metals

Article
A 4340 Steel with Superior Strength and Toughness Achieved
by Heterostructure via Intercritical Quenching and Tempering
Yi Sang 1 , Guosheng Sun 2, * and Jizi Liu 2,3, *

1 Nanjing Metro Operation Co., Ltd., Nanjing 211135, China; [email protected]

2 Nano and Heterogeneous Materials Center, School of Materials Science and Engineering, Nanjing University
of Science and Technology, Nanjing 210094, China
3 Materials Analysis and Test Center, Nanjing University of Science and Technology, Nanjing 210094, China
* Correspondence: [email protected] (G.S.); [email protected] (J.L.)

Abstract: The conventional 4340 steel was used after quenching and tempering, strengthened by the
classical pearlitic structure where cementite particles are dispersed through the ferrite matrix. In the
present study, a heterostructure microstructure consisting of micro-sized residual ferrite zones and
pearlitic zones was introduced by an optimized process of intercritical quenching and tempering,
resulting in a steel with higher strength and better toughness. The pearlite steel has a tensile strength
of 1233 MPa, yield strength of 1156 MPa, and toughness of 121.5 MJ/m3 . Compared with the pearlite
steel, the tensile strength and yield strength of the heterostructure steel have been improved by
67 MPa and 74 MPa, respectively, while the toughness has been increased by 52.5 MJ/m3 . In this
heterostructure, the micro-sized ferrite bulks serve as the soft zones surrounded by the hard zones of
the pearlite structure to achieve a remarkable work-hardening capacity. Statistical analysis shows that
the heterostructure has the best hetero-deformation-induced (HDI) hardening capability when the
residual ferrite bulk contributes ~31% by volume fraction, and the quenching temperature is around
780 ◦ C. This study opens new ways of thinking about the strengthening and toughening mechanism
of heat treatment of medium carbon steels.

Keywords: 4340 steel; heterogenous microstructure; intercritical quenching; HDI hardening;

Citation: Sang, Y.; Sun, G.; Liu, J. A strengthening mechanism
4340 Steel with Superior Strength and
Toughness Achieved by
Heterostructure via Intercritical
Quenching and Tempering. Metals 1. Introduction
2023, 13, 1139. https://doi.org/
As a high-quality quenched and tempered steel, 4340 alloys have been widely used in
10.3390/met13061139
various industrial applications such as aircraft landing gear, harmonic reducer flexsplines,
Academic Editor: Igor Yu. and transmission shafts, due to its favorable combination of strength and toughness [1–3].
Litovchenko These mechanical components, which are subjected to high pressure and adverse alter-
nating loads, usually operate in harsh environments where superior overall performance
Received: 29 May 2023
Revised: 13 June 2023
is expected. The 4340 low-alloy steels are alloyed with Cr, Ni, Mo, and Mn elements, to
Accepted: 17 June 2023
provide good hardenability and fatigue resistance [4,5]. The addition of Cr, Ni, and other
Published: 19 June 2023
elements can improve the hardenability of the alloy and improve the strength and tough-
ness of ferrite in the microstructure, while Mo and Cr elements can promote the formation
of carbide, inhibit the growth of austenite grains and prevent tempering brittleness.
Before quenching, this steel is usually normalized to completely dissolve all carbon
Copyright: © 2023 by the authors. and other alloying elements. Traditionally, austenitizing, by heating the steels to a tem-
Licensee MDPI, Basel, Switzerland. perature above the Ac3 point, is designed to obtain a fully austenitic structure at a high
This article is an open access article temperature. The austenitized steel is cooled quickly, such as by quenching in water or
distributed under the terms and an oil bath, and the dissolved carbon does not have enough time to diffuse out of the
conditions of the Creative Commons lattice despite lattice transformation, so the carbon element remains forcibly dissolved in
Attribution (CC BY) license (https://
the forming ferrite lattice, forming a tetragonally expanded lattice structure called marten-
creativecommons.org/licenses/by/
site. During the subsequent tempering process, the diffusion and redistribution cause the
4.0/).

Metals 2023, 13, 1139. https://doi.org/10.3390/met13061139 https://www.mdpi.com/journal/metals

Metals 2023, 13, 1139 2 of 11

quenched martensite to gradually decompose into cementite and/or carbide embedded

in the ferrite matrix, resulting in various combinations of strength and toughness. The
trade-off between strength and toughness depended on the morphology, size, distribution,
and composition of the embedded cementite (or carbide) and was achieved by tuning the
tempering temperature and holding time [1,6]. However, a compromise between material
properties is becoming an urgent need due to the booming industries, and it is imperative
to make a breakthrough in the traditional quenching and tempering treatment process, so
as to establish a new strengthening–toughening mechanism.
A strategy of structural heterostructuring is an emerging trend to develop new metallic
materials with superior performance that cannot be achieved by manipulating atomic or
phase composition in homogeneous counterparts [7–9]. Heterostructured metallic materials
consist of heterogeneous zones with dramatic variations in mechanical properties [10,11],
such as dual-phase steel, which consists of an island of strong martensite second phase in a
soft ferrite matrix. During plastic deformation, the plastic deformation of the soft zones is
constrained by the elastic strain of the hard zones, generating back stress in the soft zones
and forward stress in the hard zones. Back stress is a long-range internal stress generated by
geometrically necessary dislocations (GNDs), sometimes in the form of dislocation pileups.
Forward stress is generated in the hard zone to counterbalance the stress concentration at
the zone boundary caused by back stress. This interactive force causes hetero-deformation-
induced (HDI) strengthening (a kinematic stress), which increases the yield strength and
enhances strain hardening, helping to maintain the ductility [9]. At the early stage of
elastoplastic deformation before global yielding, the hard zones remain elastic and back
stress plays a dominant role in enhancing the global yield strength in heterostructured
materials [11]. The beneficial effects of the HDI strengthening have been reported to break
the strength–toughness trade-off in pure metals [12], dual-phase alloys [13], austenitic
stainless steels [14–16], high-entropy alloys [17], and so on.
The newly reported advanced strengthening and toughening mechanisms in steels
are mainly for austenite containers, such as twinning or transformation-induced plasticity
steel and dual-phase steel, based on the high work-hardening rate of FCC austenite [18–21].
In 4340 steels, austenite is stable at a high holding temperature, but nothing remains after
quenching, due to a lack of sufficient austenite-stabilizing elements. Here, the intercritical
quenching treatment [22] was employed to introduce bulk ferrite phase into tempered
pearlite, creating a topography of heterogeneous microstructure, which is different from
the conventional dual-phase steel. So far, the HDI strengthening effect in the above het-
erostructured steel has not been reported. This study focuses on this issue and investigates
the relationship between quenching temperature and microstructure property. In addition,
the contribution of the HDI strengthening and hardening effect to the improved mechanical
properties was evaluated.

2. Materials and Methods

The chemical composition of experimental steel contains Fe-0.40C-0.22Si-0.65Mn-
0.76Cr-1.35Ni-0.19Mo (wt.%). In order to achieve the above-mentioned objectives, the
experimental steels are processed in three basic steps, including normalized annealing,
quenching, and tempering; the schematic illustration is shown in Figure 1. First of all,
the 4340 steel with a thickness of ~1 mm was normalized at 860 ◦ C for 1 h followed by
forced air cooling, to eliminate chemical composition inhomogeneity and residual stress.
This is of great importance because the undissolved carbides from incomplete austeniti-
zation would have a great influence on the fracture properties of tempered samples [23].
After normalization, a mixed microstructure consisting of pearlite and a small amount of
proeutectoid ferrite would be obtained. According to the measured dilatometric curves,
the critical transformation temperature Ac1 and Ac3 were ~710 ◦ C and 790 ◦ C, respectively.
To introduce different ferrite contents in the quenched microstructure, different quenching
temperatures (720, 750, 780, 810, 840 ◦ C) were set, and the holding time was 0.5 h followed
Metals 2023, 13, x FOR PEER REVIEW 3 of 11

Metals 2023, 13, 1139 3 of 11

temperatures (720, 750, 780, 810, 840 °C) were set, and the holding time was 0.5 h followed
by
bywater
watercooling.
cooling.Finally,
Finally,all
allquenched
quenchedsamples
sampleswere
weretempered
temperedatat500
500°C
◦ Cfor
for22hhfollowed
followed
by water cooling to room temperature.
by water cooling to room temperature.

Figure 1. Schematic illustration of the applied heat treatment.

Figure 1. Schematic illustration of the applied heat treatment.
Microstructure observation of experimental steel was performed in a field emission
Microstructure
scanning observation(SEM,
electron microscope of experimental
FEI Quantasteel 250F,was
Brno,performed in a fieldand
Czech Republic) emission
a trans-
scanning electron microscope (SEM, FEI Quanta 250F, USA)
mission electron microscope (TEM, FEI TECNAI 20, Brno, Czech Republic). The and a transmission electron
SEM
microscope
samples were (TEM, FEI TECNAI
ground 20, Brno, Czech
using successively finer Republic).
SiC papersThe SEM #600,
of #320, samples were
#1000, ground
and #1500.
using successively
The ground specimensfiner were
SiC papers of #320, #600,polished
then mechanically #1000, andwith #1500.
3.5 µm The ground
particle specimens
size diamond
were then mechanically polished with 3.5 μm particle size diamond
suspensions. After polishing, the samples were finally etched with 4% nitric acid alcohol suspensions. After
polishing, the samples were finally etched with 4% nitric acid alcohol
solution for tens of seconds to reveal microstructural features. The SEM examinations were solution for tens of
seconds to reveal microstructural features. The SEM examinations
performed at an operating voltage of 15 kV and a working distance of ~10 mm. For TEM were performed at an
operating
observation,voltage of 15foils
the thin kV and
werea first
working distance of
mechanically ~10 mm.
ground to aFor TEM observation,
thickness of ~50 µm, then the
thin foils were
punched first mechanically
to prepare round disks ground
of 3 mmtoinadiameter,
thicknessand of ~50 µ m, the
finally, then punched
disks were to pre-
twin-jet
pare round disks
(Tenupol-5) of 3 mm in diameter,
electro-polished in a solution andoffinally,
80 mLthe disks were
perchloric acidtwin-jet
and 920(Tenupol-5)
mL ethanol
electro-polished in a solution of ◦ 80 mL perchloric acid and 920
at a potential of 30 V and −25 C. The TEM specimens were examined at an acceleration mL ethanol at a potential
ofvoltage
30 V and −25
of 200 kV.°C. The TEM specimens were examined at an acceleration voltage of 200
kV. The Vickers hardness was measured in a micro-hardness tester (HMV-G21DT, Shi-
TheCo.,
madzu Vickers
Tokyo,hardness
Japan)was usingmeasured
a load ofin~4.9a micro-hardness
N with a dwelltester time of(HMV-G21DT,
15 s. Each hardness Shi-
madzu Co., Tokyo,
value shown is theJapan)
averageusing
of a10load of ~4.9 N with
indentations. a dwell time
Quasi-static of 15 tensile
uniaxial s. Each tests
hardness
were
value showninisan
performed theInstron
average of 10
5982 indentations.
testing machine Quasi-static uniaxial
(Instron Company, tensile
Grove tests
City, OH,were
USA)per-at
formed
a straininrate
an of 10−3 s5982
Instron −1 attesting machine (Instron
room temperature. Company, Grove
A self-developed City, OH,
contactless strain USA) at a
gauging
strain rate of 10 s at room temperature. A self-developed contactless strain gaugingto
system based on−3 DIC
−1 (digital image correlation) technique (Nanjing, China) was applied
monitor
system the tensile
based on DICstrain during
(digital image loading. Tensiletechnique
correlation) specimens with a gauge
(Nanjing, China) length of 5 mm
was applied
toand a width
monitor theoftensile
2 mm strain
were prepared by electrical
during loading. Tensiledischarge
specimens machining from the
with a gauge annealed
length of 5
mmsheets.
and Three
a width tensile
of 2 mmtestswere
wereprepared
repeated by forelectrical
each specimen
dischargeto ensure the reproducibility
machining from the an-
of the sheets.
nealed data. TheThree cyclic load–unload–reload
tensile tests were repeated (LUR) tests
for each were carried
specimen out to
to ensure themeasure
reproduc- the
Bauschinger effect. During the LUR testing, the samples were
ibility of the data. The cyclic load–unload–reload (LUR) tests were carried out to measure tensioned to an assigned
strain,
the then unloaded
Bauschinger to 50 N
effect. During theatLURan unloading
testing, therate of 30were
samples N/s,tensioned
and thentoreloaded
an assignedand
unloaded again.
strain, then unloaded to 50 N at an unloading rate of 30 N/s, and then reloaded and un-
loaded again.
3. Results and Discussion
Typical
3. Results andSEM and TEM micrographs of the experimental steel after quenching at
Discussion
720–840 ◦ C are shown in Figures 2 and 3, respectively. After quenching at 720 ◦ C, which
Typical SEM and TEM micrographs of the experimental steel after quenching at 720–
is 10 ◦ C above the Ac1 temperature, a great amount of carbide precipitates were scattered
840 °C are shown in Figure 2 and Figure 3, respectively. After quenching at 720 °C, which
inside the ferrite grains or at the ferrite grain boundaries, and a portion of fine isolated
is 10 °C above the Ac1 temperature, a great amount of carbide precipitates were scattered
martensite (M) is also formed between the ferrite bulk, as shown in Figure 2a. These
inside the ferrite grains or at the ferrite grain boundaries, and a portion of fine isolated
ferrite grains are irregular or equiaxed with a high density of dislocations near the phase
martensite (M) is also formed between the ferrite bulk, as shown in Figure 2a. These ferrite
boundaries between martensite and ferrite (Figure 3a). As the temperature is increased up
to 750 ◦ C, the samples mainly consist of quenched martensite accompanied by ~35% (in
Metals 2023, 13, x FOR PEER REVIEW 4 of 11
Metals 2023, 13, x FOR PEER REVIEW 4 of 11

Metals 2023, 13, 1139 grains are irregular or equiaxed with a high density of dislocations near the phase bound- 4 of 11
grains are irregular or equiaxed with a high density of dislocations near the phase bound-
aries between martensite and ferrite (Figure 3a). As the temperature is increased up to 750
aries between martensite and ferrite (Figure 3a). As the temperature is increased up to 750
°C, the samples mainly consist of quenched martensite accompanied by ~35% (in area
°C, the samples mainly consist of quenched martensite accompanied by ~35% (in area
fraction) undissolved
area fraction) ferriteferrite
undissolved (Fq) and
(Fq )a small number of carbides (Figure 2b). 2b).
When an-
fraction) undissolved ferrite (Fq) and aand
smalla small
numbernumber of carbides
of carbides (Figure
(Figure 2b). When When
an-
nealed
annealed at 780 °C
at 780 ◦for 0.5
C for h followed by water quenching, the fraction of ferrite further de-
nealed at 780 °C for 0.5 0.5 h followed
h followed by water
by water quenching,
quenching, the fraction
the fraction of ferrite
of ferrite further
further de-
creases
decreasesto to
~29%
~29%andandonly a few
only a fewofof
carbides
carbidescan canbe trapped
trapped(Figure
(Figure2c).
2c).A fully
fully lath-type
creases to ~29% and only a few of carbides can bebetrapped (Figure 2c). AAfully lath-type
lath-type
martensite
martensite structure
structure can
can be
be achieved
achieved after
after quenching
quenching at
at temperatures
temperatures higher
higher than
than 810
810 °C
◦C
martensite structure can be achieved after quenching at temperatures higher than 810 °C
(20
(20 °C
◦ C above
above thethe complete
complete austenitization
austenitization temperature
temperature A Ac3c3),
), as
as shown
shown in in Figure
Figure 2d,e.
2d,e. The
The
(20 °C above the complete austenitization temperature A c3), as shown in Figure 2d,e. The
higher
higher the
the quenching
quenching temperature,
temperature, the
thelarger
largerthethe
prior-austenite
prior-austenite grains, andand
grains, the the
wider the
wider
higher the quenching temperature, the larger the prior-austenite grains, and the wider the
quenched
the quenched martensitic laths.
martensitic Obviously, the width of the martensitic lath decreases from
quenched martensitic laths.laths. Obviously,
Obviously, the width
the width of theofmartensitic
the martensitic lath decreases
lath decreases
◦ C°C
from
300
fromnm 300to nm
220 to
nm220as nm
the quenching temperature
as the quenching decreases
temperature from 840
decreases °C to
from 840780 780 ◦ C
to(Figure
300 nm to 220 nm as the quenching temperature decreases from 840 °C to 780 °C (Figure
3b,c).
(Figure 3b,c).
3b,c).

Figure
Figure 2.
2. SEM
SEMimages
imagesof experimental
experimentalsteel after quenching at at
(a) 720720
°C,◦(b) 750750
°C, ◦(c)
C, 780 °C, (d)
◦ C,
Figure 2. SEM images ofofexperimental steel
steel after
after quenching
quenching at (a)(a) C, (b)
720 °C, (b) 750 °C, (c) (c) 780
780 °C, (d)
810 °C, ◦and (e) 840 °C, ◦respectively, showing microstructural evolution features. M and Fq refer to
(d) 810
810 C, and
°C, and (e) 840
(e) 840 C, respectively,
°C, respectively, showing
showing microstructural
microstructural evolution
evolution features.
features. M and
M and Fq refer
Fq refer to
quenched martensite and undissolved ferrite, respectively.
quenched
to quenched martensite andand
martensite undissolved ferrite,
undissolved respectively.
ferrite, respectively.

Figure 3. Typical TEM micrographs of samples after quenching at (a) 720 °C, (b) 780 °C, and (c) 840
Figure
Figure 3.3.Typical
°C. TypicalTEM
TEMmicrographs of samples
micrographs afterafter
of samples quenching at (a)at720
quenching 720(b)◦ C,
(a)°C, 780(b) and◦ C,
°C,780 (c) and
840
°C. ◦
(c) 840 C.
The above results reveal that the shape, size, and volume fraction of the marten-
The
The above
above results
results reveal
reveal that
that the
the shape,
shape, size,
size, and
and volume
volume fraction
fraction ofof the
the marten-
marten-
site/ferrite phases can be tuned by changing the quenching temperature. By this way, the
site/ferrite
site/ferritephases
phasescan canbebetuned
tunedbybychanging
changingthethequenching
quenchingtemperature.
temperature.By Bythis
thisway,
way, the
the
prepared alloys will have the microstructure mixed with martensite and cementite (hard
prepared alloys
prepared alloys will
will have
have the
the microstructure
microstructure mixed
mixed with
with martensite
martensite andand cementite
cementite (hard
(hard
zones) and ferrite (soft zones). As is well known, the presence of terrible residual stresses
zones) and
zones) and ferrite
ferrite (soft
(soft zones).
zones). As
As isis well
well known,
known, thethe presence
presence of
of terrible
terrible residual
residual stresses
stresses
in the quenched martensite has been associated with harmful impacts on the processing
in the
in the quenched
quenched martensite
martensite hashas been
been associated
associated with
with harmful
harmful impacts
impacts on on the
the processing
processing
efficiency of the alloy, resulting in serious deformations; even cracking of the finished
efficiency of
efficiency of the
thealloy,
alloy,resulting
resultingin in
serious deformations;
serious deformations;even cracking
even of the
cracking offinished parts
the finished
parts and components [24]. Subsequent tempering is considered to be helpful in releasing
and components [24]. Subsequent tempering is considered to be helpful in
parts and components [24]. Subsequent tempering is considered to be helpful in releasing releasing these
terrible residual stresses. Through trial and error, holding for 2 h at 500 ◦ C was selected to
be an optimal tempering process.
In the process of tempering, the metastable martensite phase will decompose into
ferrite and cementite, and the prior ferrite bulk (i.e., Fq ) will be retained. For the sake
 these terrible residual stresses. Through trial and error, holding for 2 h at 500 °C was se-
lected to be an optimal tempering process.
Metals 2023, 13, 1139 In the process of tempering, the metastable martensite phase will decompose 5into of 11
ferrite and cementite, and the prior ferrite bulk (i.e., Fq) will be retained. For the sake of
simplicity, the quenching temperature was used to label the samples to distinguish one
from the other, such as the 840–500 sample, which means the sample was quenched from
of simplicity, the quenching temperature was used to label the samples to distinguish
840 °C and then tempered at 500 °C for 2 h. Figure 4 demonstrates the effect of quenching
one from the other, such as the 840–500 sample, which means the sample was quenched
temperature on the final tempered structure. Two types of ferrite structure can be ob-
from 840 ◦ C and then tempered at 500 ◦ C for 2 h. Figure 4 demonstrates the effect of
served in Figure 4a–c, respectively, obtained from the tempered samples quenched from
quenching temperature on the final tempered structure. Two types of ferrite structure can be
720–780 °C (intercritical quenching treatment). One is the micro-sized ferrite bulk (de-
observed in Figure 4a–c, respectively, obtained from the tempered samples quenched from
noted
720–780 as ◦FCq) without carbides (Figure 4a–c); the other is the ultra-fine ferrite matrix con-
(intercritical quenching treatment). One is the micro-sized ferrite bulk (denoted
taining dispersed
as Fq ) without carbides cementite particles
(Figure 4a–c);(pearlitic
the otherstructure, markedferrite
is the ultra-fine by P).matrix
Statistics suggest
containing
that there is
dispersed approximately
cementite particles45% bulk ferrite
(pearlitic in the
structure, area by
marked fraction in sample
P). Statistics 720–500.
suggest The
that there
corresponding bright-field TEM image (Figure 5a) shows that the
is approximately 45% bulk ferrite in the area fraction in sample 720–500. The correspondingequiaxed ultrafine-
grained ferrite
bright-field TEMgrains
imagecontained a few
(Figure 5a) of dislocations
shows and precipitates;
that the equiaxed however,
ultrafine-grained the ferrite
ferrite grains
matrix in the pearlitic structure has a significant diffraction contrast contributed
contained a few of dislocations and precipitates; however, the ferrite matrix in the pearlitic to by
abundant cementite or carbide particles and dislocations. In samples
structure has a significant diffraction contrast contributed to by abundant cementite or 750–500 and 780–500
(Figure
carbide4b,c),
particlesthe same heterostructures
and dislocations. are also750–500
In samples observed,andbut the area
780–500 fraction
(Figure of the
4b,c), the prior
same
ferrite bulk has been reduced to ~38% and 31%, respectively. A typical
heterostructures are also observed, but the area fraction of the prior ferrite bulk has been TEM micrograph
in Figureto
reduced 5b~38%
shows that
and in the
31%, 780–500 sample,
respectively. A typical cementite particles are
TEM micrograph located
in Figure 5batshows
the prior
that
austenite grain boundaries (PAGBs), lath boundary, and the interior of the
in the 780–500 sample, cementite particles are located at the prior austenite grain boundaries lath-type struc-
tures,
(PAGBs),whichlathisboundary,
in agreement and with previous
the interior of work [25]. While
the lath-type the sample
structures, whichwas quenched
is in agreement at
temperatures
with previousabove work the
[25].AWhile
c3 line,the
a representative
sample was quenchedpearlite structure is observed
at temperatures abovewithout
the Ac3
any
line,residual pure ferrite
a representative bulk,structure
pearlite as shown is in Figure without
observed 4d,e, andanya large number
residual pure of granular
ferrite bulk,
cementite
as shown precipitates
in Figure 4d,e, filled
andthe ferrite
a large matrix.ofThe
number enlarged
granular TEM image
cementite (Figure
precipitates 5c) re-
filled the
veals
ferritethat a good
matrix. Thedeal of needle-like
enlarged TEM image cementite
(Figureparticles embedded
5c) reveals that a goodin ferrite
deal ofgrains, and
needle-like
numerous film-like embedded
cementite particles cementite particles
in ferrite(the red and
grains, arrow) located film-like
numerous on the ferrite grainparticles
cementite bound-
aries.
(the red arrow) located on the ferrite grain boundaries.

Figure
Figure4.4. SEM
SEMimages
imagesofofthe
thetempered
temperedsteels
steelsafter
afterquenching
quenching from
from (a)
(a) 720
720 °C,
◦ C,(b)
(b)750
750°C,
◦ C,(c)
(c)780
780°C,
◦ C,
(d) 810 °C,
◦ and (e) 840 °C,
◦ respectively. P and Fq refer to tempered pearlite structure and retained
(d) 810 C, and (e) 840 C, respectively. P and Fq refer to tempered pearlite structure and retained
ferrite grains, respectively.
ferrite grains, respectively.

Based
Based onon the
the above,
above, aa novel
novel heterostructure
heterostructure configuration
configuration and
and aa classical
classical pearlite
pearlite
structure
structure can be achieved by controlling the quenching temperature. Besidesthe
can be achieved by controlling the quenching temperature. Besides theresidual
residual
ferrite
ferrite bulk,
bulk, the
the pearlite
pearlite zones
zones in
in the heterostructure are
the heterostructure aredifferent
differentfrom
fromthe
theclassical
classicalpearlite
pearl-
ite structure;
structure; thethe former
former hashas larger
larger granular
granular cementite
cementite particles,
particles, while
while the latter
the latter contains
contains film-
and needle-like cementite particles. Moreover, the density of carbide precipitates in the
pearlite zones in the heterostructure is higher than that in the classical pearlite structure,
because almost the same carbon content precipitates in the smaller volume.
Metals 2023, 13, x FOR PEER REVIEW 6 of 11
Metals 2023, 13, x FOR PEER REVIEW 6 of 11

film- and needle-like cementite particles. Moreover, the density of carbide precipitates in
film-
the and needle-like
pearlite cementite
zones in the particles.isMoreover,
heterostructure thethat
higher than density ofclassical
in the carbide precipitates in
pearlite struc-
Metals 2023, 13, 1139 6 of 11
the pearlite
ture, becausezones in the
almost the same
heterostructure is higher
carbon content than that
precipitates inin the
the classical
smaller pearlite struc-
volume.
ture, because almost the same carbon content precipitates in the smaller volume.

Figure 5. Typical bright-field TEM micrographs of tempered samples (a) 720–500 °C, (b) 780–500 °C,
Figure
and (c) 5. Typical°C.
840–500 bright-field TEM micrographs of tempered samples (a) 720–500 °C, (b) 780–500 °C,
Figure 5. Typical bright-field TEM micrographs of tempered samples (a) 720–500 ◦ C, (b) 780–500 ◦ C,
and (c) 840–500 °C.
and (c) 840–500 ◦ C.
Figure 6 gives the microhardness variation of the experimental steels as a function of
Figure
Figure 66 gives
the quenching the
themicrohardness
temperature.
gives As the quenching
microhardness variation
variation ofofthe
theexperimental
temperature increases
experimental steels
fromas720
steels a function
as a°C to 840
function of
the
°C, quenching
thequenching
of the temperature.
microhardness As
of both theAs
temperature. the quenching
quenched temperature
and tempered
the quenching increases
samples
temperature from
first raises
increases 720
from °C
rapidly
720 C to
◦ 840
andto
°C,
840 the
then C,microhardness
◦decreases slowly, of
the microhardness andboth
of the
theboth quenched
highest and tempered
hardness
the quenched of
and both thesamples
tempered quenched first
samples andraises rapidly
tempered
first raises and
sam-
rapidly
then
ples decreases
is
and then obtained slowly,
decreases at 780 and
slowly, the
andhighest
°C quenchingthe highest hardness
temperature.
hardnessof bothThe the
peak
of both quenched
hardness
the quenchedand oftempered
the quenched
and temperedsam-
ples
sample is obtained
samplesisisabout at 780
760 HV,
obtained at 780 °C ◦quenching
andCthat temperature.
of the corresponding
quenching temperature. The The peak
tempered hardness of the
sample isofapproximately
peak hardness quenched
the quenched
sample
450 HV.is
sample about
isFor the 760
about HV,
HV, and
quenched
760 and that
that of
steels, thethe
of the corresponding
increase in hardness
corresponding tempered
beforesample
tempered 780 °C is
sample is approximately
mainly due to
approximately
450
the HV.For
450 lattice
HV. For thequenched
quenched
distortion
the caused steels,
by the
steels, the
the increase
formation
increase in
inof hardness
supersaturated
hardness before
before 780
◦ C °C
martensitic
780 is mainly
is mainly duedue
structure. Asto
to the
the
is lattice
lattice
well distortion
distortion
documented, causedacaused
by the
higher by the formation
formation
martensite ofwould
supersaturated
of supersaturated
content cause martensitic
martensitic
greater structure.
residual structure.
As is well
stresses As
and
ais well documented,
documented,
higher a higheradensity
dislocation higher martensite
martensite content
within the content
would
adjacent would
cause cause
greater
ferrite phase, greater
residual residual
stresses
resulting stresses
in aand and
a higher
significant
adislocation
higher dislocation
enhancement density
in strengthdensity
within within
thewell
as adjacent the adjacent
ferrite
as hardness phase, ferrite phase,
resulting
of dual-phase in aresulting
steels significant
[26,27]. As in enhancement
athe
significant
quench-
enhancement
in strength
ing temperature in strength
as wellwasas hardnessas well as hardness
of dual-phase
further increased of dual-phase
steels [26,27].
to complete steels [26,27].
As the quenching
austenization As
areas (above the quench-
temperature
810 °C),
ing temperature
was further was
increased further increased
to complete to complete
austenization austenization ◦
areas (above 810 °C),
slight softening occurred. This should be ascribedareas to the(above
reduction 810 ofC), slight C
average softening
content
slight
in the softening
occurred. lath-type occurred.
This should
martensite This
be ascribed should
structure to the be reduction
and ascribed
the widening to
ofthe reduction
average
of of average
C content
martensite in the
lath, as C content
lath-type
shown in
in the lath-type
martensite
Figure 3. While martensite
structure
for theand thestructure
tempered widening and
specimens, thethe widening
of martensite lath,of
formation asofmartensite
shown lath,zones
in Figure
more pearlite as3. shown
While
should in
for
Figure
the 3.
tempered While for the
specimens, tempered
the specimens,
formation of more the formation
pearlite
be responsible for the hardness variation with increasing quenching temperature before zones of more
should pearlite
be zones
responsible should
for the
be
780 responsible
hardness
°C, and the for
variation the
withhardness
hardness increasing variation
drop results fromwith
quenching the increasing
temperature
decrease quenching
inbefore 780 ◦ C,
the density temperature
ofand before
the hardness
cementite parti-
drop
780 °C, results
and from
the the
hardness decrease
drop in the
results density
from the of cementite
decrease in particles
the
cles in the ferrite matrix with the gradual disappearance of the residual ferrite bulk, refer- density in ofthe ferrite
cementite matrix
parti-
with
cles in
ring the
to the gradual
ferrite
Figures disappearance
matrix
3 and 4. with theof the residual
gradual ferrite bulk,
disappearance referring
of the residual to Figures
ferrite bulk, 3 and 4.
refer-
ring to Figures 3 and 4.
Quenched steel
steel
Quenched & Tempered steel
800
800 Quenched & Tempered steel
760
Hardness(HV)

760 714
Hardness(HV)

714 680
600 624 680
600 624

400 450
430
400 345 430
450 408
388
345 408
388
314
314
200
200 720 750 780 810 840
720 750 780 810 840
Temperature(℃)
Temperature(℃)
Figure 6. Variation of microhardness of quenched and tempered steels as a function of quenching
Figure 6. Variation of microhardness of quenched and tempered steels as a function of quenching
temperature.
temperature.
temperature.
The engineering stress-engineering strain plots of the tempered samples exhibit con-
tinuous yielding, as shown in Figure 7a. The effect of the quenching temperature on the
tensile properties is summarized in Figure 7b and Table 1. The variation of the strength is
 Metals 2023, 13, x FOR PEER REVIEW 7 of 11

Metals 2023, 13, 1139 7 of 11

The engineering stress-engineering strain plots of the tempered samples exhibit con-
tinuous yielding, as shown in Figure 7a. The effect of the quenching temperature on the
tensile properties is summarized in Figure 7b and Table 1. The variation of the strength is
similar
similarto tothat
thatof ofthe
thehardness,
hardness,undergoing
undergoingthe theundulation
undulationofofrising risingfirst
firstand
andthen
thenfalling.
falling.In
view
In viewof the microstructure,
of the microstructure, the the
strength of the
strength steelsteel
of the varies withwith
varies the decrease
the decrease in the
in residual
the re-
ferrite
sidual zones; that is,that
ferrite zones; the strength increases
is, the strength with the
increases withdecrease in thein
the decrease residual ferriteferrite
the residual zones
at the first
zones at thestage, and then
first stage, andreaches the peak
then reaches with with
the peak 31% 31% residual ferrite
residual zones
ferrite in the
zones area
in the
fraction, and finally
area fraction, slowlyslowly
and finally decreases as the as
decreases ferrite zones gradually
the ferrite disappear.
zones gradually The highest
disappear. The
tensile ◦C
higheststrength and yieldand
tensile strength strength are 1300 are
yield strength MPa andMPa
1300 1230andMPa,1230respectively, both at 780
MPa, respectively, both
quenching temperature.
at 780 °C quenching However,However,
temperature. the tensile thestrength and yield
tensile strength andstrength of the pearlite
yield strength of the
steel quenched from 840 from ◦ C are 1233 MPa and 1156 MPa, respectively, and are reduced by
pearlite steel quenched 840 °C are 1233 MPa and 1156 MPa, respectively, and are
67 MPa and
reduced by 6774 MPa
MPa and compared
74 MPawith the peak
compared withstrength.
the peak When the quenching
strength. When thetemperature
quenching
goes down a goes
temperature to 810a◦ little
little down C, still
to above
810 °C,thestillAabove
c3 line,theit has
Ac3 little
line, itimpact on impact
has little the strength
on theof
steel withofpearlite
strength steel with structure.
pearliteHowever,
structure. as the temperature
However, drops from
as the temperature the Afrom
drops c3 line
thetoAthe
c3

Aline
c1 line,
to thethe
A strength
c1 line, the of the
strength steel
of dwindles
the steel fast,
dwindles along
fast, with
along the
withvolume
the shrinkage
volume of
shrinkage the
residual ferrite zones
of the residual ferritein the microstructure.
zones in the microstructure.The most Thenoteworthy feature feature
most noteworthy of the strength
of the
change
strengthischange
that theispeak is achieved
that the in the sample
peak is achieved in the where
sampletherewhere is about
there is31about
vol.%31residual
vol.%
ferrite
residual bulk (Figure
ferrite bulk3c), which
(Figure is which
3c), contrary to traditional
is contrary knowledge.
to traditional knowledge.

Figure 7.
Figure 7. Effects
Effects of
of quenching
quenching temperature
temperature onon mechanical
mechanical properties
properties of
of experimental
experimental steels.
steels. (a)
(a) engi-
en-
gineering stress-engineering strain curves, (b) strength and elongation of tempered steels as a func-
neering stress-engineering strain curves, (b) strength and elongation of tempered steels as a function
tion of quenching temperature, (c) true stress-true strain plots, and (d) work hardening rate-true
of quenching temperature, (c) true stress-true strain plots, and (d) work hardening rate-true strain
strain curves of tempered samples.
curves of tempered samples.
Metals 2023, 13, 1139 8 of 11

Table 1. Mechanical properties of quenched and tempered steels.

Sample Tensile Strength, MPa Yield Strength, Mpa Uniform Elongation, % Total Elongation, %
720–500 874 650 7 20
750–500 1150 870 3.8 14.5
780–500 1295 1226 4 15.2
810–500 1255 1089 3.7 14.6
840–500 1233 1156 3.1 11.3

As is well known, the strength and ductility (uniform elongation) of materials move in
perfect opposition when the materials are strengthened by traditional methods. Excitingly,
the results shown in Figure 7a,b exhibit a breakthrough against the traditional knowledge,
and the uniform elongation remains more or less constant at 4%, except for the sample
720–500, although the strength changes. The calculated true stress-strain plots and corre-
sponding work hardening rate curves are shown in Figure 7c,d, respectively. All strain
hardening rate curves include a rapid drop before 0.02 and a slow decline after 0.02. The
section after 0.02 reveals the work hardening ability of the sample in the process of plastic
deformation. Obviously, the more residual ferrite bulk there is, the higher the working
hardening rate. The introduction of residual ferrite bulk benefits the alloy in gaining good
strain-hardening capability. Thus, the 720–500 steel possessed the highest work hardening
ability due to the larger fraction of ferrite (the black line in Figure 7d). The strain energy
density, another parameter of toughness, was calculated to be 159.6 MJ/m3 in 720–500
vs. 147.8 MJ/m3 in 750–500 vs. 174 MJ/m3 in 780–500 vs. 158.7 MJ/m3 in 810–500 vs.
121.5 MJ/m3 in 840–500, according to the area below the engineering stress-engineering
strain curve. Both the enhancement strain-hardening capability and strain energy density
indicate a notable gain in toughness in the 780–500 sample with optimized heterostructure,
compared to that of the 840–500 sample with classical pearlite structure.
Combined, the heterostructured steel has excellent comprehensive mechanical proper-
ties with a higher tensile strength of 1300 MPa, an enhanced yield strength of 1230 MPa,
and better toughness, indicated by the enhancement strain-hardening capability and strain
energy density. The superior mechanical property is related to the content of residual
bulk ferrite, which optimizes carbon partition and provides dislocation motion. Generally,
ferrite is almost carbon-free, hence the average carbon content in the quenched martensite
in 780–500 steels is relatively higher than that in samples annealed at a complete austenitiz-
ing temperature, leading to a higher density of carbides in the corresponding tempered
structure. Therefore, the loss of strength and hardness caused by the formation of the ferrite
phase can be compensated by that caused by the enhanced precipitation strengthening.
In addition, strain partitioning and a strain gradient can be generated during the tensile
deformation near the boundaries between the soft ferrite zones and hard pearlite ones, to
ensure the continuity of deformation. Thus, the GNDs would be created near the soft/hard
zone boundaries, producing a long-range stress (back stress), which would provide extra
strain hardening [11].
As to validate the above assumption, the contribution of HDI hardening to the overall
strength of experimental steels is evaluated according to the measured LUR hysteresis
loops (Figure 8a) and the following equations [28].

σHDI = σflow − σeff (1)

σflow − σu σ∗
σeff = + (2)
2 2
where σflow , σeff and σu are flow stress, effective stress, and reverse yield stress, respectively,
and σ∗ represents the thermal component of the flow stress related to viscous flow at the
initiation of unloading, as schematically defined in Figure 8b.
Metals 2023, 13, 1139
x FOR PEER REVIEW 9 9of
of 11

Figure
Figure 8.
8. Bauschinger
Bauschingereffect
effectand
andHDI
HDIstress ofof
stress the tempered
the tempered steels. (a) (a)
steels. LUR stress-strain
LUR curves,
stress-strain (b)
curves,
schematic of hysteresis loops for calculating HDI stress, (c) HDI stress versus applied
(b) schematic of hysteresis loops for calculating HDI stress, (c) HDI stress versus applied strain, strain, (d)
contribution of HDI stress to total stress as a function of true strain.
(d) contribution of HDI stress to total stress as a function of true strain.

The
The calculated
calculated HDI HDI stress
stress values
values asas aa function
function of of the
the true strain are
true strain summarized in
are summarized in
Figure
Figure 8c, and it can be seen that the HDI stress grows almost linearly with the
8c, and it can be seen that the HDI stress grows almost linearly with the applied
applied
true
true stress
stress for
forthe
theselected
selectedsamples.
samples.Predictably,
Predictably, thethe
tempered
temperedsample quenched
sample quenched fromfrom
780
°C
780has
◦ C higher HDI HDI
has higher stressstress
in theinrange of 560ofMPa
the range 560 to 720to
MPa MPa
720throughout the whole
MPa throughout defor-
the whole
mation process,
deformation compared
process, to the 840–500
compared samples
to the 840–500 (470~575
samples MPa). Figure
(470~575 MPa).8d lists the
Figure 8d con-
lists
tribution of HDI stress
the contribution of HDI to stress
the total
to stress throughout
the total the deformation,
stress throughout and also the
the deformation, andcontri-
also
bution of HDI stress
the contribution of HDIto the totaltostress
stress is much
the total stresshigher
is muchin the tempered
higher in the sample
tempered quenched
sample
from 780 °C. As ◦
mentioned above, about a 31% fraction of ferrite
quenched from 780 C. As mentioned above, about a 31% fraction of ferrite was introduced was introduced in the
780–500 steel, and
in the 780–500 steel,the
andsoft
thephase (Fq) was
soft phase (Fq )constrained
was constrainedby a by
tempered
a temperedpearlite structure
pearlite (P)
structure
(regarded
(P) (regardedas the hard
as the hardzones).
zones).This
Thisprovided
provideddirectdirectexperimental
experimentalevidence
evidencefor
for the
the effects
effects
of heterostructure on mechanical properties, properties, which
which is consistent
consistent with
with the report that the
highest HDI hardening is achieved when the content of soft zones was around ~30 ~30 vol.%
vol.%
in heterostructured materials [11]. The The extra
extra strain
strain hardening
hardening provided
provided by HDI stress is
responsible for the good combination of strength and ductility achieved in the tempered
sample after quenching from 780 ◦°C. C.

4. Conclusions
4. Conclusions
Based on
Based on the
the concept
concept of
of heterogeneous
heterogeneous structure,
structure, intercritical
intercritical quenching
quenching plus
plus tem-
tem-
pering treatments were used to modify the microstructural characteristics of a 4340
pering treatments were used to modify the microstructural characteristics of a 4340 steel. steel.
The effect
The effectofofquenching
quenchingtemperature
temperature on on
thethe
microstructure evolution
microstructure and mechanical
evolution prop-
and mechanical
erty was was
property investigated, and and
investigated, the microstructure–property
the microstructure–property relationship waswas
relationship established. In
established.
addition, the contribution of HDI stress to the improvement of strength and ductility
In addition, the contribution of HDI stress to the improvement of strength and ductility was
evaluated.
was SomeSome
evaluated. interesting conclusions
interesting can be
conclusions candrawn as follows:
be drawn as follows:
Metals 2023, 13, 1139 10 of 11

(1) As the quenching temperature increased from 720 ◦ C to 840 ◦ C, the area fraction
of undissolved ferrite in the quenched samples decreased, and the cementite also
gradually decomposed completely. For the corresponding tempered steels, the mi-
crostructural constituents changed from 45% residual ferrite and tempered pearlite
in the 720–500 sample, to 31% ferrite plus pearlite structure in the 780–500 steel, and
finally to complete pearlite in the 840–500 one.
(2) The heterostructured steel (HS, i.e., 780–500 sample) exhibits superior mechanical
properties compared to the pearlite steel (PS, i.e., 840–500 sample): 1300 MPa in HS
vs. 1233 MPa in PS for tensile strength, 1230 MPa in HS vs. 1156 MPa in PS for
yield strength, 174 MJ/m3 in HS vs. 121.5 MJ/m3 in PS for strain energy density
(toughness), and better strain-hardening capability.
(3) The volume fraction of the soft ferrite bulk zone has a decisive influence on the HDI
strengthening. Here, the heterostructured steel exhibits the best HDI hardening ability
when it has 31% residual ferrite zones in the volume fraction, which can be achieved
by quenching at 780 ◦ C following the tempering at 500 ◦ C for 2 h.

Author Contributions: Conceptualization, J.L.; methodology and investigation, Y.S. and G.S.; data
collection and analysis, Y.S. and G.S.; writing—review & editing, Y.S., G.S. and J.L. All authors have
read and agreed to the published version of the manuscript.
Funding: This work was supported by the Natural Science Foundation of Jiangsu Province (grant
numbers BK20201308 and BK20220964). The authors are thankful for the technical support from the
Jiangsu Key Laboratory of Advanced Micro & Nano Materials and Technology, the Analysis and Test
Center of Nanjing University of Science and Technology.
Data Availability Statement: The data presented in this study are available on request from the
corresponding author.
Conflicts of Interest: The authors declare no conflict of interest.

References
1. Saeidi, N.; Ekrami, A. Comparison of mechanical properties of martensite/ferrite and bainite/ferrite dual phase 4340 steels.
Mater. Sci. Eng. A 2009, 523, 125–129. [CrossRef]
2. Moraes, D.A.; Almeida, G.F.C.; Couto, A.A.; Massi, M.; Caliari, F.R.; Lima, C.R.C. Creep of High-Strength Steel Coated with
Plasma Sprayed Self-Fluxing Alloy. Metals 2023, 13, 763. [CrossRef]
3. Lopez-Garcia, R.D.; Medina-Juárez, I.; Maldonado-Reyes, A. Effect of Quenching Parameters on Distortion Phenomena in AISI
4340 Steel. Metals 2022, 12, 759. [CrossRef]
4. Goant, ă, V.; Munteanu, C.; Müftü, S.; Istrate, B.; Schwartz, P.; Boese, S.; Ferguson, G.; Morăras, , C.-I.; Stefan, A. Evaluation of the
Fatigue Behavior and Failure Mechanisms of 4340 Steel Coated with WIP-C1 (Ni/CrC) by Cold Spray. Materials 2022, 15, 8116.
[CrossRef] [PubMed]
5. Clarke, A.J.; Miller, M.K.; Field, R.D.; Coughlin, D.R.; Gibbs, P.J.; Clarke, K.D.; Alexander, D.J.; Powers, K.A.; Papin, P.A.; Krauss,
G. Atomic and nanoscale chemical and structural changes in quenched and tempered 4340 steel. Acta Mater. 2014, 77, 17–27.
[CrossRef]
6. Lee, W.S.; Su, T.T. Mechanical properties and microstructural features of AISI 4340 high-strength alloy steel under quenched and
tempered conditions. J. Mater. Process. Technol. 1999, 87, 198–206. [CrossRef]
7. Wu, X.L.; Zhu, Y.T. Heterogeneous materials: A new class of materials with unprecedented mechanical properties. Mater. Res.
Lett. 2017, 5, 527–532. [CrossRef]
8. Miura, H.; Kobayashi, M.; Todaka, Y.; Watanabe, C.; Aoyagi, Y.; Sugiura, N.; Yoshinaga, N. Heterogeneous nanostructure
developed in heavily cold-rolled stainless steels and the specific mechanical properties. Scr. Mater. 2017, 133, 33–36. [CrossRef]
9. Zhu, Y.T.; Wu, X.L. Perspective on hetero-deformation induced (HDI) hardening and back stress. Mater. Res. Lett. 2019, 9, 393–398.
[CrossRef]
10. Estrin, Y.; Beygelzimer, Y.; Kulagin, R.; Gumbsch, P.; Fratzl, P.; Zhu, Y. Architecturing materials at mesoscale: Some current trends.
Mater. Res. Lett. 2021, 9, 399–421. [CrossRef]
11. Zhu, Y.T.; Ameyama, K.; Anderson, P.M.; Beyerlein, I.J.; Gao, H.; Kim, H.S.; Lavernia, E.; Mathaudhu, S.; Mughrabi, H.;
Ritchie, R.O.; et al. Heterostructured materials: Superior properties from hetero-zone interaction. Mater. Res. Lett. 2021, 9, 1–31.
[CrossRef]
12. Wu, X.L.; Yang, M.X.; Yuan, F.P.; Wu, G.; Wei, Y.; Huang, X.; Zhu, Y. Heterogeneous lamella structure unites ultrafine-grain
strength with coarse-grain ductility. Proc. Natl. Acad. Sci. USA 2015, 112, 14501–14505. [CrossRef] [PubMed]
Metals 2023, 13, 1139 11 of 11

13. Huang, J.X.; Liu, Y.; Xu, T.; Chen, X.F.; Lai, Q.Q.; Xiao, L.R.; Pan, Z.Y.; Gao, B.; Zhou, H.; Zhu, Y.T. Dual-phase hetero-structured
strategy to improve ductility of a low carbon martensitic steel. Mater. Sci. Eng. A 2022, 834, 142584. [CrossRef]
14. Wu, X.L.; Yang, M.X.; Yuan, F.P.; Chen, L.; Zhu, Y. Combining gradient structure and TRIP effect to produce austenite stainless
steel with high strength and ductility. Acta Mater. 2016, 112, 337–346. [CrossRef]
15. Sun, G.S.; Liu, J.Z.; Zhu, Y.T. Heterostructure alleviates Lüders deformation of ultrafine-grained stainless steels. Mater. Sci. Eng. A
2022, 848, 143393. [CrossRef]
16. Hu, J.; Li, X.Y.; Zhang, Z.M.; Wang, L.; Li, Y.; Xu, W. Overcoming the strength-ductility trade-off in metastable dual-phase
heterogeneous structures using variable temperature rolling and annealing. Mater. Res. Lett. 2023, 11, 648–654. [CrossRef]
17. Li, Z.; Pradeep, K.G.; Deng, Y.; Raabe, D.; Tasan, C.C. Metastable high-entropy dual-phase alloys overcome the strength–ductility
trade-off. Nature 2016, 534, 227–230. [CrossRef]
18. Hu, J.; Zhang, J.M.; Sun, G.S.; Du, L.X.; Liu, Y.; Dong, Y.; Misra, R.D.K. High strength and ductility combination in nano-/ultrafine-
grained medium-Mn steel by tuning the stability of reverted austenite involving intercritical annealing. J. Mater. Sci. 2019, 54,
6565–6578. [CrossRef]
19. Jing, S.; Ding, H.; Ren, Y.; Cai, Z. A new insight into annealing parameters in tailoring the mechanical properties of a medium Mn
steel. Scr. Mater. 2021, 202, 114019. [CrossRef]
20. He, B.B.; Hu, B.; Yen, H.W.; Cheng, G.J.; Wang, Z.K.; Luo, H.W.; Huang, M.X. High dislocation density–induced large ductility in
deformed and partitioned steels. Science 2017, 357, 1029–1032. [CrossRef]
21. Luo, Z.C.; Huang, M.X. Revisit the role of deformation twins on the work-hardening behaviour of twinning-induced plasticity
steels. Scr. Mater. 2018, 142, 28–31. [CrossRef]
22. Mehrabi, A.; Sharifi, H.; Asadabad, M.A.; Reza, A.N.; Ali, R. Improvement of AISI 4340 steel properties by intermediate
quenching–microstructure, mechanical properties, and fractography. Int. J. Mater. Res. 2020, 111, 711–779. [CrossRef]
23. Clarke, A.J.; Klemm-Toole, J.; Clarke, K.D.; Coughlin, D.R.; Pierce, D.T.; Euser, V.K.; Poplawsky, J.D.; Clausen, B.; Brown, D.;
Almer, J.; et al. Perspectives on quenching and tempering 4340 steel. Metall. Mater. Trans. A 2020, 51, 4984–5005. [CrossRef]
24. Samuel, A.; Prabhu, K.N. Residual stress and distortion during quench hardening of steels: A review. J. Mater. Eng. Perform. 2022,
31, 5161–5188. [CrossRef]
25. Lim, N.S.; Bang, C.W.; Das, S.; Jin, H.W.; Ayer, R.; Park, C.G. Influence of tempering temperature on both the microstructural
evolution and elemental distribution in AISI 4340 steels. Met. Mater. Int. 2012, 18, 87–92. [CrossRef]
26. Hosseinifar, F.; Ekrami, A. The effect of cold-rolling prior to the inter-critical heat treatment on microstructure and mechanical
properties of 4340 steel with ferrite–martensite microstructure. Mater. Sci. Eng. A 2022, 830, 142314. [CrossRef]
27. Gao, B.; Hu, R.; Pan, Z.Y.; Chen, X.; Liu, Y.; Xiao, L.; Cao, Y.; Li, Y.; Lai, Q.; Zhou, H. Strengthening and ductilization of laminate
dual-phase steels with high martensite content. J. Mater. Sci. Technol. 2021, 65, 29–37. [CrossRef]
28. Yang, M.X.; Pan, Y.; Yuan, F.P.; Zhu, Y.; Wu, X. Back stress strengthening and strain hardening in gradient structure. Mater. Res.
Lett. 2016, 4, 145–151. [CrossRef]

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