metals

Article
Effect of Quenching Conditions on the Microstructure
and Mechanical Properties of 51CrV4 Spring Steel
Lin Zhang 1, * , Dehai Gong 2 , Yunchao Li 1 , Xiaojun Wang 2 , Xixi Ren 1 and Engang Wang 1, *
1 Key Laboratory of Electromagnetic Processing of Materials (Ministry of Education), Northeastern University,
Wenhua Road, Shenyang 110819, China; liyunchaoneu@163.com (Y.L.); 13081428815@sina.cn (X.R.)
2 CRRC Guiyang Co., LTD., Dulaying Road, Guiyang 550017, China; dahai_2014@126.com (D.G.);
wxjchly@163.com (X.W.)
* Correspondence: zhanglin@epm.neu.edu.cn (L.Z.); egwang@mail.neu.edu.cn (E.W.);
Tel.: +86-24-8368-3985 (L.Z.); +86-24-8368-1739 (E.W.)




Received: 28 November 2018; Accepted: 11 December 2018; Published: 12 December 2018


Abstract: 51CrV4 steel is extensively used in large-size damping springs for trains and vehicles.
Quenching conditions play an important role in performance enhancement. The present work
investigated the effects of various oil-bath temperatures and out-of-oil temperatures on the
microstructure and the mechanical properties of this steel. The morphological examination focused
on both the quenched martensite and the tempered troostite. Tensile and hardness tests were
carried out to evaluate the mechanical properties. The results showed that a coarsening of the
martensite occurred at a high oil-bath temperature. In addition, the size and fraction of bainite
islands also increased with the increase of oil-bath temperature. In contrast, the carbide size and
the intercarbide spacing both increased with the increase of oil-bath temperature. Thus, the tensile
strength and the hardness both decreased with increasing oil-bath temperature in accordance with
the Hall-Petch relationship. Correspondingly, the ductility increased as the oil-bath temperature
increased. At a relatively high out-of-oil temperature, the martensite underwent an auto-tempering
process, which led to the precipitation of many tiny carbide particles in the as-quenched martensite
laths. This auto-tempering effect enhanced the width of large-sized carbides and reduced their length
in the final microstructure. The intercarbide spacings increased with increasing out-of-oil temperature.
As the oil-bath temperature increased, the tensile strength and hardness decreased, and the ductility
increased. The fracture morphology was examined to explain the results of mechanical properties.

Keywords: 51CrV4; spring steel; quenching; martensite; carbides; strength; hardness

1. Introduction
The development of high-speed railway trains imposes rigid requirements on the mechanical
properties of coil springs used in freight car bogies. Over the last decades, considerable efforts have
been made to develop high-performance spring steels. Most coil springs for railway applications
are made of quenched and tempered high-strength steels. Elements such as chromium, manganese,
and silicon are added to these steels [1]. 51CrV4 steel has high strength and fatigue performance due
to the addition of Cr and V, which is extensively used in large-size damping springs for trains and
vehicles [2].
The recommended properties of spring steel include high ductility and toughness at operating
temperatures and good hardenability that provides required mechanical properties even at large
dimensions [3]. One way to improve the mechanical properties of spring steel could be achieved
through the control of alloy composition [4,5]. Thermodynamic calculation was used to identify
the effects of element change on the phase fraction and transformation temperature in the soaking

Metals 2018, 8, 1056; doi:10.3390/met8121056 www.mdpi.com/journal/metals

Metals 2018, 8, 1056 2 of 16

and tempering process [6]. Thermodynamic calculation can be performed using software such as
Thermo-Calc. However, composition adjustment means to change the standard of spring steels,
which lack feasibility for spring manufacturers. Steels with a similar chemical composition may
behave differently due to various mechanical properties as a consequence of their manufacturing route.
The mechanical properties can be improved by effective heat treatment [7,8] and thermomechanical
treatment [1,9]. Quenching before tempering is a key technique to enhance the mechanical properties
of spring steels, in which the final structure is significantly affected by the processing parameters
during heat treatment. For this reason, the heat treatment parameters of spring steel are controlled
thoroughly by the producers. Large efforts have been made in recent years to investigate the effects
of heat treatment parameters during soaking and tempering process [8,10–12], such as the time and
temperature of soaking and tempering.
The emphasis in the research of spring steels has been focused on increasing the strength
while maintaining good ductility [6,13]. One way of improving steel properties is refining its
microstructure [14,15], which means to reduce the ferrite grain size, the size of carbides, and the
intercarbide spacing. The mechanical behavior of steel is influenced by the inclusions and precipitates,
which act as stress raisers [16]. Large inclusions are most harmful to mechanical properties.
Fine precipitation can be achieved through microalloying and effective heat treatment [17]. This leads
to the enhancement of hardness and strength. Retained austenite is also an important structural
component in the spring steel, whose stability is affected by the processing parameters during heat
treatment, such as the soaking temperature and the cooling rate [18].
The present work performed soaking, quenching, and tempering on 51CrV4 steel since this kind
of heat treatment is a conventional manufacturing route to improve its mechanical properties. Previous
researchers have studied the effects of various parameters during heat treatment on the microstructure
and mechanical properties of 51CrV4 steels [3,19–21]. However, very few researches have focused
on the detailed quenching conditions such as the oil-bath temperature and the out-of-oil workpiece
temperature, which is essential to obtain the required strength and ductility.
In this work, the heat treatment experiments were carried out on 51CrV4 steel under various
oil-bath temperatures and out-of-oil temperatures. The quenched martensite and tempered troostite
were examined. The microstructure of the steel was analyzed by scanning electron microscopy. Effects
of the quenching parameters on the mechanical properties were evaluated in terms of tensile strength,
elongation, hardness, and fracture. The relationship between the microstructure and the mechanical
properties was discussed. The purpose of this work is to obtain a technical reference to control the
mechanical properties using the oil-bath temperature and out-of-oil temperature.

2. Materials and Methods

51CrV4 spring steels have been processed by soaking, quenching, and tempering. Table 1 shows
the chemical composition of the commercial 51CrV4 spring steel used in this work, which was identified
by chemical analysis. The original specimens were cut from a hot deformed steel bar. The size of the
cylinder specimen was Ø20 mm × 300 mm. This work performed the heat treatment according to a
technology route usually used to fabricate a train damping spring. First, the steel bars were heated to
930 ◦ C and isothermally held for 30 min to form austenite with a uniform distribution of the alloying
elements. During this soaking process, nitrogen gas was injected into the furnace to protect the steel
bars from oxidization. Afterward, the steel bars were quenched into a stirred oil bath which was set at
various oil-bath temperatures (20 ◦ C, 50 ◦ C, and 80 ◦ C). The cooling rates were estimated to be 34 ◦ C/s,
30 ◦ C/s, and 25 ◦ C/s respectively. The surface temperature of the workpiece was measured during the
quenching process, and the workpieces were taken out of the oil bath at various temperatures (60 ◦ C,
90 ◦ C, and 120 ◦ C), which was defined as the out-of-oil temperature in this paper. After quenching,
the workpieces were cooled in the air to room temperature (about 15 ◦ C). Next, the specimens were
tempered at 450 ◦ C for 90 min. After tempering, the samples were water quenched.
Metals 2018, 8, 1056 3 of 16

Table 1. Chemical composition of the as-received 51CrV4 steel (mass percent, %).

C Si Mn S P Cr Ni Cu V Al Mo Fe
0.546 0.229 0.951 0.004 0.014 1.08 0.051 0.106 0.168 0.017 0.006 balance

Each bar was subsequently sectioned and etched to reveal the microstructure. The microstructure
was observed using an Ultra Plus field emission scanning electron microscope (Carl Zeiss AG,
Oberkochen, Germany). Image-Pro Plus software (Version 6.0, Media Cybernetics, Inc., Rockville, MD,
USA) was used to analyze the size and the area fraction of phases. The phases were identified by the
X-ray diffraction analysis using a Philips X0 Pert Pro MPD diffractometer (PANalytical Co., Almelo,
The Netherlands). In order to evaluate the mechanical properties of the samples, tensile testing and
hardness testing were performed. Hardness measurements were taken from a polished but unetched
sample, using a Rockwell apparatus (Shenyang Kejing Auto-instrument Co., LTD, Shenyang, China),
with a load of 150 kg and loading time of 5 s. Tensile testing was performed in a Shimadzu AG-X
100 kN testing machine (Shimadzu Corp., Kyoto, Japan) in accordance with the requirements and
recommendations of the ISO 6892-1:2011 [22]. The round bone-shaped tensile testing specimens were
prepared by lathe. The tensile testing specimen had an overall length of 150 mm, a gauge length of
50 mm, and a diameter of 6 mm. An extensometer was set during test to measure the strain precisely.
The strain rate was about 2.3 × 10−5 ·s−1 .

3. Results and Discussion

Figure 1a shows the microstructure of as-received commercial 51CrV4 steel used in this work.
The microstructure of the as-received steel appeared to be spheroidite, in which many spherical
carbides were distributed dispersedly in the ferrite grains. The XRD patterns of the as-received,
quenched, and tempered specimens were analyzed. The XRD result of as-received steel showed
a main phase of α-Fe (Figure 1b), which is the matrix of the microstructure shown in Figure 1a.
The carbides had a small X-ray reflection and showed no peaks in the XRD result. Figure 1b–d shows
the XRD patterns of specimens which were quenched at various oil-bath temperatures and out-of-oil
temperatures. The quenched specimens showed a pattern of martensite, which appeared to have peak
positions similar to the α-Fe phase. The pattern of quenched specimens in Figure 1b,c included the
peaks of γ-Fe phase, indicating that retained austenite existed in the two specimens quenched at an
out-of-oil temperature of 90 ◦ C. In the two patterns of the tempered specimens that corresponded to the
quenched specimens respectively, the lower peaks of γ-Fe phase indicated that the fraction of retained
austenite decreased (Figure 1b,c). The patterns of 80 ◦ C oil-bath temperature had a higher (200) peak
of γ-Fe phase compared with that of 50 ◦ C oil-bath temperature (Figure 1b,c), indicating that high
oil-bath temperature enhances the fraction of retained austenite. On the contrary, the high out-of-oil
temperature reduced the fraction of retained austenite. The quenched and tempered specimens at
120 ◦ C out-of-oil temperature appeared to have no γ-Fe peaks in the pattern (Figure 1d).
to the quenched specimens respectively, the lower peaks of γ-Fe phase indicated that the fraction of
retained austenite decreased (Figure 1b,c). The patterns of 80 °C oil-bath temperature had a higher
(200) peak of γ-Fe phase compared with that of 50 °C oil-bath temperature (Figure 1b,c), indicating
that high oil-bath temperature enhances the fraction of retained austenite. On the contrary, the high
out-of-oil
Metals 2018, 8,temperature
1056 reduced the fraction of retained austenite. The quenched and tempered4 of 16
specimens at 120 °C out-of-oil temperature appeared to have no γ-Fe peaks in the pattern (Figure 1d).
o
(b)

α(110)
(a) 50 C oil-bath temperature
o
90 C out-of-oil temperature

γ(200)

α(211)
α(200)

α(220)
intensity (a.u.)
tempered

α'-M(110)

α'-M(211)
α'-M(200)

α'-M(220)
γ(311)
γ(200)
γ(111)
quenched

α(110)

α(211)
α(200)

α(220)
as-received
Metals 2018, 8, x FOR PEER REVIEW 20 30 40 50 60 70 80 90 4100
of 16
2θ / (degree)

o o
50 C oil-bath temperature
α(110)

80 C oil-bath temperature

α(110)
(c) (d)
o o
90 C out-of-oil temperature 120 C out-of-oil temperature
γ(200)

α(211)

α(211)

α(220)
α(200)
α(200)

α(220)

intensity (a.u.)
intensity (a.u.)

tempered tempered

α'-M(110)
α'-M(110)

α'-M(211)
α'-M(211)

α'-M(220)
α'-M(200)
α'-M(200)

α'-M(220)
γ(200)

quenched quenched

20 30 40 50 60 70 80 90 100 20 30 40 50 60 70 80 90 100
2 θ / (degree) 2θ / (degree)

Figure
Figure 1.1. Microstructure
Microstructureofofas-received
as-received51CrV4
51CrV4 steel barbar
steel and X-ray
and diffraction
X-ray (XRD)
diffraction patterns
(XRD) of as-
patterns of
received,
as-received,quenched,
quenched, andand
tempered
tempered specimens:
specimens:(a)(a)microstructure
microstructureofofas-received
as-receivedsteel;
steel; (b)
(b) XRD
XRD
patterns
patternsof ofthe
theas-received
as-receivedsteel, quenched
steel, quenched and tempered
and tempered specimens
specimens at 50
at°C ◦ C oil-bath
50oil-bath temperature
temperatureand
90
and°C90 ◦ C out-of-oil
out-of-oil temperature; (c) XRD
temperature; (c) patterns of specimens
XRD patterns at 80 °C
of specimens ◦ C oil-bath
oil-bath
at 80 temperature and 90and
temperature °C
90 C out-of-oil temperature; (d) XRD patterns of specimens at 50 C oil-bath temperature and 120 ◦ C
◦
out-of-oil temperature; (d) XRD patterns of specimens at 50 °C ◦
oil-bath temperature and 120 °C out-
of-oil temperature.
out-of-oil temperature.

Figure 2a,c,e
Figure 2a,c,e presents
presents the
the microstructure
microstructure of of steel
steel bars
bars after
after quenching
quenching at at various
various oil-bath
oil-bath
temperatures of of 20 ◦ C, 50 ◦ C, and 80 ◦ C respectively (The out-of-oil temperature was 90 ◦ C). In the
20 °C,
temperatures 50 °C, and 80 °C respectively (The out-of-oil temperature was 90 °C). In the
as-quenched condition,
as-quenched condition, the
the microstructure
microstructure consisted
consisted of of untempered
untempered martensite,
martensite, bainite,
bainite, and
and retained
retained
austenite. The
austenite. Theretained
retained austenite
austenitewas wasidentified
identifiedby
by the
the XRD
XRD results,
results, whereas
whereas itit was
was not
not profound
profound in in
the structure
the structure of
of Figure
Figure 2. The
The needle-like
needle-like martensite
martensite lath
lath was
was the
the main
main component
component of of the
the quenched
quenched
structure, accompanied
structure, accompanied by by aa few
few large-sized
large-sized martensite
martensite laths.
laths. The
The martensite
martensite laths
laths were
were apparently
apparently
coarser under
coarser under higher
higher oil-bath
oil-bath temperature.
temperature. The The athermal
athermal transformation
transformation from
from austenite
austenite toto martensite
martensite
is dependent only on the amount of undercooling
is dependent only on the amount of undercooling below the below the M s temperature (∆T). The volume
Ms temperature (ΔT). The volume fraction
of martensite
fraction increases increases
of martensite with increasing ∆T [23]. The
with increasing ΔTnumber of martensite
[23]. The number of nuclei also increases
martensite nuclei with
also
the increase
increases of undercooling
with the increase ofprior to transformation
undercooling prior to[24]. The final grain
transformation [24].size
Theoffinal
the martensite
grain size will be
of the
finer as the number of nuclei is larger. Quenching at a lower oil-bath temperature
martensite will be finer as the number of nuclei is larger. Quenching at a lower oil-bath temperature tends to achieve
higherto
tends undercooling.
achieve higher Therefore, martensite
undercooling. tends to be
Therefore, finer as the
martensite oil-bath
tends temperature
to be finer as decreases.
the oil-bath
temperature decreases.
Metals 2018, 8, 1056 5 of 16
Metals 2018, 8, x FOR PEER REVIEW 5 of 16

Figure
Figure 2.
2. Microstructure
Microstructure of of the
the steel
steel bars:
bars: Specimens
Specimens quenched
quenched at
at oil-bath
oil-bath temperatures
temperatures ofof 20
20 °C
◦ C (a),
(a),
50 °C,
◦ (c) and 80 °C
◦ (e) respectively; (b), (d), and (f) are the tempered microstructures corresponding
50 C, (c) and 80 C (e) respectively; (b), (d), and (f) are the tempered microstructures corresponding
to
to specimens
specimens of of (a),
(a),(c),
(c),(e)
(e)respectively;
respectively;(g) (g)shows
showsa ahigher-magnification
higher-magnification view of of
view a bainite island
a bainite in
island
the area
in the areaoutlined
outlined bybya rectangle
a rectangleinin(a);
(a);(h)
(h)shows
showsaamorphology
morphologyof of carbide
carbide precipitation
precipitation of
of higher
higher
magnification
magnification in in the same specimen
the same specimen of of (d).
(d).

The quenched
quenchedstructure
structurecontained
contained lens-shaped
lens-shaped bainite islands,
bainite as shown
islands, in Figure
as shown 2a,c,e,g.
in Figure There
2a,c,e,g.
were carbide particles precipitated in the bainite islands (Figure 2g). A similar morphology
There were carbide particles precipitated in the bainite islands (Figure 2g). A similar morphology has been
analyzed by Sencic by
has been analyzed et al. to beetconsidered
Sencic as bainite grains
al. to be considered [3]. Gao
as bainite et al.
grains [3].also
Gaoobserved this
et al. also kind of
observed
islands
this kindin of
theislands
martensite
in thematrix and described
martensite matrix and it asdescribed
bainite islands [25]. The
it as bainite size and
islands [25].fraction
The sizeofand
the
bainite
fractionislands increased
of the bainite withincreased
islands the increase of the
with oil-bath temperature.
increase of oil-bathAt various oil-bath
temperature. temperatures,
At various oil-bath
the cooling rate of quenching was different. Thus, the diffusion distance of carbon atoms was varied
and the γ → α transition velocity was also changed. Besides, bainite formation is much slower than
martensite because it requires diffusion. Therefore, the low oil-bath temperature prevented carbon
Metals 2018, 8, 1056 6 of 16

temperatures, the cooling rate of quenching was different. Thus, the diffusion distance of carbon
atoms was varied and the γ → α transition velocity was also changed. Besides, bainite formation is
much slower than martensite because it requires diffusion. Therefore, the low oil-bath temperature
prevented carbon atom diffusion, delaying the bainite transformation and reducing the size of bainite
islands. Taken together, these results suggest that the formation of martensite and bainite islands were
both influenced by the oil-bath temperature.
In the tempering process, the martensite and retained austenite decomposed, leading to
the precipitation of carbides. The formation of fairly fine carbides was shown in Figure 2b,d,f.
The tempered structure appeared to be troostite, in which the prior martensite laths were replaced by
ferrite grains. It can be seen that the microstructure of all the three specimens contained long carbides.
The long carbides were accompanied by a certain number of short carbide particles (Figure 2h).
The carbides were located mainly at prior interlath boundaries, although some carbide particles
distributed inside the prior martensite lath. The length and width of the carbides both increased
with the increase of oil-bath temperatures. Correspondingly, the intercarbide spacings also increased.
At oil-bath temperatures of 20, 50, and 80 ◦ C, the average intercarbide spacings were measured to be
0.184, 0.212, and 0.242 µm respectively.
Carbides can easily nucleate at dislocations due to a stronger enrichment of carbon. In the
tempering process of a quenched steel bar, the carbides appeared to precipitate along the grain
boundaries and the interphase boundaries between martensite and other phases [26–28]. Therefore,
small martensite laths with more boundaries tend to prepare more locations for the nucleation of
carbides. Jang et al. found that the carbides precipitated along the surfaces of the martensite phase,
and the carbides have smaller size and were more widely dispersed due to the smaller width of
martensite phase [29]. As discussed above, the size of martensite laths decreased with the decrease of
oil-bath temperature in this work, thus the number of precipitated carbides tended to increase due to
more interfaces or boundaries in the microstructure. Correspondingly, the carbides tended to have a
smaller size. On the contrary, the number of precipitated carbides decreased and the carbides tended
to have a larger size with the increase of oil-bath temperature.
The bainite islands were also observed in the tempered microstructure (Figure 2d), which has a
similar lens-shaped morphology to those in the quenched sample.
The temperature of workpieces decreased with an increase in submerged time during the
quenching process. The surface temperatures of the steel bars were measured when they were taken
out of the oil bath (out-of-oil temperature) to identify its effects on the microstructures. Figure 3a,c,e
present the microstructures of steel bars quenching at various out-of-oil temperatures of 60 ◦ C, 90 ◦ C,
and 120 ◦ C respectively (The oil-bath temperature was 50 ◦ C). Martensite was the main phase in the
microstructures of all the three conditions. Both large-sized martensite laths and slim needle-like
martensite existed in the microstructure. There was no significant discrepancy in the size of martensite
laths in the specimens at various out-of-oil temperatures. Whereas, a high out-of-oil temperature of
120 ◦ C enhanced the chance of auto-tempering in the microstructure, which led to the precipitation of
many tiny carbide particles in the as-quenched martensite crystals (Figure 3h). In contrast, the carbide
precipitation was not observed in the specimen at a low out-of-oil temperature such as 60 ◦ C (Figure 3g),
indicating that the auto-tempering was inhibited. The auto-tempering was more profound in the
large-sized martensite lath. Morsdorf et al. found that the coarse martensite lath has a higher density
of carbide particles compared to the thinner laths, which is due to the high degree of auto-tempering
and lower dislocation density in the coarse laths [30].
Metals 2018, 8, 1056 7 of 16
Metals 2018, 8, x FOR PEER REVIEW 7 of 16

Figure
Figure 3.
3. Microstructure
Microstructureofofthethesteel
steelbars:
bars:Specimens
Specimens quenched
quenched at at
various
variousout-of-oil temperatures
out-of-oil of
temperatures
60 °C ◦(a),
of 60 C (a), °C◦ (b),
90 90 and
C (b), and120 °C◦ C(c)(c)respectively;
120 respectively;(b),(b),(d),
(d),and
and(f)
(f)are
are the
the tempered
tempered microstructures
microstructures
corresponding
corresponding totothe the specimens
specimens of (a),of (c),
(a),(e)(c), (e) respectively;
respectively; (g) show
(g) and (h) and the
(h) martensite
show the morphology
martensite
morphology of higher magnification in the specimens of
of higher magnification in the specimens of (a) and (e), respectively. (a) and (e), respectively.

Figure 3b,d,f
Figure 3b,d,fshows
showsthe
thetempered
temperedmicrostructures
microstructurescorresponding
corresponding toto
thethe quenched
quenched specimens
specimens in
in Figure
Figure 3a,c,e
3a,c,e respectively.
respectively. The
The microstructurecontained
microstructure containedlong
longcarbides
carbidesaccompanied
accompaniedby by aa certain
certain
number of
number of short
short carbide
carbide particles.
particles. The
The carbide
carbide distribution
distribution appeared
appeared to
to be
be different
different in
in the
the tempered
tempered
microstructures at various out-of-oil
microstructures out-of-oil temperatures.
temperatures. There
There were
were carbide-depleted
carbide-depleted regions
regions (large
(large black
black
regions) in
regions) in the microstructure where the distribution of carbide was sparser than other regions. The The
area of the carbide-depleted regions appeared to decrease with the increase of out-of-oil temperature.
area of the carbide-depleted regions appeared to decrease with the increase of out-of-oil temperature.
These carbide-depleted regions might correspond to the large-sized martensite laths in the quenched
specimens. As discussed above, carbides prefer to precipitate along the lath boundary, and only a
few carbide particles tended to precipitate inside the large-sized martensite lath at a low out-of-oil
 Metals 2018, 8, 1056 8 of 16

Metals 2018, 8, x FOR PEER REVIEW 8 of 16

These carbide-depleted regions might correspond to the large-sized martensite laths in the quenched
specimens. As discussed above, carbides prefer to precipitate along the lath boundary, and only a
temperature. The martensite underwent an auto-tempering process at a relatively high out-of-oil
few carbide particles tended to precipitate inside the large-sized martensite lath at a low out-of-oil
temperature, and carbide particles could nucleate inside the large martensite laths during the auto-
temperature. The martensite underwent an auto-tempering process at a relatively high out-of-oil
tempering process (Figure 3h). This provided an opportunity for them to grow into larger carbides
temperature, and carbide particles could nucleate inside the large martensite laths during the
in the subsequent principal tempering process, leading to the increase of final number density of
auto-tempering process (Figure 3h). This provided an opportunity for them to grow into larger
carbides, especially in the carbide-depleted region. Therefore, the carbide-depleted regions were not
carbides in the subsequent principal tempering process, leading to the increase of final number density
profound in the specimen at a high out-of-oil temperature such as 120 °C (Figure 3f), and the
of carbides, especially in the carbide-depleted region. Therefore, the carbide-depleted regions were
distribution of carbides appeared to be more homogeneous than that at a lower out-of-oil
not profound in the specimen at a high out-of-oil temperature such as 120 ◦ C (Figure 3f), and the
temperature. However, the carbide size increased with the increase of out-of-oil temperature.
distribution of carbides appeared to be more homogeneous than that at a lower out-of-oil temperature.
Correspondingly, the intercarbide spacings also increased. At out-of-oil temperatures of 60, 90, and
However, the carbide size increased with the increase of out-of-oil temperature. Correspondingly, the
120 °C, the average widths of the intercarbide spacing were measured to be 0.177, 0.222, and 0.231
intercarbide spacings also increased. At out-of-oil temperatures of 60, 90, and 120 ◦ C, the average
μm respectively.
widths of the intercarbide spacing were measured to be 0.177, 0.222, and 0.231 µm respectively.
Figure 4 shows the size distribution of tempered carbides in the steel bars at various out-of-oil
Figure 4 shows the size distribution of tempered carbides in the steel bars at various out-of-oil
temperatures (The statistical area in the microstructure was 600 m22). The number density of small
temperatures (The statistical area in the microstructure was 600 m ). The number density of small
carbides (with a length smaller than 0.4 μm) increased considerably as the out-of-oil temperature
carbides (with a length smaller than 0.4 µm) increased considerably as the out-of-oil temperature
increased from 60 °C to a higher degree of 90 °C or 120 °C. This was caused by the auto-tempering
increased from 60 ◦ C to a higher degree of 90 ◦ C or 120 ◦ C. This was caused by the auto-tempering
effect discussed above. The lowest number density of small carbides was observed in the specimen
effect discussed above. The lowest number density of small carbides was observed in the specimen
at out-of-oil temperature of 60 °C, when the auto-tempering has not taken effect. A relatively high
at out-of-oil temperature of 60 ◦ C, when the auto-tempering has not taken effect. A relatively high
out-of-oil temperature tended to increase the width of large-sized carbides (with a width larger than
out-of-oil temperature tended to increase the width of large-sized carbides (with a width larger than
0.24 μm). However, the length of large-sized carbides (with a length larger than 1.2 μm) tended to
0.24 µm). However, the length of large-sized carbides (with a length larger than 1.2 µm) tended to
decrease with the increase of out-of-oil temperature. This effect indicates that the fraction of long
decrease with the increase of out-of-oil temperature. This effect indicates that the fraction of long
carbides decreased, and the particle-shaped carbides tended to have a higher fraction as the out-of-
carbides decreased, and the particle-shaped carbides tended to have a higher fraction as the out-of-oil
oil temperature increased. As discussed above, the carbides nucleated inside large martensite laths
temperature increased. As discussed above, the carbides nucleated inside large martensite laths as tiny
as tiny particles during an auto-tempering process, which reduced their chance to grow into long
particles
carbides in during an auto-tempering
the later process, process,
principal tempering which reduced their
thus the chance of
fraction to grow into long carbides
particle-shaped carbidesin
the later
increased. principal tempering process, thus the fraction of particle-shaped carbides increased.

1200
(a) o (b) o
60 C out-of-oil temperature
60 C out-of-oil temperature 500 o
o 90 C out-of-oil temperature
90 C out-of-oil temperature o
1000 o 120 C out-of-oil temperature
120 C out-of-oil temperature
400

800

300
Number
Number

600

200
400

100
200

0
0 0.04 0.08 0.12 0.16 0.20 0.24 0.28 0.32 0.36
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8
Carbide width (μm)
Carbide length (μm)

Figure
Figure4.4.The
Thecarbide
carbidelength
length(a)
(a)and
andwidth
width(b)(b)distribution
distributionininthe
thetempered
temperedsteel
steelbars
barsquenched
quenchedatat
various
variousout-of-oil
out-of-oiltemperatures
temperaturesofof60 ◦
60°C,C,90 ◦
90°C,C,and
and120 ◦
120°CCrespectively.
respectively.

Thephase
The phasediagram
diagramofof51CrV4
51CrV4 steel
steel was was shown
shown in Figure
in Figure 5, which
5, which waswas calculated
calculated basedbased
on theon
the Thermo-Calc
Thermo-Calc software.
software. The composition
The composition of 51CrV4
of 51CrV4 steelsteel
was wascloseclose to the
to the eutectoid
eutectoid point.
point. The The
A1
A1 temperature
temperature was was about
about °C. ◦ C.
743 743 There
There were were several
several kindsofofprecipitations
kinds precipitationsformed
formedatat various
various
temperatures,including
temperatures, includingthe theMnS,
MnS,thethecementite,
cementite,the theM M7C7C (carbideofofFe
3 3(carbide Feand
andCr),
Cr),the
thegraphite,
graphite,the
the
MM2P 2 P (phosphide
(phosphide ofof Fe
Fe and
and Mn),
Mn), and
and the
the MM 3 C C
3 2
2 (carbide
(carbide ofofFeFe and
and Cr).
Cr). At
At the
the tempering
tempering temperature
temperature
ofofthis
thiswork,
work,the
theMM7C7C 3 -typecarbides
3-type carbideswerewereprecipitated.
precipitated.Moreover,
Moreover,MnS MnSexisted
existedas asinclusions
inclusionsatatboth
both
soaking and tempering
soaking temperingprocess.
process.Graphite
Graphite is predicted
is predictedto precipitate
to precipitate 600 ◦ C600
belowbelow in the
°C phase
in thediagram.
phase
However,However,
diagram. graphite graphite
was not observed in the microstructure
was not observed of this work.
in the microstructure of this work.
Metals 2018, 8, 1056 9 of 16
Metals 2018, 8, x FOR PEER REVIEW 9 of 16
Metals 2018, 8, x FOR PEER REVIEW 9 of 16

Figure
Figure 5.Phase
Figure5.5. Phasediagram
Phase diagramof
diagram of51CrV4
of 51CrV4 spring
51CrV4 steel (calculated
spring steel
spring (calculatedbased
(calculated basedon
based onthe
on theThermo-Calc
the Thermo-Calcsoftware).
Thermo-Calc software).
software).

Figure
Figure6 66shows
showsthe themole
molefraction
fraction ofof precipitated
precipitated phases phaseschanging
phases changingwith withtemperature,
temperature,which which was
was
Figure shows the mole fraction of precipitated changing with temperature, which was
calculated
calculated using
using Thermo-Calc
Thermo-Calc software.
software. There are are several
several kinds
kindsof ofcarbide
carbideprecipitations
precipitationsoccurring
occurring
calculated◦ using Thermo-Calc software. There are several kinds of carbide precipitations occurring
below
below740
below 740 C,
740 °C,including
°C, includingthe
including thecementite,
the cementite,the
cementite, theM
the M333C
M C222-type,
C
and the
-type, and
-type, and the M
the M777C
CC33-type
-typecarbides.
3-type carbides.A
carbides. AAsignificant
significant
significant
amount ◦
amountofof
amount ofcementite
cementiteisis
cementite isstable
stablein
stable inthe
in the temperature
the temperature range
temperature range of
range of 590–720
of 590–720°C,
590–720 °C, C,whereas
whereasit
whereas ititrapidly
rapidlydecreases
rapidly decreases
decreases
with
with decreasing
decreasing temperature
temperature below
below 590
590 ◦°C.
C. The
The cementite
cementite is completely
completely replaced
replaced bybyM M3C C -type and
with decreasing temperature below 590 °C. The cementite is completely replaced by M3C3 2-type 2 2 -type
andand
MMM
7C7
7C
C -type
3 -type
3 carbides.
carbides. M M 7 C3 carbide reaches its largest fraction and remains stable
carbide reaches its largest fraction and remains stable in the temperature
3-type carbides. M77C33 carbide reaches its largest fraction and remains stable in the temperature
in the temperature
range
range of of 420–480
420–480 ◦ C,°C,
whichwhich covers
covers the tempering
tempering
the tempering temperature
temperature ofwork,
of this this work,
work, indicating
indicating that the that the
carbides
range of 420–480 °C, which covers the temperature of this indicating that the
carbides
observed inobserved
Figures in
2 Figures
and 3 2
were and 3 were
mostly
carbides observed in Figures 2 and 3 were mostly M mostly
C
7 3 M
-type. 7C 3-type.
The The
amount
M7C3-type. The amount amount
of M C of M 7C3 carbide
carbide is is
graduallygradually
7 3of M7C3 carbide is gradually reduced
reduced
and replaced andbyreplaced by M
M3 C2 carbides M33CC22 carbides
carbides
below ◦ C. 420 °C.
below
420
reduced and replaced by below 420 °C.
0.10
0.10
Cementite
Cementite
MC
M33C22
0.08 MC
0.08 M77C33
MnS
MnS
phases
Fractionofofphases

0.06
0.06

0.04
Fraction

0.04

0.02
0.02

0.00
0.00
200 400 600 800 1000
200 400 600 o
800 1000
Temperature ( o C)
Temperature ( C)
Figure
Figure 6.The
Figure6.6. Themole
The molefraction
mole fractionof
fraction ofprecipitated
of precipitated phases
precipitated varioustemperatures
at various
phases at various temperatures(calculated
temperatures (calculated
(calculated based
based
based onon
on thethe
the
Thermo-Calc
Thermo-Calc software)
software)
Thermo-Calc software)
Metals 2018,
Metals 8, x1056
2018, 8, FOR PEER REVIEW 10 of
10 of 16
16

As indicated by the phase diagram (Figure 5), the MnS inclusions could exist in a large
As indicated by the phase diagram (Figure 5), the MnS inclusions could exist in a large temperature
temperature range below 1400 °C. Figure 7a,b shows the morphology of several MnS inclusion
range below 1400 ◦ C. Figure 7a,b shows the morphology of several MnS inclusion particles, which was
particles, which was identified by EDS elemental mapping and point analysis. Figure 7c shows the
identified by EDS elemental mapping and point analysis. Figure 7c shows the corresponding EDS
corresponding EDS elemental mapping images of the inclusions in Figure 7a, which indicate that the
elemental mapping images of the inclusions in Figure 7a, which indicate that the main elements of
main elements of the inclusions were Mn and S. Figure 7d shows the EDS point analysis of point 1 in
the inclusions were Mn and S. Figure 7d shows the EDS point analysis of point 1 in the inclusion of
the inclusion of Figure 7b. The composition appeared to be 40% Mn and 42% S, indicating that the
Figure 7b. The composition appeared to be 40% Mn and 42% S, indicating that the inclusion was MnS.
inclusion was MnS.

Figure 7. MnS Inclusion particles: (a,b) SEM image of two inclusion particles; (c) EDS elemental
Figure 7. MnS Inclusion particles: (a,b) SEM image of two inclusion particles; (c) EDS elemental
mapping around the inclusions of (a); (d) EDS point analysis of point 1.
mapping around the inclusions of (a); (d) EDS point analysis of point 1.

The
The mechanical
mechanical properties
properties of
of tempered
tempered steel
steel bars
bars were
were directly influenced by
directly influenced the intercarbide
by the intercarbide
spacing. The troostite belongs to the pearlite-type structure. The strength of the
spacing. The troostite belongs to the pearlite-type structure. The strength of the pearlite-typepearlite-type
structure
structure (ferrite
(ferrite+ +
carbide) hashas
carbide) beenbeenreported to follow
reported a Hall-Petch
to follow type relationship
a Hall-Petch with respect
type relationship to
with
the intercarbide spacing [31–34]. Both yield strength and hardness follow a Hall-Petch
respect to the intercarbide spacing [31–34]. Both yield strength and hardness follow a Hall-Petchrelationship
[33,35,36]:
relationship [33,35,36]:
σyσ ==σσ0 ++ kks λλ−−1/1/2
2 (1)
y 0 s (1)
Hrc = H0 + kh λ−1/2 (2)
−1 / 2
H rc = H 0 + k h λ (2)
where λ is the intercarbide spacing, σy is the yield strength of the steel, σ0 is the internal frictional
strength
where of the
λ is ferrite with the infinite
intercarbide spacing,mean
σy is free
the yield and ks isofa the
path, strength dislocation
steel, σ0 locking constant
is the internal during
frictional
yielding.of
strength Hrc is thewith
ferrite Rockwell
the infinite meanH0free
hardness, is the hardness
path, and ks of
is athe ferrite with
dislocation the infinite
locking mean
constant free
during
path, and k is related to the dislocation locking constant during hardness measurement.
yielding. Hrc is the Rockwell hardness, H0 is the hardness of the ferrite with the infinite mean free
h
path,Since
and kthe intercarbide spacings increased with the increase of oil-bath temperature, the tensile
h is related to the dislocation locking constant during hardness measurement.
strength
Sinceand
thehardness should
intercarbide decrease
spacings with the
increased withincrease of oil-bath
the increase temperature
of oil-bath according
temperature, to the
the tensile
strength and hardness should decrease with the increase of oil-bath temperature according to(YS)
Hall-Petch relationship. Figure 8a shows the ultimate tensile strength (UTS) and yield strength the
changing with
Hall-Petch oil-bath temperature,
relationship. Figure 8a showsin which the stress
the ultimate and strain
tensile strengthwere engineering
(UTS) and yieldvalues.
strength As(YS)
the
oil-bath temperature increased from 20 ◦
to 80 C,
changing with oil-bath temperature, in which thethe average
stress UTS decreased
and strain from 1599values.
were engineering to 1549AsMPa,
the
and the average YS decreased from 1451 to 1398 MPa. Correspondingly,
oil-bath temperature increased from 20 to 80 °C, the average UTS decreased from 1599 to 1549 the percentages ofMPa,
area
reduction
and and elongation
the average at break
YS decreased both1451
from increased
to 1398with increasing
MPa. oil-bath temperature,
Correspondingly, indicating
the percentages that
of area
a high oil-bath temperature benefits the enhancement of ductility. An extensometer
reduction and elongation at break both increased with increasing oil-bath temperature, indicating was set during
that a high oil-bath temperature benefits the enhancement of ductility. An extensometer was set
Metals 2018, 8, 1056 11 of 16
Metals 2018, 8, x FOR PEER REVIEW 11 of 16

the tensile
during the test to measure
tensile the strain
test to measure precisely.
the The elastic
strain precisely. Themodulus was calculated
elastic modulus from the from
was calculated slopesthe
of
elastic part of the stress-strain curves. The elasticity modulus, which is an important
slopes of elastic part of the stress-strain curves. The elasticity modulus, which is an important parameter relating
to the spring
parameter behavior,
relating also
to the decreased
spring withalso
behavior, increasing oil-bath
decreased withtemperature, as shown
increasing oil-bath in Figure 8b.
temperature, as
Figure 8c shows the hardness results tested along a diameter in a cross section of
shown in Figure 8b. Figure 8c shows the hardness results tested along a diameter in a cross sectionthe tempered steel
bar.the
of The hardnesssteel
tempered value showed
bar. a small discrepancy
The hardness value showed between
a smallthe center andbetween
discrepancy surface, indicating that
the center and
the steel indicating
surface, bar was fully thathardened during
the steel bar wasthe quenching
fully hardened process.
duringThe hardness ofprocess.
the quenching tempered workpieces
The hardness
decreased with the increase of oil-bath temperature. As discussed in Figure
of tempered workpieces decreased with the increase of oil-bath temperature. As discussed in1, the fraction of austenite
Figure
was higher in samples at 80 ◦ C oil-bath temperature than that at 50 ◦ C, which also contribute to °C,
the
1, the fraction of austenite was higher in samples at 80 °C oil-bath temperature than that at 50
decrease of strength and hardness.
which also contribute to the decrease of strength and hardness.

1700 280
Elongation at break,A(%) / Utimate Strength,Rm(Mpa)

1700
(a) (b)

Yield strength,RP0.2(MPa) / Reduction of area, Z(%)

1600 Rm 1600 260

1500 1500

Elasticity modulus (GMPa)

240
1400
Rp0.2
1400
220
1300 1300
9.8

8.4 200
35
7.0 Z
A 180
5.6 30

4.2 160
25

10 20 30 40 50 60 70 80 90 10 20 30 40 50 60 70 80 90 100
o
Oil-bath temperature( C) o
Oil-bath temperature( C)

50
(c) Oil-bath temperature 20 C
o
49 o
Oil-bath temperature 50 C
o
48 Oil-bath temperature 80 C
47

46
Hardness(HRC)

45

44

43

42

41

40
-12 -10 -8 -6 -4 -2 0 2 4 6 8 10 12
Distance from center(mm)

Figure
Figure 8.
8. Mechanical
Mechanical properties
properties ofof the
the steel
steel bars
bars at
at various
various oil-bath
oil-bath temperatures:
temperatures: (a)
(a) ultimate
ultimate tensile
tensile
strength,
strength, yield strength, elongation at break, and reduction of area (The stress and strain and
yield strength, elongation at break, and reduction of area (The stress strain are
are engineering
engineering value); (b)
value); (b) elasticity elasticity
modulus; (c)modulus; (c) rockwell
rockwell hardness hardness
(HRC) (HRC) samples.
of tempered of tempered samples.

As discussed above, the the intercarbide

intercarbide spacings
spacings decreased
decreased withwith the increase of out-of-oil
temperature. According to the Hall-Petch relation, the tensile strength and hardness should decrease
with increasing oil-bath temperature. FigureFigure 9a shows the ultimate tensile strength (UTS) and yield
strength (YS) changing with out-of-oil temperature,
temperature, in which the stress and strain were engineering
values. As the
theout-of-oil
out-of-oiltemperature
temperatureincreased
increased from
from 60 60
to 120 ◦ C,°C,
to 120 the the average
average UTSUTS decreased
decreased fromfrom
1615
1615 to MPa,
to 1513 1513 andMPa,
theand the average
average YS decreased
YS decreased from 1461from 1461
to 1404 to 1404
MPa. MPa. Correspondingly,
Correspondingly, the
the percentages
percentages of area
of area reduction andreduction
elongation andatelongation
break bothatincreased
break both increased
with with of
the increase theout-of-oil
increase temperature,
of out-of-oil
temperature,
indicating that indicating that a high
a high out-of-oil out-of-oil resulted
temperature temperaturein theresulted in the enhancement
enhancement of ductility.
of ductility. The elasticity
The elasticity
modulus also modulus
decreasedalso
withdecreased withofthe
the increase increasetemperature,
out-of-oil of out-of-oil temperature, as shown
as shown in Figure 9b. in Figure
9b.
Metals 2018, 8, 1056 12 of 16
Metals 2018, 8, x FOR PEER REVIEW 12 of 16

(a) (b)
Elongation at break,A(%) / Utimate Strength,Rm(Mpa)

Yield strength,RP0.2(MPa) / Reduction of area, Z(%)

1700 1700
260
1600 Rm
1600

1500 240
1500

Elasticity modulus (GMPa)

Rp0.2
1400
1400
220
1300
9.6 1300

8.0 200
35
6.4 A
Z 180
4.8 30

3.2 160
25

50 60 70 80 90 100 110 120 130

50 60 70 80 90 100 110 120 130
o
Out-of-oil temperature( C) o
Out-of-oil temperature( C)

50
o
(c) Out-of-oil temperature 60 C
49 o
Out-of-oil temperature 90 C
o
48 Out-of-oil temperature 120 C
47

46
Hardness(HRC)

45

44

43

42

41

40
-12 -10 -8 -6 -4 -2 0 2 4 6 8 10 12
Distance from center(mm)

Figure
Figure 9.
9. Mechanical
Mechanical properties
properties of
of the
the steel
steel bars
bars at
atvarious
variousout-of-oil
out-of-oil temperatures:
temperatures: (a)
(a) ultimate
ultimate tensile
tensile
strength, yieldstrength,
strength, yield strength, elongation
elongation at break,
at break, and reduction
and reduction of area of area
(The (The
stress andstress
strain and strain are
are engineering
engineering value); (b)
value); (b) elasticity elasticity
modulus; (c)modulus; (c) rockwell
rockwell hardness hardness
(HRC) (HRC) of
of tempered tempered samples.
samples.

The auto-tempering
The auto-temperingwas wasa possible
a possible reason
reason to cause
to cause the change
the change of mechanical
of mechanical properties
properties at a highat
a high out-of-oil
out-of-oil temperature.
temperature. The auto-tempering
The auto-tempering process generated
process generated carbide particles
carbide particles inside theinside the
carbide-
carbide-depleted
depleted region atregion
a highatout-of-oil
a high out-of-oil temperature
temperature (Figure(Figure
3), and3), and reduced
reduced the volume
the volume fraction
fraction of such of
areas in theinfinal
such areas microstructure
the final microstructure after subsequent
after subsequent principal
principaltempering.
tempering.Besides,
Besides,the theauto-tempering
auto-tempering
reduced
reduced thethelength
lengthofoflarge-sized
large-sized carbides
carbidesand enhanced
and enhancedtheir width
their widthat the
at same time time
the same (Figure 4). This
(Figure 4).
coarsening behavior
This coarsening of theofcarbides
behavior at high
the carbides out-of-oil
at high temperature
out-of-oil temperature contributed
contributed to atorelative drop
a relative of
drop
tensile strength.
of tensile strength.
As theout-of-oil
As the out-of-oil temperature
temperature increased,
increased, the hardness
the hardness decreased
decreased due to the due to the
increase increase of
of intercarbide
intercarbide spacing(Figure
spacing of carbides of carbides (Figure
9c). In 9c). In the
the tempered tempered
specimen specimen
quenched at 60 ◦ C out-of-oil
quenched at 60 °C out-of-oil
temperature,
temperature, most ofresults
most of the hardness the hardness
were in the results
rangewere in the
of 46~47 range
HRC; whenof the
46~47 HRC; temperature
out-of-oil when the out-of-oil
changed
to 120 ◦ C, most
temperature changed
of thetohardness
120 °C, most of the
results hardness
were in the results
range were in the
of 44~45 range
HRC, of 44~45
and HRC, andwas
the decrement the
decrement
about 4.3%.was about 4.3%.
The
The yield
yield strength
strength andand hardness
hardness of the steel samples with various intercarbide intercarbide spacings
spacings are
shown
shown inin Figure
Figure 10. Two
Two dashed lines are plotted as functions of the the inverse
inverse of of the
the square
square root
root of
of the
the
intercarbide
intercarbide spacing −
spacing (λ ) in1/2
−1/2 ) inFigure
Figure10a,b
10a,brespectively.
respectively.From
Fromthetheplot,
plot,intercepts
intercepts and and slopes
slopes were
were
calculated,
calculated, and the following empirical relationships were obtained:

σσ = 973 + 206λ−−1/1/2
2
(3)
y y= 973 + 206λ (3)

−1/2
HHrcrc== 34.5
34.5+ 5.1λ − 1 / 2
+ 5.1λ (4)
(4)

This implies that the yield strength and the hardness both decreased with increasing intercarbide
in accordance with the Hall-Petch relationship. Both high oil-bath temperature and high out-of-oil
Metals 2018, 8, x FOR PEER REVIEW 13 of 16

temperature resulted in an increase in intercarbide spacing, which led to the decrease of strength
Metals 2018, 8, 1056 13and
of 16
hardness.

1550 49

various oil-bath temperature various oil-bath temperature

various out-of-oil temperature various out-of-oil temperature
1500 48
Yield Strength (MPa)

Hardness (HRC)
1450 47

1400 46

1350 45

1300 44
0.18 0.20 0.22 0.24 0.16 0.18 0.20 0.22 0.24

Intercarbide spacing (μm) Intercarbide spacing (μm)

(a) (b)
Figure
Figure 10.
10. Yield
Yield strength
strength and
and hardness
hardness of
of the
the steel
steel bars
bars with
with various
various intercarbide
intercarbide spacings:
spacings: (a)
(a) yield
yield
strength;
strength; (b)
(b) hardness.
hardness.

This implies
According tothat
the the yield
above strength and
discussions on the hardnessproperties,
mechanical both decreased bothwith
highincreasing intercarbide
oil-bath temperature
in accordance with the Hall-Petch relationship. Both high oil-bath temperature
and high out-of-oil temperature benefited the enhancement of the ductility, which correspondingly and high out-of-oil
temperature
reduced resultedand
the strength in an increase
hardness. in intercarbide
These effects werespacing, which led
further proved to the
by the decrease
fracture of strength
analysis. Figure
and
11 hardness.
shows the SEM microfractographs of the steel bars investigated. The fractures were uneven and
showed According
randomtofluctuations.
the above discussions
Fractures on of mechanical
all the fourproperties,
conditionsboth werehigh oil-bath temperature
composed by dimple and and
high out-of-oil temperature
quasi-cleavage morphology,benefited the enhancement
which indicated of the ductility,
the experimental steel hadwhich
highcorrespondingly
toughness. Many reduced
deep
the strength
dimples wereand hardness.
observed, andThese
manyeffects
smallwere further
dimples were proved by thearound
distributed fracturelarge
analysis.
dimples.Figure 11 shows
There were
the SEMexisting
pockets microfractographs
in all the four of conditions,
the steel bars investigated.
which containedThe fractures
features that were uneven
resemble and showed
localized quasi-
random fluctuations.
cleavage. Figure 11a,bFractures
presentsofthe all fracture
the four conditions
morphology were composed
of the specimens by dimple
at 20 and and 80
quasi-cleavage
°C oil-bath
temperatures, respectively. The specimen at 80 °C oil-bath temperature had a larger dimple were
morphology, which indicated the experimental steel had high toughness. Many deep dimples size,
observed, and
indicating thatmany small dimples
this specimen hadwere distributed
a higher around
ductility. large11c,d
Figure dimples.
showsTherethewere pockets
tensile existing
fractures of
in all the four
tempered conditions,
51CrV4 which
spring steel contained
bars at variousfeatures that resemble
out-of-oil localized
temperatures. At 60quasi-cleavage. Figure 11a,b
°C out-of-oil temperature,
presents
the dimplesthe fracture
appearing morphology of thefracture
in the tensile specimenswereat 20 andand
small 80 ◦ C oil-bath temperatures,
uniformly distributed, most respectively.
of the
The specimen ◦
at 80lessC oil-bath temperature had a larger temperature,
dimple size, indicating that this specimen had
dimples had sizes than 1 μm. At 120 °C out-of-oil many large dimples with sizes
a higher
larger ductility.
than 1 μm were Figure 11c,d shows
observed. the tensile
Therefore, the fractures of tempered
fracture was more ductile51CrV4 at aspring
higher steel bars at
out-of-oil
various out-of-oil
temperature. temperatures.
The fracture At 60 ◦ C
morphology out-of-oil
could temperature,
explain the mechanicalthe dimples
property appearing in the tensile
results presented in
fracture8were ◦C
Figures and small
9. It isand uniformly
noted distributed,
that a fine inclusion most
wasofobserved
the dimples had sizes
in Figure 11d,less than
and the1 inclusion
µm. At 120 was
out-of-oil
MnS temperature,
compound according many large
to the EDS dimples with sizes larger than 1 µm were observed. Therefore,
analysis.
the fracture was more ductile at a higher out-of-oil temperature. The fracture morphology could
explain the mechanical property results presented in Figures 8 and 9. It is noted that a fine inclusion
was observed in Figure 11d, and the inclusion was MnS compound according to the EDS analysis.
Metals 2018, 8, 1056 14 of 16
Metals 2018, 8, x FOR PEER REVIEW 14 of 16

Figure 11. Fracture morphology of tempered steel bars: specimens quenched at oil-bath temperature
Figure 11. Fracture morphology of tempered steel bars: specimens quenched at oil-bath temperature
of 20 °C (a) and 80 °C (b), respectively; specimens quenched at out-of-oil temperature of 60 °C (c) and
of 20 ◦ C (a) and 80 ◦ C (b), respectively; specimens quenched at out-of-oil temperature of 60 ◦ C (c) and
120 ◦°C (d), respectively.
120 C (d), respectively.

The
The size
size of
of the
thedimples
dimpleson onthe
thefracture
fracturesurface
surfacewas
wasgoverned
governed bybythe number
the number and
anddistribution
distributionof
microvoids that are nucleated at regions of localized strain discontinuity, such as that associated
of microvoids that are nucleated at regions of localized strain discontinuity, such as that associated with
grain grain
with boundaries or second
boundaries phase particles
or second [37]. The[37].
phase particles microvoids grew to a large
The microvoids grew size
to aand ledsize
large to large
and
dimples when the nucleation sites were few and widely spaced. As discussed above,
led to large dimples when the nucleation sites were few and widely spaced. As discussed above, the average
intercarbide spacing increased
the average intercarbide with both
spacing increased withthe increase
both of oil-bath
the increase temperature
of oil-bath temperatureandand out-of-oil
out-of-oil
temperature.
temperature. The large intercarbide spacing caused a small number density of nucleation sites
The large intercarbide spacing caused a small number density of nucleation and
sites and
resulted in large
resulted in large dimple
dimple size.
size.

4.
4. Conclusions
Conclusions
The
The present work performed
present work performed soaking,
soaking, quenching,
quenching, andand tempering
tempering on on 51CrV4
51CrV4 steel.
steel. The
The effects
effects of
of
various oil-bath temperatures and out-of-oil temperatures on the quenching
various oil-bath temperatures and out-of-oil temperatures on the quenching microstructure, tempering microstructure,
tempering
microstructure,microstructure, and the mechanical
and the mechanical propertiesproperties were investigated,
were investigated, the mainthe main conclusions
conclusions can be
can be summarized
summarized as follows: as follows:
The
The as-quenched
as-quenched microstructure
microstructure of of 51CrV4
51CrV4 steel
steel consisted
consisted of of needle-like
needle-like martensite,
martensite, large-sized
large-sized
martensite laths, lens-shaped bainite islands, and retained austenite. The tempered
martensite laths, lens-shaped bainite islands, and retained austenite. The tempered microstructure microstructure
contained
contained longlongcarbides,
carbides,accompanied
accompanied byby a certain
a certain number
number of carbide
of carbide particles.
particles. According
According to the to the
phase
phase
diagram diagram calculated
calculated based onbased on Thermo-Calc
Thermo-Calc software,software,
the M7the M7C3carbides
C3 -type -type carbides were precipitated
were precipitated at the
at the tempering temperature
tempering temperature of this work. of this work.
A lower oil-bath
A lower oil-bath temperature
temperature tended
tended to to achieve
achieve higher
higher cooling
cooling rate
rate and
and higher
higher undercooling,
undercooling,
which led
which led to
to the
the finer
finer size
size ofof martensite.
martensite. A A coarsening
coarsening of of the
the martensite
martensite occurred
occurred at at aa high
high oil-bath
oil-bath
temperature. In addition, the size and fraction of the bainite islands increased
temperature. In addition, the size and fraction of the bainite islands increased with the increase with the increase of oil-
bath temperature.
of oil-bath temperature.In theIn tempered
the temperedspecimens
specimens which
whichhavehavebeen
been quenched
quenchedatataa high oil-bath
high oil-bath
temperature,
temperature, the number of precipitated carbides decreased and the carbides tended to have aa larger
the number of precipitated carbides decreased and the carbides tended to have larger
size. Sincethe
size. Since theintercarbide
intercarbide spacings
spacings increased
increased withwith increasing
increasing oil-bath
oil-bath temperature,
temperature, thestrength
the tensile tensile
strength
and hardnessand hardness both decreased
both decreased with increasing
with increasing oil-bath temperature
oil-bath temperature in accordance in accordance with the
with the Hall-Petch
Hall-Petch relationship. Correspondingly, the ductility increased with
relationship. Correspondingly, the ductility increased with the increase of oil-bath temperature. the increase of oil-bath
temperature.
Metals 2018, 8, 1056 15 of 16

A high out-of-oil temperature enhanced the chance of auto-tempering, which led to the
precipitation of tiny carbide particles in the as-quenched martensite laths. This auto-tempering
effect reduced the length of large-sized carbides and enhanced their width in the final tempered
microstructure. The intercarbide spacings between carbides increased with the increase of out-of-oil
temperature. The tensile strength and hardness decreased with increasing oil-bath temperature, and the
ductility increased correspondingly.
The fracture of 51CrV4 steel was composed by dimple and quasi-cleavage morphology. Both a
higher oil-bath temperature and a higher out-of-oil temperature resulted in larger dimples, which can
explain the enhancement of ductility.

Author Contributions: Methodology, L.Z. and E.W.; Investigation, L.Z. and Y.L.; Formal Analysis, X.R. and D.G.;
Data Curation, X.W. and D.G.; Writing—Original Draft Preparation, L.Z.
Funding: This research was funded by the National Natural Science Foundation of China, grant number 51674083,
the project of heat treatment optimization and product quality control of springs used in urban rail train (funded
by the CRRC Guiyang Co., LTD.), and the Programme of Introducing Talents of Discipline to Universities (the 111
Project of China), grant number B07015.
Conflicts of Interest: The authors declare no conflict of interest.

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