materials

Article
Microstructure Evolution and Mechanical Properties
of 0.4C-Si-Mn-Cr Steel during High
Temperature Deformation
Fei Zhang 1,2 , Yang Yang 1,2 , Quan Shan 1,2, * , Zulai Li 1,2, *, Jinfeng Bi 1,2 and Rong Zhou 1,2
1 School of Material Science and Engineering, Kunming University of Science and Technology,
Kunming 650093, China; 15096694110@163.com (F.Z.); yangyang72199@163.com (Y.Y.);
jfsd1015@126.com (J.B.); zhourong@kmust.edu.cn (R.Z.)
2 National & Local Joint Engineering Laboratory of Advanced Metal Solidification Forming and Equipment
Technology, Kunming University of Science and Technology, Kunming 650093, China
* Correspondence: quanshan.ms@gmail.com (Q.S.); lizulai@126.com (Z.L.)




Received: 8 November 2019; Accepted: 27 December 2019; Published: 1 January 2020


Abstract: Herein, the effects of height-diameter ratios (H/D) on the microstructure evolution and
mechanical properties of 0.4C-Si-Mn-Cr steel during high temperature deformation are reported.
The compression experiments were performed on steel samples using Gleeble to obtain a reasonable
deformation temperature, and the degree of deformation was assessed in the range of 1.5 to 2.0 H/D via
forging. The forged specimens were quenched using the same heat treatment process. The hardness
and impact toughness of the steel samples were tested before and after heat treatment. Grain sizes
gradually increased with an increase in the compression temperature from 950 ◦ C to 1150 ◦ C, and the
grain sizes decreased with an increase in H/D. The microstructure of the steel samples contained
pearlite, bainite, martensite, and retained austenite phase. The microstructure after forging was more
uniform and finer as compared to that of as-cast steel samples. The hardness and impact toughness
of the steel samples were evaluated after forging; hardness first increased and then decreased with an
increase in H/D, while the impact toughness continuously increased with an increase in H/D. Hence,
the microstructure and properties of steel could be improved via high temperature deformation,
and this was primarily related to grain refinement.

Keywords: deformation; height-diameter ratio; pearlite; impact toughness

1. Introduction
Owing to their excellent comprehensive performance, medium carbon steels have been widely
used in essential fields such as energy development, machine manufacturing, and rail traffic [1–4].
In recent years, there has been an intense focus on the improvement of material properties through
deformation technologies such as hot rolling, cold rolling, and forging [5–8]. Forging is a method for
refining the grain size of steel via severe plastic deformation to enhance the strength and toughness.
Internal cracks and defects of raw materials can be reduced during forging, and the microstructure and
grain distribution are more uniform and compact after forging [9,10].
Grain refinement during deformation has a positive effect on the microstructure and properties
of steel. G.P. Chaudhari et al. [11–14] found that the grain was clearly refined after multidirectional
forging of steel, which induced fine austenite grains because of continuous dynamic recrystallization
and dynamic recovery. The formation of fine grains is beneficial for enhancement of tensile strength
and hardness. Crystal slips are the primary mode of deformation, and the mechanism of ferrite
refinement is comprised grain segmentation and recovery. Sumit et al. [15] found that when the steel
was forged in pure ferrite regions, the mechanical properties of steel had the best combination of yield

Materials 2020, 13, 172; doi:10.3390/ma13010172 www.mdpi.com/journal/materials

Materials 2020, 13, 172 2 of 11

strength and ductility. Hot compression deformation at different temperatures (950–1150 ◦ C) and
rates (0.01–10 s−1 ) can significantly promote grain refinement of as-cast samples [16]. Yang et al. [17]
conducted hot deformation experiments of 35CrMoV steel with a degree of deformation that was
about 50% at temperatures of 850 ◦ C, 950 ◦ C, and 1050 ◦ C and concluded that grain size increased
gradually with an increase in the deformation temperature under the same strain rate. Furthermore,
the performance of the forging can be further enhanced via heat treatment. Smaropoulos [18] achieved
excellent tensile strength, hardness, and toughness of a low alloy steel after forging followed by
heat treatment. The as-obtained medium carbon steel had extraordinary mechanical properties,
and this was achieved by alternating timed quenching in water and air [19,20]. However, the current
research on microstructure evolution and mechanical properties of 0.4C-Si-Mn-Cr steel under different
degrees of deformation is still limited, especially in the high temperature forging process. Therefore,
understanding of microstructure evolution in steels and the associated mechanism is beneficial for
further formulating and improving the deformation process.
Herein, to determine an appropriate forging temperature, Gleeble simulated compression
deformation of medium carbon (0.4C-Si-Mn-Cr) steel under different temperatures. Samples
with different height-diameter ratios (H/D) were forged and quenched. The microstructures of
specimens were characterized using optical microstructure (OM) analysis, scanning electron microscopy
(SEM), X-ray diffraction (XRD), and transmission electron microscopy (TEM). The hardness and
impact toughness were investigated, and the microstructure evolution and mechanical properties
of 0.4C-Si-Mn-Cr steel contributed towards providing a theoretical basis for the change rule of the
deformation process.

2. Experimental Methods
The chemical composition of the steel investigated in this work is listed in Table 1. The steel was
smelted and poured into a cylindrical billet in an intermediate frequency furnace. A direct reading
spectrometer was used to determine the chemical composition of the tested alloy. A schematic diagram
of the experimental process is provided in Figure 1. The billet was processed into a round rod of
size Φ8 × 12 mm. Specimens were heated to 50 ◦ C below the predetermined temperature at a rate of
10 ◦ C/s on a Gleeble-1500D dynamic thermal simulator (Data Sciences International INC, St. Paul, MI,
USA), and then, the heating rate was reduced to 2 ◦ C/s. The strain rate was 5 s−1 , and deformation
was 50%. Compression tests were conducted at temperatures of 950 ◦ C, 1050 ◦ C, and 1150 ◦ C and
maintained at the specified temperatures for 5 min followed by water quenching to cool the sample
to room temperature (Figure 1a,b). The round bar was subjected to multidirectional force and then
formed into a ball in a high temperature forging process (Figure 1c). Cylindrical billets with different
H/D values (1.5, 1.7, and 2.0) were taken to 1050 ◦ C for hot forging, and the billets were forged into a
sphere of 150 mm (Figure 1d). The heat treatment was carried out by alternating the cycle cooling
process in water and air (Figure 1e). After forging, samples were subjected to a quenching treatment
under the same conditions. Moreover, all the samples were heated to 900 ◦ C for 3 h, followed by
alternating cycle cooling in water and air (after water cooling, the sample was cooled in air). Because
the cooling rate of steel in water was higher than that in air, the temperature of samples could be
reduced relatively uniformly to the isothermal region. As the quenching temperature decreased, the
slope of the curve during water cooling was reduced gradually. The time of water cooling was 10 s,
and that of air cooling was 15 s. The samples were treated at 330 ◦ C for 3 h in a salt bath and further
cooled to room temperature in air.

Table 1. Chemical composition of the 0.4C-Si-Mn-Cr steel.

Element C Si Mn Cr Fe
Content (wt.%) 0.37–0.60 1.60–2.0 2.0–2.5 0.55–0.85 Balance
Oregon State, U.S.).

Table 1. Chemical composition of the 0.4C-Si-Mn-Cr steel.

Element C Si Mn Cr Fe
Materials 2020, 13, 172 3 of 11
Content (wt.%) 0.37–0.60 1.60–2.0 2.0–2.5 0.55–0.85 Balance

Schematic diagram
Figure 1. Schematic diagram of of the experimental process. (a) High
process. (a) High temperature
temperature compression
deformation process T =T950
processatat = ◦950 °C, ◦1050
C, 1050 C, and°C,
1150 ◦ C; (b) specimens under unidirectional compression
and 1150 °C; (b) specimens under unidirectional
in Gleeble; (c)instress
compression and(c)
Gleeble; deformation of a cylinderof
stress and deformation during high during
a cylinder temperature forging; (d) forging
high temperature forging;and(d)
pressingand
forging process of casting
pressing rod
process of with height-diameter
casting ratios (H/D)ratios
rod with height-diameter values(H/D)
of 1.5,values
1.7, and 2.0; 1.7,
of 1.5, (e) heat
and
treatment
2.0; (e) heatprocess of casting
treatment processand forging.and forging.
of casting

The specimens were prepared at half the distance from the center of the instrument before and after
3. Results
heat treatment. The samples were then processed into unnotched impact specimens with dimensions
× 10 × 55 mm.
of 10Stress–strain Hardness
curves and theandgrain
impactsizetests were
of the performed steels
compressed using ata Rockwell tester (HR-150A,
various temperatures are
Dongshan,
shown China)
in Figure andshape
2. The semi-automatic tester was
of the flow curve (JB-300B,
mainlyDongshan,
unimodal. China). Thetemperatures,
At different specimens used witha
mixture
an of saturated
increase in strain,picric acid,stress
the true purified
firstwater, detergent,
increased and hydrochloric
to a maximum value and acidthen
to corrode the grains.
decreased to the
The diameter of the grain in different fields was measured using the cut line method
steady-state region. When the temperature increased from 950 to 1150 °C, the maximum flow stress in the experiment,
and then, the
decreased fromaverage
219.93value was counted
to 117.23 MPa. Thisas the
maygrain size. Theofsamples
be because were corroded
the increase using 4%
in temperature andnitric
the
acid alcohol
activation solution
energy and picric
of thermal acid solution.
deformation. XRD (MiniFlex
Furthermore, the 600, Rigaku,
kinetic energy Japan) was performed
of atoms increased, onanda
diffractometer
the critical shear(Copper Kα line
stress slip radiation)
decreased. /minbehavior
at 10◦The for the counting
of strain time 30◦ to
from was
softening 100◦ . Furthermore,
considered to be due
for TEM, the specimens were prepared via electrolytic double spraying of 5% perchloric acid and 95%
alcohol solution. The microstructure of the steel was observed using an optical microscope (Nikon
ECLIPSE MA200, Japan), scanning electron microscope (ZEISS EVO18, Baden-Wurttemberg, Germany),
and transmission electron microscope (FEI G220, Hillsboro, Oregon State, U.S.).

3. Results
Stress–strain curves and the grain size of the compressed steels at various temperatures are
shown in Figure 2. The shape of the flow curve was mainly unimodal. At different temperatures,
with an increase in strain, the true stress first increased to a maximum value and then decreased to
the steady-state region. When the temperature increased from 950 to 1150 ◦ C, the maximum flow
Materials 2020, 13, 172 4 of 11

stress decreased from 219.93 to 117.23 MPa. This may be because of the increase in temperature4 and
Materials 2019, 13, x FOR PEER REVIEW of 11
the activation energy of thermal deformation. Furthermore, the kinetic energy of atoms increased,
and thedynamic
to new critical shear stress slip line
recrystallization decreased.
(DRX), and theThe behaviorbehavior
asymptotic of strainwassoftening was considered
characteristic of dynamicto
be due to new dynamic recrystallization (DRX), and the asymptotic behavior
recovery (DRV) [21,22]. The shape of the grains was a polygon or a block. With an increase in was characteristic of
dynamic
compression recovery (DRV) [21,22].
temperature, Thesize
the grain shape of the grains
increased was a polygon
significantly. or a block.
The maximum With
value an size
grain increase
was
in compression
obtained under atemperature,
compressionthe grain sizeof
temperature increased
1150 °C. significantly. The maximum
When the compression value grain
temperature size
was more
was ◦
thanobtained
1050 °C,under a compressionappeared
the microstructure temperature of 1150
to be clearlyC.the
When the compression
feature of an equiaxedtemperature was
crystal. DRX
more than 1050 ◦ C, the microstructure appeared to be clearly the featureMoreover,
of an equiaxed crystal. grain
DRX
incompletely produced granular crystal grains at a low temperature. the average
incompletely produced granular crystal grains at a low temperature. Moreover,
size gradually increased from 6.2 to 17.8 μm with an increase in the compression temperature. The the average grain
size gradually
variation rule ofincreased
the actualfrom 6.2 size
grain to 17.8
wasµm with anvia
obtained increase in thefitting.
numerical compression temperature.
The relationship The
between
variation
grain sizeruleand of the actual grain
compression size wasisobtained
temperature as follows:via numerical fitting. The relationship between
grain size and compression temperature is as follows:

GG==2.95 e −−4
2.95e
4 2
TT2 −− 0.561
0.561TT++273.2125
273.2125 (1)
(1)

◦ C).
where G
where G is
is the
the grain
grain size
size (µm) and TT is
(μm) and is the
the compression
compressiontemperature
temperature((°C).

2. Stress–strain
Figure 2. Stress–strain curves
curves (a) and grain size data (b) of
of compressed
compressed 0.4C-Si-Mn-Cr
0.4C-Si-Mn-Cr steel under
from 950
temperatures from 950 to 1150 ◦°C
to 1150 C..

The ◦ C. Therefore,
The grain
grainsizes
sizeswere
werefinefine
for the
for compression
the compression temperatures in the range
temperatures in theof range
950–1050of 950–1050 °C.
to obtain fine original austenite grains before heat treatment, the forging temperature
Therefore, to obtain fine original austenite grains before heat treatment, the forging temperature was was selected to
be ◦
1050 to C,bewhich ◦
selected 1050is°C,in which
the rangeis inofthe
950–1050
range of C. The sizes
950–1050 °C.ofThegrains
sizeswith different
of grains withH/D valuesH/D
different are
provided in Figure 3. The results showed that the shape of the samples was elliptical
values are provided in Figure 3. The results showed that the shape of the samples was elliptical and and band-like,
and the grain
band-like, andsize
thedecreased
grain sizewith an increase
decreased withinanthe H/D value.
increase in theFor castvalue.
H/D steel, the
Forgrain size was
cast steel, the about
grain
26.4 and the
µm, about
size was grains
26.4 μm, were
and theshaped
grains aswere
irregular
shapedblocks. Furthermore,
as irregular blocks.the distributionthe
Furthermore, was relatively
distribution
dispersed, anddispersed,
was relatively the grain roundness
and the grain wasroundness
not good enough.
was not When the H/D When
good enough. value was fromvalue
the H/D 1.5 towas
2.0,
the grains were mainly elliptical. After forging, the grain size decreased to 3.6 µm,
from 1.5 to 2.0, the grains were mainly elliptical. After forging, the grain size decreased to 3.6 μm,and the distribution
of
andgrains was relatively
the distribution uniform
of grains wasand dense. uniform
relatively With forging, the variations
and dense. in grain
With forging, the size with different
variations in grain
H/D values were obtained via numerical fitting:
size with different H/D values were obtained via numerical fitting:

Gi = −0.755x3i3 + 7.545x2i2 − 29.78xi + 51.02(i ∈ R, i , 0) (2)

G i = − 0 .7 5 5 x i + 7 .5 4 5 x i − 2 9 .7 8 x i + 5 1 .0 2 ( i ∈ R , i ≠ 0 ) (2)
where Gi is the grain size (µm) and xi is the height-diameter ratio (H/D).
where Gi is the grain size (μm) and xi is the height-diameter ratio (H/D).
Materials 2020, 13, 172 5 of 11
Materials 2019, 13, x FOR PEER REVIEW 5 of 11

Grainsize
Figure 3. Grain sizeofof0.4C-Si-Mn-Cr
0.4C-Si-Mn-Crsteelsteel with
with different
different H/D
H/D values
values forfor
thethe deformation
deformation process.
process. (a)
(a) As-cast,
As-cast, (b) (b)
H/DH/D = 1.5,
= 1.5, (c) H/D
(c) H/D = 1.7,
= 1.7, andand (d) H/D
(d) H/D = 2.0.
= 2.0.

The
The optical
optical microstructure
microstructure (OM) (OM) of of 0.4C-Si-Mn-Cr
0.4C-Si-Mn-Cr steelsteel before
before and
and after
after heat
heat treatment
treatment withwith
different H/D values is shown in Figure 4. The microstructure was primarily
different H/D values is shown in Figure 4. The microstructure was primarily composed of pearlite composed of pearlite
and
and ferrite
ferrite before
before the heat treatment,
the heat treatment, andand the
the pearlite
pearlite and
and ferrite
ferrite were
were distributed
distributed among
among each each grain.
grain.
As shown in Figure 4a–d, the size of the pearlite in the forged samples was finer
As shown in Figure 4a–d, the size of the pearlite in the forged samples was finer than that of thethan that of the pearlite
in the as-cast
pearlite in thesteel.
as-castThe pearlite
steel. in the forged
The pearlite in thesteel wassteel
forged mainly
wasdistributed on the shear
mainly distributed on the bands,
shearand the
bands,
pearlite
and thewas deformed
pearlite in the growth
was deformed direction.
in the growthCompared
direction.with forged steels,
Compared the as-cast
with forged specimen
steels, had
the as-cast
aspecimen
distinct grain orientation, which could be because a temperature gradient field
had a distinct grain orientation, which could be because a temperature gradient field was was formed in the
crystal
formedbodyin thedue to the
crystal quantitative
body due to theloss of heat in the
quantitative lossuncompressed state. This led state.
of heat in the uncompressed to theThisformation
led to
of
thefibrous
formationtissue
of parallel to the parallel
fibrous tissue directiontooftheheat dissipation.
direction of heat The microstructures
dissipation. of samples after
The microstructures of
heat treatment for different H/D values are shown in Figure 4e–h. The microstructure
samples after heat treatment for different H/D values are shown in Figure 4e–h. The microstructure was mainly
composed
was mainlyofcomposed
acicular bainite, martensite,
of acicular bainite,and retained austenite.
martensite, and retained Compared with
austenite. Figure 4e,with
Compared the bainite
Figure
and martensite of specimens were finer and had a dispersed distribution, as
4e, the bainite and martensite of specimens were finer and had a dispersed distribution, as shown shown in Figure 4f–h.
in
According to the color metallographic techniques [19], with an increase in
Figure 4f–h. According to the color metallographic techniques [19], with an increase in H/D, theH/D, the bainite content
increased gradually
bainite content whilegradually
increased the martensite
whilecontent decreased.
the martensite content decreased.

4. Optical microstructure (OM) of 0.4C-Si-Mn-Cr steel before and after heat treatment
Figure 4. treatment with
with
different H/D values
values for
for the
the deformation
deformation process.
process. (a–d) Before heat treatment and (e–h) after heat
treatment. P: pearlite, F: ferrite, B: bainite, M: martensite, and RA:
treatment. RA: retained austenite.
retained austenite.

Figure
Figure 55 shows
showsSEM
SEMimages
imagesofofsteel
steelbefore
beforeand
andafter
afterheat
heattreatment.
treatment. Figure
Figure5a5a
is is
anan
SEMSEMimage of
image
the sample
of the withwith
sample an H/D
an value
H/D of 2.0 before
value of 2.0 heat treatment.
before Different pearlite
heat treatment. Differentclusters were
pearlite distributed
clusters were
and grew along
distributed and the grain
grew boundary.
along the grainThe sizes of ferrite
boundary. and of
The sizes cementite in all
ferrite and the grains
cementite inwere different
all the grains
and
wereregularly
differentarranged in a specific
and regularly direction.
arranged The SEM
in a specific microstructure
direction. The SEMofmicrostructure
steel after heatof
treatment is
steel after
heat treatment is shown in Figure 5b, and the microstructure was similar to that shown in Figure 4e–
h. Figure 6 shows the XRD spectra for the steel samples before and after heat treatment, and the peaks
Materials 2020, 13, 172 6 of 11

shown
Materials in Figure
2019, 5b, and
13, xx FOR
FOR PEERthe microstructure was similar to that shown in Figure 4e–h. Figure 6 shows
REVIEW
Materials 2019, 13, PEER REVIEW 66 of
of 11
11
the XRD spectra for the steel samples before and after heat treatment, and the peaks observed before
and after heat
observed
observed before
beforetreatment
and after
and corresponded
after heat treatment
heat to the
treatment body-centered
corresponded
corresponded to cubic
to structure. These
the body-centered
the body-centered results
cubic
cubic showed
structure.
structure. that
These
These
the sample
results showedhad the
that face
the centered
sample cubic
had the structure
face after
centered heat
cubictreatment.
structure With
after
results showed that the sample had the face centered cubic structure after heat treatment. With thethe combined
heat treatment. analysis
With of
the
Figures 4 and
combined analysis
combined 5, it
analysis of could be
of Figuresconfirmed
Figures 44 and
and 5, that
5, it
it couldbefore
could be treatment,
be confirmed
confirmed that the body
that before centered cubic
before treatment,
treatment, the structure
the body of
body centered
centeredthe
steel
cubic structure of the steel was ferrite, while after treatment, there was a mixed structure ofThe
cubic was ferrite,
structure ofwhile
the after
steel treatment,
was ferrite,there
while was a
aftermixed structure
treatment, thereof bainite
was a and
mixed martensite.
structure of face
bainite
bainite
centered
and cubic
martensite. structure
The face was the
centered retained
cubic austenite
structure wasphase
the after
retainedquenching,
austenite
and martensite. The face centered cubic structure was the retained austenite phase after quenching, and
phase these results
after were
quenching,
consistent
and these
and with the
these results
results experimental
were
were consistentresults.
consistent with the
with the experimental
experimental results.
results.

Figure 5.
Figure 5. SEM
SEM micrographs
SEMmicrographs ofofthe
micrographsof the microstructure
themicrostructure ininthe
microstructurein the tested
thetested steel.
steel.
tested (a)(a)
(a)
steel. Before
Before heat
heat
Before treatment
treatment
heat andand
and
treatment
(b) after
(b) after heat
heat treatment.
treatment.

Figure 6.
Figure XRD spectra
6. XRD
XRD spectra of
of the
the tested
tested steel
steel treated
treated under different conditions.
under different conditions.
conditions.

Figure
Figure 777shows
Figure showsTEM
shows TEMimages
TEM imagesand
images and
andthetheselected
the selected
selected area electron
area
area diffraction
electron
electron (SAED)
diffraction
diffraction pattern
(SAED)
(SAED) of steel
pattern
pattern of with
of steel
steel
an H/D
with an
with value
an H/D of
H/D value 2.0.
value of As shown
of 2.0.
2.0. As in
As shownFigure
shown in 7a,
in Figureafter
Figure 7a, forging,
7a, after the steel
after forging,
forging, thehad a large
the steel
steel had number
had aa large of dislocation
large number
number of of
lines and
dislocation dislocation
lines and tangles
dislocation between
tangles the ferrite
between and
the cementite.
ferrite and Furthermore,
cementite.
dislocation lines and dislocation tangles between the ferrite and cementite. Furthermore, cementite cementite
Furthermore, (<100 nm)
cementite
is observed
(<100
(<100 nm) is
nm) isin Figure 7b.
observed
observed in The deformation
in Figure
Figure 7b. The
7b. ability of ability
The deformation
deformation pearlite
ability of ofwith ferrite
pearlite
pearlite with
withand cementite
ferrite
ferrite was variable
and cementite
and cementite was
was
because
variable of different
because of stresses
different during
stresses high
during temperature
high forging.
temperature A dislocation
forging.
variable because of different stresses during high temperature forging. A dislocation in the ferrite A in the
dislocation ferrite
in theformed
ferrite
because
formed of the plastic
formed because
because of thedeformation
of the plastic deformation
plastic of the pearlite
deformation theduring
of the
of pearlite
pearlite forging.
duringWhen
during there
forging.
forging. When
Whenwas a largewas
there
there amount
was of
aa large
large
deformation,
amount of
amount the layer
of deformation,
deformation, the size and
the layergrain
layer size size
size and of
and grain pearlite
grain size
size ofwere fine.
of pearlite The
pearlite were deformation
were fine.
fine. The resistance
The deformation decreased
deformation resistance
resistance
via adjustments
decreased via in the
adjustments orientation
in the of lamella
orientation during
of lamellacontinuous
during impact
continuous
decreased via adjustments in the orientation of lamella during continuous impact compression. The compression.
impact The
compression.cementite
The
in the pearlite
cementite in grain
the group
pearlite gradually
grain group fractured,
gradually and the
fractured, ferrite
and formed
the
cementite in the pearlite grain group gradually fractured, and the ferrite formed a high density of a high
ferrite density
formed a of
high dislocations
density of
and a substructure
dislocations and
dislocations that could
and aa substructure reduce
substructure that the
that could strain
could reduce energy
reduce the [23].
the strainTEM images
strain energy
energy [23].of the
[23]. TEMmorphology
TEM imagesimages of of the
of the
the
steel after
morphology heatof treatment
the steel with
after an
heat H/D value
treatment of
with 2.0
an are
H/D shown
value in
of Figure
2.0
morphology of the steel after heat treatment with an H/D value of 2.0 are shown in Figure 7c–d. After are 7c–d.
shown After
in heat
Figure treatment,
7c–d. After
the
heatsteel
heat obtained
treatment,
treatment, the
the thesteel
multiphase
steel obtainedmicrostructure
obtained the multiphase
the multiphase that included dislocation-type
microstructure
microstructure that included
that included lath martensite, bainite,
dislocation-type
dislocation-type lath
lath
and retained austenite
martensite, bainite,
martensite, bainite, and and a
and retained number
retained austenite of dislocations
austenite and gathered
and aa number
number of around the
of dislocations martensite.
dislocations gathered According
gathered aroundaround the to
the
the inserted According
martensite.
martensite. SAEDP in Figure
According to the7d,
to the the orientation
inserted
inserted SAEDP in
SAEDP relationships
in Figure. 7d,
Figure. 7d,ofthe
the orientation
the multiphase relationships
orientation microstructure
relationships of ofwere
the
the
(110)α // (111)γ. In addition, the retained __ austenite
__ __ was mainly found to be film-like and blocks.
multiphase microstructure
multiphase microstructure were were (1(110)α
10)α // // (1
(11111)γ.
)γ. In
In addition,
addition, the the retained
retained austenite
austenite was was mainly
mainly found
found
to be film-like and blocks.
to be film-like and blocks.
Materials 2020, 13, 172 7 of 11
Materials
Materials 2019,
2019, 13,
13, xx FOR
FOR PEER
PEER REVIEW
REVIEW 77 of
of 11
11

Figure
Figure 7.7.
Figure TEM
7.TEM images
TEMimages
images of
of the
of the morphology
morphology
the and
and SAED
and SAED
morphology of steelof
SAED steel
with
of an with
steel H/D an
an H/D
withvalue value
of 2.0
H/D in theof
value 2.0
2.0 in
in the
deformation
of the
deformation
process. (a,b)process.
Before (a–b)
heat Before
treatmentheat
and treatment
(c,d) afterand
heat(c–d) after
treatment. heat treatment.
deformation process. (a–b) Before heat treatment and (c–d) after heat treatment.

The mechanical
The mechanicalproperties
mechanical propertiesof
properties ofsteel
of steelwith
steel withdifferent
with differentH/D
different H/D
H/D values
values
valuesareareshown
are shown
shown in in
Figure
in Figure
Figure8. 8.
As shown
8. As
As shown
shown in
Figure
in
in Figure
Figure8a,8a,
thethe
8a, hardness
the values
hardness
hardness (40–45
values
values (40–45HRC)
(40–45 of the
HRC)
HRC) of steel
of the
the steelsamples
steel afterafter
samples
samples heat heat
after treatment
heat werewere
treatment
treatment largerlarger
were than
larger
the
thanhardness
the values
hardness (21–29
values HRC)
(21–29 of
HRC) the
ofsteel
the samples
steel samples before heat
before treatment.
heat treatment.
than the hardness values (21–29 HRC) of the steel samples before heat treatment. As shown in Figure As shown
As shownin Figure
in 8b,
Figure
the impact toughness after heat treatment was greater than 12 J/cm 2 , which was higher than that of
8b,
8b, the
the impact
impact toughness
toughness after
after heat
heat treatment
treatment was
was greater
greater thanthan 1212 J/cm
J/cm ,, which
22 which was was higher
higher than
than that
that
the steel samples before heat treatment (3–9 J/cm 2
of
of the
the steel
steel samples
samples before
before heat
heat treatment
treatment (3–9
(3–9 J/cm).2).).The
J/cm 2
Thehardness
The hardnessand
hardness andthe
and theimpact
the impact toughness
impact toughness were
toughness were
significantly enhanced after heat treatment. Before
Before heat
heat treatment,
treatment, with
with an
an increase
increase
significantly enhanced after heat treatment. Before heat treatment, with an increase in the H/D value, in
in the
the H/D
H/D value,
value,
hardness
hardnessfirst
hardness firstincreased
first increasedand
increased andthen
and then
then decreased.
decreased.
decreased. However,
However,
However, thethe
impact
the impacttoughness
impact toughness
toughness of the
of samples
of the
the samplesbefore
samples and
before
before
after
and heat heat
and after
after treatment
heat increased
treatment
treatment linearly.
increased
increased linearly.
linearly.

Figure 8.
8. Mechanical
Figure 8.
Figure Mechanical properties
properties of
of the
the 0.4C-Si-Mn-Cr
0.4C-Si-Mn-Cr steel
0.4C-Si-Mn-Cr steel showing
showing the
the development
development of
development of (a)
of (a) hardness
(a) hardness
hardness
and
and (b)
(b) impact
impact toughness
toughness before
before and
and after
afterheat treatment.
heattreatment.
treatment.

4.
4. Discussion
4. Discussion
Discussion
Figure
Figure 999 presents
Figure presents aaa series
presents series of
series of schematic
of schematic diagrams
schematic diagrams
diagrams ofof
of the
the microstructure
the microstructure evolution
microstructure evolution of
of steel
evolution of steel during
steel during
during
the
the process
process of
of compression-forging-heat
compression-forging-heat treatment.
treatment. When
When the
the temperature
temperature waswas greater
greater
the process of compression-forging-heat treatment. When the temperature was greater than point than than point
point A11,,
A
A , pearlite
pearlite
pearlite and
1 and ferrite
and ferrite dissolved
ferrite dissolved
dissolved and and
and formedformed austenite
formed austenite
austenite grains. grains.
grains. When When
When the the specimens
the specimens
specimens began began
began to
to yield,to yield,
yield, plastic
plastic
plastic
strain strain
strain and
and and recrystallization
recrystallization
recrystallization driving
drivingdriving
force force increased
force increased
increased with
with anwith
an an increase
increase
increase in in compression
in compression
compression temperature.
temperature.
temperature. The
The
The
grain grain boundary
boundary migration
migration rate rate accelerated,
accelerated, and and
this this promoted
promoted rapid
rapid
grain boundary migration rate accelerated, and this promoted rapid grain growth. grain
grain growth.
growth.
Materials 2020, 13, 172 8 of 11
Materials 2019, 13, x FOR PEER REVIEW 8 of 11

Figure9.9. Microstructure
Figure Microstructure evolution
evolution mechanism
mechanism ofof medium
medium carbon
carbon 0.4C-Si-Mn-Cr
0.4C-Si-Mn-Crsteel
steelduring
duringthe
the
process
processofofcompression-forging-heat
compression-forging-heattreatment.
treatment.

According
Accordingto
tothe
thekinetics
kineticsof
of grain
grain growth
growth [24]:
[24]:

Gm m
t − Gt0 = k(t − t0 ) (3)
Gtm −Gtm0 = k ( t −t0 ) (3)
where Gt0 and Gt are the grain diameter (µm) at the times t0 and t, respectively. m is the average
mobility
where Gt of0 the
andgrain
Gt areboundary,
the grainand m depends
diameter (μm)onatthe timesoft0Gand
theindex t /Gt0 .t,krespectively.
= k0 exp(−Q/RT), m iswhere Q is the
the average
activation
mobility of energy of the
the grain grain boundary
boundary, and T is the
and m depends heating
on the indextemperature.
of Gt/Gt0. k = k0exp(−Q/RT), where Q is
Accordingenergy
the activation to Equation
of the (3), when
grain time isand
boundary T is themheating
constant, is proportional
temperature. to exp(−Q/RT); thus, the rate
of grain growth is related to m. When the temperature is higher,
According to Equation (3), when time is constant, m is proportional to exp(−Q/RT); the grain boundary migration and
thus, the rate
the growth
of grain rate were
growth fastertodue
is related to the increased
m. When the temperature atomicisdiffusion
higher, the rate; also,boundary
grain the grainmigration
size increased
and
exponentially
the growth rate withwere anfaster
increase
due in temperature.
to the increased atomic Temperature
diffusion affects the plastic
rate; also, the grain deformation
size increased of a
material,
exponentially with an increase in temperature. Temperature affects the plastic deformation of aof
which as a consequence, directly influences the microstructure evolution. The growth rate
grains
material,at awhich
low temperature
as a consequence,was lower thaninfluences
directly that at a high temperature, which
the microstructure was because
evolution. The growth recovery
rate
and recrystallization
of grains were more
at a low temperature pronounced
was lower thanat a high
that temperature.
at a high temperature, which was because recovery
and Therecrystallization
diameter of the were more pronounced
cross-section at a high
of the round bartemperature.
decreased during forging. Under the action
The diameter
of external force, the of round
the cross-section of the round
bar was deformed and bar decreased
expanded outwardduringinforging.
the radial Under the action
direction. The
of external
two end faces force,
were theelongated
round baralongwas deformed
the vertical andaxis
expanded
(Figureoutward
1c). Thein the radial direction.
dislocation density ofThe two
pearlite
end faces
during thewere
forgingelongated along the
deformation vertical
process axis (Figure
increased, and 1c).
itsThe dislocation
value changeddensityfrom 2.02 of pearlite m−2 to
× 1014during
the ×
6.07 14
forging −2
10 mdeformation
; this provided process increased,
nucleation sitesandfor its value changed
cementite and promoted from 2.02 × 10 of
diffusion 14 m iron
−2 to 6.07 × 1014
and carbon
m ; this
−2
atoms. Anprovided
increase in nucleation sites for
the H/D value cementitethe
accelerated and promoted
migration of diffusion
atoms along of iron and carbonline,
the dislocation atoms.and
An increase in the H/D value accelerated the migration of atoms along
this led to a decrease in the deformation resistance. When the strain was higher than the critical strain, the dislocation line, and this
ledlattice
the to a decrease
was distortedin the because
deformation resistance.
the number When theand
of slippages strain was higher
twinning than via
increased the atoms
criticalthrough
strain,
the lattice was distorted because the number of slippages and twinning
dislocation. The initial grains began to break, and the slip resistance increased in this case. Dislocation increased via atoms through
dislocation.
density The initial grains
and deformation energybegan
were to formed
break, and the ferrite,
in the slip resistance
and thisincreased in this for
was beneficial case. Dislocation
obtaining fine
density
grains and deformation
during DRX [25,26].energy were formed
Furthermore, in the ferrite,
the temperature ofand
the this
corewas slowlybeneficial
decreased for obtaining
because offine the
grains during DRX [25,26]. Furthermore, the temperature of the core
large volume of steel, providing sufficient time for grain recovery in the forging process. However, slowly decreased because of the
largea volume
with continuous of steel, providing
decrease sufficient during
in temperature time forthe grain recovery
forging process,in the forging
it was process.
difficult However,
to recrystallize
with a continuous
deformed austenitedecrease in temperature
because delayed nucleationduring the forging
inhibited DRX process, it was difficult
[27]. In addition, the highto recrystallize
content of Si
deformed austenite because delayed nucleation inhibited DRX [27].
increased the hot deformation energy and reduced the rate of DRX, which made the steel deformation In addition, the high content of
Si increased the hot deformation energy and reduced the rate
difficult, and the grain growth gradually stopped [28–30]. The microstructure of the undeformed of DRX, which made the steel
billet
deformation difficult, and the grain growth gradually stopped [28–30].
was relatively stable under same heating conditions and still retained a large grain size. When the billet The microstructure of the
undeformed billet was relatively stable under same heating conditions and still retained a large grain
was air cooled to room temperature after forging, transformation of the ferrite and pearlite occurred
size. When the billet was air cooled to room temperature after forging, transformation of the ferrite
during the cooling process [31]. Because of nucleation and grain growth during the transformation
and pearlite occurred during the cooling process [31]. Because of nucleation and grain growth during
process, it was difficult to obtain quantitative information for DRX during deformation.
the transformation process, it was difficult to obtain quantitative information for DRX during
The hardness and impact toughness of the steel sample obviously increased under the same
deformation.
quenching conditions. The grain size decreased after forging, and microstructure refinement improved
The hardness and impact toughness of the steel sample obviously increased under the same
the hardness and toughness of the metal [32]. After heat treatment, the pearlite of the forged state
quenching conditions. The grain size decreased after forging, and microstructure refinement
transformed into bainite, martensite, and retained austenite. The increase in the martensite content was
improved the hardness and toughness of the metal [32]. After heat treatment, the pearlite of the
beneficial for enhancing the hardness, and bainite and film-like retained austenite clearly improved
forged state transformed into bainite, martensite, and retained austenite. The increase in the
the impact toughness [33]. The transformation induced plasticity (TRIP) effects resulted from the
martensite content was beneficial for enhancing the hardness, and bainite and film-like retained
deformation during forging, and this contributed to the enhanced toughness because the austenite
austenite clearly improved the impact toughness [33]. The transformation induced plasticity (TRIP)
was rich in manganese and carbon [34]. Smaller prior austenite grains formed a finer martensite
effects resulted from the deformation during forging, and this contributed to the enhanced toughness
because the austenite was rich in manganese and carbon [34]. Smaller prior austenite grains formed
Materials 2020, 13, 172 9 of 11

lath after heat treatment, whereas the longer martensite in the specimens also meant that there were
larger grains before austenite transformed to bainite and martensite [35,36]. With an increase in
deformation, the hardness of the forged billet slightly decreased before and after heat treatment.
The work hardening effect was inherited by the subsequent microstructural transformation process
due to thermal deformation. The material appeared to undergo dynamic recovery and flow softening
because of the influence of the annihilation of dislocation when the strain was further increased
to some extent [37,38]. With increased deformation at different values of H/D, the specimens were
completely recrystallized, and this reduced the deformation energy storage and led to decreased
hardness. However, the hardness of steel was improved compared to that of the as-cast steel because
of deformation.

5. Conclusions
(1) With an increase in deformation temperature in the range of 950–1150 ◦ C, the grain size of samples
increased from 6.2 µm to 17.8 µm. The relationship between the grain size and temperature
conformed to the fitting formula (Equation (1)). The steel had an abundance of blocky grains
during the deformation process. Moreover, the grain size decreased from 26.4 µm to 3.6 µm
with an increase in the H/D value. The relationship between the grain size and H/D was close to
Equation (2).
(2) The microstructure was pearlite, ferrite, bainite, martensite, and retained austenite with different
H/D values. The microstructure was clearly more uniform and finer than that of the as-cast steel.
The optimum deformation process was a heating temperature that was less than 1050 ◦ C, and
the H/D value was 2.0. Changes in grain size depended on the grain nucleation and dislocation
movement during forging.
(3) Compared with steel that was not subjected to heat treatment, the hardness and impact toughness
of the steel samples after heat treatment showed obvious improvements. When the H/D value was
2.0, the maximum impact toughness was 87 J/cm2 . Heat treatment had a significant contribution
to improving the mechanical properties of the forged samples. Hardness decreased slightly with
an increase in the H/D value. Furthermore, the impact toughness gradually increased, and this
was related to the microstructure, dynamic recovery, and softening of the grains.

Author Contributions: The study was designed by Q.S., Z.L. and R.Z. The data was collected by F.Z., Y.Y. and
J.B., and the literature was searched by Y.Y. and J.B. The figures and data analysis wereperformedby F.Z. and Z.L.
The data interpretation was carried out by Q.S. The manuscript was written by F.Z. and Q.S. All authors have read
and agreed to the published version of the manuscript.
Funding: This research was funded by [National key R&D Program of China] grant number [2017YFB0305100,
2017YFB0305101] and [National Natural Science Foundation of China] grant number [51561018, 51871116].
Conflicts of Interest: The authors declare no conflict of interest.

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