materials

Article
Effect of Reverse-phase Transformation Annealing
Process on Microstructure and Mechanical Properties
of Medium Manganese Steel
Yan Zhao, Lifeng Fan * and Bin Lu
School of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010000, China;
13623455180@163.com (Y.Z.); lubinbt@126.com (B.L.)
* Correspondence: fanlf@imut.edu.cn; Tel.: +86-188-4712-5671




Received: 15 August 2018; Accepted: 3 September 2018; Published: 6 September 2018


Abstract: In order to develop a third-generation automobile steel with powerful strength and
elongation, we propose a method through high temperature quenching and two-phase region
reverse-phase transformation annealing to develop such steel with 0.13% C and 5.4% Mn.
To investigate the microstructure evolution and mechanical properties of manganese steel, SEM, XRD
and TEM are employed in our experiments. Experimental results indicate that the microstructure
after quenching is mainly lath martensite microstructure with average of lath width at 0.5 µm.
The components of the steel after along with reverse-phase transformation annealing are ultra-fine
grain ferrite, lath martensite and different forms of austenite microstructure. When the temperature
at 625 ◦ C, the components of the steel mainly includes lath martensite microstructure and ultra-fine
grain ferrite and the fraction of austenite volume is only 5.09%. When the annealing temperature of
reverse-phase transformation increase into 650 ◦ C and 675 ◦ C, the austenite appears in the boundary
of the ferritic grain boundary and the boundary of lath martensite as the forms of bulk and lath.
The phenomenon appears in the bulk of austenite, and the size of is 0.22 µm, 0.3 µm. The fraction
of austenite volume is 22.34% at 675 ◦ C and decreases into 9.32% at 700 ◦ C. The components of
austenite mainly includes ultra-fine grained ferrite and lath martensite. Furthermore, the density
of decreases significantly, and the width of martensite increases into 0.32 µm. In such experimental
settings, quenching at 930 ◦ C with 20 min and at 675 ◦ C with 30 min reverse-phase transformation
annealing, the austenite volume fraction raises up to 22.34%.

Keywords: medium manganese steel; reverse transformation annealing; ultra-fine grained ferrite;
austenite; strength-ductility combination

1. Introduction
With the rapid development, people pay more attention to energy, environment and resource
issues, which poses new challenges to the light weight and safety of automobiles. Strength and
plasticity are important indexes of steel materials. In general, the high strength which reflects in
plasticity and toughness are low, and good matching with high strength as well as high plasticity
is a necessary condition for automobile components [1–5]. The first generation of automotive steel,
represented by IF steel and DP steel cannot meet the dual requirements of light weight and high safety.
The second generation of automotive steels are included by TWIP steel, having a strength-ductility
combination level of 60 GPa %. However, it added a large number of alloying elements, which make
the cost higher and the manufacturing process complicated [6,7]. Therefore, it is very significant for
us to investigate and develop third generation automotive steel with good matching of strength and
plasticity. In 1970s, professor Miller [8] and Morris [9] obtained austenite with a volume fraction of

Materials 2018, 11, 1633; doi:10.3390/ma11091633 www.mdpi.com/journal/materials

Materials 2018, 11, 1633 2 of 12
Materials 2018, 11, x FOR PEER REVIEW 2 of 12

20–30% fraction
volume and ultra-fine grains
of 20–30% ferrite
and microstucture
ultra-fine in low
grains ferrite carbon 5% Mn
microstucture steelcarbon
in low by austenite
5% Mnreverted
steel by
transformation
austenite (ART).
reverted Arlazarov [10]
transformation gained
(ART). a multiphase
Arlazarov [10] microstructure
gained a multiphaseof ferrite, martensite and
microstructure of
retainedmartensite
ferrite, austenite by andaustenite
retainedreverse-phase transformation
austenite by austenite annealing.
reverse-phase Yin’s [11] research
transformation groupYin’s
annealing. used
the continuous
[11] research group annealing
used the process
continuousto provide 28 GPa
annealing % fortostrength-ductility
process provide 28 GPa %combination by using
for strength-ductility
the TRIP effect
combination by of metastable
using the TRIP austenite
effect ofand ultrafineaustenite
metastable ferrite. Cao
and [12] adopted
ultrafine theCao
ferrite. different cooling
[12] adopted
methods
the differentafter annealing
cooling to acquire
methods the austenite
after annealing volume
to acquire thefraction after
austenite air cooling
volume fractionwas greater
after than
air cooling
the austenite
was greater thanvolume fraction of
the austenite the furnace
volume cooling,
fraction of the obtaining the third-generation
furnace cooling, automotive steel
obtaining the third-generation
with a strength-ductility
automotive combination of 26.5
steel with a strength-ductility GPa %. Itofis26.5
combination alsoGPa
well%.known thatwell
It is also the first
known generation
that the
of automotive
first generationsteel is mainly bcc
of automotive as the
steel microstructure,
is mainly bcc as thebut fcc phase plays
microstructure, buta vital role in
fcc phase the second
plays a vital
role in the second
generation generation
of automotive steel,ofthe
automotive steel, the
third generation of third generation
automotive steel of automotive
obtains the dualsteel obtains the
microstructure
dual
of themicrostructure
bcc + fcc phaseofthrough
the bcc a+ reasonable
fcc phase through a reasonable
heat treatment heat treatment process.
process.
In this
this paper,
paper,we westudy
studythe the 0.13%
0.13% C-5.4%
C-5.4%MnMn lowlow carbon coldcold
carbon rolled medium
rolled manganese
medium steel
manganese
through austenite reverse-phase transformation annealing heat treatment process and the effectthe
steel through austenite reverse-phase transformation annealing heat treatment process and of
different reverse-phase
effect of different transformation
reverse-phase transformation annealing
annealingtemperatures
temperatures on on microstructure
microstructureevolution.
evolution.
Meanwhile,
Meanwhile, we we investigate
investigate the mechanical properties, provide provide theoretical
theoretical guidance
guidance for the
development and application of the third generation of automobile steel.

2. Materials
2. Materials and
and Methods
Methods
The chemical
The chemical composition
composition(mass (massfraction
fraction%) %)ofofthe studied
the studied steel is demonstrated
steel is demonstrated in Table 1. The
in Table test
1. The
is carried
test out by
is carried outusing a 50-Kg
by using vacuum
a 50-Kg induction
vacuum furnace
induction and pour
furnace andintopour a mold
into aofmold
150 mm × 150
of 150 mmmm × 150×
250 mm. Firstly, slab first heats to 450 ◦ C with 50 min, then continue heating to 700 ◦ C heat preservation
mm × 250 mm. Firstly, slab first heats to 450 °C with 50 min, then continue heating to 700 °C heat
50 min, finally50heats
preservation 1150 ◦ C
min,tofinally holding
heats 90 min
to 1150 to ensure90
°C holding themin
temperature
to ensureof thetemperature
the slab inside and outside
of the slab
is uniform. Followed by hot rolling theby rolling temperature is 1150 ◦ C, the finishing temperature is
inside and outside is uniform. Followed hot rolling the rolling temperature is 1150 °C, the finishing
controlled at 900 ◦ C. The final rolling thickness is 5 mm and with furnace cooling to room temperature.
temperature is controlled at 900 °C. The final rolling thickness is 5 mm and with furnace cooling to
The hot
room rolled plate The
temperature. is subjected
hot rolled to normalization
plate is subjected treatment at a normalizing
to normalization temperature
treatment at 850 ◦ C
at a normalizing
and the normalizing
temperature at 850 °C time
andwith 8 min and airtime
the normalizing cooling.
withThe8 minnormalized plate is The
and air cooling. pickled by hydrochloric
normalized plate is
acid to remove the surface iron oxide scale, and the pickled sample is cold-rolled
pickled by hydrochloric acid to remove the surface iron oxide scale, and the pickled sample is cold- by a cold rolling mill
and the
rolled bythickness of themill
a cold rolling coldandrolling
the is 1.5 mm.ofThe
thickness theonset
cold temperature
rolling is 1.5 AC mm. 1 of
Thetheonset
sample austenite
temperature
transformation and the end temperature
AC1 of the sample austenite transformation AC 3 of the austenite transformation are
and the end temperature AC3 of the austenite measured on a DSC
differential thermal analyzer to be 591 ◦ C and 736 ◦ C, respectively. Differential Scanning Calorimeter
transformation are measured on a DSC differential thermal analyzer to be 591 °C and 736 °C,
(DSC) analyzer is to use 1 mm thick, radius of (DSC)
1.5 mm small rounds by1 10 ◦ ·min−1 heating speed
respectively. Differential Scanning Calorimeter analyzer is to use mmCthick, radius of 1.5 mm
heat to 1000 ◦ C, and observe the inflection point on the analyzer. The heat treatment process is
small rounds by 10 °C·min heating speed heat to 1000 °C, and observe the inflection point
−1 on the
shown in The Figure 1, treatment
the sampleprocess
is annealed ◦
at 930in Figure
C with 1, 20the
minsample
and quenched to room
analyzer. heat is shown is annealed at 930temperature
°C with 20
then and
annealed in a two-phase region at 625, ◦ C with 30 min, air cooling to room
min quenched to room temperature then650, 675 and
annealed in 700
a two-phase region at 625, 650, 675 and
temperature. ◦ ◦ C, choosing the four temperatures for two
700 °C with 30Because
min, airAC 1 is 591
cooling to C,
roomACtemperature.
3 reaches 736 Because AC1 is 591 °C, AC3 reaches 736 °C,
phase region reverse transformation annealing temperature. ◦ C is austenitic phase region, aim to
choosing the four temperatures for two phase region reverse930 transformation annealing temperature.
fully achieve austenitizing.
930 °C is austenitic phase region, aim to fully achieve austenitizing.

930°C holding 20min

Temperature/°C

625°C/650°C/675°C/700°C holding 30min

AC3=736°C
AC1=591°C

Austenitiziaion ART

Water air
quenching cooling

Holding time/min
Figure 1. Heat treatment process of studied steel.
Figure 1. Heat treatment process of studied steel.
Materials 2018, 11, 1633 3 of 12

Table 1. Composition of studied steel/(wt%).

C Mn Cu Al Si Ni Nb Ti S
0.13 5.4 0.24 0.043 0.072 0.24 0.032 0.017 0.0069

Using a standard specimen with a gauge length size of 50 mm a tensile force of 20 KN, and a
displacement speed of the chuck of 2 mm·min−1 . Tensile tests are carried out on a SHT-4605
microcomputer, controlled electronic universal testing machine to measure the tensile strength,
yield strength and elongation of the studied steel. The heat treatment samples are finely ground
mechanically polished and finally etch with 4% nitric acid. The corroded samples are observed under
QUANTA 650 field emission Scanning Electron Microscopy (SEM). The heat treatment sample is first
mechanically ground to 30~50 µm, then it is punched into a sample with a diameter of 3 mm adopting
a punching machine. The double-spray is used as it is thinner. The electrolyte is a 4% HClO4 alcohol
solution and the temperature of the double spray is −20 ◦ C. The microstructure of the studied steel is
investigated by Tecnai G2F20 Transmission Electron Microscope (TEM). The retained austenite in the
studied steel is measured by the Dutch PANaco X Pert PRO MPD X-ray diffractometer. The studied
steel sample is selected to be 25 mm × 20 mm, and the austenite γ peak (200)γ, (220)γ (311)γ is
selected, three diffraction lines and martensite α peak (200)α, (211)α two diffraction lines, a total of
five diffraction lines are scanned, accurately. Measuring the corresponding diffraction angle 2θ and
cumulative intensity IM , IA , calculating the retained austenite volume fraction with the following
formula [13]:
1 − VC
VA = (1)
1 + G IIM
A

VA is the austenite volume fraction, VC is the volume fraction of the carbide phase content of the
studied steel, IM is the cumulative strength of the martensitic plane diffraction peak in the studied
steel, and IA is the accumulation of the austenite plane diffraction line in the studied steel. G is the
ratio of the intensity related factors corresponding to the austenite plane and the martensite plane.
Calculating one VA for each IM /IA value and the corresponding G value, calculating six VA one by
one, then get in the arithmetic mean. This value is the volume fraction of the retained austenite.

3. Results and Discussion

3.1. Microstructure
Figure 2 depicts an SEM image of studied steel after the reverse-phase transformation annealing
at 625, 650, 675 and 700 ◦ C. Figure 2a shows the SEM image of studied steel after austenitizing water
quenching at 930 ◦ C with 20 min. It could be found that the microstructure after quenching is complete
lath martensite. It can be seen that there are small amounts of dark black martensite lath bundles
and a small amount of carbides in the bundle. Meanwhile, no austenite microstructure is discovered.
From Figure 2b, we can conclude that after quenching and annealing at 625 ◦ C, the lath martensite still
exists. When reverse-phase transformation annealing occurs in the two-phase region, the quenched
martensite lath is broken to form the annealed martensite (ultra-fine grained ferrite), and a small
quantity of carbides are precipitated on the ferrite grain boundary while no carbides are found in the
lath martensite bundle. Meanwhile, the volume fraction of austenite after annealing at 625 ◦ C is 5.09%
and the percent of the content is relatively low. This is because that annealing at 625 ◦ C, it will generate
a large number of carbide precipitation and the precipitation is not completely dissolved, however, the
austenite volume fraction still maintains at 5.09%. Most nucleation regions of austenite are dissolved
in ferritic crystal and carbide, however, a large amount of carbides in Figure 2b are concentrated on
ferritic grain boundary and a small amount of carbides are dissolved in ferritic crystal to form a small
amount of austenite [14]. As the annealing temperature raises to 650 ◦ C, the lath martensite is almost
completely broken to form ultra-fine grained ferrite, as shown in Figure 2c. The strip austenite is shown
Materials 2018, 11, 1633 4 of 12

up inMaterials
the lath beam
2018, of lath
11, x FOR PEERmartensite,
REVIEW and the austenite volume fraction austenite is 10.39%.4 However, of 12
with the increase of the annealing temperature, the carbides do not dissolve completely and, instead, a
smallThe strip austenite
amount of themisare shown up in thein
distributed lath
thebeam of lath
ferrite martensite,
crystal. As theand the austenite
annealing volume fraction
temperature goes up to
◦ austenite is 10.39%. However, with the increase of the annealing temperature, the carbides do not
675 C, the austenite lath becomes wider and the same strip bundle of austenite is combined to form
dissolve completely and, instead, a small amount of them are distributed in the ferrite crystal. As the
bulk austenite, and the volume fraction is increased into 22.34%, as illustrated in Figure 2d. At the same
annealing temperature goes up to 675 °C, the austenite lath becomes wider and the same strip bundle
time,ofthe components
austenite of thetomicrostructure
is combined are ultra-fine
form bulk austenite, grained
and the volume ferrite,isbulk
fraction and strip
increased austenite
into 22.34%, as and
not completely broken lath martensite. As the annealing temperature raises up to 700 ◦ C, martensite
illustrated in Figure 2d. At the same time, the components of the microstructure are ultra-fine grained
rapidly transforms
ferrite, bulk andinto austenite,
strip austenite because
and not such temperature
completely broken is close
lath to the austenite
martensite. single-phase
As the annealing
region temperature.
temperature raisesIt up
is believed thatmartensite
to 700 °C, the higher annealing
rapidly temperature,
transforms the bigger
into austenite, the such
because austenite
volumetemperature
fraction.isWith closethe
to the austeniteofsingle-phase
increment region temperature.
the temperature, the diffusion It rate
is believed
of C andthatMn
the elements
higher is
annealing temperature, the bigger the austenite volume fraction. With the
increased so that the average C and Mn content in austenite decreases [11,15]. Under this situation, increment of the
temperature,
the stability the diffusion
of austenite rate ofsignificantly
decreases C and Mn elements
and theis volume
increasedfraction
so that of theaustenite
average Creduces
and Mn from
content in austenite decreases [11,15]. Under this situation, the stability of austenite decreases
22.34% to 9.32%. Finally, martensite is formed during the cooling process [11]. The final microstructure
significantly and the volume fraction of austenite reduces from 22.34% to 9.32%. Finally, martensite
at 700 ◦ C incorporates ultra-fine grained ferrite, lath martensite and a small amount of austenites,
is formed during the cooling process [11]. The final microstructure at 700 °C incorporates ultra-fine
as shown
grained in ferrite,
Figurelath 2e. martensite and a small amount of austenites, as shown in Figure 2e.

(a) (b) (c)

(d) (e)

FigureFigure 2. SEM
2. SEM image
image after
after annealingtemperature
annealing temperature of
of reverse-phase
reverse-phasetransformation
transformation (a) At
(a)930
At °C ◦ C with
930with
20 min austenitizing quenching; austenitiic reverse anealing 30 min; (b) 625 C; (c) 650 C; (d) 675 ◦ C;
20 min austenitizing quenching; austenitiic reverse anealing 30 min; (b) 625 ◦
°C; (c) 650 °C; ◦
(d) 675 °C;
(e)◦700
(e) 700 C. °C.

FigureFigure 3 depicts
3 depicts thethe
TEMTEMimage
image of of studied
studied steel
steel after
afterthethereverse
reverseannealing
annealingat different
at different
temperatures of 650, 675 and 700 °C◦with austenitizing water quenching at 930 °C. Figure 3a◦ indicates
temperatures of 650, 675 and 700 C with austenitizing water quenching at 930 C. Figure 3a
the TEM image after water quenching for 20 min at 930 °C, and we find that lath martensite
indicates the TEM image after water quenching for 20 min at 930 ◦ C, and we find that lath martensite
microstructure is the completely thick after the water quenching, with average lath width up to 0.5
microstructure
μm. There isarethe completely
many thickinafter
dislocations the water lath
the martensite quenching, with average
bundle along with some lath width up slide
dislocations to 0.5 µm.
Therealong
are many dislocations in the martensite lath bundle along with some dislocations
the dislocation lines to form multi-slip and cross-slip to form dislocation entanglement which slide along the
dislocation lines
increases theto form multi-slip
dislocation density.and
Aftercross-slip
quenching to at
form dislocation
a high entanglement
temperature, the stackingwhich increases
fault energy of the
dislocation
studieddensity. After quenching
steel is relatively high, andat the
a high temperature,
stacking fault is nottheeasy
stacking fault
to carry out.energy of studied steel
The deformation is is
mainly
relatively caused
high, andbythedislocations, and new
stacking fault is notdislocations
easy to carryare formed
out. The asdeformation
shown in Figure 3a. Thecaused
is mainly new by
dislocations, and new dislocations are formed as shown in Figure 3a. The new dislocation resistance is
Materials 2018, 11, x1633
FOR PEER REVIEW 55 of 12
12

dislocation resistance is small. It is necessary to form multiple slips, high stacking fault energy, easy
small. It isrecrystallization,
dynamic necessary to form and multiple
easy toslips, high stacking fault energy, easy dynamic recrystallization,
slippage.
and easy to slippage.
Figure 3b shows that the ultra-fine-grained ferrite after annealing at 650 °C. The average lath
◦
widthFigure
is 0.193b μm shows
whilethatthe the ultra-fine-grained
average lath width of the ferrite after annealing
unbroken martensite at is
650
0.23C.μm. TheThere
average lath
exists a
width is 0.19 µm while the average lath width of the unbroken martensite
large amount of carbides and acres of dislocations between the ferrite and martensite laths. The ultra- is 0.23 µm. There exists
a large amount
fine-grained of carbides
ferrite formed after and annealing
acres of dislocations between the
is in the martensite withferrite and martensite
relatively laths.
high dislocation
The ultra-fine-grained
density. Nevertheless,ferrite formed
after the after annealing
annealing, is in thedensity
the dislocation martensite with relatively
of retained martensite highisdislocation
relatively
density. Nevertheless, after the annealing, the dislocation density of retained
low. It is mainly because that ultra-fine-grained ferrite is formed during reverse-phase transformation martensite is relatively
low. It is mainly
annealing and the because that ultra-fine-grained
dislocation density in martensiteferrite isisformed duringquenching
low during reverse-phase and transformation
reverse-phase
annealing and the dislocation density in martensite is low during
transformation annealing. However, the volume expansion caused by the subsequent cooling of quenching and reverse-phase
transformation
martensitic annealing. However,
transformation process leads the to
volume expansion
boundaries of thecaused by the
ultra-fine subsequent
grained cooling
ferrite and formsof
martensiticlines
dislocation transformation process leadsontothe
which are concentrated boundaries
lath martensiteof the[16,17].
ultra-fine grained ferrite and forms
dislocation lines which are concentrated on the lath martensite
Figure 3c demonstrates the TEM image after annealing at 675 °C. The composition of [16,17].
Figure 3c isdemonstrates
microstructure mainly ultra-fine the grained
TEM image ferrite,after annealingand
lath martensite 675 ◦ C. The
at austenite with composition
different forms. of
microstructure
The average lath is width
mainlyofultra-fine
martensite grained ferrite,
increases lath
into martensite
0.29 and austenite
μm and plentiful with different
of carbides forms.
are dissolved
The average lath width of martensite increases into 0.29 µm and plentiful
on the martensite lath bundle boundary. The dissolution of carbides provides energy for the austenite of carbides are dissolved on
the martensite
nucleation so that laththe
bundle boundary.
austenite appears Thein dissolution of carbides
a lath-like shape at the provides
martensite energy for theboundary
lath bundle austenite
nucleation so that the austenite appears in a lath-like shape at the martensite
[14]. As the annealing temperature increases, the dislocation lines in the ferrite grain boundaries and lath bundle boundary [14].
As the annealing temperature increases, the dislocation lines in the
martensite laths almost disappear. With the annealing temperature rises to 700 °C, the lath-like ferrite grain boundaries and
martensite laths ◦ C, the lath-like
microstructure of almost disappear.
alternating light andWithdarkthe annealing
martensite temperature
laths are clearlyrises to as
visible, 700revealed in Figure
microstructure of alternating light and dark martensite laths are clearly
3d. The average lath width of martensite serves as 0.32 μm, and a small amount of lath martensite visible, as revealed in Figure 3d.
The average
ruptures lath width
to form of martensite
ultra-fine grained serves
ferrite.asOnly
0.32 µm, and a small
a handful amount microstructure
of austenite of lath martensite ruptures
exists and
to form ultra-fine grained ferrite. Only a handful of austenite microstructure
carbide precipitation is less. As the annealing temperature increases, the dislocation lines and exists and carbide
precipitation
dislocation is less.decrease
density As the annealing
so that C temperature
and Mn cannot increases,
diffuse themoredislocation lines and dislocation
into the austenite. Due to the
density decrease
inability of C, Mnso that C and
elements Mn cannot
to diffuse morediffuse more into
into austenite the austenite.
which the stabilityDue to the
is too inability
weak of C,
to reserve
Mn elements to
to room temperature. diffuse more into austenite which the stability is too weak to reserve to room temperature.

(a) (b)

(c) (d)
Figure 3. TEM
TEM image
image after
after annealing
annealing temperature
temperature of reverse-phase transformation.
transformation. (a) At 930 °C ◦ C with

20 min austenitizing quenching; austenitiic reverse anealing

anealing 30
30 min;
min; (b)
(b) 650 ◦ ◦ C; (d) 700 ◦°C.
C; (c) 675 °C;
650 °C; C.
Materials 2018, 11, 1633 6 of 12
Materials 2018, 11, x FOR PEER REVIEW 6 of 12

Figure ◦
Figure 4a,b
4a,b are
arethe
theTEM
TEMimage
imageofofaustenite
austeniteafter
afterannealing
annealing ofof
the studied
the studiedsteel at 650
steel at 650C.°C.
Figure 4c
Figure
illustrates the austenite diffraction spot. Austenite mainly appears in ferrite grain boundaries
4c illustrates the austenite diffraction spot. Austenite mainly appears in ferrite grain boundaries and and
martensite lath bundles
martensite lath bundlesin inthe
theform
formofofbulk.
bulk. During
During thethe reverse-phase
reverse-phase transformation
transformation annealing,
annealing, the
the
enrichment of C and Mn elements contribute increment into austenite stability [17]. FigureFigure
enrichment of C and Mn elements contribute increment into austenite stability [17]. 4d
4d shows
shows the TEM image of dislocation entanglements after annealing at 650 ◦ C. Admittedly, the studied
the TEM image of dislocation entanglements after annealing at 650 °C. Admittedly, the studied steel
steel after annealing at 650 ◦ does not completely eliminate dislocations and there exists more
after annealing at 650 °C does C not completely eliminate dislocations and there exists more dislocation
dislocation lines in the
lines in the ultra-fine ultra-fine
grained grained
ferrite. Theseferrite. These
dislocation dislocation
lines lines
slip to form slip to form
dislocation dislocation
entanglements
entanglements
and the dislocationand the dislocation
density density is large.
is tremendously tremendously large.

(a) (b)

(c) (d)
TEMimage
Figure 4. TEM imageofofaustenite
austeniteininreverse
reverse transformation
transformation annealing
annealing °C.◦(a)
at 650
at 650 C. bright-field;
(a) bright-field;
(b)
(b) dark-field;
dark-field; (c) austenite
(c) austenite diffraction
diffraction spot;
spot; (d) (d) dislocation
dislocation entanglement.
entanglement.

Figure ◦ C.
Figure 55reveals
revealsthethe austenitic
austenitic TEM TEM images
images of different
of different forms forms after annealing
after annealing at 675 °C.atThe
675lath-
The lath-like with
like austenite austenite withorientation
the same the same orientation
combines tocombines
form bulkto form bulk
austenite and austenite and there
there are stacking are
faults
stacking faults and austenite twins in bulk austenite as illustrated in Figure 5a.
and austenite twins in bulk austenite as illustrated in Figure 5a. Figure 5b demonstrates the bulkFigure 5b demonstrates
the bulk austenite
austenite diffractiondiffraction
spot. Figurespot.5c,dFigure 5c,dthe
illustrate illustrate
lath-liketheaustenite
lath-likemorphology
austenite morphology and
and diffraction
diffraction spots, separately. The austenite volume fraction is relatively high
spots, separately. The austenite volume fraction is relatively high when the annealing at the when the annealing at
the temperature of 675 ◦
temperature of 675 °C. C. Since
Since thethe nucleation
nucleation andgrowth
and growthofofaustenite
austeniteinvolves
involves thethe migration
migration of of
interfacial boundaries to the ferrite phase and the diffusion of interstitial C atoms
interfacial boundaries to the ferrite phase and the diffusion of interstitial C atoms and substituted Mn and substituted
Mn atoms
atoms between
between the the ferrite
ferrite andand austenite
austenite phases
phases gapgaptype.
type.[14,16,17].
[14,16,17].TheThediffusion
diffusioncoefficient
coefficient of
of C
C
atom
atom and
and replacement
replacement Mn Mn atom
atom inin ferrite
ferrite is
is greater
greater than
than inin austenite.
austenite. As As aa result,
result, as
as the
the annealing
annealing
temperature
temperature increases,
increases, the
the alloying
alloying elements
elements cancan diffuse
diffuse rapidly
rapidly which
which will
will lead
lead toto the
the final
final alloying
alloying
elements
elements being
being continuously
continuously diffused
diffused andand enriched
enriched from
from ferrite
ferrite to
to austenite
austenite [18].
[18].
Materials 2018, 11, 1633 7 of 12
Materials 2018, 11, x FOR PEER REVIEW 7 of 12

(a) (b)

(c) (d)
Figure 5. Morphology TEM image of austenite at 675 ◦°C C reverse transformation annealing of studied
steel (a) bulk austenite; (b) bulk austenite diffraction spot; (c) strip austenite; (d) strip austenite
diffraction spot.

3.2. Mechanical Properties

3.2. Mechanical Properties
The variation of
The variation of mechanical
mechanical properties
properties of studied steel
of studied steel with
with annealing
annealing temperature
temperature is is illustrated
illustrated
in
in Figure
Figure 6. The variation
6. The variation of of tensile
tensile strength
strength and and yield
yield strength
strength are
are indicated
indicated inin Figure
Figure 6a.6a. As
As the
the
annealing
annealing temperature increases, the tensile strength increases continuously, obtaining 1360 MPa at
temperature increases, the tensile strength increases continuously, obtaining 1360 MPa at
700 ◦ C while the yield strength decreases constantly, gaining 825 MPa at 625 ◦ C. The elongation and
700 °C while the yield strength decreases constantly, gaining 825 MPa at 625 °C. The elongation and
strength-ductility combination are
strength-ductility combination are shown
shown in in Figure
Figure 6b. The elongation
6b. The elongation and and the
the strength-ductility
strength-ductility
combination
combination increase first, which gradually decrease with the annealing temperature increases,
increase first, which gradually decrease with the annealing temperature increases, andand
the maximum value is obtained at 675 ◦ C (22% and 23.1 GPa %, respectively). Figure 6c is X-ray
the maximum value is obtained at 675 °C (22% and 23.1 GPa %, respectively). Figure 6c is X-ray
diffraction
diffraction patterns
patternsat atdifferent
differentannealing
annealingtemperatures,
temperatures, showing
showing that thethe
that retained austenite
retained peaks
austenite are
peaks
the highest and the cumulative strength is the highest after annealing at 675%. Figure
are the highest and the cumulative strength is the highest after annealing at 675%. Figure 6d indicates 6d indicates the
variation of annealing
the variation temperature
of annealing on theon
temperature retained austenite
the retained volumevolume
austenite fractionfraction
and the andstrength-ductility
the strength-
combination, which both increase first and then decrease with the increase of
ductility combination, which both increase first and then decrease with the increase of temperature. temperature. With the
retained austenite volume fraction reaches 22.34%, and the strength-ductility
With the retained austenite volume fraction reaches 22.34%, and the strength-ductility combination combination gets to
23.1
gets GPa % at
to 23.1 the%
GPa maximum. Figure 6eFigure
at the maximum. is an engineering stress-strain
6e is an engineering curve withcurve
stress-strain different
withannealing
different
temperatures. After annealing with ART, the tensile strength is 1360 MPa;
annealing temperatures. After annealing with ART, the tensile strength is 1360 MPa; the lowest the lowest is 890 isMPa,
890
the engineering strain is 22% and the lowest
MPa, the engineering strain is 22% and the lowest is 12%. is 12%.
Materials 2018, 11, 1633 8 of 12
Materials 2018, 11, x FOR PEER REVIEW 8 of 12

Tensile strength 40 40
1400

Tensile strength×Elongation/GPa%
Yield strength Elongation
35 TS×E 35
1200 30 30
Strength/MPa

Elongation/%
25 25
1000
20 20
800
15 15

600 10 10

630 660 690 5 5

620 640 660
680 700
Annealing temperature/°C Annealing temperature/°C
(a) (b)
30 30

Retained austenite volume fraction/%

Elongation and strength-ductility combination

Tensile strength×Elongation/GPa%
RA%
(211)α
(200)α 25 25
(200)γ (220)γ (311)γ
700°C
20 20
Intensity

675°C
15 15

10 10
650°C
5 5

625°C 0 0
630 660 690
60 80 100 120
2θ/° Annealing temperature/°C
(c) (d)
1600
700°C
1400
Engineering stress/MPa

1200 675°C

1000 650°C
800 625°C
600
400
200
0
0 5 10 15 20 25 30 35 40
Engineering strain/%
(e)

FigureFigure 6. Effect
6. Effect of reverse-phasetransformation
of reverse-phase transformation annealing
annealing temperature
temperature on mechanical properties
on mechanical of
properties
experimentalsteel.
of experimental steel. (a)
(a) tensile
tensile strength
strength and
and yield
yieldstrength;
strength;(b)(b)elongation andand
elongation strength-ductility
strength-ductility
combination;
combination; (c) volume
(c) volume fraction
fraction ofof retainedaustenite
retained austenite and
and strength-ductility
strength-ductility combination; (d) XRD
combination; (d) XRD
patterns and the measured RA volume fractions of the samples at different annealing temperatures;
patterns and the measured RA volume fractions of the samples at different annealing temperatures;
(e) Engineering stress–strain curves of the different annealing samples.
(e) Engineering stress–strain curves of the different annealing samples.
With the increase of the temperature, the tensile strength increases. However, this phenomenon
With the increase of the temperature, the tensile strength increases. However, this phenomenon is
is not conspicuous when the temperature anneals from 625 to 650 °C. As depicted in Figure 6, with
not conspicuous when the temperature anneals from 625 to 650 ◦ C. As depicted in Figure 6, with the
the annealing temperature accesses to 675 °C, the austenite volume fraction reaches its maximum at
annealing temperature
22.34%. accesses
The TRIP effect to 675 ◦ C,
is enhanced the austenite
when volume
the stability fraction
of austenite reaches
stays in theitsroom
maximum at 22.34%.
temperature
The TRIP effect is enhanced when the stability of austenite stays in the room temperature and the
tensile deformation is improved. The dislocation entanglement exists at 675 ◦ C, as shown in Figure 5c.
During the slip process, dislocation interacts with each other and the process generates dislocation
entanglements and plugging, which prevents the further movement and enhances the tensile strength
Materials 2018, 11, x FOR PEER REVIEW 9 of 12

and the2018,
Materials tensile deformation is improved. The dislocation entanglement exists at 675 °C, as shown
11, 1633 in
9 of 12
Figure 5c. During the slip process, dislocation interacts with each other and the process generates
dislocation entanglements and plugging, which prevents the further movement and enhances the
of experimental
tensile strength steel. Figure 7a,b steel.
of experimental illustrates
Figurethe7a,b
TEMillustrates
morphology the and
TEM energy spectrumand
morphology of Nb and
energy
Ti precipitates. From those two figures, we can conclude that from 200 to
spectrum of Nb and Ti precipitates. From those two figures, we can conclude that from 200 to 300 300 nm, precipitates are
dispersed
nm, in the ferrite
precipitates matrix. Under
are dispersed this ferrite
in the circumstance,
matrix.the dislocation
Under movement is retrained
this circumstance, and the
the dislocation
tensile strength is improved. At the same time, with the temperature increases to 700 ◦ C, martensite
movement is retrained and the tensile strength is improved. At the same time, with the temperature
rapidly transforms
increases into austenite
to 700 °C, martensite because
rapidly this temperature
transforms is close
into austenite to the
because temperature
this temperature ofisaustenite
close to
single-phase
the temperature region. However,
of austenite the component
single-phase of C
region. and Mn in
However, theaustenite
component decreases to aMn
of C and low
inlevel, and
austenite
this causes the stability of austenite to reduce into a lower stage. Finally, during the
decreases to a low level, and this causes the stability of austenite to reduce into a lower stage. Finally, cooling process,
almost the
during the whole
coolingmartensite is completely
process, almost the wholeformed. Considering
martensite the analysis
is completely andConsidering
formed. demonstrations the
above, we find that the tensile strength reaches the peak at 700 ◦ C.
analysis and demonstrations above, we find that the tensile strength reaches the peak at 700 °C.

(a)
Mn
Fe
800 Fe
Fe
600
Counts

Nb
400
Nb Nb
200 N Nb
Fe Nb
C Nb
Ti Ti Mn Nb
Nb
0.0 10 20
Energy (keV)

(b)
PrecipitationofofNb,
Nb,TiTicarbides
carbidesafter
afterannealing
annealingatat675
675 ◦ C. (a) the TEM morphology of Nb,
Figure 7. Precipitation °C. (a) the TEM morphology of Nb, Ti
Ti carbides;
carbides; (b)(b) spectral
spectral diagram
diagram of of Nb,
Nb, Ti Ti carbides.
carbides.

As the
As the annealing temperature increases,
annealing temperature increases, thethe grain
grain constantly
constantly grows
grows andand the
the microstructure
microstructure
becomes more
becomes more uniform.
uniform. Due Due to to the
the recrystallization
recrystallization of of crystal
crystal grains, even the
grains, even the dislocations
dislocations areare
rearranged, the dislocation density reduces and the dislocation entanglement
rearranged, the dislocation density reduces and the dislocation entanglement decreases during decreases during tensile
deformation,
tensile which which
deformation, lowerslowers
the yield
the strength [19]. With
yield strength the increase
[19]. With of annealing
the increase of annealingtemperature,
temperature,the
average grain size of ferrite at 650 ◦ C acts as 0.22 µm and 0.30 µm at 675 ◦ C, respectively. Calculating by
the average grain size of ferrite at 650 °C acts as 0.22 μm and 0.30 μm at 675 °C, respectively.
the Hall–Petch
Calculating by formula, we could
the Hall–Petch conclude
formula, wethat with
could the increment
conclude that withof the
the average
increment sizeofofthe
grain, the yield
average size
strength ◦
of grain, of
thethe material
yield strengthdecreases [20]. At 700
of the material C, although
decreases [20]. Atthe700austenite volume
°C, although thefraction
austenitedecreases,
volume
the formeddecreases,
fraction ultra-fine-grained
the formedferrite provides better elongation
ultra-fine-grained ferriteandprovides
spontaneously
betterstimulates
elongationthe yield
and
strength to decrease.
spontaneously stimulates the yield strength to decrease.
From Figure
From Figure 6d,
6d, we
we find
find that
that with
with the
the annealing
annealing temperature
temperature increases,
increases, the
the variational
variational trends
trends of
of
austenite volume fraction and the strength-ductility combination are similar. All
austenite volume fraction and the strength-ductility combination are similar. All of the austenite of the austenite volume
fraction, fraction,
volume elongation and strength-ductility
elongation combination
and strength-ductility increase first
combination and then
increase first decrease.
and then When the
decrease.
annealing temperature increases from 625 to 675 ◦ C, the ultra-fine-grained ferrite and austenite formed
When the annealing temperature increases from 625 to 675 °C, the ultra-fine-grained ferrite and
by reversing
austenite phase
formed byannealing,
reversing which provides better
phase annealing, which elongation. Nevertheless,
provides better the Nevertheless,
elongation. austenite volume the
fraction is volume
only 5.09%. Withis theonly
annealing ◦
austenite fraction 5.09%. atWith
625 theC while the strength-ductility
annealing at 625 °C whilecombination represents
the strength-ductility
relatively low.represents
combination When therelatively
annealing temperature
low. When theincreasing, the austenite increasing,
annealing temperature volume fraction rises to
the austenite
10.48% at 650 ◦ C and reaches to its peaked of 22.34% at 675 ◦ C. It is also well known that with the
volume fraction rises to 10.48% at 650 °C and reaches to its peaked of 22.34% at 675 °C. It is also well
increment
known thatofwith
austenite volume fraction,
the increment the TRIP
of austenite volume effect facilitates
fraction, the martensitic
the TRIP transformation
effect facilitates more
the martensitic
easily. After the martensitic transformation, the partial strength is naturally improved whereas it is
Materials 2018, 11, x FOR PEER REVIEW 10 of 12
Materials 2018, 11, 1633 10 of 12
transformation more easily. After the martensitic transformation, the partial strength is naturally
improved whereas it is difficult to continue deformation. Because the deformation transforms to the
difficult
parts to continue
where deformation.
the martensite Becausehappens,
seldom the deformation transforms
the formation of tonecking
the partsiswhere the martensite
delayed and the
seldom happens, the formation of necking is delayed and the concentration
concentration at the crack tip is loosened. When this phenomenon occurs, the formation of at the crack tip is loosened.
When this phenomenon
microcracks is preventedoccurs, so that thethe formation
elongationof is microcracks is prevented
increased [15,21,22]. The Nb so that
and the elongation
Ti carbides from is
increased [15,21,22]. The Nb and Ti carbides from 200 to 300 nm precipitates at 675 ◦ C and they interact
200 to 300 nm precipitates at 675 °C and they interact with dislocations as a second phase particle.
with will
This dislocations
hinder the as acontinuing
second phase slip particle. This will
of dislocations andhinder
increasethethe
continuing slip ofof
strengthening dislocations
material. With and
increase
the the strengthening
precipitated spacing reaches of material. With the
to a certain precipitated
critical spacing reaches
value, dislocations willto a certain
bypass thecritical value,
precipitated
dislocations will bypass the precipitated phase particles and maximum
phase particles and maximum strengthening effect will be generated [23]. At 700 °C, the austenitic strengthening effect will be
generatedgradually
[23]. At 700 ◦ C, the austenitic
stability deteriorated due tostability gradually
the decrease of C deteriorated due to the decrease
and Mn components. Therefore,of C and
the
◦ can
elongation as well as the strength-ductility combination at 700 °C can be significantly reduced. CSo,
Mn components. Therefore, the elongation as well as the strength-ductility combination at 700 it
beeffectively
is significantly reduced.the
to increase So,strength-ductility
it is effectively tocombination
increase the strength-ductility
of studied steel bycombination
enhancing the of volume
studied
steel by enhancing
fraction of austenitethe volume fraction of austenite [24].
[24].
Figure 8a,b are tensile
Figure 8a,b are tensile fracture fracture morphology
morphology after after reverse-phase
reverse-phase transformation
transformation annealing
annealing at at 625
625
and 650 ◦ C, respectively. There are smaller dimples at the fractures of steel annealing at 625 ◦ C and
and 650 °C, respectively. There are smaller dimples at the fractures of steel annealing at 625 °C and
◦ C and some brittle intergranular fractures appear in the fracture morphology. Figure 8c shows
650 °C
650 and some brittle intergranular fractures appear in the fracture morphology. Figure 8c shows
the fracture
fracture after
after annealing
annealing at at 675 ◦ C. The smaller dimples mainly belong to ductile fracture at 675 ◦ C.
675 °C.
the The smaller dimples mainly belong to ductile fracture at 675 °C.
In addition, at 700 ◦ C, the dimples almost completely disappear; the fracture are mainly based on
In addition, at 700 °C, the dimples almost completely disappear; the fracture are mainly based on
brittle intergranular
brittle intergranularfracturesfracturesand andare arealso
alsocleavage
cleavage streaks.
streaks.ByByobserving
observing the the
fracture morphology
fracture morphology and
mechanical properties, we find that with the increment of temperature,
and mechanical properties, we find that with the increment of temperature, the increment of tensile the increment of tensile strength
is not significant
strength from 625 tofrom
is not significant 650 ◦625
C. After
to 650the °C.
reverseAftertransformation annealing, the plasticity
the reverse transformation annealing, of the
the
steel is low, and the type of fracture in the surface is intergranular fracture.
plasticity of the steel is low, and the type of fracture in the surface is intergranular fracture. As the As the temperature raises
to 650 ◦ C, theraises
temperature elongation
to 650 becomes poor. The becomes
°C, the elongation austenitepoor.volume Thefraction
austenitepeaks
volume
◦ C, and we can
at 675fraction peaks at
see that more dimples ◦ ◦ C, the tensile
675 °C, and we can seeinthat the more
fracture, the elongation
dimples reaches
in the fracture, theitselongation
peak at 675reachesC. At its700peak at 675 °C.
strength
At 700 °C, reaches its peak
the tensile with the
strength lowest
reaches its elongation.
peak with the Thelowest
exhibition of fracture
elongation. The intergranular fracture
exhibition of fracture
and cleavage streaks
intergranular fractureare andillustrated
cleavage in Figureare
streaks 8d.illustrated in Figure 8d.

(a) (b)

(c) (d)

Tensile fracture morphology at reverse-phase transformation

Figure 8. Tensile transformation annealing
annealing temperature
temperature (SEM)
(SEM)
◦ C; ◦ C; (c) 675 ◦ C; (d) 700 ◦ C.
(a) 625 °C; (b) 650 °C; (c) 675 °C; (d) 700 °C.
Materials 2018, 11, 1633 11 of 12

4. Conclusions
(1) The main microstructure of steel is lath martensite after quenching. The microstructure
incorporates ultra-fine grained ferrite, lath martensite and different morphology austenite
microstructure after reverse-phase transformation annealing. With the increment of reverse-phase
transformation annealing temperature, the microstructure is mainly lath martensite and ultra-fine
grained ferrite at 625 ◦ C. The austenite volume fraction is only 5.09%. When the annealing temperature
increases to 650 ◦ C and 675 ◦ C, the different morphology and strip shape appears on the ferrite
grain boundary and the martensite lath bundle boundary. The bulk austenite exhibits austenite
stacking fault and twin crystal. At 700 ◦ C, the austenite volume fraction reduces into 9.32% and the
mainly components of the microstructure are ultra-fine grained ferrite, lath martensite and minority
of austenite.
(2) With the increment of annealing temperature, the tensile strength increases but the yield
strength declines. Both of the elongation and the strength-ductility combination increases firstly and
then decreases. The intergranular fracture at 625 ◦ C proves that the strength should be high while
the elongation is poor in the reverse-phase transformation annealing. When the temperature rises to
650 ◦ C, there exists more mixed fractures in the fractured dimples. At 675 ◦ C, the fracture is ductile
fracture and the elongation and strength-ductility combination become higher than before. At 700 ◦ C,
the tensile strength reaches the peak and the elongation achieves its lowest value. The main fracture
has an intergranular fracture and cleavage streaks.
Quenching at 930 ◦ C with 20 min and at 675 ◦ C with 30 min reverse-phase transformation
annealing, the austenite volume fraction increases up to 22.34%. Beside a large number of dislocation
entanglements, there exists some precipitation composited with 200 nm~300 nm Nb, Ti carbides.
The best comprehensive mechanical properties are obtained under the process. The tensile strength is
1100 MPa, the elongation is 22% and the strength-ductility combination is 23.1 GPa %.

Author Contributions: Conceptualization, Y.Z. and L.F.; Methodology, L.F.; Validation, B.L. and L.F.; Formal
Analysis, L.F. and B.L; Investigation, Y.Z.; Resources, B.L.; Data Curation, Y.Z.; Writing: Original Draft Preparation,
Y.Z.; Writing: Review and Editing, L.F. and B.L.; Supervision, L.F.
Funding: This research was funded by [National Natural Science Foundation of China] grant number [51661026],
[China Postdoctoral Science Foundation] grant number [2016M602914XE], [Advanced Education Research Project
in Inner Mongolia Autonomous Region] grant number [NJZZ18076].
Conflicts of Interest: The authors declare no conflict of interest.

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