1.50~1.80 1.40~1.70 0.20~0.30
Coatings 2021, 11, x FOR PEER REVIEW 3 of 15

Table 1. 18CrNiMo7-6 chemical composition (wt.%).

Element C Si Mn P S Cr Ni Mo
Table 1. 18CrNiMo7-6 chemical composition (wt.%).
Coatings 2021, 11, 1482
18CrNiMo7-6 0.16~0.19 0.15~0.35 0.45~0.65 ≤0.0015 ≤0.0020 1.50~1.80 1.40~1.70 0.20~0.30 3 of 15
Element C Si Mn P S Cr Ni Mo
18CrNiMo7-6 0.16~0.19 0.15~0.35 0.45~0.65 ≤0.0015 ≤0.0020
carburized 1.50~1.80 1.40~1.70 0.20~0.30

carburized
930℃/6.5 h 930℃/6 h

,℃
860℃/1 h 840℃/2 h

Temperature
650℃/2 h

Nitroge
930℃/6.5 h 930℃/6 h

,℃
860℃/1 h 840℃/2 h

n slow gen slow cool

1.20 % 0.68 % 0.68 %

Temperature

OQ
650℃/2 h

Nitro

AC
cooling
0.70 %
180℃/3 h 180℃/3 h
1.20 % 0.68 % 0.68 %

AC

AC
OQ
AC
0.70 %
180℃/3 h 180℃/3 h

ing

AC

AC
Time,t

Time,t
Figure 1. Carburizing heat treatment process, and the underlined data indicates the carbon poten-
Figure 1. Carburizing heat treatment process, and the underlined data indicates the carbon potential.
tial.
Figure 1. Carburizing heat treatment process, and the underlined data indicates the carbon poten-
tial.

Figure
Figure 2. 2. Final
Final machined
machined dimensions
dimensions and
and shape
shape of of
thethe specimen.
specimen.

In order to better characterize the microstructure of the specimens after carburizing,

FigureIn2.order to better characterize
Final machined theshape
dimensions and microstructure of the specimens after carburizing,
of the specimen.
several 2020
several mm mm× 20 × mm20 mm× 30×mm 30 mm
cuboid cuboid metallographic
metallographic specimens
specimens werewere
placed placed
insideinside
the
the same
sameInfurnace. furnace.
order toThe better The specimens
characterize
specimens that needed
the microstructure
that needed to be characterized
of the specimens
to be characterized were cut
were cut after by linear cutting.
carburizing,
by linear cutting.
Aftercarburizing,
several
After carburizing,
20 mm × 20the thecarburizing
mm carburizing
× 30 mm cuboid layermetallographic
layer structureof
structure ofthe
thespecimens
specimenswere
specimens was observed
was observed
placed inside by
by optical
the
opti-
calmicroscopy
same furnace. (OM,
microscopy The
(OM, Olympus
specimens
Olympus GX51,
that Tokyo,
needed
GX51, toJapan),
Tokyo, and
beJapan), thethe
characterized
and residual
were austenite
cut
residual by linear
austenite content was
cutting.
content
measured by XRD (Bruker, Karlsruhe, Germany), with martensite by scanning electron
After carburizing,
was measured by the
XRD carburizing layer structure
(Bruker, Karlsruhe, of the with
Germany), specimens
martensitewas observed
by scanning by opti-
elec-
microscopy (SEM, FEI Company, Hillsboro, OR, USA). Due to the hardness gradient, the
cal
tronmicroscopy
microscopy(OM, (SEM, Olympus
FEI Company,GX51, Hillsboro,
Tokyo, Japan), and the
OR, USA). Due residual austenitegradient,
to the hardness content
microstructure and carbon contents from the surface to the center were not homogeneous,
was measured by XRD
the microstructure and (Bruker, Karlsruhe,
carbon contents from Germany),
the surface with martensite
to the by scanning
center were not homoge- elec-
and the distribution of residual austenite was also different. The retained austenite contents
tron
neous,microscopy (SEM, FEI Company,
and the distribution of residualHillsboro,
austenite was OR, also
USA). Due to the
different. Thehardness
retained gradient,
austenite
were measured at 0, 0.3, 0.6, 0.9, 1.2, and 1.5 mm from the surface, respectively. The sectional
the microstructure
contents were measured and carbon contents
at 0, 0.3, 0.6, 0.9, from
1.2,the
andsurface
1.5 mmtofrom the center were not
the surface, homoge-
respectively.
hardness distribution from the surface to the center was measured using a Vickers hardness
neous, and thehardness
The sectional distribution of residual
distribution austenite
from was also
the surface to thedifferent.
center was The retained
measured austenite
using a
tester (Wilson Wolpert, Norwood, MA, USA).
contents were measured
Vickers hardness at 0, 0.3,Wolpert,
tester (Wilson 0.6, 0.9, Norwood,
1.2, and 1.5MA, mmUSA).
from the surface, respectively.
In the present experiment, the ultra-high cycle fatigue test (USF-2000, Shimadzu, Ky-
The sectional hardness
In the present distribution
experiment, thefrom the surface
ultra-high cycletofatigue
the center
test was measured
(USF-2000, using a
Shimadzu,
oto, Japan) was carried out under axial ultrasonic loading in the VHCF regime. The stress
Vickers hardness
Kyoto, Japan) was tester (Wilson
carried Wolpert,
out under axialNorwood,
ultrasonic MA, USA).in the VHCF regime. The
loading
ratio was R = −1, and the frequency was about 20 kHz. The fatigue test was carried out
stressInratio
the was
present
R = experiment,
−1, and the the ultra-high
frequency was cycle20
about fatigue
kHz. test fatigue
The (USF-2000, was Shimadzu,
◦
at room temperature (25 C). Due to the faster frequency, the stress parttest carried
of the specimens
Kyoto,
out at Japan)
room was
temperaturecarried out
(25 under
°C). Due axial
to the ultrasonic
faster loading
frequency,
heated up faster. In order to prevent overheating, compressed air was used for cooling, in
the the VHCF
stress part regime.
of the The
speci-
stress
mens ratio
heated wasup R = −1,
faster. and
In the
order frequency
to prevent was about
overheating, 20 kHz. The
compressed
and an intermittent loading mode of 150 s was adopted to further decrease the influence fatigue
air wastest was
used carried
for cool-
outofat
ing, and
theroom temperature
an intermittent
ultra-high (25 °C).
loading
frequency. Due
mode
The toofthe
fracture faster
s wasfrequency,
150morphology adopted andtothe stress
further
the partcomposition
decrease
chemical of the
thespeci-
influ-of
mens
ence heated
of up faster.frequency.
the ultra-high
nonmetallic inclusions Inwere
orderanalyzed
toThe
prevent byoverheating,
fracture morphology
scanning compressed
electron and air was
the chemical
microscopy used
(SEM) for cool-
composition
and energy
ing,
dispersive X-ray spectrometer (EDS), and the distribution and size of the FIE and influ-
and an intermittent loading mode of 150 s was adopted to further decrease the GBF re-
ence of the
gions wereultra-high
measured. frequency. The fracture
Using transmission morphology
observation, FIBandwasthe usedchemical composition
to cut small specimens
for the transmission electron microscopy (TEMFEI Company, Hillsboro, OR, USA) test. The
TEM and electron back scatter diffraction (EBSD) methods were also used to observe the
cross-section of the GBF area of the fracture surface, after the fractured specimen was cut
and prepared according to References [25,26].
 to observe the cross-section of the GBF area of the fracture surface, after the fractured
specimen was cut and prepared according to References [25,26].

3. Results and Discussion

Coatings 2021, 11, 1482 4 of 15
3.1. Microstructure and Hardness
Figure 3 presented the microstructural features of the carburized layer on the surface
of the carburized3.specimen,
Results andand Figure 4 presented the microstructural features 1.0 mm
Discussion
away from the surface of the carburized
3.1. Microstructure and Hardnessspecimen by OM and SEM, respectively. Figure
3 illustrates that the microstructure
Figure 3 presented ofthe
themicrostructural
carburized layer consisted
features of acicular
of the carburized layermartensite
on the surface
and retained austenite, and carbides
of the carburized could
specimen, andbe observed
Figure in thethecarburized
4 presented layer.
microstructural Figure
features 1.0 4
mm
shows that the microstructure at 1.0 mm away from the surface of the carburized speci- 3
away from the surface of the carburized specimen by OM and SEM, respectively. Figure
illustrates that the microstructure of the carburized layer consisted of acicular martensite
men mainly consisted of lath martensite and carbide, and there was a little residual aus-
and retained austenite, and carbides could be observed in the carburized layer. Figure 4
tenite and acicular martensite.
shows The microstructure
that the microstructure characteristics
at 1.0 mm away of these
from the surface different specimen
of the carburized loca-
tions are differentmainly
mainly because
consisted themartensite
of lath carbon content of the
and carbide, andsection
there wasisanot
littleuniform after
residual austenite
and acicular martensite. The microstructure characteristics
the carburizing heat treatment. The carbon content of the surface is the highest, and the of these different locations
are different
carbon content decreases mainly
with because the
the distance carbon
from thecontent
surface of and
the section is not uniform
eventually tends toafter
thethe
carburizing heat treatment. The carbon content of the surface is the highest, and the
matrix carbon content
carbon[27]. Due
content to the difference
decreases in carbon
with the distance contents,
from the the eventually
surface and martensite phase
tends to the
transformation structure and phase transformation temperature are different [28].
matrix carbon content [27]. Due to the difference in carbon contents, the martensite phase The
high carbon will form acicular structure
transformation martensite, and low
and phase carbon will
transformation form lathare
temperature martensite. TheThe
different [28].
transformation of high-carbon martensite in the formation process is not complete, with aThe
high carbon will form acicular martensite, and low carbon will form lath martensite.
transformation of high-carbon martensite in the formation process is not complete, with
certain amount of residual austenite and low-carbon martensite with a little amount of
a certain amount of residual austenite and low-carbon martensite with a little amount of
residual austenite.residual austenite.

(a) (b)
Figure 3. OM
Figure 3. and
OMSEM
andofSEM
the carburizing layer: (a) layer:
of the carburizing optical(a)
microscope microstructure
optical microscope of the carburizing
microstructure layercarbu-
of the and
(b) electron microscope microstructure of the carburizing layer.
rizing layer and (b) electron microscope microstructure of the carburizing layer.
Since the surface of the carburized layer contains a large amount of residual austenite,
it has a significant effect on the hardness and fatigue. The content of the retained austenite
at different depths of the carburized specimen was measured by XRD, with the spectra
shown in Figure 5. According to the peak strength measured by XRD, the peak strength
of martensite and austenite was calculated by using Jade software, and the content of
residual austenite was calculated according to different peak strengths. The maximum
residual austenite content of the carburized specimen is 32% on the largest surface of the
specimen, and the residual austenite content decreases gradually with the increase of the
depth from the surface. The residual austenite contents at 0.3, 0.6, 0.9, 1.2, and 1.5 mm
of distance from the sample surface are 21%, 11%, 11%, 4%, and 3%, respectively. From
the distribution of the residual austenite content in the carburized layer, the relationship
between the residual austenite content and the depth of the carburized layer is nonlinear.
The carburization process can increase the surface hardness and improve the fatigue and
wear resistance of the material; at the same time, due to the high surface carbon content of
carburizing, the residual austenite content of the surface due to high-carbon martensite
cannot be completely transformed and increased [15,29].
 (a) (b)
Figure 4. OM and SEM images of the area 1.0 mm from the surface: (a) optical microscope micro-
structure image and (b) scanning electron microscope microstructure image.
R PEER REVIEW
Coatings 2021, 11, 1482
5 of 15 5 of 15
Since the surface of the carburized layer contains a large amount of residual austen-
ite, it has a significant effect on the hardness and fatigue. The content of the retained aus-
tenite at different depths of the carburized specimen was measured by XRD, with the
spectra shown in Figure 5. According to the peak strength measured by XRD, the peak
strength of martensite and austenite was calculated by using Jade software, and the con-
tent of residual austenite was calculated according to different peak strengths. The maxi-
mum residual austenite content of the carburized specimen is 32% on the largest surface
of the specimen, and the residual austenite content decreases gradually with the increase
of the depth from the surface. The residual austenite contents at 0.3, 0.6, 0.9, 1.2, and 1.5
mm of distance from the sample surface are 21%, 11%, 11%, 4%, and 3%, respectively.
From the distribution of the residual austenite content in the carburized layer, the rela-
tionship between the residual austenite content and the depth of the carburized layer is
nonlinear. The carburization process can increase the surface hardness and improve the
fatigue and wear resistance (a) of the material; at the same time, due (b)to the high surface car-
bon content of carburizing, the residual austenite content of the surface due to high-car-
Figure
Figure 4. 4.
OM OMandand
SEMSEM images
images of the of the
area 1.0area 1.0 mm
mm from from the
the surface: (a)surface: (a) optical
optical microscope microscopeimage
microstructure micro-
and
bon(b)martensite
scanningimage
structure
cannot
electronand be
microscope completely
microstructure
(b) scanning
transformed
image.
electron
and increased
microscope microstructure image.
[15,29].

35
Since
(110)α
the surface of the carburized layer contains a large amount of residual austen-
carburized
ite, it has a significant effect on the hardness and fatigue. 30 The content of the retained aus-
Residual austenite content/%

tenite at different depths of the carburized specimen 25 was measured by XRD, with the
(111)g
spectra shown in Figure 5. According to the peak strength measured by XRD, the peak
Intensity

20
strength of martensite and austenite was calculated by using Jade software, and the con-
(200)g (211)α
tent of residual austenite
(200) α(220)g
was calculated according15to different peak strengths. The maxi-
(311)g RA : 32%
0.0

mum residual austenite contentRA of :the

21% carburized specimen is 32% on the largest surface
0.3
10
RA : 11%
0.6
of the specimen, and the residual austenite
RA : 11%
0.9
content decreases gradually with the increase
5
RA ：4%
of the depth from the surface. The residual austenite contents at 0.3, 0.6, 0.9, 1.2, and 1.5
1.2
RA ：3%
1.5
mm of distance from the sample surface are 21%,011%, 0.0
11%,
0.2
4%,0.6and
0.4 0.8
3%,1.0
respectively.
1.2 1.4 1.6
40 50 60 70 80 90 100 110 120 130 140
From the distribution 2q/°of the residual austenite content in the carburized
Distance from layer,
surface/μm the rela-
tionship between the (a)residual austenite content and the depth of the (b)carburized layer is
nonlinear. The carburization process can increase the surface hardness and improve the
The XRD patterns
Figure5.5.The
Figure of theofexperimental steel at different depths of 0~1.5depths
mm from the0~1.5 carburized surface show
fatigue andXRD wear patterns
resistance the
of experimental
the material; at steel
theatsame
different
time, due toof the highmm fromcar-
surface the car-
different fractions of retained austenite (RA): (a) XRD RA results and (b) RA changes with the surface distance.
burized surface show
bon content different fractions
of carburizing, the residual of retained
austenite austenite
content(RA):of the(a)surface
XRD RA due results and (b) RA
to high-car-
changes with the surface
bon martensite cannotdistance.
beThe cross-sectional
completely distributionand
transformed of the microhardness
increased in the carburized specimen is
[15,29].
shown in Figure 6. It can be seen that the hardness decreased linearly with the distance
The cross-sectional from about 705 HV of
distribution in the
thenear-surface
microhardness
35 case to aboutin the 530carburized
HV in the core. If a harnessisof
specimen
(110)α 550 HV is defined as the critical value of hardening, the effective case depth was about
shown in Figure 6. It 1.4 can mm, beindicating
seen that that the hardness
the specimens 30
weredecreased linearly
carburized deeply under with the distance
carburized
the present carburizing
Residual austenite content/%

from about 705 HV in process. the near-surface

Compared with casethetomatrix
about 530 HV
25 hardness in the
of 442 HV forcore.the If a harnesssteel
experimental of 550
after
(111)g
HV is defined as the pseudo-carburizing
critical value of[22,30], the hardness
hardening, of the carburized
the effective case depthspecimens was wasabout
remarkably
1.4
Intensity

20
increased by the carburizing treatment. Figure 6 presents the cross-section microhardness
mm, indicating that the
(200)g
specimens
of the fatigue
(211)
were carburized
specimens deeplyprocess.
after the carburizing underItthe canpresent
be seen that carburizing
the hardness
α 15
(200)α(220)g (311) RA0.0: 32%
decreased linearly g with the distance, from about 705 HV in the near-surface case to about
RA0.3: 21%
10
530 HV in the RA core.
0.6 : If
11% a harness of 550 HV is defined as the critical value of hardening,
the effective case RA0.9depth
: 11% was about 1.4 mm, indicating that the specimens were carburized
5
RA1.2：4%
deeply under RA the
1.5
present
：3%
carburizing process. Compared with a matrix hardness of
442 HV for the pseudo-carburizing 0steel 0.0 [22],
0.2 the
0.4 hardness
0.6 0.8 of1.0the1.2
carburized
1.4 1.6 specimens
40 50 60 70 80 90 100 110 120 130 140
was
2q/°
tremendously increased. Zhao et al. [30] indicated that,
Distance from although the carburization
surface/μm
changed the distribution of the microstructure and hardness, the distribution of the elastic
(a) (b)
Figure 5. The XRD patterns of the experimental steel at different depths of 0~1.5 mm from the car-
burized surface show different fractions of retained austenite (RA): (a) XRD RA results and (b) RA
changes with the surface distance.
 530 HV in the core. If a harness of 550 HV is defined as the critical value of harden
effective case depth was about 1.4 mm, indicating that the specimens were car
deeply under the present carburizing process. Compared with a matrix hardnes
HV for the pseudo-carburizing steel [22], the hardness of the carburized specim
Coatings 2021, 11, 1482 6 of 15
tremendously increased. Zhao et al. [30] indicated that, although the carbu
changed the distribution of the microstructure and hardness, the distribution of th
modulus on the cross-section did not change much, mainly because the elastic m
modulus on the cross-section did not change much, mainly because the elastic modulus
was aninherent
was an inherent property
property of theof the material,
material, and the
and the elastic elasticwas
modulus modulus was almost c
almost constant
when theatomic
when the atomic bond
bond wasdestroyed.
was not not destroyed.

720

700 Carburized
680

660
Hardness/HV

640

620

600

580

560

540
Effective carburized case depth
520

500
0 200 400 600 800 1000 1200 1400 1600

Distance from surface/μm

Figure 6.6.Cross-sectional
Figure Cross-sectionaldistributions of microhardness
distributions of the experimental
of microhardness steel.
of the experimental steel.
3.2. S-N Curve
3.2. S-N
For aCurve
long time, the safety life method has been used to replace the defect tolerance
methodFor in athe
long time,
fatigue the safety
strength design life
and method
analysis ofhas been used
structural members to replace the defect to
in engineering.
The design and analysis procedures are based on smooth
method in the fatigue strength design and analysis of structural members specimens obtained from fa-in engin
tigue tests of S-N or Wöhler curves obtained from fatigue testing on smooth specimens.
The design and analysis procedures are based on smooth specimens obtained from
A traditional S-N data curve is characterized by three asymptotic lines. The middle part
tests
of the of S-Nwith
curve, or Wöhler
a constant curves
slope, obtained from
presents that fatiguelife
the fatigue testing
in terms onofsmooth
the number specimen
ditional
of cycles toS-N data
failure Nfcurve
increasesis characterized
with the decreaseby of three asymptotic
the stress amplitude.lines.
FigureThe middle pa
7 shows
the S-N curve of VHCF of carburized gear steel 18CrNiMo7-6 by the
curve, with a constant slope, presents that the fatigue life in terms of the number oup–down method.
As shown in Figure 7, with the decrease of the stress amplitude, the number of failure cycles
to failure Nf increases with the decrease of the stress amplitude. Figure 7 shows
increased gradually. When the stress amplitude was lower than 600 MPa, the sample failed
curve
beyondof 107VHCF
cycles. ofThecarburized
fatigue limitgear steelby
calculated 18CrNiMo7-6 by thewas
the up–down method up–down
510 MPa method.
with As
in Figure 7, with
9 the decrease of the stress amplitude, the number
the power of 10 cycles. When the stress was reduced to 500 MPa, the fatigue life exceeded of failure cy
9
the 10 cycles, but the fatigue
creased gradually. Whenspecimen stillamplitude
the stress did not fail. The
wascurve has than
lower an obvious platform,
600 MPa, the samp
and there is no double S-N curve or continuous descending
beyond 10 cycles. The fatigue limit calculated by the up–down method was
7 curve [1,2], which is similar to 510 M
the traditional fatigue S-N curve [31,32].
the power of 10 cycles. When the stress was reduced to 500 MPa, the fatigue life ex
9

the 109 cycles, but the fatigue specimen still did not fail. The curve has an obvio
3.3. Fractography
form, and
The there
typical is nosurfaces
fracture doubleofS-N curve or specimens
the carburized continuous descending
after curve
the VHCF tests are [1,2], w
shown in Figure 8. It can be seen that the fatigue
similar to the traditional fatigue S-N curve [31,32].crack initiated from the interior of the
specimen with an obvious fisheye feature, as shown in Figure 8a,c. The granular bright
facet (GBF) area can be clearly seen around a nonmetallic inclusion, which acted as the
crack initiation site (Figure 8b,d). According to the typical fracture morphology in Figure 8,
the crack initiated in the internal inclusion, and the size of GBF area was different with
the distance between the inclusions and the surface, all of which were related to the stress
amplitude and cycle times of loading.
 Stress amplititude s
550 σ-1=510MPa

Coatings 2021, 11, x FOR PEER REVIEW 1

Coatings 2021, 11, 1482 7 of 15

500 4

1
650
450 Failure
106 107 108 109 1010 Pass 1011

Stress amplititude sa / MPa

Number of cycles to failure, Nf
600
Figure 7. S-N curve of a carburized specimen during an ultra-high cycle.

550 σ-1=510MPa
3.3. Fractography
The typical fracture surfaces of the1 carburized specimens after the VHCF tes
shown 500in Figure 8. It can be seen that the 4
fatigue crack initiated from the interior
specimen with an obvious fisheye feature, as shown in Figure 8a,c. The granular
1
facet (GBF) area can be clearly seen around a nonmetallic inclusion, which acted
crack 450
initiation site (Figure 8b,d). According to the typical fracture morphology in F
106
8, the crack initiated
7
10in the 10
8 9
1010 and
internal10inclusion, 1011the size of GBF area was differen
Number of cycles to failure, Nf
the distance between the inclusions and the surface, all of which were related to the
amplitude
Figure and
Figure7.7.S-N
S-N cycle
curve
curve times
of a of ofspecimen
carburized loading.
a carburized during anduring
specimen ultra-high
ancycle.
ultra-high cycle.

3.3. Fractography
The typical fracture surfaces of the carburized specimens after the VHCF t
shown in Figure 8. It can be seen that the fatigue crack initiated from the interio
specimen with an obvious fisheye feature, as shown in Figure 8a,c. The granula
facet (GBF) area can be clearly seen around a nonmetallic inclusion, which acte
crack initiation site (Figure 8b,d). According to the typical fracture morphology in
8, the crack initiated in the internal inclusion, and the size of GBF area was differ
the distance between the inclusions and the surface, all of which were related to th
amplitude and cycle times of loading.

(a) (b)

(a) (b)
(c) (d)
Figure
Figure8.8.Typical fracture
Typical fracturediagrams
diagrams ofof carburized samplesduring
carburized samples during ultra-high
ultra-high cyclecycle fatigue: (a,
fatigue:
(a,b) σ = 590 MPa for N = 6.66 × 10 7 and (c,d) σ = 570 MPa for N = 9.53 × 7107 .
590 MPaa for Nf = 6.66 ×f 10 and (c,d) σa = 570a MPa for Nf = 9.53
7 f × 10 .
The VHCF fracture had a GBF characteristic area, so it was particularly important to
The
study theVHCF fracture
size and had
properties a GBF
of the GBF,characteristic area,
FIE, and inclusion so By
(Inc.). it was
SEM particularly
observation of import
study the size
the fracture and itproperties
surface, is found thatofthe
the GBF,
GBF FIE, and
is formed inclusion
around (Inc.). Byinclusions
Al2 O3 nonmetallic SEM observat
containing a scruple Ca element, and the size of the GBF was different under different
stress amplitudes and different cycles. The sizes of the inclusion, GBF, and FIE were

(c) (d)
Coatings 2021, 11, 1482 8 of 15

analyzed systematically. The sizes of the inclusion, GBF, and FIE were represented by
√ √ √
areaInc , areaGBF , and areaFiE , respectively. Are shown in Table 2, it can be seen that
the fatigue life increases with the decrease of the stress amplitude, but it is difficult to
√ √ √
directly find a relationship between the areaInc , areaGBF , or areaFiE and fatigue life of
√
the specimens. The sizes areaInc of the inclusion range from 9 to 39 µm, with an average
√
value of 22 µm. The areas areaGBF of the GBF range from 22 to 86 µm, with an average
√
value of 39 µm. The average size of area areaFiE was 1549 µm and ranged from 1138
to 1918 µm.

Table 2. Data of the VHCF fracture origins measured from the fracture surfaces.
√ √ √
Stress Nf areaInc areaGBF areaFiE Depth
No.
/MPa /Cycle /µm /µm /µm /µm
1 560 1.79 × 108 17.00 39.12 1488 947
2 540 4.75 × 107 15.60 36.29 1751 1406
3 520 3.57 × 108 29.46 29.85 1693 1212
4 520 3.74 × 108 10.42 42.76 1918 1378
5 540 3.29 × 108 37.99 86.52 1869 1290
6 520 1.83 × 108 34.85 51.25 1138 646
7 500 2.26 × 107 33.52 49.87 1690 1340
8 520 2.32 × 106 38.84 38.84 1610 1106
9 520 1.67 × 107 26.85 34.37 1680 1269
10 570 2.82 × 107 21.21 37.36 1304 933
11 570 6.33 × 106 38.95 43.15 1440 916
12 570 9.53 × 107 12.35 29.79 1420 953
13 590 6.66 × 107 9.01 36.47 1540 1192
14 590 2.09 × 106 22.01 22.01 1510 1215
15 590 3.32 × 107 12.02 29.53 1512 1173
16 610 1.91 × 107 21.05 46.55 1160 650
17 610 1.56 × 107 15.25 26.40 1536 1091
18 610 1.32 × 107 12.19 28.86 1629 1350

Figure 9 shows the depth of the VHCF crack initiation sites from the carburized surface
against the number of cycles to failure. It can be seen that most of the crack initiation sites
of the fracture specimens were located at a depth of 0.9–1.4 mm. It can be seen from the
hardness distribution curve that this region is a transition zone with an average hardness
of 580 HV. We tried to find out the relationship between the area size of the GBF and the
location of initiation but failed to find a direct relationship. In other words, there was
no obvious correlation between the size of the GBF area and the crack initiation position,
which was random and may be related to different stress amplitudes and the loading stress
of damaged samples. Ultra-high cycle fatigue stress belongs to axial loading stress, namely
the tension and compression fatigue test. Theoretically, the stress level is even throughout
the whole section of the specimen. Numerical analyses of the static tests showed that the
highest level of stress one can find was in the center of the cylindrical specimen, but in
the case of fatigue after some cycles, the maximum stress could be found close to the free
surface. The carburized specimens had a hardness gradient, the closer it was to the surface,
the higher the carbon content, the higher the martensite hardness and microhardness,
and the higher the strength, which had a protective effect on the fatigue. The hardness
and strength decreased with the increasing distance from the surface, and weakened the
protection effect on fatigue failure.
Coatings 2021, 11, x FOR PEER REVIEW
Coatings 2021, 11, 1482 9 of 15

1600

depth from specimen surface，D/μm

540
1400

Micro Vickers hardness，HV

560
1200
580
1000 600
800 620

600 640

400 10-20μm 660

20-30μm
680
200 >30μm
700
0
106 107
10 8
10 9

Number of cycles to failure, Nf

Figure
Figure The
9. 9. relationship
The betweenbetween
relationship the inclusion
thedepth from thedepth
inclusion specimen surface,
from theVickers hardness,
specimen surface, V
and number of cycles to failure.
and number of cycles to failure.
3.4. Detailed Characterization of GBF and Discussion
3.4. Figure
Detailed Characterization
10 shows of GBFwith
a TEM image together andselected
Discussionarea diffraction (SAD) patterns
of the cross-section and GBF for a carburizing specimen around the inclusion, which was
Figure
fractured beyond 1010shows a TEM
7 cycles under image
a 590 together
MPa stress amplitude.withDuring
selected a TEM area diffraction
analysis of (
of the
the cross-section
longitudinal and
profile, the GBFsurface
fracture for acould
carburizing
be roughlyspecimen
divided into around the inclusi
the GBF region,
transition region, and matrix. GBF region I was the refined
fractured beyond 107 cycles under a 590 MPa stress amplitude. During a TE nanograin, the transition region
was the partially refined microstructure, and the final region, III, was the martensite of the
the longitudinal
matrix, profile,
as shown in Figure 10a.the fracture
It could also be surface
found that could be roughly
the width of the GBF divided
region into th
transition
varied due to region, and matrix.
the “unevenness” GBF region
of the fracture, I was the
and its average value refined
was about nanograin,
500 nm. the
According to the comparison of light and dark fields in Figure
gion was the partially refined microstructure, and the final region, III, was 10b,c, it could be seen that
the GBF region and matrix had two different tissue forms. In Figure 10d, it specified the
of the of
location matrix, as shown
the selected in Figure
area diffraction, showing10a.thatIt the
could alsonear
location bethe found
fracturethat
zonethe wid
region
was variedpolycrystalline
a continuous due to the diffraction
“unevenness” of the that
ring. It indicated fracture, and itsformed
the nanocrystals average va
during the fatigue process under high stress and plastic
500 nm. According to the comparison of◦ light and dark fields in Figure strain. Below the fracture was 10b
greater than 400 nm (transition area), which was a 5 misalignment angle diffraction spot,
seen showed
which that the GBF
that region
the plastic and matrix
deformation of thehad
grains two different
at that tissue
position was forms.
small. It couldIn Figu
ified
be seenthethatlocation
the factureof the selected
surface in the GBF area areawas diffraction,
rough, and the showing
near-surface thatareathewaslocation
much finer than the areas deeper beneath the surface, where
ture zone was a continuous polycrystalline diffraction ring. It indicated that martensitic laths could be
clearly observed in the center and right sides of the image.
tals Hong
formed et al.during the fatigue
[13] proposed process
a large number under
of cyclic high(NCP)
pressing stressmodels
and plastic
to explain strain. B
ture
the was greater
formation mechanismthanof400 nmon
the GBF (transition
the basis of area),
revealing which was a 5°properties
the microscopic misalignmen
of the spot,
tion crack initiation
which region.
showed Fatigue
thatcrack
the initiation
plastic may occur due toof
deformation thethe
evolution
grains of at tha
the local plastic deformation near the activated inclusion after the initial loading period.
small.
Crack It could
wakes be seen
are subjected that the
to repeated facture
extrusion surface
by cyclic in the
loading, which GBF areatowas
is related crackrough,
surface
closure area
[33] andwas much
residual stressfiner
releasethan
[34].the areas
Under the deeper
action of beneath the surface, whe
the local concentrated
plastic
laths could be clearly observed in the center and right sides ofand
deformation, the microstructure of the crack surface layer will fracture the form
image.
nanoparticles. This process continues, and after millions of loading cycles, the crack surface
Hong et al. [13] proposed a large number of cyclic pressing (NCP) mod
becomes a thin layer of coarse nanoparticles. Under the transient conditions from crack
the formation
initiation mechanism
to steady-state propagation,of the
the NCPGBFprocess
on the basis of
terminates andrevealing
reaches thethe microsco
critical
size of the
of the GBF. According
crack initiationto region.
the morphology
Fatigue of the GBF region
crack represented
initiation may inoccurFiguredue 10, to th
it basically conformed to the NCP model, and a large number of dislocation aggregation
the local plastic deformation near the activated inclusion after the initial lo
can be observed in Figure 10c, which proved that, under a large amount of cyclic stress,
aCrack
certain wakes are subjected
internal plastic deformationto ledrepeated
to a dislocation extrusion
movement. by cyclic loading, whic
crack closure [33] and residual stress release [34]. Under the action of the
trated plastic deformation, the microstructure of the crack surface layer wi
form nanoparticles. This process continues, and after millions of loading cy
surface becomes a thin layer of coarse nanoparticles. Under the transient co
crack initiation to steady-state propagation, the NCP process terminates an
 Coatings 2021, 11, x FOR PEER REVIEW

ings 2021, 11, x FOR PEER REVIEW 10 of

Coatings 2021, 11, 1482 10 of 15

Figure 10. TEM bright field image together with the SAD patterns in the GBF area of the carburized specimen after
VHCF tests at σa = 590 MPa for Nf = 6.66 × 107. (a) is transmission morphology of GBF region, transition region
Figure
matrix, (b)10. TEM bright field
is transmission image together
morphology ofwith
GBFthe SAD patterns
region, in the
(c) is GBF GBF area
region of the carburized
transmission specimen after
amplification the
morphology, (d) is
7
Figurelocation
10. VHCF
TEMoftests
bright σfield
a = 590image
theatselected MPa
areafortogether
Nf = 6.66 with
diffraction. × 10 .the
(a) isSAD patterns
transmission in the GBF
morphology area
of GBF of the
region, carburized
transition region specimen
and matrix, after the
σa = 590 MPa
VHCF tests(b)atis transmission for Nf of= GBF
morphology 6.66region,
× 107.(c)(a)
is GBF region transmission
is transmission amplification
morphology of morphology,
GBF region, (d)transition
is the location
region and
of the selected area diffraction.
matrix, (b) is transmission morphology Figure of GBF region, (c) is GBF region
11 shows a TEM imagetransmission amplificationofmorphology,
with the morphology (d) is the
carbide precipitation
location of the selected area diffraction.
crack origin.
Figure The precipitates
11 shows a TEM image arewithCr-rich carbides
the morphology of in longprecipitation
carbide strip formsnearin the
the matrix
crack origin. The precipitates are Cr-rich carbides in long strip forms in the
carbides have lower dissolution temperatures, and most of them dissolve after c matrix. Cr-rich
Figure
carbides11 shows
loweradissolution
TEM image with the and
morphology ofdissolve
carbideafter
precipitation
carburizing near t
ing for ahave
long time. However, temperatures,
the carbidesmost of them
precipitated after high-temperature tem
crack for
origin. The
a long precipitates
time. However, thearecarbides
Cr-richprecipitated
carbides inafter
longhigh-temperature
strip forms in the matrix. Cr-ri
tempering
werenot
were not completely dissolved in the subsequent short austenitizing, and the und
carbides havecompletely dissolved
lower dissolution intemperatures,
the subsequent short
andaustenitizing,
most of them anddissolve
the undissolved
after carburi
carbideswere
carbides were distributed
distributed in longinstrips
longinstrips in the matrix.
the matrix.
ing for a long time. However, the carbides precipitated after high-temperature temperin
were not completely dissolved in the subsequent short austenitizing, and the undissolv
carbides were distributed in long strips in the matrix.

Figure11.11.
Figure TEMTEM characterization
characterization of the carbide
of the carbide precipitates.
precipitates.

Figure 12 shows EBSD maps of the same carburized specimen cross-section

Figure 11. TEM characterization of the carbide precipitates.
the inclusion and GBF. It also indicated that the near-surface area was much finer
Coatings 2021, 11, 1482 11 of 15

Figure 12 shows EBSD maps of the same carburized specimen cross-section around
Coatings 2021, 11, x FOR PEER REVIEW
theinclusion and GBF. It also indicated that the near-surface area was much finer than 11 ofthe
15
areas deeper beneath the surface (Figure 12a). As shown in Figure 12b, retained austenite,
as shown by the peak areas, was distributed between the martensitic boundaries. Figure 12
shows
12 that
shows a large
that number
a large of nanocrystallines
number of nanocrystallinesexistexist
in the
in GBF region,
the GBF which
region, is consistent
which is con-
with the
sistent transmission
with results,results,
the transmission furtherfurther
verification that nanocrystalline
verification layers are
that nanocrystalline formed
layers are
aroundaround
formed inclusions under millions
inclusions of cycles
under millions ofofcycles
ultra-high cycle fatigue.
of ultra-high cycle fatigue.

(a) (b)
Figure
Figure12.12.EBSD
EBSDmap
mapshowing
showingthethefracture
fracturesurfaces
surfacesof
ofthe
thecarburized
carburizedspecimens
specimensafter
afterVHCF
VHCFtests
testsat
at
σσaa ==590
590 MPa
MPa for Nff == 6.66
for N 6.66 ×
× 10
107. .(a)
7
(a)The
Thenear-surface
near-surfacearea
areamicrostructure
microstructureand
and(b)
(b)the
thenear-surface
near-surface
area
areaRA.
RA.

3.5.Stress
3.5. StressIntensity
IntensityFactor
Factor
ByBycalculating
calculatingthe the stress
stress intensity
intensity rangerange∆K,∆K,
the the influence
influence ofinclusion,
of the the inclusion, GBF, GBF,
and
andon
FIE FIE
theonfatigue
the fatigue
life andlifefatigue
and fatigue
strengthstrength was studied.
was studied. The calculation
The calculation formulaformula
is as fol- is
as follows:
lows: q √
∆K = 0.5∆σ π area , ∆σ = 2σa (1)
∆K = 0.5∆σ√π√area , ∆σ = 2σa (1)
√
where area is a crack size defined as the square root of the measurement area, and σ is
where √𝑎𝑟𝑒𝑎 is a crack size defined as the square root of the measurement area, and a𝜎𝑎
the stress amplitude. Figure 13 shows the relationship between the stress intensity factor
is the stress amplitude. Figure 13 shows the relationship between the stress intensity factor
∆K and fatigue life N . The crack propagation process of the fatigue specimens was GBF-
∆K and fatigue life Nf.f The crack propagation process of the fatigue specimens was GBF-
FIE-FCGZ-MFZ [21], where 99% of the life of the crack initiation was mainly consumed
FIE-FCGZ-MFZ [21], where 99% of the life of the crack initiation was mainly consumed in
in the GBF region [10], and ∆KGBF can be regarded as the threshold value ∆Kth [21] of
the GBF region [10], and ∆KGBF can be regarded as the threshold value ∆Kth [21] of the
the crack initiation. When the stress intensity factor at the crack edge was ∆K < ∆Kth ,
crack initiation. When the stress intensity factor at the crack edge was ∆K < ∆Kth, the fa-
the fatigue short crack did not expand and directly formed a fisheye; when ∆K > ∆Kth ,
tigue short crack did not expand and directly formed a fisheye; when ∆K > ∆Kth, the short
the short crack formed a GBF nanograin layer. Similarly, ∆KFiE can also be regarded as
crack formed a GBF nanograin layer. Similarly, ∆KFiE can also be regarded as the critical
the critical value of crack growth. When ∆K < ∆KFiE , the fatigue long crack did not grow,
value
and aoffatigue
crack growth.
fracture When occur ∆K < ∆KFiE,As
suddenly. theindicated
fatigue long crack did
in Figure not the
13a,b, grow, and of
values a fatigue
∆KGBF
fracture occur suddenly. As indicated in Figure 13a,b, the values
and ∆KFiE did not change with the increase of Nf but fluctuated within a small range, of ∆K GBF and ∆KFiE did

not change
which was with the increase
consistent with theofresearch
Nf but fluctuated
results of manywithin a small range,
researchers [31,32].which was con-
sistentItwith the research results of many researchers [31,32].
assumed that ∆KGBF and ∆KFiE were regarded as constants; the average values
of ∆K It assumed that ∆KGBF and ∆KFiE were regarded as constants; the average values of
GBF and ∆KFiE after the carburization of low-carbon gear steel 18CrNiMo7-6 were
∆K GBF and ∆KFiE after
3.04 and 20 MPa·m−1/2 the carburization
, respectively. of low-carbon
According to the gear
abovesteel 18CrNiMo7-6
analysis, the thresholdwerevalue3.04
and 20 MPa· m −1/2, respectively. According to the above analysis, the threshold value
formed by the GBF region was far less than that formed by FIE, and it was inevitable that
formed
the crack byfront
the GBFend region
of the GBFwasgrew
far less than thus
slowly, that formed
consuming by FIE,
mostand it was
of the inevitable
fatigue life. Atthat
low
the crack front end of the GBF grew slowly, thus consuming most
cyclic stresses of millions of times, the dislocations moved and piled up, further slowing of the fatigue life. At
low
down cyclic
thestresses
propagation of millions
of shortof times,
cracks.the The dislocations
value of ∆K moved and piled up, further slow-
Inc decreased with the increase of
ing
Nf ,down
while the propagation
Nf increased onlyofwhen
shortthecracks.
stressThe value ofdecreased;
amplitude ∆KInc decreased
that is,with
in thethe increase
case of low
of Nf, while
stress, Nf increased
the cracks were first only when the
initiated at an stress amplitude
inclusion a withdecreased;
small size.that
As canis, inbethe case
seen fromof
Figure 13c, the ratio of ∆KGBF /∆KInc increased with the increase of the number of cycles,
low stress, the cracks were first initiated at an inclusion a with small size. As can be seen
from
furtherFigure 13c, the
indicating ratio
that theofformation
∆KGBF/∆Kof increased
Inc GBF with the
consumed the increase of theofnumber
vast majority the life ofof cy-
the
cles, further indicating that
VHCF at a lower stress amplitude. the formation of GBF consumed the vast majority of the life of
the VHCF at a lower stress amplitude.
Coatings 2021, 11, 1482 12 of 15
Coatings 2021, 11, x FOR PEER REVIEW 12 of 15

3.0
30 5.0 ΔKGBF/ΔKinc
Stress intensity factor, K / MPa·m1/2

ΔKFiE ΔKinc

Stress intensity factor, K / MPa·m1/2

4.5 2.5
ΔKGBF
25 Average value=20MPa·m1/2 4.0 Average value=3.04MPa·m1/2
2.0

ΔKGBF/ΔKinc
3.5

20 3.0 1.5

2.5
1.0
15 2.0

1.5 0.5

10 1.0
106 107 108 109 106 107 108 109 0.0
107 108
Number of cycles to failure, Nf Number of cycles to failure, Nf
Number of cycles to failure, Nf
(a) (b) (c)
Figure
Figure 13.13.The
Therelationship between ∆K
relationship between , ,∆K
∆Kincinc ∆KGBF, ∆K Fish-eye, and the fatigue life of experimental steel: (a) ∆KFish-eye changes
GBF , ∆KFish-eye , and the fatigue life of experimental steel: (a) ∆KFish-eye
with the fatigue cycle life, (b) ∆K inc and ∆KGBF changes with the fatigue cycle life, and (c) ∆KGBF/ ∆Kinc changes with the
changes with the fatigue cycle life, (b) ∆Kinc and ∆KGBF changes with the fatigue cycle life, and (c) ∆KGBF /∆Kinc changes
fatigue cycle life.
with the fatigue cycle life.
Table33lists
Table liststhe
the results
results of
of the VHCF
VHCF limits
limitsandand△K ∆KGBF
GBFvalues
valuesofofsome
some high-strength
high-strength
steels[22,35,36].
steels [22,35,36]. The
The VHCF
VHCF limits
limits of
of the
thecarburized
carburizedspecimen
specimen ofofthe experimental
the experimental steel
steel
were not only lower than those of bearing steel SUJ2 and quenched
were not only lower than those of bearing steel SUJ2 and quenched and tempered steel and tempered steel
SNCM439but
SNCM439 but also
also lower
lower than
than that
that of
of the
the same
samesteel
steel18CrNiMo7-6
18CrNiMo7-6thorough-carburized
thorough-carburized
with the same cross-section hardness of 719 HV.
with the same cross-section hardness of 719 HV. The ∆KGBF The △K of the experimental steel was
GBF of the experimental steel was
thelowest
the lowestamong
among the the listed
listed steels.
steels. Thus,
Thus,the thetransition
transitionarea
areaininthe
thecarburized
carburized specimen
specimen
had the lowest VHCF properties than both cases, which had a high
had the lowest VHCF properties than both cases, which had a high hardness and hardness and core thatthat
core
did not show the VHCF phenomenon, as reported in a previous study
did not show the VHCF phenomenon, as reported in a previous study [22]. This indicates [22]. This indicates
that much attention should be paid to the transition area for real carburized gears with
that much attention should be paid to the transition area for real carburized gears with
very high cycle life requirements in service.
very high cycle life requirements in service.
Table3.3.Comparison
Table Comparisonof
of the
the VHCF
VHCF limits andK
limits and ∆KGBF values of high-strength steels.
GBF values of high-strength steels.

σ−1
σ− Hardness
Hardness
Steel
Steel 1 △KGBF
∆K Ref.
Ref.No
No
/MPa
/MPa /HV
/HV GBF

18CrNiMo7-6 (Carburized) 500 705–510 3.04 present

18CrNiMo7-6 (Carburized) 500 705–510 3.04 present
18CrNiMo7-6 (Thorough-carburized)
18CrNiMo7-6 (Thorough-carburized) 600
600 719
719 3.49
3.49 [22]
[22]
SUJ2
SUJ2 765
765 707
707 4.65
4.65 [35]
[35]
SNCM439
SNCM439 925
925 586
586 4.00
4.00 [36]
[36]

3.6.Fatigue
3.6. FatigueLife
Life Prediction
Prediction
Lotsofofparts
Lots partsreached
reachedthe thefatigue
fatiguelife
lifelimit
limitbut
butdid
did
notnot fail,
fail, andand thethe cycles
cycles of of lots
lots of of
parts
inparts in the operation
the actual actual operation
processprocess far exceeded
far exceeded the design
the design safetysafety
life, alllife, all of which
of which brought
brought
about about enormous
enormous safety
safety risks, risks,
so the so the accurate
accurate predictionprediction of the fatigue
of the fatigue life became
life became the focus
the focus of research [37,38]. Especially for very high cycle fatigue,
of research [37,38]. Especially for very high cycle fatigue, it was difficult to evaluate it was difficult to eval-and
verify its fatigue safety life through actual service, not only because it would cost acost
uate and verify its fatigue safety life through actual service, not only because it would lot of
a lot of manpower
manpower and financial
and financial resources resources
but also,but in also,
mostin mostthe
cases, cases,
time theandtime and conditions
conditions were not
were notFuruya
allowed. allowed. FuruyaTanaka-Akimina’s
revised revised Tanaka-Akimina’s model and model and proposed
proposed a new predic-
a new prediction model
tion model of ultra-high cycle fatigue strength [39]. The
of ultra-high cycle fatigue strength [39]. The solid line near the carburizingsolid line near the carburizing
pattern in
pattern
Figure 14inisFigure 14 is fitted to
fitted according according
this newtomodel.
this newIn model. In this
this fitting, thefitting,
R2 valuethe R(determination
2 value (de-

termination coefficient) reflecting the goodness of fit is 0.78. According to these results,
coefficient) reflecting the goodness of fit is 0.78. According to these results, the fatigue life
the fatigue life curves (dashed lines) of the minimum inclusion √ size of √𝑎𝑟𝑒𝑎 = 15 μm
curves (dashed lines) of the minimum inclusion size of area = 15 µm and the maximum
and the maximum √ inclusion size √𝑎𝑟𝑒𝑎 = 26 μm are predicted, and it can be seen that the
inclusion size area = 26 µm are predicted, and it can be seen that the measured points
measured points are basically between these two curves. The ultra-high cycle fatigue
are basically between these two curves. The ultra-high cycle fatigue strength of 1010 cycles
strength of 1010 cycles is predicted, and the fatigue strength is about 490 MPa. However,
is predicted, and the fatigue strength is about 490 MPa. However, the accuracy of the
the accuracy of the 1010 cycles’ fatigue life prediction needs further study. Formula (1) is
1010 cycles’ fatigue life prediction needs further study. Formula (1) is the new law of crack
growth instead of this model. The related formula of this model are as follows:
√
d area  √ α m

= C ∆K × area (2)
dN
 the new law of crack growth instead of this model. The related formula of this mo
as follows:
𝑑 √𝑎𝑟𝑒𝑎 𝛼
Coatings 2021, 11, 1482 = 𝐶(∆𝐾 × √𝑎𝑟𝑒𝑎 )𝑚 13 of 15
𝑑𝑁

1 1 1 1
1
𝜎𝑎 =
𝜋
(𝐷)𝑚 × (𝑁𝑓 )−𝑚 × (√𝑎𝑟𝑒𝑎𝑖𝑛𝑐 )(𝑚−2−𝛼)
1 √ √
1 1 ( 1 − 1 −α)
σa = √ (D) m × (Nf )− m × ( areainc ) m 2 (3)
π 1
𝛼 𝑚 𝑁𝑓 2
1−𝑚( +𝛼)
2 −1
√ (∆𝐾𝑖𝑛𝑐
×√𝑎𝑟𝑒𝑎
N 𝑖𝑛𝑐 ) (2√1𝑎𝑟𝑒𝑎
 −m( 12 +)α)=− 1 1 =𝐷
α m 𝐶(1−𝑚( +𝛼)
∆Kinc × areainc √ f = 𝑖𝑛𝑐
  =D 2 (4)
areainc C(1 − m 12 + α
where m, D, and α are constants that determine the crack propagation properties
where m, D,
constant andsimplifies
that α are constants
the that determine
right side of the crack propagation
Formula properties.
(3). Through D is a fitting,
nonlinear
obtain the parameters for the carburized specimens of the experimentalcan
constant that simplifies the right side of Formula (3). Through nonlinear fitting, we steel as
obtain the parameters for the carburized specimens of the experimental steel as follows:
D = 2.04 × 1087, m = 37.17, and α =
D = 2.04 × 1087, m = 37.17, and α = −0.28. −0.28.

650
carburized steel
Stress amplititude sa / MPa

√𝒂𝒓𝒆𝒂𝒊𝒏𝒄=21.8 μm

600 √𝒂𝒓𝒆𝒂𝒊𝒏𝒄=15 μm

550
√𝒂𝒓𝒆𝒂𝒊𝒏𝒄=26 μm

σ-1=490 MPa
500

450
105 106 107 108 109 1010 1011
Number of cycles to failure , Nf

14.Fatigue
Figure 14.
Figure FatigueS-NS-N
curve of theof
curve carburized specimens
the carburized of the experimental
specimens steel.
of the experimental steel.
4. Conclusions
4. Conclusions
The VHCF properties of low-carbon gear 18CrNiMo7-6 were studied by means of
ultrasonic
The fatigue
VHCFtests in this work.
properties The GBF region
of low-carbon was18CrNiMo7-6
gear characterized in were
detail, studied
and its by m
formation mechanism was revealed, and the applicability of the fatigue life prediction
ultrasonic fatigue tests in this work. The GBF region was characterized in detail,
model for carburized gear steel was verified. The following conclusions can be drawn.
formation mechanism
(1) The carburized was revealed,
specimens and the
of the experimental applicability
steel showed typicalofVHCF
the fatigue
behavior, life pre
model
and the for carburized
fatigue gear
limit at the 10 steel
9 cyclewas
wasverified.
measuredThe to befollowing
500 MPa. conclusions
The VHCF S-N can be dr
curve(1) The carburized specimens of the experimental steel showed typical VHCF
could be predicted by a theoretical model taking into account the nonmetallic
inclusion
ior, and sizes.
the fatigue limit at the 109 cycle was measured to be 500 MPa. The VH
(2) The fatigue crack initiation sites of the carburized specimens were located mostly
curve could be predicted by a theoretical model taking into account the nonmetall
in the transition area at a distance of 0.9–1.4 mm from the surface, where the hardness was
sion
aboutsizes.
580 HV. It was because the core did not show VHCF phenomena, and the case had a
higher(2) The fatigue crack initiation sites of the carburized specimens were located
hardness.
(3) A fine microstructure
in the transition was observed
area at a distance in the GBF
of 0.9–1.4 mmarea fromby means of TEM where
the surface, and EBSD,the hardn
and the stress intensity factor value ∆KGBF at the GBF area was measured to be around
about 580 −HV. It was because the core did not show VHCF phenomena, and the c
3.04 MPa·m 1/2 . The GBF region was mainly a nanograin layer formed by a small plastic
adeformation
higher hardness.
caused by long-time circulation under low stress.
(3) A fine microstructure was observed in the GBF area by means of TEM and
Author
and theContributions: Conceptualization,
stress intensity factor valueS.Y.,
∆KP.C., C.Z.
GBF at and
the M.W.
GBF andwas
area experiment and data
measured to be arou
processing, K.W., F.H. and W.Y. All authors have read and agreed to the published version of
MPa· m . The GBF region was mainly a nanograin layer formed by a small plasti
−1/2
the manuscript.
mation caused by long-time circulation under low stress.
Funding: This research was financially supported by Industrial Strong Foundation Engineering
(Tender No. TC180A3Y1/Subcontract No. 14).
Author Contributions: Conceptualization, S.Y., P.C., C.Z., and M.W. and experiment and d
Institutional Review Board Statement: Not applicable.
cessing, K.W., F.H., and W.Y. All authors have read and agreed to the published versio
manuscript.
Funding: This research was financially supported by Industrial Strong Foundation Eng
(Tender No. TC180A3Y1/Subcontract No. 14).
Coatings 2021, 11, 1482 14 of 15

Informed Consent Statement: Not applicable.

Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

References
1. Sakai, T.; Lian, B.; Takeda, M.; Shiozawa, K.; Oguma, N.; Ochi, Y.; Nakajima, M.; Nakamura, T. Statistical duplex S–N characteristics
of high carbon chromium bearing steel in rotating bending in very high cycle regime. Int. J. Fatigue 2010, 32, 497. [CrossRef]
2. Li, W.; Sakai, T.; Wakita, M.; Mimura, S. Influence of microstructure and surface defect on very high cycle fatigue properties of
clean spring steel. Int. J. Fatigue 2014, 60, 48. [CrossRef]
3. Furuya, Y. Gigacycle fatigue properties of double-melted SCM440 steel and size effects. ISIJ Int. 2014, 52, 1436. [CrossRef]
4. Yang, Z.G.; Li, S.X.; Zhang, J.M.; Zhang, J.F.; Li, G.Y.; Li, Z.B.; Hui, W.J.; Weng, Y.Q. On the critical inclusion size of high strength
steels under ultra-high cycle fatigue. Acta Mater. 2004, 52, 5235. [CrossRef]
5. Bathias, C.; Drouillac, L.; le Francois, P. How and why the fatigue S–N curve does not approach a horizontal asymptote.
Int. J. Fatigue 2001, 23, 143–151. [CrossRef]
6. Sakai, T.; Takeda, M.; Shiozawa, K.; Ochi, Y.; Nakajima, M.; Nakamura, T. Experimental reconfirmation of characteristic S-
N property for high carbon chromium bearing steel in wide life region in rotating bending. J. Soc. Mater. Sci. 2000, 49,
779–785. [CrossRef]
7. Sakai, T.; Sato, Y.; Oguma, N. Characteristic S-N property of high carbon chromium bearing steel under axial loading in long life
fatigue. Mater. Struct. 2002, 25, 765–773. [CrossRef]
8. Murakami, Y.; Yokoyama, N.N.; Nagata, J. Mechanism of fatigue failure in ultralong life regime. Fatigue Fract. Eng. Mater. Struct.
2002, 25, 735–746. [CrossRef]
9. Hong, Y.; Zhao, A.; Qian, G.; Zhou, C. Fatigue strength and crack initiation mechanism of very-high-cycle fatigue for low alloy
steels. Mater. Trans. A 2012, 43, 2753–2762. [CrossRef]
10. Hong, Y.; Lei, Z.; Sun, C.; Zhao, A. Propensities of crack interior initiation and early growth for very-high-cycle fatigue of high
strength steels. Int. J. Fatigue 2014, 58, 144–151. [CrossRef]
11. Tanaka, K.; Akiniwa, Y. Fatigue crack propagation behaviour derived from S–N data in very high cycle regime. Fatigue Fract. Eng.
Mater. Struct. 2002, 25, 775–784. [CrossRef]
12. Liu, X.; Sun, C.; Hong, Y.S. Effects of stress ratio on high-cycle and very-high cycle fatigue behavior of a Ti–6Al–4V alloy.
Hong Mater. Sci. Eng. A 2015, 622, 228–235. [CrossRef]
13. Hong, Y.; Liu, X.; Lei, Z.; Sun, C. The formation mechanism of characteristic region at crack initiation for very-high-cycle fatigue
of high-strength steels. Int. J. Fatigue 2016, 89, 108–118. [CrossRef]
14. Yukun, C.; Xiangnan, P.; Liang, Z. Microstructure refinement and grain size distribution in crack initiation region of very-high-
cycle fatigue regime for high-strength alloys. Int. J. Fatigue 2020, 134, 105473.
15. Krauss, G. The microstructure and fracture of a carburized steel. Metall. Mater. Trans. A 1978, 9, 1527. [CrossRef]
16. Erdogan, M.; Tekeli, S. The effect of martensite volume fraction and particle size on the tensile properties of a surface-carburized
AISI 8620 steel with a dual-phase core microstructure. Mater. Charact. 2003, 49, 445. [CrossRef]
17. Liu, Y.; Wang, M.Q.; Shi, J.; Hui, W.J.; Fan, G.; Dong, H. Fatigue properties of two case hardening steels after carburization.
Int. J. Fatigue 2009, 31, 292. [CrossRef]
18. Naito, T.; Ueda, H.; Kikuchi, M. Fatigue behavior of carburized steel with internal oxides and nonmartensitic microstructure near
the surface. Metall. Mater. Trans. 1984, 15, 1431. [CrossRef]
19. Nehila, A.; Li, W.; Gao, N.; Xing, X.; Zhao, H.; Wang, P.; Sakai, T. Very high cycle fatigue of surface carburized CrNi steel at
variable stress ratio: Failure analysis and life prediction. Int. J. Fatigue 2018, 111, 112. [CrossRef]
20. Marines-Garcia, I.; Paris Paul, C.; Tada, H. Fatigue crack growth from small to long cracks in VHCF with surface initiations.
Mater. Sci. Eng. A 2007, 468–470, 120–128. [CrossRef]
21. Li, W.; Sun, Z.; Zhang, Z.; Deng, H. Tatsuo Sakai. Influence of case-carburizing and micro-defect on competing failure behaviors
of Ni–Cr–W steel under gigacycle fatigue. J. Mater. Res. 2015, 30, 2247–2257. [CrossRef]
22. Cheng, P.F.; Li, Y.K.; Yu, W.C.; Yang, S.P.; Hu, F.Z.; Shi, J.; Wang, M.Q.; Li, L. Comparison of very high cycle fatigue properties of
18CrNiMo7-6 steel after carburizing and pseudo-carburizing. Mater. J. Eng. Perform. 2020, 29, 8340. [CrossRef]
23. Sun, C.; Xie, J.; Zhao, A.; Lei, Z.; Hong, Y.A. cumulative damage model for fatigue life estimation of high-strength steels in
high-cycle and very-high-cycle fatigue regimes. Fatigue Fract. Eng. Mater. Struct. 2012, 35, 638–647. [CrossRef]
24. Mayer, H. Recent developments in ultrasonic fatigue. Fatigue Fract. Eng. Mater. Struct. 2016, 39, 3–29. [CrossRef]
25. Wang, C.F.; Wang, M.Q.; Shi, J.; Hui, W.J.; Dong, H. Effect of microstructural refinement on the toughness of low carbon
martensitic steel. Scr. Mater. 2008, 58, 492. [CrossRef]
26. Chen, W.; He, X.F.; Yu, W.C.; Shi, J.; Wang, M.Q.; Yao, K.F.; Mater, J. Nano and microhardness distribution in the carburized case
of nb microalloyed gear steel. Eng. Perform. 2020, 29, 4626. [CrossRef]
27. Liu, H.; Wang, W.; Zhu, C. A microstructure sensitive contact fatigue model of a carburized gear. Wear 2019, 436–437, 203035. [CrossRef]
28. Shen, Y.; Moghadam, S.; Mobasher, S.F. Effect of retained austenite—Compressive residual stresses on rolling contact fatigue life
of carburized AISI 8620 steel. Int. J. Fatigue 2015, 75, 135–144. [CrossRef]
Coatings 2021, 11, 1482 15 of 15

29. Roy, S.; Sundararajan, S. The effect of heat treatment routes on the retained austenite and tribomechanical properties of carburized
AISI 8620 steel. Surf. Coat. Technol. 2016, 308, 236. [CrossRef]
30. Zhao, M.H.; Han, X.C.; Wang, G. Determination of the mechanical properties of surface-modified layer of 18CrNiMo7-6 steel
alloys after carburizing heat treatment. Int. J. Mech. Sci. 2018, 148, 84–93. [CrossRef]
31. Hong, Y.; Sun, C. The nature and the mechanism of crack initiation and early growth forvery-high-cycle fatigue of metallic
materials—An overview. Theor. Appl. Fract. Mech. 2017, 92, 331–350. [CrossRef]
32. Li, W.; Yuan, H.; Sun, Z. Surface vs. interior failure behaviors in a structural steel under gigacycle fatigue: Failure analysis and
life prediction. Int. J. Fatigue 2014, 64, 42–53. [CrossRef]
33. Pippan, R.; Hohenwarter, A. Fatigue crack closure: A review of the physical phenomena. Fatigue Fract. Eng. Mater. Struct. 2017,
40, 471–495. [CrossRef] [PubMed]
34. Sattari-Far, I.; Akbari, D.; Alderliesten, R. Effect of residual stresses on crack behaviour in single edge bending specimens.
Mater. Struct. 2013, 36, 115–126.
35. Shiozawa, K.; Murai, M.; Shimatani, Y.; Yoshimoto, T. Transition of fatigue failure mode of Ni–Cr–Mo low-alloy steel in very high
cycle regime. Int. J. Fatigue 2010, 32, 541. [CrossRef]
36. Li, Y.D.; Xu, N.; Ma, H.; Li, Y.Z. Granular bright fact crack propagating under very high cycle fatigue. Mater. Sci. Technol. 2016,
31, 1894. [CrossRef]
37. Sakai, T.; Oguma, N.; Morikawa, A. Microscopic and nanoscopic observations of metallurgical structures around inclusions at
interior crack initiation site for a bearing steel in very high-cycle fatigue. Fatigue Fract. Eng. Mater. Struct. 2015, 38, 1305. [CrossRef]
38. Lei, Z.Q.; Hong, Y.S.; Xie, J.; Sun, C.Q.; Zhao, A.G. Effects of inclusion size and location on very-high-cycle fatigue behavior for
high strength steels. J. Mater. Sci. Eng. A 2012, 558, 234. [CrossRef]
39. Furuya, Y. A New model for predicting the gigacycle fatigue strength of high-strength. J. Mater. Sci. Eng. 2019, 743, 445. [CrossRef]