metals
Article
Study on High-Temperature Mechanical Properties of
Fe–Mn–C–Al TWIP/TRIP Steel
Guangkai Yang 1,2 , Changling Zhuang 1,2, *, Changrong Li 1,2 , Fangjie Lan 1,2 and Hanjie Yao 1,2






Citation: Yang, G.; Zhuang, C.; Li, C.;
Lan, F.; Yao, H. Study on
High-Temperature Mechanical
Properties of Fe–Mn–C–Al
TWIP/TRIP Steel. Metals 2021, 11,
821. https://doi.org/10.3390/
met11050821
Academic Editor: Colin Scott
Received: 28 April 2021
Accepted: 15 May 2021
Published: 18 May 2021
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
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iations.
Copyright: © 2021 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
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4.0/).
Metals 2021, 11, 821. https://doi.org/10.3390/met11050821
1 School of Materials and Metallurgy, Guizhou University, Guiyang 550025, China;
18085037568@163.com (G.Y.); crli@gzu.edu.cn (C.L.); fangjielan@163.com (F.L.);
yhj1394542756@163.com (H.Y.)
2 Guizhou Key Laboratory of Metallurgical Engineering and Process Energy Conservation,
Guiyang 550025, China
* Correspondence: clzhuang@gzu.edu.cn; Tel.: +86-186-0851-4532
Abstract: In this study, high-temperature tensile tests were carried out on a Gleeble-3500 thermal
simulator under a strain rate of ε = 1 × 10−3 s−1 in the temperature range of 600–1310 ◦ C. The hot
deformation process of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP at different temperatures was studied.
In the whole tested temperature range, the reduction of area ranged from 47.3 to 89.4% and reached
the maximum value of 89.4% at 1275 ◦ C. Assuming that 60% reduction of area is relative ductility
trough, the high-temperature ductility trough was from 1275 ◦ C to the melting point temperature, the
medium-temperature ductility trough was 1000–1250 ◦ C, and the low-temperature ductility trough
was around 600 ◦ C. The phase transformation process of the steel was analyzed by Thermo-Calc
thermodynamics software. It was found that ferrite transformation occurred at 646 ◦ C, and the
austenite was softened by a small amount of ferrite, resulting in the reduction of thermoplastic and
formation of the low-temperature ductility trough. However, the small difference in thermoplasticity
in the low-temperature ductility trough was attributed to the small amount of ferrite and the low
transformation temperature of ferrite. The tensile fracture at different temperatures was characterized
by means of optical microscopy and scanning electron microscopy. It was found that there were
Al2 O3 , AlN, MnO, and MnS(Se) impurities in the fracture. The abnormal points of thermoplasticity
showed that the inclusions had a significant effect on the high-temperature mechanical properties.
The results of EBSD local orientation difference analysis showed that the temperature range with
good plasticity was around 1275 ◦ C. Under large deformation extent, the phase difference in the
internal position of the grain was larger than that in the grain boundary. The defect density in
the grain was large, and the high dislocation density was the main deformation mechanism in the
high-temperature tensile process.
Keywords: TWIP/TRIP steel; high-temperature mechanical properties; reduction of area;
ductility trough
1. Introduction
Fe–Mn–C–Al TWIP/TRIP steel has great potential in automotive structural compo-
nents, the construction industry, and oil and gas exploration due to its excellent tensile
strength, ductility, and high energy absorption capacity [1]. In modern automotive struc-
tural parts, excellent stamping ductility is expected. This steel provides high-strength
structural performance and can absorb a lot of energy to enhance crashworthiness, which
is very important for vehicles. In addition, large-scale use of such high-grade steel can
reduce vehicle density, reduce the weight of the vehicle itself, reduce greenhouse gas
emissions, increase gasoline mileage, and improve passenger safety [2]. The good me-
chanical properties required can be achieved by strain-induced martensitic transformation
or twin materials, which are called TRIP (transformation-induced plasticity) steel and
TWIP (twinning-induced plasticity) steel [1]. The difference in the deformation mechanism
https://www.mdpi.com/journal/metals
Metals 2021, 11, 821 2 of 15

between the two steels is caused by stacking fault energy (SFE) of the austenite matrix.
The main factors affecting SFE are alloy composition and deformation temperature [3].
Jin et al. [4] studied the effect of Al content in the range of 0–2% on SFE of TWIP steel with
Fe–18Mn–0.6C–xAl composition. The results showed that the SFE increased linearly with a
constant slope of 7.8 mJ/m2 for every 1 wt % Al addition. Frommeyer et al. [5] showed that
TRIP was the main effect when the manganese content was lower than 20%, while the TWIP
became the main effect when the manganese content was higher than 25%. Lee et al. [6]
studied the tensile properties of medium manganese steel with Mn% in the range of 9–12%.
They found that the plastic deformation mechanism was related to the strain rate, and the
TRIP and TWIP effects occurred simultaneously when the strain rate was in the range of
10−4 s−1 to 10−2 s−1 . However, there have been few studies on the thermoplasticity of steel
with TWIP/TRIP effects, which will affect the surface cracking of steel billets during the
hot rolling and continuous casting processes. Gennari et al. [7] carried out an innovative
heat treatment (intercritical annealing at 780 ◦ C and austempering at 400 ◦ C for 30 min)
for a new high-silicon steel with TRIP effect. Higher hardness and higher tensile strength
were obtained by isothermal quenching. The high amount of martensite was responsible
for the low fracture strain and ductility. Improvement of austenite stability increased the
ultimate tensile strength and total elongation of TRIP steel [8]. Furthermore, Mou et al. [9]
found that lamellar austenite was more likely to cause stress relaxation during martensitic
transformation, resulting in a discontinuous TRIP effect and thus higher ductility. Peng
et al. [10] carried out extension experiment at elevated temperature on Fe–22Mn–0.7C
TWIP steel in the temperature range of 700–1250 ◦ C and found that the reduction of area
was extremely low, all below 40%. Barbieri et al. [11] carried out tensile tests of Fe–22Mn–
0.65C TWIP steel at 25–400 ◦ C. Metallographic observation showed that mechanical twins
were the main feature of the microstructure at 25 ◦ C. At 350 ◦ C, twins were observed
only in some dispersed grains, with dislocation bands observed. Koyama et al. [12] tested
tensile Fe–18Mn–1.2C TWIP steel in the temperature range of −150 to 250 ◦ C and analyzed
the twin density at different temperatures by EBSD. It was found that the twin density
decreased monotonously with the increase in deformation temperature from −50 to 200 ◦ C
and became nearly zero at 200 ◦ C. It is well known that deformation-induced ε-martensitic
transformation occurs at a lower temperature range than deformation twins, both of which
are suppressed with increasing SFE.
The purpose of this study was to examine the mechanical properties and fracture
mechanism of TWIP/TRIP steel at temperatures of 600–1310 ◦ C, which is a more represen-
tative range. The tensile test was carried out by a thermal simulator at high temperature,
and the fracture behavior, phase transformation, and dynamic recrystallization (DRX)
were characterized by optical microscopy (OM), scanning electron microscopy (SEM),
energy-dispersive spectrometry (EDS), electron backscattered diffraction (EBSD), and the
Thermo-Calc thermodynamic software. The high-temperature mechanical properties of
Fe–Mn–C–Al TWIP/TRIP were analyzed. The change of SFE in the temperature range
of 600–1310 ◦ C was calculated by a formula. The reduction of area (RA) was used to
quantify the thermoplasticity, which was compared with Fe–24.2Mn–3Al–2.6Si TWIP steel
and 12Cr1MoVG steel. The TWIP/TRIP steel studied here had excellent thermoplasticity
in the whole tensile temperature range. There was no traditional ductility trough (≤40%).
The high- and low-temperature ductility troughs shifted to the high- and low-temperature
zones, respectively, resulting in the excellent performance of the steel in the whole high-
temperature zone. This is a very interesting phenomenon. The fracture mechanism and
high-temperature mechanical properties are described in detail below.

2. Sample Processing and Experimental Methods

2.1. Sample Preparation and Sampling
First, 20 kg of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel ingot was produced in a 25 kg
medium frequency vacuum induction furnace (Santai Electric Furnace Factory, Jinzhou,
China). After removing the riser, the section size was Φ120 mm. The edge of the billet
 2. Sample Processing and Experimental Methods
2.1. Sample Preparation and Sampling
Metals 2021, 11, 821 First, 20 kg of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel ingot was produced in 3aof2515
kg medium frequency vacuum induction furnace (Santai Electric Furnace Factory, Jin-
zhou, China). After removing the riser, the section size was Ф120 mm. The edge of the
billet was selected
was selected alongalong the direction
the direction shownshown
by thebyred
thearrow
red arrow in Figure
in Figure 1. Aoftotal
1. A total of 14
14 tensile
tensile specimens with the size of Ф10 × 121.5 mm were selected by wire cutting.
specimens with the size of Φ10 × 121.5 mm were selected by wire cutting. The length Theof
length of the two ends of the thread was 15.25 mm, and the thread spacing
the two ends of the thread was 15.25 mm, and the thread spacing was 1.5 mm. was 1.5 mm.

Samplingdiagram
Figure1.1.Sampling
Figure diagramofofhigh-temperature
high-temperaturetensile
tensilesample.
sample.

Themass
The massfraction
fraction of
of the
the main
main elements
elements in
in this
this steel
steelisisshown
shownininTable
Table1. 1.
The concen-
The con-
centrations of carbon and sulfur were determined by the infrared absorption methodafter
trations of carbon and sulfur were determined by the infrared absorption method af-
combustion
ter combustionin oxygen using
in oxygen a CS-230
using high-frequency
a CS-230 high-frequency infrared carbon
infrared sulfur
carbon analyzer
sulfur (Yan-
analyzer
rui Instrument
(Yanrui Co.,Co.,
Instrument Ltd.,Ltd,
Chongqing, China).
Chongqing, In addition,
China). In addition,the concentrations of nitrogen
the concentrations of ni-
and oxygen were measured by the thermal conductivity and infrared absorption methods
trogen and oxygen were measured by the thermal conductivity and infrared absorption
using a NO-330 nitrogen oxygen analyzer (Yanrui Instrument Co., Ltd., Chongqing, China)
methods using a NO-330 nitrogen oxygen analyzer (Yanrui Instrument Co., Ltd, Chong-
and helium as carrier gas. The contents of other alloying elements (Mn and Al) were
qing, China) and helium as carrier gas. The contents of other alloying elements (Mn and
determined by X-ray fluorescence (XRF) (Shimadzu Enterprise Management (China) Co.,
Al) were determined by X-ray fluorescence (XRF) (Shimadzu Enterprise Management
Ltd., Shanghai, China) under vacuum.
(China) Co., Ltd, Shanghai, China) under vacuum.
Table 1. Chemical composition of specimens (wt %).
Table 1. Chemical composition of specimens (wt %).
Element
Element FeFe MnMn CC Al
Al N
N OO SS
Content(%)
Content (%) Bal.
Bal. 15.3
15.3 0.58
0.58 2.3
2.3 0.0057
0.0057 0.0049
0.0049 0.0099
0.0099

2.2.High-Temperature
2.2. High-TemperatureTensile
TensileTest
Test
Theprocessed
The processedtensile
tensile sample
sample bar was subjected
subjected toto high-temperature
high-temperaturetensile
tensiletest
testusing
us-
a Gleeble-3500
ing a Gleeble-3500 thermal
thermalsimulator
simulator(Fuller
(FullerInstrument
Instrument Technology (Shanghai)
(Shanghai) Co.,
Co.,Ltd,
Ltd,
Shanghai,China),
Shanghai, China),and
and the
the tensile temperature rangerange was 600–1310◦ C.
was600–1310 °C.The
Thetensile
tensilesample
sam-
was
ple horizontally
was horizontallyfixed in the
fixed vacuum
in the vacuumchamber.
chamber.After vacuum
After pumping,
vacuum the the
pumping, sample was
sample
heated by a resistor in an Ar-filled atmosphere to prevent oxidation. The
was heated by a resistor in an Ar-filled atmosphere to prevent oxidation. The effective effective length
of heating
length was 20was
of heating mm.20Temperature was measured
mm. Temperature using anusing
was measured R-type
an platinum–rhodium
R-type platinum–
thermocouple
rhodium wire. Thewire.
thermocouple processing flow chart
The processing of the
flow high-temperature
chart tensile specimen
of the high-temperature tensile
is shownisinshown
specimen Figurein2.Figure
The 12 2. tensile
The 12 specimens were heated
tensile specimens at roomattemperature
were heated room tempera- at a
rate of 10 ◦ C/s to 1250 ◦ C for 180 s. The purpose of this operation was to carry out solid
ture at a rate of 10 °C/s to 1250 °C for 180 s. The purpose of this operation was to carry
solution treatment and simulate the conditions appearing in the straightening operation
process of continuous casting as much as possible. It was ensured that the steel was fully
austenitized, internal stress was eliminated, and a larger grain size was obtained, similar
to the grain size of the continuous casting process. Then, it was heated or cooled at a rate
of 3 ◦ C/s to predetermined test temperatures (600, 700, 800, 900, 1000, 1100, 1200, 1250,
1275, 1285, 1300, and 1310 ◦ C). After holding for 60 s, the specimens were stretched to
 out solid solution treatment and simulate the conditions appearing in the straightening
operation process of continuous casting as much as possible. It was ensured that the
steel was fully austenitized, internal stress was eliminated, and a larger grain size was
obtained, similar to the grain size of the continuous casting process. Then, it was heated
Metals 2021, 11, 821 or cooled at a rate of 3 °C/s to predetermined test temperatures (600, 700, 800, 900, 1000,4 of 15
1100, 1200, 1250, 1275, 1285, 1300, and 1310 °C). After holding for 60 s, the specimens
were stretched to fracture failure at a strain rate of 1 × 10−3∙s−1. Quick cooling was imme-
diately carried out to retain the high-temperature fracture morphology and microstruc-
fracture failure at a strain rate of 1 × 10−3 s−1 . Quick cooling was immediately carried out
ture. During the high-temperature tensile process, the stress and strain values of the
to retain the high-temperature fracture morphology and microstructure. During the high-
specimen were recorded in real time by a Gleeble-3500 thermal simulator. The curves
temperature tensile process, the stress and strain values of the specimen were recorded
processed by the Origin software (2021, OriginLab, Hampton, USA). The maximum ten-
in real time by a Gleeble-3500 thermal simulator. The curves processed by the Origin
sile stress in the tensile process at each temperature was obtained from the recorded data
software (2021, OriginLab, Hampton, USA). The maximum tensile stress in the tensile
and then compared with Fe–24.2Mn–3Al–2.6Si TWIP steel [13] and 12Cr1MoVG steel
process at each temperature was obtained from the recorded data and then compared with
[14].
Fe–24.2Mn–3Al–2.6Si TWIP steel [13] and 12Cr1MoVG steel [14].

Figure 2. Flowchart of high-temperature tensile specimen processing.

Figure 2. Flowchart of high-temperature tensile specimen processing.
As shown in Figure 3, the end with relatively complete morphology after fracture was
selected, the fracture
As shown was
in Figure 3,sealed,
the endand samples
with of appropriate
relatively complete size were cut by
morphology wire.
after Quanta
fracture
FEG 250 (FEI, Hillsboro, OR, USA)
was selected, the fracture was sealed, and Zeiss-Utra55 (Zeiss, Oberkochen, German)
samples of appropriate size were cut by wire. field
emission
Quanta FEGscanning
250 (FEI,electron microscopes
Hillsboro, OR, USA)were and used for SEM (Zeiss,
Zeiss-Utra55 and EDS tests, respectively.
Oberkochen, Ger-
SEMfield
man) wasemission
used to observe
scanningtheelectron
morphology of typicalwere
microscopes inclusions nearSEM
used for the fracture.
and EDSEDS was
tests,
used to analyze
respectively. SEM thewascomposition of thethe
used to observe inclusions and the
morphology of mass fraction
typical of each
inclusions element.
near the
The fracture
fracture. EDS was wasused
cut longitudinally
to analyze thealong the tensile
composition direction.
of the Afterand
inclusions a series of standard
the mass frac-
grinding and polishing processes, the metallographic surface was etched by
tion of each element. The fracture was cut longitudinally along the tensile direction. Af- 4% nitric acid
alcohol solution. The microstructure near the fracture was observed by
ter a series of standard grinding and polishing processes, the metallographic surface wasOLYMPUSGX71
optical
etched bymicroscope
4% nitric acid(Olympus,
alcohol Tokyo,
solution.Japan). Oxford Nordlys
The microstructure Max3
near the(Oxford,
fracture UK)
was EBSD
ob-
was used
served to detect and analyze
by OLYMPUSGX71 themicroscope
optical section. Finally, Thermo-Calc
(Olympus, Tokyo, thermodynamic
Japan). Oxford software
Nord-
lys(TCFEC7, Stockholm,
Max3 (Oxford, Sweden)
UK) EBSD wasofused
TCFE7 database
to detect andwas used the
analyze to predict
section.the phaseTher-
Finally, change
behavior in the whole tensile temperature range.
mo-Calc thermodynamic software (TCFEC7, Stockholm, Sweden) of TCFE7 database
was used to predict the phase change behavior in the whole tensile temperature range.
Metals2021,
Metals 2021,11,
11,821
x FOR PEER REVIEW 55 of
of 15
15

Figure 3. Fracture topography.

Figure 3. Fracture topography.

3. Results
3. Results and
and Analysis
Analysis
3.1.
3.1. Calculation
Calculation of
of SFE
SFE
In
In Olson’s
Olson’s work
work [15,16],
[15,16], the
the thermodynamic
thermodynamic model of stacking fault energy is ex-
pressed
pressed as
as follows:
follows:
γSF = 2ρA ∆Gγ→ ε
(1)
γSF = 2ρAΔGγ→ε (1)
In Equation (1), ρA is the atomic surface stacking density in the face-centered cubic
In and
phase, Equation →(1),
∆Gγγ→ε ε ρA is the atomic surface stacking density in the face-centered cubic
is the free energy difference between the face-centered cubic and
phase, and ΔG
close-packed hexagonal is the free energy
phases, which isdifference
the key tobetween thethe
calculating face-centered cubic
stacking fault and
energy.
close-packed hexagonal phases, which is the key to2 calculating the stacking
Allain et al. [17] gave the average value of 10 mJ/m for the range of 5–15 mJ/m . fault
2 energy.
Allain et al. [17] gave the average value of 10 mJ/m2 for the range of 5–15 mJ/m2.
4 4 11
ρA =ρA√ = ·α ∙ (2)
(2)
3√3 α2 2NN
In Equation (2), N is the Avogadro constant and N = 6.02 × 1023, and α is the lattice
In Equation (2), N is the Avogadro constant and N = 6.02 × 1023 , and α is the lattice
constant of the alloy. According to the work done in [18,19], the empirical formula of the
constant of the alloy. According to the work done in [18,19], the empirical formula of
lattice parameters of Fe–Mn–Al–C alloy and the lattice constant of austenite at any
the lattice parameters of Fe–Mn–Al–C alloy and the lattice constant of austenite at any
transformation temperature can be derived.
transformation temperature can be derived.
αγ0 = 0.35721 + 0.0001166 (Mn) + 0.0044089 (C) + 0.0002771(Al) (3)
αγ0 = 0.35721 + 0.0001166 (Mn) + 0.0044089 (C) + 0.0002771(Al) (3)
αγ = αγ0[1 + βγ(T − 300)] (4)
αγ = αγ0 [1 + βγ (T − 300)] (4)
In Equation (3), the brackets denote the mass fraction of the element. In Formula (4),
In Equation
βγ denotes (3), the
the linear brackets
thermal denote the
expansion mass fraction
coefficient of the element.
of austenite, In ×Formula
βγ = 2.065 10−5 K−1.(4),
αγ0
βγ denotes the linear thermal expansion coefficient of austenite, βγ = 2.065
is the lattice parameter of austenite at room temperature, T is Kelvin temperature. × 10−5 K−1 .
αγ0 is the lattice parameter of austenite at room temperature,
γ→ε T is Kelvin temperature.
γ→ε
ΔGγ→ε = ∑Xx ΔGγ→ε x + ∑Xx XFe ΔGFex + XC ΔGFeMnAl/C + ΔGγ→ε mg (5)
In Equation (5),∑ΔGx xis the ∑
γ→ε γ→ε γ→ε γ→ε γ→ε
∆G = X ∆G
γ→ε + X X ∆G
free xenergy
Fe Fex + X ∆G
C between
difference + ∆G mg
FeMnAl/Cthe face-centered (5)
cu-
x
bic and close-packed hexagonal
→ε phases of Fe, Mn, Al, and C alloy elements. Xx is the
In Equation (5), ∆Gγ
x is the free energy difference between
γ→ε the face-centered cubic
molar fraction of Fe, Mn, Al, and C alloy elements, and ΔGFex is the interaction param-
and close-packed hexagonal phases of Fe, Mn, Al, and C alloy elements. Xx is the molar
eter difference between Fe and Mn, Al, and C alloy elements.
→ε Here, only the interaction
fraction of Fe, Mn, Al, and C alloy elements, and ∆Gγ is the interaction parameter
between Fe and Mn is considered, and the interaction Fex between iron and other alloy ele-
difference between Fe and
γ→ε Mn, Al, and C alloy elements. Here, only the interaction between
ments is ignored. ΔGFeMnAl/C is the effect of interaction between Fe, Mn, Al, and C on
Fe and Mn is considered, and the interaction between iron and other alloy elements is
phase transition free energy.
γ→ε 1246
ΔGFeMnAl/C = [1 − exp(-24.29XC )] − 17175XMn (6)
XC

ΔGγ→ε
mg is the difference of molar magnetic free energy between the γ and ε phases.
Metals 2021, 11, 821 6 of 15

→ε
ignored. ∆Gγ FeMnAl/C is the effect of interaction between Fe, Mn, Al, and C on phase
transition free energy.

→ε 1246
∆Gγ
FeMnAl/C = [1 − exp(−24.29 XC )] − 17175XMn (6)
XC
→ε
∆Gγ
mg is the difference of molar magnetic free energy between the γ and ε phases.

γ→ε
∆Gmg = Gεm −Gγ
m (7)

In Equation (7), Gεm and Gγ

m represent the molar magnetic free energy of the ε and γ
phases, respectively.

Gεm = RT ln (βε +1)fε (τε ), Gγ γ γ γ

m = RT ln (β +1)f (τ ) (8)

1 τ−5 τ−15 τ−25

f(τ)= − ( + + ) (9)
D 10 315 1500
T T
τε = ε , τγ = γ (10)
TN TN
In Equation (10), T is the actual temperature, and TN is the temperature of the antifer-
romagnetic transition point.

Tγ
N = 250lnXMn −4750XMn XC −6.2XAl + 720(k) (11)

TεN = 580XMn (k) (12)

βγ = 0.7XFe +0.62XMn +0.64XFe XMn −4XC (13)
ε
β = 0.62XMn −4XC (14)
518 11692 1
D= + ( −1) (15)
1125 15975 P
For fcc and hcp crystal structures, P = 0.28 in Equation (15). In addition, the physical
parameters involved are shown in Table 2.

Table 2. Relevant physical parameters required to calculate SFE.

1
Physical Parameter [20] Value/(J·mol− )
→ε
∆Gγ
Fe→ε −2243.38 + 4.309T
∆Gγ
Mn −1000.00 + 1.123T
→ε
∆Gγ
C −22,166
γ→ε
∆GAl 2800 + 5T
→ε
∆Gγ
FeMn 2873 − 717(XFe − XMn )
→ε
∆Gγ
FeC 42,500
γ→ε
∆GFeAl 3339

Through the above formula and related physical parameters, the SFE value of this steel
at 25 ◦ C was 15.6 mJ/m2 , and the SFE value range at the tensile temperature of 600–1310 ◦ C
was 120.8–221 mJ/m2 . When the composition of TRIP/TWIP steel was unchanged, the SFE
value increased with the increase in temperature, which is consistent with the conclusions
of Akbari [21] and Allain et al. [17]. In addition, martensitic transformation occurred when
SFE was <18 mJ/m2 , which is beneficial to martensite-induced plasticity. When the SFE
value was 18–45 mJ/m2 , the martensitic transformation was inhibited, and the mechanical
twinning was enhanced. When the SFE value is ≥45 mJ/m2 , the dislocation slip is a single
deformation mechanism [15]. Combined with the above, the TRIP effect was the main
deformation mechanism of steel at room temperature. The dislocation slip mechanism was
dominant between 600 and 1310 ◦ C.
Metals 2021, 11, x FOR PEER REVIEW 7 of 15
Metals 2021, 11, 821 7 of 15

3.2. Tensile Strength Analysis

3.2. The effect
Tensile of deformation
Strength Analysis temperature on the tensile properties of Fe–Mn–C–Al
TWIP/TRIP steel is shown in Figure
The effect of deformation temperature 4. Figureon4athe is the trueproperties
tensile stress–strain curve in the
of Fe–Mn–C–Al
temperature range of 600–1310 °C. As can be seen from
TWIP/TRIP steel is shown in Figure 4. Figure 4a is the true stress–strain curve the curve, there was a single
in the
peak stress from 600 to 800 °C, ◦and the maximum stress was
temperature range of 600–1310 C. As can be seen from the curve, there was a single about 395 Mpa at 600peak
°C.
The stress
stress from decreased
600 to 800 ◦
sharply
C, and after
thereaching
maximum thestress
peak was value, and 395
about the specimen
Mpa at 600 ◦
wasC.frac-
The
tured.
stress Moreover, the decreasing
decreased sharply trend slowed
after reaching the peak down
value, withandthetheincrease
specimen in was
temperature.
fractured.
As can be seen
Moreover, from the curve,
the decreasing trendthere
slowedwasdown
fluctuation
with the atincrease
900 °C and a short processing
in temperature. As canri- be
gidification area on the true stress–strain curve ◦ of the subsequent
seen from the curve, there was fluctuation at 900 C and a short processing rigidification temperature. The
stress
area on increased
the truerapidly with the
stress–strain increase
curve of thein strain andtemperature.
subsequent then reachedThe the stress
maximum ten-
increased
sile stress,
rapidly which
with is the ultimate
the increase in straintensile strength
and then reached[22].the Then,
maximuma longtensile
post ultimate tensileis
stress, which
strength was tensile
the ultimate formed,strength
which [22].mightThen,
be related
a long to theultimate
post occurrence of DRX
tensile [23].was
strength Figure 4b
formed,
compares
which might the tensile strength
be related to the ofoccurrence
Fe–24.2Mn–3Al–2.6Si
of DRX [23]. TWIP steel4b
Figure and 12Cr1MoVG
compares steel
the tensile
with that of Fe–24.2Mn–3Al–2.6Si
strength the steel tested in thisTWIP study.steel
It canandbe12Cr1MoVG
seen that thesteel peak stress
with thatofofthe
thethree
steel
testeddecreased
steels in this study.
withItthecan be seeninthat
increase the peak
tensile stress of In
temperature. thethe
three steels
range decreased
of 600–850 °C,with
the
the increase in tensile ◦
tensile strength of thistemperature.
steel was betweenIn the range of 600–850
the other two steels. C, the tensile strength
However, above 850 of °C,
this
steel
the was between
tensile strengththe otherrelatively
became two steels.excellent.
However,This above 850 ◦that
proved C, the tensile strength became
Fe–15.3Mn–0.58C–2.3Al
relatively excellent.
TWIP/TRIP steel hadThis proved
better thatstrength
tensile Fe–15.3Mn–0.58C–2.3Al
than the two other TWIP/TRIP steel had
steels at high better
tempera-
tensile strength than the two other steels at high temperature.
ture.

Figure 4. (a) True stress–strain curve and (b) curve of peak stress versus temperature.
Figure 4. (a) True stress–strain curve and (b) curve of peak stress versus temperature.
3.3. Thermoplastic Analysis
3.3. Thermoplastic
Elongation at Analysis
break complicates the interpretation of the curve due to necking. Ther-
moplastic is quantified
Elongation at breakas the percentage
complicates reduction
the in the cross-sectional
interpretation of the curve area
due oftothe sample
necking.
at fracture. The
Thermoplastic cross-sectional
is quantified as thearea after fracture
percentage reduction wasinmeasured by standard
the cross-sectional areavernier
of the
caliper, and the RA of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel was calculated
sample at fracture. The cross-sectional area after fracture was measured by standard using
Equation (16). The variation trend of the RA of this steel with temperature
vernier caliper, and the RA of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel was calculated is shown by the
red curve in Figure 5. In addition, for comparison, the RA of Fe–24.2Mn–3Al–2.6Si
using Equation (16). The variation trend of the RA of this steel with temperature is and
12Cr1MoVG
shown by the were compared.
red curve in Figure 5. In addition, for comparison, the RA of Fe–24.2Mn–
A0 −Af
3Al–2.6Si and 12Cr1MoVG were compared. ϕ= ×100% (16)
A0
A0 − Af
In Equation (16), A0 and Af are φ= the cross-sectional
×100% areas of the specimen before(16) and
A0
after fracture, respectively.
In Equation (16), A0 and Af are the cross-sectional areas of the specimen before and
after fracture, respectively.
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Temperature dependence
Figure 5. Temperature dependence of
of reduction
reduction of
of area
area of
of Fe–15.3Mn–5.8C–2.3Al
Fe–15.3Mn–5.8C–2.3AlTWIP/TRIP
TWIP/TRIP steel
and Fe–24.2Mn–3Al–2.6Si
and Fe–24.2Mn–3Al–2.6Si and
and 12Cr1MoVG
12Cr1MoVG steel.
steel.

According to the the thermoplastic

thermoplastic curve curve of ofFe–15.3Mn–0.58C–2.3Al
Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP TWIP/TRIP steel,
temperature, the plasticity increased in the
with the increase in temperature, the temperature
temperature range range of of
600–900 ◦°C, C, and the RA was 71.5% at 900 900 ◦°C.C. Between
Between 1000 1000 and 1250 ◦°C,
and 1250 C, thethe medium
medium
temperature
temperature ductility
ductilitytrough
troughofofthis thissteel
steelhad
hadthe
theworst
worst plasticity
plasticity in the whole
in the whole temperature
tempera-
range at 1200 ◦ C, with RA of 47.3%. Because this experiment was carried out at a low
ture range at 1200 °C, with RA of 47.3%. Because this experiment was carried out at a
strain
low strain (1 ×(1
rate rate 10×−10 −1−1
3 s−3
s),),the
theembrittlement
embrittlementwould wouldnot notbe beserious.
serious. As As thethe temperature
temperature
continued to rise, the plasticity increased rapidly. At 1275 °C, ◦ C, the RA reached the maxi-
mum, increasing ◦ C to the
increasingto to89.4%.
89.4%.The Thehigh-temperature
high-temperature ductility
ductilitytrough
trough was from
was from 12751275 °C to
melting point. However, withwiththe the
increase in temperature of only ◦
25 25 C, i.e., at 1300 ◦ C,
the melting point. However, increase in temperature of only °C, i.e., at 1300
the
°C, thermoplastic
the thermoplastic curve appeared
curve as anas
appeared anomalous
an anomalous point.point.
Plasticity suddenly
Plasticity suddenlydeteriorated
deteri-
sharply, and a brittle fracture occurred; the RA was only 12.8%.
orated sharply, and a brittle fracture occurred; the RA was only 12.8%. Through Through in-depth analysis
of the anomalous
in-depth analysis point,
of the it was foundpoint,
anomalous that there
it waswas a large
found thatnumber
there was of Al 2 O3 , AlN,
a large numberMnO, of
and MnS(Se) inclusions at the fracture of the sample. According
Al2O3, AlN, MnO, and MnS(Se) inclusions at the fracture of the sample. According to the to the thermodynamic
calculation
thermodynamic and experimental
calculation and study in [24], it was
experimental studyfound that the
in [24], AlNfound
it was precipitated
that theinAlN
the
liquid phase, and as the heterogeneous nucleation core, MnS(Se)
precipitated in the liquid phase, and as the heterogeneous nucleation core, MnS(Se) and and other inclusions pre-
cipitated locally on
other inclusions its surface.locally
precipitated The aggregation of brittle
on its surface. The inclusions
aggregation seriously
of brittle deteriorated
inclusions
the high-temperature mechanical properties, which was
seriously deteriorated the high-temperature mechanical properties, which was thethe fundamental reason forfun-
the
significant reduction in RA. The fracture morphology observation
damental reason for the significant reduction in RA. The fracture morphology observa- in Figure 3 shows that
there
tion inwas no obvious
Figure 3 shows necking phenomenon
that there was no in the tensile
obvious specimen
necking at this temperature.
phenomenon in the tensile In
Figure 5, the RA of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel
specimen at this temperature. In Figure 5, the RA of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP in this study is compared
with that of Fe–24.2Mn–3Al–2.6Si TWIP steel in Li et al. [13] and 12Cr1MoVG steel in
steel in this study is compared with that of Fe–24.2Mn–3Al–2.6Si TWIP steel in Li et al.
Dong et al. [14] at high temperature. As can be seen, the TWIP/TRIP steel in this study
[13] and 12Cr1MoVG steel in Dong et al. [14] at high temperature. As can be seen, the
had better plasticity at high temperature. In the temperature range of 600–1310 ◦ C, the
TWIP/TRIP steel in this study had better plasticity at high temperature. In the tempera-
RA was 47.3–89.4%. According to the experimental study of several steel grades in the
ture range of 600–1310 °C, the RA was 47.3–89.4%. According to the experimental study
literature, 40% RA is the critical value of ductility trough [25]. When the reduction of area
of several steel grades in the literature, 40% RA is the critical value of ductility trough
is less than 40%, cracks will increase. No traditional ductility trough in the temperature
[25]. When the reduction of area is less than 40%, cracks will increase. No traditional
range of 600–1310 ◦ C has been measured in this steel. In this study, the relative ductility
ductility trough in the temperature range of 600–1310 °C has been measured in this steel.
trough was below 60% RA. The RA of Fe–24.2Mn–3Al–2.6Si TWIP steel and 12Cr1MoVG
In this study, the relative ductility trough was below 60% RA. The RA of Fe–24.2Mn–
steel in the same temperature range were 0–90% and 40–82%, respectively. There was an
3Al–2.6Si TWIP steel and 12Cr1MoVG steel in the same temperature range were 0–90%
obvious ductility trough below 850 ◦ C.
and 40–82%, respectively. There was an obvious ductility trough below 850 °C.
Research has shown that it is easy to generate holes and cracks on the ferrite pre-
Research
cipitated on the has shown that
austenite grain it boundary,
is easy to generate
which isholes and cracks
the possible on the
reason for ferrite precip-
intergranular
itated on the austenite grain boundary, which is the possible
fracture. The Thermo-Calc thermodynamic calculation of this steel (see Section 3.6) showed reason for intergranular
Metals 2021, 11, 821 9 of 15

a small amount of ferrite was precipitated on austenite between 600 and 700 ◦ C, resulting in
the decrease in RA from 65.7 to 55.9%. However, ferrite was found in Fe–24.2Mn–3Al–2.6Si
TWIP steel at 850 ◦ C. Therefore, the decrease in ferrite transformation temperature caused
the low-temperature ductility trough to shift to the low-temperature section. The small
amount of ferrite precipitation meant there was only a slight effect on the RA. In addition,
it was found that the high-temperature ductility trough of the steel in this study was
obviously shifted to the high-temperature zone compared to the other two steels. Zero duc-
tility temperature (ZDT) and zero strength temperature (ZST) were estimated at about
1330 ◦ C. In summary, the Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel had comparatively
good plasticity in the whole tensile temperature range.

3.4. Fracture Morphology

The fracture of Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel at different temperatures
was observed by Quanta FEG 250 and Zeiss-Utra55 field emission scanning electron mi-
croscopy, as shown in Figure 6. The red box in the lower left corner is a local zoom of
the area referred to by the blue arrow. When the test temperature was 600 ◦ C, as shown
in Figure 6a, there were a large number of small-sized circular or elliptical dimples, but
large-sized dimples, which belong to intergranular dimple fracture, were rare. With the
increase in temperature, the dimple size increased, and some large and deep equiaxed
dimples appeared. In addition, there were many small dimples around the large dimples.
As can be seen from Figure 6b,c, with smaller inclusions, there were second-phase par-
ticles or micropores between the large dimples [26]. As plastic deformation continued,
the connection between large dimples could be carried out through secondary dimples.
MnS(Se) + MnO + Al2 O3 + AlN composite inclusions were observed near the wedge cracks.
Figure 6d clearly shows the morphology characteristics of the above small dimples and the
MnS (Se) + MnO inclusions in the concave dimples. There were many typical dimples with
small size, shallow depth, and tearing ridge. In addition, there were some large dimples
with a diameter of about 400 µm at 900 ◦ C. As the dimple diameter increased, the deeper
the depth, the better was the plasticity. This was consistent with the phenomenon of the RA
increasing from 55.9 to 71.5% in the temperature range of 600–900 ◦ C, as shown in Figure 5.
From Figure 6f, it can be observed that the number of dimples decreased at 1100 ◦ C. The
fracture was smooth, there was no characteristic small plane, and a large number of wedge
cracks appeared. This is the intergranular debonding phenomenon caused by slip due
to the weakening of grain boundary strength during the tensile process [27,28], which
belongs to intergranular brittle fracture. As Mejía et al. [29] reported, local cracking is
a natural result of inhomogeneous plastic deformation. At the temperature of 1200 ◦ C,
no dimples were found in the whole fracture field. As shown in Figure 6g, the structure
between the dendrites was in a layered state after tearing and breaking. With the increase
in temperature, the plasticity reached the best value at 1275 ◦ C, as shown in Figure 6h,i,
and the fracture was cup–cone. Strong plastic deformation occurred in the unfractured
area, which gradually formed a cavity. MnS (Se) inclusions were observed near the dimples.
In addition, it was also found that there was a hunting slip pattern on the inner wall of the
larger dimple. This is because when the dimple surface is perpendicular to the principal
stress direction, new slip occurs on the surface of the dimple under the action of stress.
The primary slip trace was sharp. With the continuous slip, it developed smoothly into a
hunting pattern and further flattened, which is a typical ductile fracture feature.
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Figure
Figure 6.
6. Fracture
Fracture morphology
morphologyof ofsamples
samplesatatdifferent
differenttest
testtemperatures.
temperatures.(a)(a)
600 °C;◦ C;
600 (b,c) 700700
(b,c) °C;◦ C;
(d)(d)
800800
°C;◦ (e) 900900
C; (e) °C;◦(f)
C;
1100 °C;◦(g) 1200 °C;◦(h,i) 1275 °C. ◦
(f) 1100 C; (g) 1200 C; (h,i) 1275 C.

3.5.
3.5. Microstructure
Microstructure
Figure
Figure 77 shows
shows the the microstructure
microstructure of of the
the samples
samples with with different
different tensile
tensile temperatures
temperatures
and
and without tensile at room temperature. The stretching direction has been
without tensile at room temperature. The stretching direction has been marked
marked by by aa
white arrow. Figure 7a is the microstructure of the sample at
white arrow. Figure 7a is the microstructure of the sample at 25 C, where a large number 25 °C,
◦ where a large number
of
of isometric austenite grains
isometric austenite grainscan canbebeobserved.
observed.Figure Figure7b–f 7b–f is is a picture
a picture of of
thethe microstruc-
microstructure
ture around the fracture at different tensile temperatures. Figure
around the fracture at different tensile temperatures. Figure 7c is a microstructure about 7c is a microstructure
about
5 mm 5away mm from awaythe from the fracture
fracture at Compared
at 700 ◦ C. 700 °C. Compared with Figure with7b,Figure
it can 7b, it can be that
be observed ob-
served that the number of cracks and voids at the trifurcate
the number of cracks and voids at the trifurcate grain boundary was significantly reduced, grain boundary was signifi-
cantly
and thereduced,
austeniteand grain thewas austenite grain was
not elongated. not cavities
Large elongated. were Large cavities
initially formed were initially
at the early
formed at the early stage of deformation due to grain boundary
stage of deformation due to grain boundary sliding. Grain boundary sliding is the main sliding. Grain boundary
sliding
fractureismechanism
the main fracture mechanism at
at this temperature. this when
Then, temperature.
the crack Then, when the
propagates, crack prop-
it distorts into
agates,
slenderitcavity
distortsuntilinto slenderfails
it finally cavity untilDislocation
[23,30]. it finally fails [23,30].
pile-up canDislocation
be easily formed pile-up at can
the
be easily
triple lineformed
boundary, at the triple line
resulting boundary,
in stress resultingand
concentration, in stress
tensileconcentration,
microcracks can andbetensile
easily
microcracks
generated. With can the
be extension,
easily generated. With thecontinue
the microcracks extension, the microcracks
to expand and connect continue
with each to
expand and connect with each other, resulting in the fracture
other, resulting in the fracture of the sample. At 1200 and 1250 C, an obvious dendritic of ◦the sample. At 1200 and
1250 °C, an
structure wasobvious
observed dendritic
near the structure
fracture. was observedwith
Combined nearthe theobservation
fracture. Combined
in Figurewith 6f,g,
the observation
it was found that in Figure
in this 6f,g, it was found
temperature range, thatsomein this temperature
fracture surfacesrange,had thesome fracture
re-melting
surfaces
phenomenon. had the Thisre-melting
might have phenomenon.
been due toThis might haveofbeen
the segregation P, S,due
and to the elements
other segregation on
theP,grain
of S, and boundary, which reduced
other elements the melting
on the grain boundary, pointwhich
of thereduced
grain boundary
the melting and point
was theof
main
the factor
grain leading toand
boundary thewas occurrence
the main of afactor
dendritic structure.
leading to theThe thermoplasticity
occurrence in this
of a dendritic
temperature
structure. Therange was reduced,inand
thermoplasticity thisthe RA, shown range
temperature in Figure was5,reduced,
was also and significantly
the RA,
shown in Figure 5, was also significantly reduced. A large number of intergranular
Metals 2021, 11, 821 11 of 15
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reduced.
cracks andAmicropores
large number of intergranular
were formed near thecracks and micropores
fracture surface and were formed
existed nearden-
between the
fracture surface and existed between dendrites, which meant that cracks could
drites, which meant that cracks could easily occur and propagate along the dendrite easily occur
and propagate
boundary. When along
the the dendrite are
micropores boundary.
seriousWhen
enough,thethe
micropores
cracks arequickly
can seriousconnect
enough,and
the
cracks can quickly connect and fracture. Especially at 1200 ◦ C, there were a large number
fracture. Especially at 1200 °C, there were a large number of micropores, which led to
of micropores, which led to the occurrence of brittle fracture and a decrease of section
the occurrence of brittle fracture and a decrease of section shrinkage. When the temper-
shrinkage. When the temperature reached 1275 ◦ C, there were subgrain boundaries in
ature reached 1275 °C, there were subgrain boundaries in some slender grains near the
some slender grains near the fracture front, which might be partially related to dynamic
fracture front, which might be partially related to dynamic recovery and dynamic re-
recovery and dynamic recrystallization. The decrease in grain size could be attributed
crystallization. The decrease in grain size could be attributed to continuous DRX caused
to continuous DRX caused by dislocation accumulation [31]. Some grain sizes increase
by dislocation accumulation [31]. Some grain sizes increase because the essence of ther-
because the essence of thermally activated process is thermal activation [32]. Under high
mally activated process is thermal activation [32]. Under high temperature tensile pro-
temperature tensile process and low strain rate, the ability of thermal activation is strong. It
cess and low strain rate, the ability of thermal activation is strong. It is easy to overcome
is easy to overcome energy barriers, and grain boundary migration can easily occur, which
energy barriers, and grain boundary migration can easily occur, which promotes the nu-
promotes the nucleation and growth of DRX [33]. This is also the main reason for the high
cleation and growth of DRX [33]. This is also the main reason for the high section
section shrinkage in this temperature range.
shrinkage in this temperature range.

Figure 7. Microstructure morphology near the high-temperature tensile fracture. (a) 25 °C; (b–c) 700 °C; (d) 1200 °C; (e)
Figure 7. Microstructure morphology near the high-temperature tensile fracture. (a) 25 ◦ C; (b,c) 700 ◦ C; (d) 1200 ◦ C;
1250 °C; (f) 1275 °C.
(e) 1250 ◦ C; (f) 1275 ◦ C.

3.6.
3.6. Phase
Phase Transition Process and
Transition Process and EBSD
EBSD Analysis
Analysis
The phase change
The phase changeprocess
processofof thethe steel
steel waswas calculated
calculated by Thermo-Calc
by Thermo-Calc thermody-
thermodynamic
namic software. It should be noted that in order to be rigorous,
software. It should be noted that in order to be rigorous, sulfur, oxygen, and nitrogen sulfur, oxygen, and ni-
trogen elements with relatively low content should be considered
elements with relatively low content should be considered in the calculation process. in the calculation pro-
cess. According to the thermodynamic calculation, as shown
According to the thermodynamic calculation, as shown in Figure 8a, there was no single in Figure 8a, there was no
single austenite structure in the whole tensile temperature range.
austenite structure in the whole tensile temperature range. The main phases were austenite The main phases were
austenite
face-centered face-centered
cubic phase, cubic
MnS,phase,
AlN,MnS, and AlAlN, and Al2O3. It can be observed from Fig-
2 O3 . It can be observed from Figure 8b that
ure 8b that austenite began to appear
◦
austenite began to appear at 1429.3 C. Among them, at 1429.3 °C.AlN
Among them,
(1458.9 AlNAl(1458.9
◦ C) and °C) and
2 O3 (2029.8 C)
◦
Al O (2029.8 °C) were formed at a temperature higher than their
were formed at a temperature higher than their liquidus, and the solidus was 1343.1 C. The
2 3 liquidus, and the
◦ soli-
dus was 1343.1
formation °C. The of
temperature formation
MnS was temperature of MnSwas
1328.1 ◦ C, which wasslightly
1328.1 lower
°C, which
thanwas slightly
the solidus.
lower
The results showed that AlN and Al2 O3 began to form in liquid high manganeseliquid
than the solidus. The results showed that AlN and Al 2 O 3 began to form in steel.
high
With the manganese steel.process,
solidification With the solidification
inclusions gradually process,
increasedinclusions gradually
and eventually increased
tended to be
and eventually
stable. AlN tendedtended to stable
to be be stable.
at about 1000 ◦ Ctowith
AlN tended be stable
a molar at fraction
about 1000 °C ×
of 4.2 10−a4 .mo-
with As
lar
shownfraction of 4.28a,
in Figure × there
10 . As
−4
wasshown
a smallinamount
Figure of 8a,ferrite
there body-centered
was a small amount of ferrite
cubic phase and
body-centered
cementite between cubic600phase
and 700 and◦ C,
cementite between 600
with the cementite and 700
generated ◦ C. It
°C, with
at 665.3 the cementite
disappeared
generated at 665.3 °C. It disappeared quickly ◦
when the temperature
quickly when the temperature dropped to 621.7 C. Thus, the presence of cementite dropped to 621.7
had °C.
no
Thus,
effect onthethepresence
tensile of cementite in
temperature had theno effect on the tensile temperature in the experi-
experiment.
ment.
 Metals2021,
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Figure 8. Predicted phase change behavior of steel by Thermo-Calc thermodynamic calculation. (a) 600–1300 ◦ C;
Figure 8. Predicted
(b) 1425–1460 ◦ C. phase change behavior of steel by Thermo-Calc thermodynamic calculation. (a) 600–1300 °C; (b)
1425–1460 °C.
It was found that large deformation increased dislocation density and increased the
It was
driving found
force that large deformation
of transformation increased
from austenite dislocation
to ferrite. density and increased
The thermodynamic the
calculation,
driving
shown force
in the of transformation
diagram above, showedfrom that
austenite
a ferriteto body-centered
ferrite. The thermodynamic
cubic phase appearedcalcula-at
646 ◦shown
tion, C and in a small amount above,
the diagram of ferrite precipitated,
showed that a which
ferrite softened the austenite.
body-centered However,
cubic phase ap-
due toatthe low ◦C
peared 646 °Cformation
and a small temperature
amount of and lowprecipitated,
ferrite content of ferrite,
which the RA atthe
softened 600–700
austen-
was
ite. less affected
However, due to andthethe
lowcurve decreased
formation gently, asand
temperature shown in Figure
low content of5.ferrite,
Compared
the RAwith
at
Fe–24Mn–2.6Si–3Al
600–700 °C was less steel, affectedthe and
liquidus temperature
the curve decreased of this steel as
gently, was increased
shown by about
in Figure 5.
100 ◦ C, which
Compared withwould greatly improve
Fe–24Mn–2.6Si–3Al thethe
steel, temperature of the high-temperature
liquidus temperature of this steel ductility
was in-
trough and
creased by delay
about the 100embrittlement
°C, which would caused by the liquid
greatly improvefilm atthe
the temperature
crystal interface of [34].
the
Oxford Nordlys Max3 EBSD was used for surface scan,
high-temperature ductility trough and delay the embrittlement caused by the liquid film and the scan results were
atanalyzed
the crystal byinterface
local misorientation.
[34]. The dislocation density is very high in the deformed
grains produced
Oxford Nordlys by high-temperature
Max3 EBSD was used stretching. Thesescan,
for surface dislocations
and the arescanarranged in the
results were
dislocation
analyzed structure,
by local resulting inThe
misorientation. different degrees
dislocation of local
density misorientation
is very high in the [35]. Local
deformed
misorientation can be used to study the orientation change
grains produced by high-temperature stretching. These dislocations are arranged in the within grains during plastic
deformation
dislocation so as to measure
structure, resultingthe in relative
differentsize of dislocation
degrees of local density in deformed
misorientation [35]. metals.
Local
The higher the whole dislocation density, the larger is the average
misorientation can be used to study the orientation change within grains during plastic local misorientation [36].
Figure 9a,b shows the grain boundary distribution and local
deformation so as to measure the relative size of dislocation density in deformed metals. orientation difference distri-
bution as characterized by EBSD density,
at 1200 and ◦
The higher the whole dislocation the 1275
largerC. is The
the orientation
average local deviation near the
misorientation
fracture is also shown. In the color scale, yellow-green color represents
[36]. Figure 9a,b shows the grain boundary distribution and local orientation◦ difference a large orientational
angle. Although
distribution the upper threshold
as characterized by EBSD of at local
1200 misorientation
and 1275 wasorientation
°C. The set to 5.0 , deviation
the actual
local misorientation was mostly concentrated below 2.0 ◦ . It can be seen intuitively that at
near the fracture is also shown. In the color scale, yellow-green color represents a large
1200 ◦ C, most
orientational areasAlthough
angle. are blue areas with small
the upper local of
threshold misorientation. Only a small
local misorientation was setnumber
to 5.0°,of
green regions with large local misorientation are distributed on the grain boundaries of
the actual local misorientation ◦was mostly concentrated below 2.0°. It can be seen intui-
subgrains. In contrast, at 1275 C, the yellow-green region accounts for most of the area. It
tively that at 1200 °C, most areas are blue areas with small local misorientation. Only a
is mostly located in the grain interior, and a small amount is located in the grain bound-
small number of green regions with large local misorientation are distributed on the
ary. This indicates that when the temperature increased from 1200 to 1275 ◦ C, the grain
grain boundaries of subgrains. In contrast, at 1275 °C, the yellow-green region accounts
orientation deviation angle increased compared with the grain boundary. The deformation
for most of the area. It is mostly located in the grain interior, and a small amount is lo-
occurred in most areas of the grain, and the deformation was large. The defect density
cated in the grain boundary. This indicates that when the temperature increased from
increased and the internal stress increased, resulting in a large number of dislocations.
1200 to 1275 °C, the grain orientation deviation angle increased compared with the grain
The dislocation density was high, and the speed of dislocation disappearance was also
boundary. The deformation occurred in most areas of the grain, and the deformation
accelerated. This further indicates that the dislocation slip mechanism was dominant.
was large. The defect density increased and the internal stress increased, resulting in a
large number of dislocations. The dislocation density was high, and the speed of dislo-
cation disappearance was also accelerated. This further indicates that the dislocation slip
mechanism was dominant.
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Metals 2021, 11, 821 13 of 15

Figure 9. EBSDanalysis
9. EBSD analysis near
near tensile
tensile fracture
fracture at
at 1200
1200 and
and 1275 ◦ C. (a) 1200 ◦ C; (b) 1275 ◦ C.
1275 °C.
Figure (a) 1200 °C; (b) 1275 °C.
4. Conclusions
4. Conclusions
(1) The Fe–15.3Mn–0.58C–2.3Al TWIP/TRIP steel studied in this work had a good
(1)temperature
plastic The Fe–15.3Mn–0.58C–2.3Al
range (600–1310 ◦TWIP/TRIP
C). Compared steel studied
with in this work
the traditional had atrough
ductility good
plastic
(RA of temperature
less than 40%), range
there(600–1310 °C). Compared
was no traditional with
ductility the traditional
trough ductility
in this steel. Taking trough
the RA
(RA of less than 40%), there was no traditional ductility trough in
of 60% as the relative ductility trough, the high-temperature ductility trough (from this steel. Taking
1275the◦C
RA of 60% as the relative ductility trough, the high-temperature ductility
to the melting point) shifted to the high-temperature range due to the high temperature of trough (from
1275 °C toline.
the solid the The
melting point) shifted to the
medium-temperature high-temperature
ductility trough wasrange between due1000
to the
andhigh
1250tem-
◦ C.
perature
Due to the of low
the precipitation
solid line. The medium-temperature
temperature ductility
and low content troughthe
of ferrite, was between 1000
low-temperature
and 1250trough
ductility °C. Due to the
shifted to low precipitation temperature
the low-temperature and low
range and existed in content of ferrite,
the temperature the
range
near 600 ◦ C.
low-temperature ductility trough shifted to the low-temperature range and existed in the
temperature range to
(2) According near
the600 °C.
thermodynamic calculation of SFE, the SFE value of this steel was
2
According ◦
15.6 mJ/m at 25 C, which belongs to lowcalculation
(2) to the thermodynamic SFE metal, of SFE,
and the aSFE
it had value of this
TWIP/TRIP steel
effect. In
was 15.6 mJ/m
the tested 2
tensileat temperature
25 °C, whichrange
belongs(600–1310 ◦
to low SFE C),metal, and
the SFE it had
value was a TWIP/TRIP
120.8–221 mJ/meffect.2 .
In
A the tested
higher SFEtensile temperature
will make range (600–1310
the dislocation slip become°C),the
thedominant
SFE valuemechanism
was 120.8–221 mJ/m2.
of thermal
deformation in the high-temperature tensile process.
Metals 2021, 11, 821 14 of 15

(3) When the local misorientation in grains was large, the dislocation density increased
and the dislocation disappearance rate accelerated. Moreover, the hindering effect of DRX
on crack propagation was the main reason for good plasticity in the temperature range
of 1250–1285 ◦ C. Through OM and EBSD observation at 1200 ◦ C, it was found that the
rapid connection of many micropores near the fracture under tensile stress was the main
factor for the brittle fracture at this temperature. In addition, the aggregation of Al2 O3 ,
AlN, MnO, and MnS (Se) inclusions reduced the thermoplasticity and the RA, which was
the fundamental factor affecting the high-temperature mechanical properties of this steel.

Author Contributions: Conceptualization, G.Y. and C.Z.; methodology, G.Y., C.Z. and C.L.; software,
G.Y., C.Z., F.L. and H.Y.; writing—original draft preparation, G.Y. and C.Z.; writing—review and
editing, G.Y. and C.Z.; funding acquisition, C.L. and C.Z. All authors have read and agreed to the
published version of the manuscript.
Funding: This project is financially supported by the “National Science Foundation of China with the
grant numbers 51704083 and 51864013”, Guizhou Science and Technology Plan Project ([2017]5788,
[2018]1026, [2019]1115, and [2019]2163), Education Department Foundation of Guizhou Province
(No. [2017]118), Guizhou Science Cooperation platform talents [2018] 5781 subsidy, and Research
Foundation for Talents of Guizhou University (No. 201628).
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

References
1. Asghari, A.; Zarei-Hanzaki, A.; Eskandari, M. Temperature dependence of plastic deformation mechanisms in a modified
transformation-twinning induced plasticity steel. Mater. Sci. Eng. A 2013, 579, 150–156. [CrossRef]
2. De Cooman, B.C.; Estrin, Y.; Kim, S.K. Twinning-induced plasticity (TWIP) steels. Acta Mater. 2018, 142, 283–362. [CrossRef]
3. Krüger, L.; Meyer, L.W.; Brux, U.; Frommeyer, G.; Grässel, O. Stress-deformation behaviour of high manganese (AI, Si) TRIP and
TWIP steels. J. Physi. IV 2003, 110, 189–194. [CrossRef]
4. Jin, J.E.; Lee, Y.K. Effects of Al on microstructure and tensile properties of C-bearing high Mn TWIP steel. Acta Mater. 2012, 60,
1680–1688. [CrossRef]
5. Frommeyer, G.; Brüx, U.; Neumann, P. Supra-Ductile and High-Strength Manganese-TRIP/TWIP Steels for High Energy
Absorption Purposes. ISIJ Int. 2003, 43, 438–446. [CrossRef]
6. Lee, S.; Estrin, Y.; Cooman, B. Effect of the Strain Rate on the TRIP-TWIP Transition in Austenitic Fe-12 pct Mn-0.6 pct C TWIP
Steel. Metall. Mater. Trans. A 2014, 45, 717–730. [CrossRef]
7. Franceschi, M.; Pezzato, L.; Gennari, C.; Fabrizi, A.; Polyakova, M.; Konstantinov, D.; Brunelli, K.; Dabalà, M. Effect of Intercritical
Annealing and Austempering on the Microstructure and Mechanical Properties of a High Silicon Manganese Steel. Metals 2020,
10, 1448. [CrossRef]
8. Zhou, N.; Song, R.; Li, X.; Li, J. Dependence of austenite stability and deformation behavior on tempering time in an ultrahigh
strength medium Mn TRIP steel. Mater. Sci. Eng. A 2018, 738, 153–162. [CrossRef]
9. Mou, Y.; Li, Z.; Zhang, X.; Misra, D.; He, L.; Li, H. Design of an Effective Heat Treatment Involving Intercritical Hardening for
High Strength/High Elongation of 0.2C-3Al-(6-8.5)Mn-Fe TRIP Steels: Microstructural Evolution and Deformation Behavior.
Metals 2019, 9, 1275. [CrossRef]
10. Lan, P.; Tang, H.; Zhang, J. Hot ductility of high alloy Fe–Mn–C austenite TWIP steel. Mater. Sci. Eng. A 2016, 660, 127–138.
[CrossRef]
11. De Barbieri, F.; Castro Cerda, F.; Pérez-Ipiña, J.; Artigas, A.; Monsalve, A. Temperature Dependence of the Microstructure and
Mechanical Properties of a Twinning-Induced Plasticity Steel. Metals 2018, 8, 262. [CrossRef]
12. Koyama, M.; Sawaguchi, T.; Tsuzaki, K. TWIP Effect and Plastic Instability Condition in an Fe–Mn–C Austenitic Steel. ISIJ Int.
2013, 53, 323–329. [CrossRef]
13. Li, S.; Liu, J.; Liu, H.; Zhuang, C.; Liu, J.; Han, Z. Study on High-Temperature Mechanical Properties of Low-Carbon Fe-Mn-Si-Al
TWIP Steel. High Temp. Mater. Process. 2017, 36, 505–513. [CrossRef]
14. Dong, K.; Liu, J.; Zhang, P.; Zheng, G.; Li, Y.; He, Y. Research on Elevated Temperature Mechanical Properties of 12Cr1MoVG
Steel Continuous Casting Billet. Iron Steel Vanadium Titan. 2020, 41, 124–129.
15. Curtze, S.; Kuokkala, V.T. Dependence of tensile deformation behavior of TWIP steels on stacking fault energy, temperature and
strain rate. Acta Mater. 2010, 58, 5129–5141. [CrossRef]
Metals 2021, 11, 821 15 of 15

16. Olson, G.B.; Cohen, M. A general mechanism of martensitic nucleation: Part I. General concepts and the FCC→HCP transforma-
tion. Metall. Mater. Trans. A 1976, 7, 1897–1904.
17. Allain, S.; Chateau, J.-P.; Bouaziz, O.; Migot, S.; Guelton, N. Correlations between the calculated stacking fault energy and the
plasticity mechanisms in Fe–Mn–C alloys. Mater. Sci. Eng. A 2004, 387–389, 158–162. [CrossRef]
18. Tian, X. Effect of Aluminium, Chromium and Silicon on the Lattice Parameter for Fe-Mn-C Austenite. Chin. J. Mater. Res. 1991, 25,
48–51.
19. García de Andrés, C.; García Caballero, F.; Capdevila, C.; Bhadeshia, H.K. Modelling of kinetics and dilatometric behavior of
non-isothermal pearlite-to-austenite transformation in an eutectoid steel. Scr. Mater. 1998, 39, 791–796. [CrossRef]
20. Dumay, A.; Chateau, J.-P.; Allain, S.; Migot, S.; Bouaziz, O. Influence of addition elements on the stacking-fault energy and
mechanical properties of an austenitic Fe–Mn–C steel. Mater. Sci. Eng. A 2008, 483–484, 184–187. [CrossRef]
21. Saeed-Akbari, A.; Imlau, J.; Prahl, U.; Bleck, W. Derivation and Variation in Composition-Dependent Stacking Fault Energy Maps
Based on Subregular Solution Model in High-Manganese Steels. Metall. Mater. Trans. A 2009, 40, 3076–3090. [CrossRef]
22. Salas-Reyes, A.E.; Mejía, I.; Bedolla-Jacuinde, A.; Boulaajaj, A.; Calvo, J.; Cabrera, J.M. Hot ductility behavior of high-Mn austenitic
Fe-22Mn-1.5Al-1.5Si-0.45C TWIP steels microalloyed with Ti and V. Mater. Sci. Eng. A 2014, 611, 77–89. [CrossRef]
23. Crowther, D.N.; Mintz, B. Influence of grain size and precipitation on hot ductility of microalloyed steels. Mater. Sci. Technol.
1986, 2, 1099. [CrossRef]
24. Lan, F.; Du, W.; Zhuang, C.; Li, C. Effect of Niobium on Inclusions in Fe-Mn-C-Al Twinning-Induced Plasticity Steel. Metals 2021,
11, 83. [CrossRef]
25. Mintz, B. The Influence of Composition on the Hot Ductility of Steels and to the Problem of Transverse Cracking. ISIJ Int. 1999,
39, 833–855. [CrossRef]
26. Hamada, A.S.; Karjalainen, L.P. Hot ductility behaviour of high-Mn TWIP steels. Mater. Sci. Eng. A 2011, 528, 1819–1827.
[CrossRef]
27. Carpenter, K.R.; Dippenaar, R.; Killmore, C.R. Hot Ductility of Nb- and Ti-Bearing Microalloyed Steels and the Influence of
Thermal History. Metall. Mater. Trans. A 2009, 40, 573–580. [CrossRef]
28. Abushosha, R.; Vipond, R.; Mintz, B. Influence of sulphur and niobium on hot ductility of as cast steels. Metal. Sci. J. 1991, 7,
1101–1107. [CrossRef]
29. Mejía, I.; Altamirano, G.; Bedolla-Jacuinde, A.; Cabrera, J.M. Effect of Boron on the Hot Ductility Behavior of a Low Carbon
Advanced Ultra-High Strength Steel (A-UHSS). Metall. Mater. Trans. 2013, 44, 5165–5176. [CrossRef]
30. Zhang, S.; Kim, D.-U.; Jiang, W.; Tonk, M.R. A phase field model of crack propagation in anisotropic brittle materials with
preferred fracture planes. Comput. Mater. Sci. 2021, 193, 110400. [CrossRef]
31. Liu, X.; Ye, L.; Tang, J.; Shan, Z.; Ke, B.; Dong, Y.; Chen, J. Superplastic deformation mechanisms of an Al–Mg–Li alloy with
banded microstructures. Mater. Sci. Eng. A 2021, 805, 140545. [CrossRef]
32. Yang, S.; Shen, J.; Chen, L.; Li, X. Dynamic evolution of microstructure of Al-Cu-Li alloy during hot deformation. Trans. Nonferrous
Met. Soc. China 2019, 29, 674–683.
33. Khosravifard, A.; Hamada, A.; Moshksar, M.; Ebrahimi, R.; Porter, D.; Karjalainen, L. High temperature deformation behavior of
two as-cast high-manganese TWIP steels. Mater. Sci. Eng. A 2013, 582, 15–21. [CrossRef]
34. Yang, Z.; Zhao, Y.; Wang, R.; Che, Y.; Ma, Y.; Chen, Q. Formation of Ultra-Fine Ferrite Grains in Low Carbon Steels Through low
Temperature Heavy Deformation. Acta Metall. Sin. 2000, 36, 1061–1066.
35. Salas-Reyes, A.E.; Mejía, I.; Cabrera, J.M. Microstructure and Crystallographic Texture Development of Microalloyed Twinning
Induced Plasticity (TWIP) Steels Under Uniaxial Hot-Tensile Conditions. MRS Proc. 2015, 1765, 103–108. [CrossRef]
36. Meng, Y.; Ren, Q.; Ju, X.H. Evaluation of dislocation density by local grain misorientation in deformed metals. Trans. Mater. Heat
Treat. 2014, 35, 122–128.