metals

Article
Effect of Heterogeneous Microstructure on Refining
Austenite Grain Size in Low Alloy Heavy-Gage Plate
Shengfu Yuan 1 , Zhenjia Xie 2 , Jingliang Wang 2 , Longhao Zhu 3 , Ling Yan 3 ,
Chengjia Shang 2,3, * and R. D. K. Misra 4
1 School of Materials Science and Engineering, University of Science and Technology Beijing,
Beijing 100083, China; yuansf_77@163.com
2 Colarborative Innovation Center of Steel Technology, University of Science and Technology Beijing,
Beijing 100083, China; zjxie@ustb.edu.cn (Z.X.); jlwang@ustb.edu.cn (J.W.)
3 State Key Laboratory of Steel for Marina Equipment and Application, Anshan Steel, Anshan 114021, China;
zlhdut@163.com (L.Z.); yanling_1101@126.com (L.Y.)
4 Laboratory for Excellence in Advanced Steel Research, Department of Metallurgical and Materials
Engineering, University of Texas at El Paso, El Paso, TX 79912, USA; dmisra2@utep.edu
* Correspondence: cjshang@ustb.edu.cn; Fax: +8610-6233-2428




Received: 18 November 2019; Accepted: 13 January 2020; Published: 16 January 2020


Abstract: The present work introduces the role of heterogeneous microstructure in enhancing the
nucleation density of reversed austenite. It was found that the novel pre-annealing produced a
heterogeneous microstructure consisting of alloying elements-enriched martensite and alloying-depleted
intercritical ferrite. The shape of the martensite at the prior austenite grain boundary was equiaxed and
acicular at inter-laths. The equiaxed reversed austenite had a K-S orientation with adjacent prior austenite
grain, and effectively refined the prior austenite grain that it grew into. The alloying elements-enriched
martensite provided additional nucleation sites to form equiaxed reversed austenite at both prior
austenite grain boundaries and intragranular inter-lath boundaries during re-austenitization. It was
revealed that prior austenite grain size was refined to ~12 µm by pre-annealing and quenching, while it
was ~30 µm by conventional quenching. This is a practical way of refining transformation products by
refining prior austenite grain size to improve the strength, ductility and low temperature toughness
of heavy-gage plate steel.

Keywords: alloying element enrichment; heterogeneous microstructure; nucleation site; grain

refinement

1. Introduction
Low carbon low alloy steels have been widely used in fields of marine engineering, engineering
machines, and other structural applications due to their high strength, excellent toughness, good
weldability and low cost [1–3]. With the structural components becoming large and the need for cost
effectiveness, there is a significant demand for heavy gauge plate steel. However, for low carbon
low alloy heavy-gage plate steel manufactured by thermomechanical controlling process (TMCP),
austenite grains in the center of the plate gradually become larger due to insufficient reduction in
thickness during controlled rolling. This leads to the deterioration of mechanical properties, especially
low-temperature toughness [4–6]. Therefore, a heat treatment process should be applied to optimize
the mechanical properties of heavy plate.
Austenite grain refinement is well recognized as being of great importance in enhancing mechanical
properties of high strength low alloy steels [7–9]. Several efforts have been made towards the refining
of austenite grain size. Grange [10] reported that the thermal cycling process between martensite
and austenite is helpful in refining austenite grain size by reversed transformation. The effect of the

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effect of the two-step quenching (TSQ) and one-step quenching (OSQ) heat treatment process on
austenite grain size was studied [11], and the results showed that the prior austenite grain size of
TSQ heat-treated
two-step quenching specimen
(TSQ) and wasone-step
50% finer than OSQ
quenching heat heat
(OSQ) treatment.
treatment Further studies
process [12–14] found
on austenite grain
two
size morphologies
was studied [11], of reversed austenite
and the results from martensite
showed that the prior or bainite:
austenite equiaxed
grain size austenite
of TSQ and acicular
heat-treated
austenite
specimen during
was 50%thermalfiner than cycling
OSQ heatprocess and multi-step
treatment. heat treatment
Further studies [12–14] found process.two In addition, the
morphologies of
mechanism of prior
reversed austenite fromaustenite
martensite grain refinement
or bainite: was attributed
equiaxed austenite and to acicular
the enhancement
austenite during of nucleation
thermal
density of equiaxed
cycling process and austenite
multi-stepby thermally
heat treatment activated
process. nucleation
In addition, or static recrystallization
the mechanism of prior [15].
austenite
grainThere is a vast
refinement was literature
attributed [13,14,16–21] reportingof
to the enhancement that reverseddensity
nucleation austenite nucleates austenite
of equiaxed at the prior by
austenite
thermally grain boundary,
activated nucleation intersection of multiple-grains,
or static recrystallization [15].packet boundary, block boundary and
cementite.
There Miyamoto [22] pointed
is a vast literature out thatreporting
[13,14,16–21] austenitethat preferentially
reversed austenite nucleates at the at
nucleates high
the angle
prior
boundary of pearlite-ferrite.
austenite grain Studies [23,24]
boundary, intersection on the crystallographic
of multiple-grains, characteristics
packet boundary, blockdetermined
boundary that and
acicular
cementite.austenite
Miyamoto [22] had pointed
Kurdjumov–Sachs
out that austenite (K-S) orientation
preferentially relationship
nucleates at the high((111) //(011)bcc,
anglefccboundary
[−101] fcc//[−1–11]bcc) Studies
of pearlite-ferrite. with the[23,24]
matrix, on while equiaxed austenite
the crystallographic nucleated determined
characteristics at prior austenite grain
that acicular
boundaries
austenite had grew into the adjacent
Kurdjumov–Sachs prior
(K-S) austeniterelationship
orientation grain at high angle
((111) fcc //(011)
misorientation
bcc , [−101] [23].
fcc //[−1–11]
This also
bcc )
suggested that the
with the matrix, equiaxed
while equiaxedaustenite was nucleated
austenite beneficial inat refining austenite
prior austenite grain
grain size. In addition,
boundaries grew into some
the
literatures
adjacent prior [25–28] published
austenite grain that
at highcementite was the core [23].
angle misorientation of austenite
This alsonucleation.
suggested However, in this
that the equiaxed
study,
austenitethewascontent of carbon
beneficial is 0.08
in refining wt. %,grain
austenite whichsize.was too low to
In addition, some grow to the [25–28]
literatures core of published
austenite
nucleation.
that cementite In contrast,
was the core the cementite
of austenite was easily decomposed.
nucleation. However, in Inthis
thisstudy,
study,the a novel
content pre-annealing
of carbon is
process
0.08 wt. prior
%, which to quenching
was too low was introduced
to grow to increase
to the core nucleation
of austenite nucleation.density of equiaxed
In contrast, reversed
the cementite
austenite
was easilyand refine austenite
decomposed. In thisgrain
study,size in the
a novel core of heavy
pre-annealing plate.prior
process Microstructure
to quenching evolution during
was introduced
heat treatment
to increase was studied
nucleation densitytoof elucidate
equiaxed the mechanism
reversed austenite of and
austenite
refine grainaustenite refinement
grain size byinpre-
the
annealing
core of heavy and plate.
quenching. Microstructure evolution during heat treatment was studied to elucidate the
mechanism of austenite grain refinement by pre-annealing and quenching.
2. Experimental Material and Procedure
2. Experimental Material and Procedure
The chemical composition of experimental steel was C 0.08, Si 0.23, Mn 1.21, P 0.011, S 0.002, Ni
The+chemical
1.1, (Cu Cr + Mo)composition
< 2.0, Nb 0.022, of experimental
B 0.0012 andsteel was in
Ti 0.014 C 0.08,
weight Si 0.23,
percent Mn(wt.1.21,%). P 0.011,
The ASC10.002,and ANi C3

1.1, (Cu + Cr +
temperatures were < 2.0, Nb by
Mo)measured 0.022, B 0.0012 to
dilatometry andbeTi7150.014
andin863
weight percent (wt. Three
°C, respectively. %). The AC1 and
specimens
AC3 temperatures
(denoted as 1#, 2#,were measured
3#) with by dilatometry
dimensions of 10 mmto(rolling and 863 ◦ C,
be 715 direction) × 3respectively.
mm (transverse Threedirection)
specimens ×
(denoted as 1#, 2#, 3#) with dimensions of 10 mm (rolling direction)
10 mm (thickness) were cut from the center of the experimental plate steel which was hot rolled to× 3 mm (transverse direction) ×
10 mm
100 mm (thickness)
by TMCP, were cut from
because the center
of inferior of the experimental
mechanical properties plate steel which
of center plate.was Heat hottreatments
rolled to 100were mm
by TMCP,
carried outbecause
as shown of inferior
in Figure mechanical
1. Specimen properties
1# was of reheated
center plate.
to 900Heat °Ctreatments
for 30 min were
for carried
complete outre-
as
shown in Figure 1. Specimen 1# was reheated to 900 ◦ C for 30 min for complete re-austenitization, and
austenitization, and then quenched to room temperature (Figure 1a). To isolate the effect of
then quenched
intercritical to room temperature
annealing, specimen 2#(Figure 1a). To isolate
was isothermally thefor
held effect of intercritical
30 min at 740 °C annealing,
followed specimen
by water
2# was isothermally held for 30 min at 740 ◦ C followed by water quenching to room temperature
quenching to room temperature (Figure 1b), to distinguish the microstructure after intercritical
(Figure 1b),Intothe
annealing. distinguish the microstructure
case of specimen 3#, two-step after
heatintercritical
treatment annealing. In the caseannealing
process: intercritical of specimen 3#,
at 740
two-step
°C for 30 heat treatmentby
min followed process:
quenchingintercritical annealing
and reheating to at
900740°C◦ C
forfor
3030minmin followedbybyquenching,
followed quenching was and
reheatingastoshown
applied, 900 ◦ Cinfor 30 min
Figure 1b.followed by quenching, was applied, as shown in Figure 1b.

Figure 1. Heat treatment scheme of experimental specimens: (a) conventional quenching process; and
Figure 1. Heat treatment scheme of experimental specimens: (a) conventional quenching process; and
(b) intercritical annealing, and intercritical annealing + conventional quenching processes.
(b) intercritical annealing, and intercritical annealing + conventional quenching processes.
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The microstructure was characterized by optical microscope (OM) (OLYMPUS, Beijing, China),
field
field emission
emissionscanning
scanning electron microscope
electron (FEG-SEM;
microscope ULTRAULTRA
(FEG-SEM; 55) and 55)
electron
and backscatter diffraction
electron backscatter
(EBSD, Oxford
diffraction Instruments,
(EBSD, OxfordEngland, UK). For England,
Instruments, OM, the specimens
UK). For wereOM,metallographically
the specimens polished
were
and etched by Picric acid
metallographically (China
polished andelectron microscope
etched by Picricscientific instrument,
acid (China China)
electron consisting scientific
microscope of 10 mL
detergent
instrument, (Diao Pai made
China) in Nice
consisting of Group), 2 mL CCl4,
10 mL detergent 0.2 gPai
(Diao NaCl, 4.5 in
made g picric acid and 260mL
Nice Group), mLCCl4,
deionized
0.2 g
water ◦
NaCl,in 50–55
4.5 C water
g picric acid bath
and 60in order to observewater
mL deionized the equiaxed
in 50–55austenite
°C water grain
bathsize. The specimens
in order to observewere
the
etched by 4% nital for SEM observation. The local chemical composition in specimen
equiaxed austenite grain size. The specimens were etched by 4% nital for SEM observation. The local 2# was examined
by energycomposition
chemical dispersive x-ray spectrometer
in specimen (EDS)
2# was facility available
examined by energywith transmission
dispersive x-ray electron microscope.
spectrometer (EDS)
The austenite
facility availabletransformation
with transmission vs temperature during reheating
electron microscope. was simulated
The austenite transformationby dilatometer at a
vs temperature
heating rate of 0.1 ◦ C/s for the one-step and two-step processes. The specimens for EBSD analysis were
during reheating was simulated by dilatometer at a heating rate of 0.1 °C/s for the one-step and two-
ground and electrolytically
step processes. The specimens polished in ananalysis
for EBSD electrolyte
wereofground
10% perchloric acid, 5% glycerol
and electrolytically andin85%
polished an
ethanol at 15ofV 10%
electrolyte for 30perchloric
s. The EBSD measurements
acid, 5% glycerolwere andperformed at a voltage
85% ethanol at 15 V of 20
forkv30with a step
s. The size
EBSD
of 0.1 µm.
measurements were performed at a voltage of 20 kv with a step size of 0.1 μm.

3. Results and
3. Results and Discussion
Discussion

3.1. Refining Prior Austenite Grain

3.1. Refining Prior Austenite Grain
Figure 2 shows the effect of two-step heat treatment on the refinement of austenite grain size
Figure 2 shows the effect of two-step heat treatment on the refinement of austenite grain size in
in the core of heavy-gage plate processed by TMCP. The austenite grain size of hot rolled specimen
the core of heavy-gage plate processed by TMCP. The austenite grain size of hot rolled specimen was
was ~105 µm in the core, as presented in Figure 2a, because the cooling rate was lower in the core of
~105 μm in the core, as presented in Figure 2a, because the cooling rate was lower in the core of the
the hot rolled plate; the microstructure was composed of bainite with large martensite and austenite
hot rolled plate; the microstructure was composed of bainite with large martensite and austenite
constituents (M/A). After conventional one-step quenching of hot rolled plate (specimen 1#), the prior
constituents (M/A). After conventional one-step quenching of hot rolled plate (specimen 1#), the prior
austenite grain was inhomogeneous, the large austenite grain (γb : ~78 µm) was surrounded by small
austenite grain was inhomogeneous, the large austenite grain (γb: ~78 μm) was surrounded by small
austenite grain (γa : ~29 µm), as shown in Figure 2b. For the specimen 2# (intercritical annealed at
austenite grain (γa: ~29 μm), as shown in Figure 2b. For the specimen 2# (intercritical annealed at 740
740 ◦ C for 30 min), as shown in Figure 2c, where it can be seen that austenite grain size was as large as
°C for 30 min), as shown in Figure 2c, where it can be seen that austenite grain size was as large as
that of the hot rolled sample (~106 µm), but there was fresh martensite formed at the prior austenite
that of the hot rolled sample (~106 μm), but there was fresh martensite formed at the prior austenite
grain boundary (G-M) and the inter-lath (L-M). The microstructure of specimen 2# was composed
grain boundary (G-M) and the inter-lath (L-M). The microstructure of specimen 2# was composed of
of G-M, L-M and intercritical ferrite (I-F); as indicated in Figure 2c, G-M and L-M was transformed
G-M, L-M and intercritical ferrite (I-F); as indicated in Figure 2c, G-M and L-M was transformed from
from equiaxed reversed austenite (ERA) and distributed at the prior austenite grain boundary, and
equiaxed reversed austenite (ERA) and distributed at the prior austenite grain boundary, and acicular
acicular reversed austenite (ARA) was present at bainite-lath. However, after the two-step heat
reversed austenite (ARA) was present at bainite-lath. However, after the two-step heat treatment
treatment (specimen 3#), fine and uniform austenite grains were obtained, as shown in Figure 2d. The
(specimen 3#), fine and uniform austenite grains were obtained, as shown in Figure 2d. The average
average grain size was ~12 µm, which was twice as fine as specimen 1#. It can be seen that the novel
grain size was ~12 μm, which was twice as fine as specimen 1#. It can be seen that the novel pre-
pre-annealing heat treatment process enhanced the nucleation of reversed austenite and refined the
annealing heat treatment process enhanced the nucleation of reversed austenite and refined the
coarse prior austenite grains.
coarse prior austenite grains.

Figure 2. Cont.
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Figure 2. SEM images of hot rolled plate steel (a) and specimen 2# (c) by nital etching; optical
microscope images of specimen 1# (b) and specimen 3# (d) by picric etching; M/A: martensite and
SEM images
Figure 2. SEM images of
of hot
hot rolled
rolled plate
plate steel
steel (a)
(a) and specimen 2# (c) by nital etching; optical
austenite constituent; I-F: intercritical ferrite; L-M: martensite distributed at laths; G-M: martensite
images of specimen
microscope images specimen 1# (b) and specimen 3# (d) by picric etching; M/A: martensite and
distributed at prior austenite grain boundary; γa and γb: austenite grain.
constituent; I-F:
austenite constituent; I-F: intercritical
intercritical ferrite; L-M: martensite distributed
distributed at laths; G-M: martensite
distributed at prior austenite grain boundary; γ γa and γγbb:: austenite
austenitegrain.
grain.
3.2. Crystallographic Characteristics of Pre-Annealed Microstructure
3.2. Crystallographic
The pre-annealed Characteristics
specimenofof (2#)
Pre-Annealed Microstructure
was investigated by EBSD in order to analyze the
3.2. Crystallographic Characteristics Pre-Annealed Microstructure
crystallographic orientation
The pre-annealed specimenof fresh martensite
(2#) was at prior
investigated austenite
by EBSD grain
in order boundary,
to analyze as presented in
the crystallographic
The pre-annealed specimen (2#) was investigated by EBSD in order to analyze the
Figure
orientation of fresh martensite at prior austenite grain boundary, as presented in Figurewas
3. A typical fresh martensite ‘b’ between two prior austenite grains γ-A and γ–B 3. A selected,
typical
crystallographic orientation of fresh martensite at prior austenite grain boundary, as presented in
as shown
fresh in Figure
martensite 3a. From
‘b’ between theprior
two poleaustenite
figures, grains
Figureγ-A3b–d,
anditγ–B
waswasfound that the
selected, position
as shown of “one”
in Figure 3a.
Figure 3. A typical fresh martensite ‘b’ between two prior austenite grains γ-A and γ–B was selected,
particular Bainfigures,
From the pole group of selected
Figure fresh
3b–d, martensite
it was in the
found that the(100) pole figure
position of “one”was identical Bain
particular to “one”
groupBain
of
as shown in Figure 3a. From the pole figures, Figure 3b–d, it was found that the position of “one”
group of prior austenite grain γ–B, which indicated that the selected fresh martensite
selected fresh martensite in the (100) pole figure was identical to “one” Bain group of prior austenite held the K-S
particular Bain group of selected fresh martensite in the (100) pole figure was identical to “one” Bain
orientation relationship
grain γ–B, which indicatedwiththat
the the
prior austenite
selected grain
fresh γ-B, butheld
martensite no orientation relationship
the K-S orientation with the
relationship
group of prior austenite grain γ–B, which indicated that the selected fresh martensite held the K-S
with the prior austenite grain γ-B, but no orientation relationship with the prior austenite grainfresh
prior austenite grain γ-A. In addition, from the pole figures, Figure 3b,c, it was found that the γ-A.
orientation relationship with the prior austenite grain γ-B, but no orientation relationship with the
martensite
In addition,between
from the inter-laths
pole figures,had the 3b,c,
Figure sameitBain groupsthat
was found with
theintercritical annealed
fresh martensite ferrite,
between which
inter-laths
prior austenite grain γ-A. In addition, from the pole figures, Figure 3b,c, it was found that the fresh
suggested
had the same that thegroups
Bain fresh martensite kept the
with intercritical K-S orientation
annealed ferrite, whichrelationship
suggestedwith the fresh
that the priormartensite
austenite
martensite between inter-laths had the same Bain groups with intercritical annealed ferrite, which
grain. The fresh martensite between the inter-laths was formed by acicular reversed
kept the K-S orientation relationship with the prior austenite grain. The fresh martensite between austenite when
suggested that the fresh martensite kept the K-S orientation relationship with the prior austenite
cooling to room
the inter-laths wastemperature. This illustrated
formed by acicular reversed that the acicular
austenite reversed
when cooling austenite
to room held the This
temperature. K-S
grain. The fresh martensite between the inter-laths was formed by acicular reversed austenite when
orientation relationship
illustrated that the acicularwithreversed
the prioraustenite
austeniteheldgrain.
theSadovskii [29] showed
K-S orientation that itwith
relationship is possible to
the prior
cooling to room temperature. This illustrated that the acicular reversed austenite held the K-S
reconstruct the prior austenite by growth and impingement of acicular
austenite grain. Sadovskii [29] showed that it is possible to reconstruct the prior austenite by growth austenite during
orientation relationship with the prior austenite grain. Sadovskii [29] showed that it is possible to
austenitization.
and impingement of acicular austenite during austenitization.
reconstruct the prior austenite by growth and impingement of acicular austenite during
austenitization.

Figure 3. Cont.
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Figure 3. (a)
(a) Bandcontrast
contrast images of
of 2#specimen;
specimen; two polepole figures(b,c)
(b,c) corresponding to to theprior
prior
Figure 3. (a) Band
Figure 3. Band contrast images
images of 2#
2# specimen; two two pole figures
figures (b,c) corresponding
corresponding to thethe prior
austenite grainγ-A
austenite γ-A andγ-B
γ-B in image(a);
(a); polefigures
figures (d) corresponding to the selected sections of in
‘b’
austenitegrain
grain γ-Aand
and γ-Bininimage
image (a);pole
pole figures(d) corresponding
(d) correspondingto to
thethe
selected sections
selected of ‘b’
sections of ‘b’
in image
image (a).
(a).(a).
in image
3.3.
3.3. Enrichment
Enrichment of of Alloying
Alloying Elements
Elements
3.3. Enrichment of Alloying Elements
The
The distribution
distribution of of alloying
alloying elements
elements in in specimen
specimen 2# 2# was
was examined,
examined, as as presented
presented in in Figure
Figure 4. 4.
From The distribution
intercritical ferriteoftoalloying
martensiteelements
to in specimen
intercritical 2#on
ferrite was
the examined,
other side,as
linepresented
scanning in
of Figure
alloying 4.
From intercritical ferrite to martensite to intercritical ferrite on the other side, line scanning of alloying
From intercritical
elements ferrite to martensite theto intercritical ferrite on the otherMn,
side,Ni,
lineCu
scanning of alloying
elements (Figure
(Figure 4a)
4a) showed
showed that that the contents
contents ofalloying
of alloying elements,
elements, Mn, Ni, Cu and andCrCr increased
increased in
elements
in (Figure
martensite and 4a) showed in
decreased that the contents
intercritical of alloying
ferrite aselements, inMn, Ni, Cu4b. and Cr increased in
martensite and decreased in intercritical ferrite (I-F),(I-F),
as shown shown
in FigureFigure
4b. Five-lineFive-line
scanning scanning
results
martensite
results are and decreased in1.
shown intercriticalbeferrite (I-F),the
as shown in Figure 4b. Five-line scanningMn, results
are shown in Tablein1.Table
It can beItseencan that seen that
the concentration concentration
of alloyingofelements
alloying elements
Mn, Ni, Cu andNi, Cr
are
Cu shown in Table 1. It can be seen that the concentration of alloying elements Mn, Ni, Cu and Cr
wasand Cr was significantly
significantly highertointheir
higher in contrast contrast
nominalto their nominal compositions,
compositions, which formedwhich formed the
the heterogeneous
was significantly
heterogeneous higher in contrast to their nominal compositions, which formed the heterogeneous
microstructuremicrostructure
of alloying of alloying
element element
enriched enriched
martensite martensite and depleted
and depleted intercritical
intercritical ferrite.
ferrite. In
microstructure
In combination of
with alloying
the image element
of Figure enriched
2d, the martensite
heterogeneous and depleted
microstructure intercritical
is related ferrite.
to fine In
and
combination with the image of Figure 2d, the heterogeneous microstructure is related to fine and
combination
uniform with the image of Figure 2d, the heterogeneous microstructure is related to fine and
uniformaustenite
austenitegrains
grainsobtained
obtainedby bythe
thetwo-step
two-stepheatheattreatment.
treatment.
uniform austenite grains obtained by the two-step heat treatment.
4.0
4.0 Mn
3.5
(b) M Ni
Mn
3.5
(b) M Cu
Ni
I-F/M interface Cr
Cu
3.0 I-F/M interface M/I-F interface Cr
3.0
M/I-F interface
(wt%)

I-F
2.5
(wt%)

I-F
2.5
I-F
Content

2.0 I-F
Content

2.0
1.5
1.5
1.0
1.0
0.5
0.5
0.0
0.0 0.0 0.5 1.0 1.5 2.0
0.0 0.5 Distance
1.0 (μm) 1.5 2.0
Distance (μm)
Figure4.4. Examined
Figure Examined schematic
schematic image
image of
of fresh
fresh martensite
martensite after
afterintercritical
intercritical annealing
annealing (a);
(a);examined
examined
Figure 4. Examined schematic image of fresh martensite after intercritical annealing (a); examined
resultsof
results ofalloying
alloyingelements
elementsdistribution
distributionbybyFEG-SEM
FEG-SEM(b).
(b).
results of alloying elements distribution by FEG-SEM (b).
Table 1. Concentration of alloying elements in M for specimen 3#.
Table 1. Concentration of alloying elements in M for specimen 3#.
Table 1. Concentration of alloying elements in M for specimen 3#.
Position Mn
Position Mn NiNi Cu Cu Cr Cr
Position Mn Ni Cu Cr
1# 1.89
1# 1.89 1.59
1.59 0.68 0.68 0.51 0.51
2# 1#
2.08 1.89 1.59
1.67 0.68 0.51
0.85 0.68
2# 2.08 1.67 0.85 0.68
3# 2#
1.81 2.08 1.56
1.67 0.85 0.720.68 0.56
4#
3#
1.95
1.81 1.56 0.72 0.79 0.56
3# 1.81 1.57
1.56 0.72 0.56 0.59
5# 4#
2.09 1.95 1.74
1.57 0.79 0.82 0.59 0.65
4# 1.95 1.57 0.79 0.59
Mean 5#
1.96 2.09 1.63
1.74 0.82 0.77 0.65 0.60
5# 2.09 1.74 0.82 0.65
Mean 1.96 1.63 0.77 0.60
Mean 1.96 1.63 0.77 0.60
3.4. Role of Heterogeneous Microstructure
3.4. Role of Heterogeneous Microstructure
3.4. Role
The of Heterogeneous
role Microstructure
of the heterogeneous microstructure in phase transformation of austenite was studied
The role
by thermal of the heterogeneous
simulation microstructure
(dilatometer) experiments,inasphase
showntransformation
in Figure 5. ofThe
austenite was studied
start temperature
The role of the heterogeneous microstructure in phase transformation of austenite was studied
and finish temperature of austenite transformation were 718 C and 877 C, respectively, for and
by thermal simulation (dilatometer) experiments, as shown in◦ Figure 5. The
◦ start temperature the
by thermal simulation (dilatometer) experiments, as shown in Figure 5. The start temperature and
finish temperature of austenite transformation were 718 °C and 877 °C, respectively, for the one-step
finish temperature of austenite transformation were 718 °C and 877 °C, respectively, for the one-step
Metals 2020, 10, 132 6 of 11
Metals 2020, 10, x FOR PEER REVIEW 6 of 11

one-step heat treatment ◦C

heat treatment specimen,specimen,
and for theand for theheat
two-step two-step heat specimen,
treatment treatment they
specimen, they
were 695 °Cwere 695 °C,
and 881
and ◦
881 C, respectively,
respectively, as presentedasinpresented in Figure
Figure 5a,c. We can 5a,c.
see We
thatcan see the
from thatplot
fromofthe
theplot
rateofofthe rate of
austenite
austenite transformation
transformation andtemperature,
and heating heating temperature,
there wasthere
only was only
a peak a peak transformation
transformation rate
rate for the for the
one-step
one-step heat treatment
heat treatment specimenspecimen (Figure
(Figure 5b), 5b), and
and there werethere
two were
peak two
ratespeak rates
for the for theheat
two-step two-step heat
treatment
treatment specimen (Figure 5d). This indicated that the alloying elements-enriched fresh
specimen (Figure 5d). This indicated that the alloying elements-enriched fresh martensite had lower martensite
had lower transformation
transformation temperature
temperature and alloying
and alloying elements-depleted
elements-depleted intercritical
intercritical ferritehad
ferrite had higher
transformation temperature.
temperature.

100 718℃ 12
(a)

Transformation Rate of reversed austenite

(b)
10
80
Change in length

877℃ 8
60
6
40
4

20 2

0 0

-2
-20
-4
0 100 200 300 400 500 600 700 800 900 740 760 780 800 820 840 860
TeTTeTatTTeT℃ Temperature/℃

120 4.0
695℃
Transformation Rate of reversed austenite

(c) 3.5
100 (d)
3.0
80
2.5
Change in length

60 881℃
2.0
40
1.5
20 1.0

0 0.5

-20 0.0

-0.5
-40
-1.0
0 200 400 600 800 1000 700 725 750 775 800 825 850 875
TeTTeTatTTeT℃ Temperature/℃

Figure
Figure 5. Gleeble simulated
5. Gleeble simulated curves
curves of
of one-step
one-step (a)
(a) and
and two-step
two-step (c)
(c) heat
heat treatment;
treatment; the
the austenite
austenite
transformation rate curves of one-step (b) and two-step (d) heat treatment.
transformation rate curves of one-step (b) and two-step (d) heat treatment.

The austenite nucleation during reheating for intercritically annealed specimen can be discussed
The austenite nucleation during reheating for intercritically annealed specimen can be discussed
from the viewpoint of thermodynamics. As is well known, the thermal activated nucleation needs to
from the viewpoint of thermodynamics. As is well known, the thermal activated nucleation needs to
overcome the energy barrier before the formation of embryo. According to the nucleation theory [30],
overcome the energy barrier before the formation of embryo. According to the nucleation theory [30],
under ideal state, the relationship of the nucleation energy barrier, interface energy and intrinsic energy
under ideal state, the relationship of the nucleation energy barrier, interface energy and intrinsic
difference of fcc phase and bcc phase can be expressed by:
energy difference of fcc phase and bcc phase can be expressed by:
3 2
△G0 0== 16πγ
4G 16πγ3/(3*(4g)
/(3*(△g)2)) (1)
(1)
where ∆G∆G0 is nucleation energy barrier, γ is interface energy, ∆g is intrinsic energy difference of fcc
where 0 is nucleation energy barrier, γ is interface energy, ∆g is intrinsic energy difference of fcc
phase and
phase and bcc
bcc phase
phase when
when bcc
bcc phase
phase transformed
transformed into
into fcc
fcc phase.
phase. The
The nucleation
nucleation energy
energy barrier
barrier is
is
decreased when the interface energy is low (in our case, the interface energy was low
decreased when the interface energy is low (in our case, the interface energy was low because of because of
alloying elements
alloying elements enriched
enriched atat the
the interface)
interface) and
and the
the intrinsic
intrinsic energy
energy difference
difference of
of fcc
fcc phase
phase and
and bcc
bcc
phase increased.
phase increased. Thus,
Thus, the
the necessary
necessary driving
driving energy
energy for
for nucleation
nucleation was
was small,
small, which
which enhanced
enhanced the
the
nucleation rate of reversed austenite via thermally activated nucleation.
nucleation rate of reversed austenite via thermally activated nucleation.
∆g = gfcc − gbcc (2)
∆g = gfcc − gbcc (2)
where gfcc or gbcc represent intrinsic energy of α phase or γ phase, respectively, at a temperature and
at a given
where chemical
gfcc or composition.
gbcc represent intrinsic energy of α phase or γ phase, respectively, at a temperature and at
Thechemical
a given composition of G-M/L-M and I-F after intercritical annealing at 740 °C was calculated by
composition.
Thermo-calc 3.0 based on TCFE 7.0 according to the nominal composition (NC). The alloying element
contents in G-M/L-M and I-F were 0.15C-0.21Si-2.03Mn-1.87Ni-0.52Cr-0.36Mo-0.80Cu (wt. %) and
Metals 2020, 10, 132 7 of 11

The composition of G-M/L-M and I-F after intercritical annealing at 740 ◦ C was calculated by
Thermo-calc 3.0 based on TCFE 7.0 according to the nominal composition (NC). The alloying element
Metals 2020, 10, x FOR PEER REVIEW 7 of 11
contents in G-M/L-M and I-F were 0.15C-0.21Si-2.03Mn-1.87Ni-0.52Cr-0.36Mo-0.80Cu (wt. %) and
0.05C-0.24Si-0.79Mn-0.74Ni-0.43Cr-0.48Mo-0.35Cu
0.05C-0.24Si-0.79Mn-0.74Ni-0.43Cr-0.48Mo-0.35Cu (wt. (wt. %),
%), respectively.
respectively. Figure
Figure 66 shows
shows the
the intrinsic
intrinsic
energy
energy difference of fcc phase and bcc phase for the nominal composition, martensite (G-M/L-M) and
difference of fcc phase and bcc phase for the nominal composition, martensite (G-M/L-M) and
I-F,
I-F, respectively,
respectively, during reheating. ItItcan
during reheating. canbebe seen
seen that
that thethe intrinsic
intrinsic energy
energy difference
difference of G-M/L-M
of G-M/L-M was
was higher ◦ C, and the intrinsic energy difference
higher thanthan NC when
NC when the temperature
the temperature was below
was below 763and
763 °C, the intrinsic energy difference of I-F
of I-Fgreater
was greater ◦ C. Thus, the heterogeneous
was than than
NC NCas theas the temperature
temperature waswas greaterthan
greater than815815°C. Thus, the heterogeneous
microstructure
microstructure can reduce the energy barrier and driving energy for nucleation, and
can reduce the energy barrier and driving energy for nucleation, and enhance
enhance thethe
nucleation of equiaxed reversed austenite.
nucleation of equiaxed reversed austenite.

NC
51000 G-M/L-M
IF
48000

45000
(gfcc-gbcc)(J)

42000

39000

36000

33000
763℃ 815℃
30000
700 725 750 775 800 825 850 875 900
Temperature (℃)

Figure 6. The intrinsic energy difference of fcc phase and bcc phase when bcc phase transformed into
Figure 6. The intrinsic energy difference of fcc phase and bcc phase when bcc phase transformed into
fcc phase for the compositions of NC, G-M/L-M and I-F calculated by thermo-calc 3.0 based on TCFE 7.
fcc phase for the compositions of NC, G-M/L-M and I-F calculated by thermo-calc 3.0 based on TCFE
3.5. Nucleation
7. Rate of Reversed Austenite
The effect of heterogeneous microstructure on reaustenitization during reheating was studied
3.5. Nucleation Rate of Reversed Austenite
via step by step experiments. Experiments were designed every 20 ◦ C in the temperature range of
720–860The◦ C
effect of heterogeneous
for one-step and two-stepmicrostructure
heat treatmenton processes,
reaustenitization
and theduring
resultsreheating
are shownwas studied
in Figure 7.
via step by step experiments. Experiments were designed every 20 °C in the temperature
Two optical microscope images show the distribution of equiaxed reversed austenite grain (Figure 7a,b) range of
720–860
for °C for one-step
the one-step and two-step
and two-step heat treatment
heat treatment processes,
processes. It can beandseen
the that
results
theare shown reversed
equiaxed in Figure
7. Two optical
austenite grainmicroscope
was large andimages
mainlyshow the distribution
distributed at priorofaustenite
equiaxedgrainreversed austenite
boundary grain (Figure
for one-step heat
7a,b) for the one-step and two-step heat treatment processes. It can be seen that
treatment specimen (Figure 7a); however, the fine equiaxed reversed austenite grain obtained by the equiaxed reversed
austeniteheat
two-step grain was large
treatment wasand mainly
present distributed
at the at prior
prior austenite austenite
grain grainand
boundary boundary for one-step
intragranular (Figureheat
7b).
treatment specimen (Figure 7a); however, the fine equiaxed reversed austenite
The results in Figure 7b showed the heterogeneous microstructure can enhance the nucleation of grain obtained by two-
step heatreversed
equiaxed treatment was present
austenite. at the prior
The number austenite
of equiaxed grain boundary
reversed and intragranular
austenite grains for different (Figure 7b).
intercritical
The results
annealing in Figure 7b
temperature showed
were theas
counted, heterogeneous
shown in Figure microstructure
7c (note: the can enhance
statistical thesize
grain nucleation of
was for an
equiaxed reversed austenite. The number of equiaxed reversed austenite
area greater than 2 square micro-meters; for the two-step experimental specimens, the grain below grains for different
intercritical
820 ◦ C was tooannealing
small totemperature
count). Thewere counted,
austenite grainasnumber
shown for in Figure 7c (note:
the two-step the statistical
specimen grain
was higher
size was for an area greater than 2 square micro-meters; for the two-step experimental
than for the one-step specimen for every intercritical annealing temperature, which indicated that specimens, the
grain below 820 °C was too small to count). The austenite grain number for the
the nucleation density of equiaxed grain for two-step specimen was higher in contrast to that of the two-step specimen
was higher
one-step than for the one-step specimen for every intercritical annealing temperature, which
specimen.
indicated that the nucleation density of equiaxed grain for two-step specimen was higher in contrast
to that of the one-step specimen.
Metals 2020, 10, 132 8 of 11
Metals 2020, 10, x FOR PEER REVIEW 8 of 11

400
NTTbeT of eqTiaxed TeveTsed aTstentie gTain

one-step:760~860℃ (interval:20℃)
two-steps: 740℃(30min) (c)
350 +820~860℃ (interval:20℃)

300

250

200

150

100

760 780 800 820 840 860

Annealing teTTeTatTTe

Theoptical
opticalmicroscope
microscopeimages
imagesofofone-step
one-step ◦ C holding 1 min;
Figure 7.
Figure 7. The (a)(a)
andand two-step
two-step (b)(b) at 820
at 820 °C holding 1 min; (c)
(c) the
the number
number of statistically
of statistically equiaxed
equiaxed reversed
reversed austenite
austenite graingrain (within
(within theofsize
the size 165of× 114 × 114 square
165 square micro
micro meter).
meter).

In a summary, a schematic image of austenitized behavior during one-step and two-step

In a summary, a schematic image of austenitized behavior during one-step and two-step
austenitization is proposed, as shown in Figure 8. For the one-step heat treatment specimen, the
austenitization is proposed, as shown in Figure 8. For the one-step heat treatment specimen, the
equiaxed reversed austenite (ERA) grains only occurred at the prior austenite grain boundary and grew
equiaxed reversed austenite (ERA) grains only occurred at the prior austenite grain boundary and
fast during austenitization (Figure 8b) to form the austenite grain γ (Figure 8c), the acicular reversed
grew fast during austenitization (Figure 8b) to form the austenitea grain γa (Figure 8c), the acicular
austenite (ARA) grew and impinged to reconstitute the prior austenite γb (Figure 8c), as presented
reversed austenite (ARA) grew and impinged to reconstitute the prior austenite γb (Figure 8c), as
in Figure 2b. For the two-step specimen, the heterogeneous microstructure of alloying elements
presented in Figure 2b. For the two-step specimen, the heterogeneous microstructure of alloying
enriched fresh martensite (including G-M and L-M) and depleted intercritical ferrite was obtained after
elements enriched fresh martensite (including G-M and L-M) and depleted intercritical ferrite was
intercritical annealing (Figure 8d), which enhanced the equiaxed reversed austenite grain nucleated at
obtained after intercritical annealing (Figure 8d), which enhanced the equiaxed reversed austenite
the intragranular and prior austenite grain boundary during reaustenitization (Figure 8e). Finally, fine
grain nucleated at the intragranular and prior austenite grain boundary during reaustenitization
and uniform austenite grain size was obtained after complete austenitization, (Figures 8f and 2d).
(Figure 8e). Finally, fine and uniform austenite grain size was obtained after complete austenitization,
(Figures 8f and 2d).
Metals 2020, 10, 132 9 of 11
Metals 2020, 10, x FOR PEER REVIEW 9 of 11

Figure 8. Schematic of direct austenitization (a–c) or partition and reaustenitization (a,d–f) for hot
Figure 8. Schematic of direct austenitization (a–c) or partition and reaustenitization (a,d–f) for hot
rolled experimental steel. ERA: equiaxed reversed austenite; ARA: acicular reversed austenite.
rolled experimental steel. ERA: equiaxed reversed austenite; ARA: acicular reversed austenite.
4. Conclusions
4. Conclusions
In this study, coarse prior austenite grains in the core of heavy plate processed by TMCP were
In this
studied study, coarse
by two-step prior austenite
heat treatment, grains
and the in the core
conclusions areofconcluded
heavy plate processed by TMCP were
as follows:
studied by two-step heat treatment, and the conclusions are concluded as follows:
• The heterogeneous microstructures of alloying elements-enriched fresh martensite and -depleted
• The heterogeneous microstructures of alloying elements-enriched fresh martensite and -depleted
intercritical ferrite were obtained after intercritical annealing. The fresh martensite was distributed
intercritical ferrite were obtained after intercritical annealing. The fresh martensite was
at prior austenite grain boundary (G-M) and inter-lath (L-M). G-M was transformed by equiaxed
distributed at prior austenite grain boundary (G-M) and inter-lath (L-M). G-M was transformed
reversed austenite and the L-M was formed by acicular reversed austenite, when the reversed
by equiaxed reversed austenite and the L-M was formed by acicular reversed austenite, when the
austenite obtained during intercritical annealing was quenched to room temperature.
reversed austenite obtained during intercritical annealing was quenched to room temperature.
• The heterogeneous microstructure increased the intrinsic energy difference of fcc phase and bcc
• The heterogeneous◦ microstructure increased the intrinsic energy difference of fcc phase and bcc
phase below 763 C or above 815 ◦ C, and the interface energy decreased because of alloying
phase below 763 °C or above 815 °C, and the interface energy decreased because of alloying
element enrichment at the interface, which reduces the nucleation energy barrier according to the
element enrichment at the interface, which reduces the nucleation energy barrier according to the
nucleation theory under ideal state. Therefore, the nucleation driving energy of equiaxed reversed
nucleation theory under ideal state. Therefore, the nucleation driving energy of equiaxed
austenite is less. The heterogeneous microstructure can enhance the equiaxed reversed austenite
reversed austenite is less. The heterogeneous microstructure can enhance the equiaxed reversed
nucleation at intragranular and prior austenite grain boundary during reheating, which effectively
austenite nucleation at intragranular and prior austenite grain boundary during reheating, which
refined the coarse prior austenite grains in the core of hot rolled heavy plate processed by TMCP.
effectively refined the coarse prior austenite grains in the core of hot rolled heavy plate processed
• The prior austenite grains in the core of heavy plate processed by TMCP was very large (~105
by TMCP.
µm). The austenite grains were inhomogeneous when the hot rolled specimen was reheated
• The prior austenite grains in the core of heavy plate processed by TMCP was very large (~105
by one-step heat treatment process. However, for the two-step heat treatment process, fine and
μm). The austenite grains were inhomogeneous when the hot rolled specimen was reheated by
uniform austenite grain size (~12 µm) was obtained, which was two times finer compared to the
one-step heat treatment process. However, for the two-step heat treatment process, fine and
one-step heat treatment. An effective way of improving strength, ductility and low temperature
uniform austenite grain size (~12 μm) was obtained, which was two times finer compared to the
toughness in alloy steel is to refine the prior austenite grain size. This study provides a possible
one-step heat treatment. An effective way of improving strength, ductility and low temperature
way of effectively refining prior austenite grain size.
toughness in alloy steel is to refine the prior austenite grain size. This study provides a possible
way of effectively refining prior austenite grain size.
Author Contributions: S.Y.: conceptualization, data curation, formal analysis, investigation, writing—original
Author Contributions:
draft; Z.X.: S.Y.: conceptualization,
review & editing; datareview
J.W.: formal analysis, curation, formal analysis,
& editing; investigation,
L.Z.: data writing—original
curation; L.Y.: dcuration; C.S.:
conceptualization,
draft; funding
Z.X.: review & acquisition,
editing; supervision,
J.W.: formal review&&editing;
analysis, review editing;L.Z.:
R.D.K.M.: review &L.Y.:
data curation; editing. All authors
dcuration; C.S.:
have read and agree
conceptualization, to the published
funding version
acquisition, of the manuscript.
supervision, review & editing; R.D.K.M.: review & editing. All authors
have read and agree to the published version of the manuscript.
Metals 2020, 10, 132 10 of 11

Funding: This research received no external funding.

Conflicts of Interest: The authors declare no conflict of interest.

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