Materials Science & Engineering A 669 (2016) 437–446

Contents lists available at ScienceDirect

Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

On the work-hardening behaviour of a high manganese TWIP steel

at different deformation temperatures
Vadim Shterner, Ilana B. Timokhina, Hossein Beladi n
Institute for Frontier Materials, Deakin University, Geelong, Victoria 3216, Australia

art ic l e i nf o a b s t r a c t

Article history: In the current study, the work-hardening behaviour of a high manganese TWIP steel was investigated at
Received 17 December 2015 different deformation temperatures. At room temperature, the steel exhibited an excellent combination
Received in revised form of mechanical properties due to a unique work-hardening behaviour. There were four distinct stages
20 April 2016
observed in the work-hardening behaviour as a result of complex dynamic strain induced micro-
Accepted 25 May 2016
Available online 27 May 2016
structural reactions consisted of dynamic recovery, dislocation dissociation, stacking fault formation,
mechanical twining and dynamic strain aging. An increase in the deformation temperature significantly
Keywords: influenced the microstructure evolution, resulting in a remarkable alteration in the work-hardening
Work-hardening behaviour behaviour. Consequently, the mechanical properties of the TWIP steel were gradually deteriorated with
Temperature
the deformation temperature. The mechanical twins appeared to have a restricted influence on the work-
Mechanical twinning
hardening behaviour of the TWIP steel at room temperature and remarkably diminished with the
TWIP steel
Stacking faults temperature. The enhanced work-hardening behaviour was mostly attributed to the interaction of glide
Dynamic strain aging dislocations with stacking faults.
& 2016 Elsevier B.V. All rights reserved.

1. Introduction experiment revealed that mechanical twinning contribution to

Development of new materials to improve the strength-ducti-
lity balance led to a recent development of high manganese
TWinning Induced Plasticity (TWIP) steels [1–3]. This type of steel
can offer  1 GPa ultimate tensile strength combined with  50%
elongation at room temperature [1–3]. These exceptional me-
chanical properties at room temperature are due to the remark-
able work-hardening behaviour of the TWIP steel [1–5].
The work-hardening of TWIP steel is mostly attributed to the
nano-scale mechanical twins formed in austenitic microstructure
during straining [5–10]. Mechanical twins contribute to the plastic
strain directly by inducing back stress, so called Bauschinger effect
[11,12], and indirectly through the formation of obstacles against
the dislocation motion, which reduces the mean free path and
enhances the dislocation multiplications, referred as the dynamic
Hall-Petch effect [6–10]. Although the contribution of mechanical
twins to the work-hardening behaviour of TWIP steels is well-
known [4,11,13–31], other microstructural phenomena on strain-
ing may influence the work-hardening behaviour, such as stacking
faults (SFs) formation [27,32], clustering and short range ordering
(SRO) of solute atoms, [25,33,34] and dynamic strain aging (DSA)
[4,35]. Moreover, recent study [36] using synchrotron XRD
n
Corresponding author.
E-mail address: hossein.beladi@deakin.edu.au (H. Beladi).
flow stress is very limited and the enhanced work-hardening can
be attributed to the forest hardening resulted by extensive dis-
location evolution.
In a number of publications [4,35], the DSA effect was con-
sidered as a main contributor to the enhanced work-hardening
behaviour of the TWIP steel. The DSA effect occurs only in the
explicit temperature range, and the work-hardening behaviour
decreases at the temperatures above and below that range [4,35].
It has also been shown [35] that a short range reorientation of the
C-Mn couples, which tend to pin the dislocations and prevent
them from gliding, can contribute to the work-hardening. To un-
derstand the clustering and short range ordering in high-Mn TWIP
steels, C and Mn distribution was analysed using atom probe to-
mography [25,34], which did not reveal any clear conclusion.
There have been several attempts to model the constitutive
behaviour and/or the work-hardening behaviour in austenitic
metals with low SFE [8–11,23,24,29,30,37–42] and all the models
rely on the presence of the mechanical twins in the micro-
structure. In addition to the mechanical twinning, some models
considered the DSA effect [29] or dislocation substructure evolu-
tion [24] such as highly dense dislocation walls or dislocation cells
as a contributor to the enhanced work-hardening behaviour.
The ambiguity in the contribution of the mechanical twinning
to the work-hardening behaviour may also be related to the size of
the mechanical twins and/or to the characterisation technique
approach used to analyse the twinning. Each characterisation

http://dx.doi.org/10.1016/j.msea.2016.05.104
0921-5093/& 2016 Elsevier B.V. All rights reserved.
438 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446
method has its own advantages and limitations. For example,
optical microscopy [27] could be used to characterize a large area
but could not resolve the nano-scale twins. Another method ex-
tensively used [4,6,10,17,21,29,40] was TEM, which can resolve the
nano-twins, however the observation area is limited. Alternative
method was scanning electron microscopy (SEM) in conjunction
with EBSD detector [13,14,17,22,23,28], which can cover a larger
area but could not successfully reveal the twin thickness of less
than 100 nm. A newly developed Electron Channelling Contrast
Imaging (ECCI) technique [21,24,25], overcomes these limitations.
However, the observations of twins appeared to be limited for the
grains with specific orientations [32,43,44].
The current paper will meticulously investigate the micro-
structure of TWIP steel, in particularly mechanical twins, formed
during deformation at different temperatures. The microstructure
then would be correlated with the work-hardening behaviour to
understand the extent of microstructural features contribution to
the work-hardening behaviour at different stage of straining.
2. Experimental procedure
The TWIP steel used in this study was provided by POSCO Steel,
South Korea. The composition of steel was Fe-18Mn-0.6C-1Al
(wt%). The average austenite grain size was about 2.5 70.2 mm.
The standard tensile specimens with a gauge length of 30 mm
were wire cut from sheet product, perpendicular to the rolling
direction, with a thickness of 1.25 mm. The grip section of a tensile
sample was modified to be wider than the standard grip area to
prevent any sliding during the tensile experiment. The tensile
experiments were conducted at a strain rate of 10 3 s 1 using
Instron tensile test machine with 30 kN load cell and at the tem-
perature range of ambient ≤T [°C ] ≤ 400°C (room temperature, 100,
200, 300, 400 °C). To examine the microstructural evolution dur-
ing straining, interrupted tensile tests were performed at testing
temperatures of ambient, 100 and 200 °C.
Mechanical twinning is a stress-assisted mechanism. However,
as stress and strain are interdependent, the analysis of the me-
chanical twinning as a function of strain does not change the
nature of the results. Therefore, it was easier to interrupt the tests
at a given strain level and analyse the evolution of the mechanical
twinning parameters as a function of strain.
At ambient temperature, the tensile tests were interrupted at a
strain of 0.04, 0.1, 0.2, 0.3, 0.4 and fracture, which was equal to
0.5 of true strain. At 100 °C, the tensile tests were interrupted at
0.1 true strain intervals (i.e. 0.1, 0.2, 0.3, 0.4 and fracture, which
occurred at about 0.5 of true strain). At 200 °C, the tensile tests
were interrupted at a true strain of 0.1, 0.2, 0.25, 0.3, 0.35 and
fracture, corresponding to about 0.4 of true strain. Four tensile
samples were tested for each temperature conditions. The samples
used for microstructural characterisation were cut in width of
10 mm from the middle of the sample or about 5 mm away from
the fracture edge.
The samples at room temperature were characterised using
transmission electron microscopy (TEM) by Jeol 2100 with the
voltage of 200 V. The TEM samples were sliced (2–3 slices from
each sample) in the longitudinal (tensile) direction and manually
ground to a thickness of  70 mm. They were then electro-polished
with 5% of perchloric acid in methanol using a twin-jet Tenupol
unit, operating at 50 V and the temperature of 25 °C. Although
TEM is a very powerful technique to reveal the mechanical twin-
ning and dislocation substructure development, it was not possi-
ble to characterise the extent of twinning as a function of strain
statistically.
To overcome this problem, SEM equipped with AsB detector
was employed to statistically examine the microstructure
evolution of TWIP steel at different deformation conditions.
The microstructure characterisation at different tensile testing
conditions was performed using Zeiss Supra 55VP SEM operating at
20 kV in conjunction with the angle selected backscattered (AsB)
detector. AsB detector empowers to reveal nano-scale mechanical
twinning. This enables to statistically analyse nano-scale mechan-
ical twinning in a large area. The microstructure examination was
conducted on 26 SEM images containing a total of more than 100
grains covering an area of about 300 mm2 at each deformation
condition. The volume fraction of twinned grains and the volume
fraction of mechanical twins were measured using a point counting
technique with a statistical significance of po0.05 [45].
The work-hardening rate was estimated at all tensile testing
temperatures using Eq. (1):
∂σ
θ=
∂ε (1)
where θ is the work-hardening rate and ∂σ and ∂ε are the differ-
entials of the engineering stress and strain, respectively. The data
were smoothened every 25 points to reduce the serration.
3. Results
3.1. Mechanical properties of the samples deformed at different
temperatures
The TWIP steel revealed unique mechanical properties at room
temperature, having a yield strength (YS) of 500 MPa, ultimate
tensile strength (UTS) of  1000 MPa and a total elongation (TE) of
 60% (Figs. 1 and 2). Similar uniform and total elongations in-
dicate that the deformation was mostly uniform and ultimate
tensile stress occurred at a strain level close to the fracture (Fig. 2
(a)). The tensile testing temperature significantly affected the
mechanical behaviour of the TWIP steel (Figs. 1 and 2). The YS and
UTS continuously decreased as the temperature increased from
ambient temperature to 400 °C. The TE showed a slight increase at
100 °C, followed by a significant drop at higher tensile tempera-
tures of 200, 300 and 400 °C (Fig. 2(a)). Similar to the room tem-
perature condition, the uniform elongation (UE) was close to the
total elongation at all elevated temperature testing conditions,
suggesting that the deformation was mostly uniform at all tensile
temperatures (Fig. 2(a)). A decrease in both elongation and
strength with an increase in the tensile testing temperature re-
sulted in a significant deterioration in the strength-ductility bal-
ance of the TWIP steel, represented by the UTS and total elonga-
tion (Fig. 2(b)).
1800
Room temperature 100 C
o
1500
True stress (MPa)
o
200 C
1200
o
300 C
900
o
400 C
600
300
0
0.0 0.1 0.2 0.3 0.4 0.5
True strain
Fig. 1. True stress-strain curves at different tensile testing temperatures.
 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446
Fig. 2. (a) Mechanical properties of TWIP steel (i.e. yield strength, ultimate tensile strength (UTS), total and uniform elongations) and (b) the strength-ductility balance of
TWIP steel represented by the product of UTS and total elongation (TEL), at different tensile testing temperatures.
The stress-strain curves revealed the serration for all tensile
testing temperatures, although the extent of serration was sig-
nificantly influenced by the temperature (Fig. 1). The serration was
the most prominent at 100 °C and initiated at a true strain level of
about 0.15, showing continuously growing amplitude with the
deformation (Fig. 1). For other deformation temperatures, the
serration was seen only at a very late stage of the deformation (e.g.
a true strain level of about 0.4 and above at room temperature,
Fig. 1).
3.2. Work-hardening behaviour during tensile testing at different
temperatures
The work-hardening behaviour curve, i.e. dσ /dε vs. ε (Fig. 3,
Table 1) of TWIP steel at room temperature can be divided into
four stages: (I) a sharp decrease in the work-hardening until it
reached a minimum value of 2800 MPa at a true strain of about
0.025; (II) a gradual increase in the work-hardening with the de-
formation up to a true strain of about 0.05; (III) plateau behaviour
from strain of 0.05 up to a true strain of about 0.07. During stage
III, the work-hardening value remained almost constant
(  2800 MPa); and (IV) a gradual decrease with local fluctuation in
the overall work-hardening behaviour with straining until the
fracture occurred (Fig. 3(a)).
The tensile testing temperature had a vital effect on the work-
hardening behaviour, influencing stages (II) and (III), (Table 1). The
stages (II) and (III) gradually diminished with an increase in the
tensile testing temperature up to 200 °C (Fig. 3(b) and (c)), above
which these stages were nearly disappeared (Fig. 3(d) and (e)). At
the tensile testing temperature of 300 and 400 °C, the work-
hardening behaviour showed only the stages (I) and (IV) (Table 1,
Fig. 3d, e).
3.3. Characterisation of the microstructure development at different
deformation conditions
The TEM in the current study was used to reveal the nano-scale
twins and the dislocation substructure development at each stage
of deformation. At the as-received condition, the TEM showed the
presence of annealing twins, having a thickness of 0.2–1 mm
(shown by white arrows in Fig. 4). An increase in strain to 0.04 led
to the formation of dislocations, stacking faults (Fig. 5) and me-
chanical twins (Fig. 6). However, the stacking faults formation was
the predominant deformation mechanism at this condition. The
diffraction pattern analysis confirmed the formation of stacking
faults, which were mostly nucleated at the grain boundaries and
propagated into the grain interior, pinning the gliding dislocations
(indicated by blue arrows in Fig. 5). The TEM analysis also revealed
439
the formation of the mechanical twins in some austenite grains
(Fig. 6). Mechanical twin thickness was 20–50 nm and high dis-
location density was often observed in the vicinity of the me-
chanical twins (Fig. 6).
At the strain level of 0.1, the formation of stacking faults was
observed homogeneously within grains (Fig. 7). Moreover, in some
grains stacking faults with different burger vectors were observed
(Fig. 7(b) and (c)), which significantly increased the interaction of
the dislocations with the stacking faults (indicated by blue arrows
in Fig. 7). At this stage, stacking faults were still the predominant
deformation mechanism. Moreover, the number of austenite
grains with twins increased with an increase in strain (Fig. 8). The
mechanical twins were mostly nucleated at the grain boundaries,
propagating across the grain interior (Fig. 8). Similar to the TEM
observation, the mechanical twins revealed using AsB-SEM tech-
nique, were very fine having a thickness of 20–50 nm (Fig. 9(a–e).
Furthermore, some dislocation activity was observed in both
twinned and twin-free grains. The volume fraction of twins and
twinned grains were progressively increased with an increase in
the strain (Fig. 10). The volume fraction of twinned grains and the
volume fraction of twins enhanced from 397 6 and 0.6 70.2% at a
true strain level of 0.1 to 84 74 and 18.6 71.7% at a true strain
level of  0.5 (at fracture), respectively (Fig. 10).
The deformation temperature significantly affected the changes
in the microstructure development occurred during straining. The
extent of the mechanical twinning was remarkably reduced with
an increase in the deformation temperature (Figs. 11 and 12), so
that no mechanical twinning was observed at a deformation
temperature of 300 °C and above even at fracture (Fig. 13). At this
temperature regime, the grains only contained dislocation sub-
structure (i.e. twin-free grains, Fig. 13). Furthermore, the initiation
of the mechanical twin formation was postponed from 0.04 at
room temperature to a true strain of 0.2 and 0.25 at 100 and
200 °C, respectively (Figs. 9(a), 11(b) and 12(b)). Mechanical twin
thickness remains almost constant throughout the deformation
regardless the deformation conditions (Figs. 9a–e, 11b–e and 12b–
e). In general, the volume fraction of twins significantly decreased
with an increase in the tensile deformation temperatures at a gi-
ven strain. At a strain level of 0.4, the volume fraction of me-
chanical twins reduced from 11.2 70.7% at room temperature to
5 70.7 and 2.9 70.4% at 100 and 200 °C, respectively (Fig. 10(a)). A
similar trend was observed for the volume fraction of twinned
grains, where it was reduced from 72 75 at room temperature to
567 6 and 44 7 7% at 100 and 200 °C, respectively, at a strain level
of 0.4 (Fig. 10(b)).
440 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446

Fig. 3. Work-hardening behaviour as a function of true strain at different tensile testing temperatures, (a) at room temperature (b) 100 °C, (c) 200 °C, (d) 300 °C and
(e) 400 °C.

Table 1. 4. Discussion
Work-hardening behaviour as a function of strain at different deformation
temperatures.
The current TWIP steel reveals the exceptional mechanical
Tensile testing The stages of the work-hardening behaviour properties at room temperature, although the mechanical prop-
temperature erties are deteriorated at the elevated tensile temperatures
I II III IV
(Figs. 1 and 2). The mechanical properties are directly related to
True strain the work-hardening behaviour of the material during straining
(Fig. 3(a)). The work-hardening behaviour of the TWIP steel is
Ambient 0–0.025 0.025–0.05 0.05–0.07 0.07 onwards
highly dependent on the deformation mechanisms, which are
100 °C 0–0.018 0.018– 0.022– 0.041 onwards
0.022 0.041 associated with the stacking fault energy. Three different
200 °C 0–0.021 0.021– 0.023– 0.027 onwards deformation mechanisms are identified in austenitic materials
0.023 0.027
during straining as a function of SFE [5,23,26,42,46]: (i) slip
300 °C 0–0.024 – – 0.024 onwards
400 °C 0–0.024 – – 0.024 onwards mechanism, which is always expected to take place during
deformation, although it would be a dominant mechanism at a SFE
 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446
30 µm
Fig. 4. The as-received microstructure of the TWIP steel; (a) EBSD map; red and black lines represent annealing twin and high angle grain boundaries, respectively and
(b) TEM image, arrows show the annealing twins. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)
002
131
[310]
0.2µm
Fig. 5. Bright field image of 0.04 strained TWIP steel showing stacking faults
emitted from the grain boundary. The inset is diffraction pattern of austenite matrix
with zone axis of [310]γ. The red arrows and dash line represent the stacking faults
and the grain boundary, respectively. The interactions of the glide dislocations with
the stacking faults are shown by blue arrows. (For interpretation of the references
to color in this figure legend, the reader is referred to the web version of this
article.)
greater than 60 mJ/m2 [5,23,26,42,46]; (ii) transformation of aus-
tenite to martensite, Transformation Induced Plasticity (TRIP) ef-
fect, in austenitic steels with a SFE lower than 20 mJ/m2
[5,23,26,42,46]; and (iii) twinning of austenite (TWIP effect) in
austenitic steels with a SFE between 20–60 mJ/m2 [5,23,26,42,46].
The last two deformation mechanisms result in the formation of
new obstacles against dislocations during deformation, which
enhances the work-hardening rate. As a result, necking is delayed,
which improves the plasticity of the material. At room tempera-
ture, the SFE of current TWIP steel is measured in a range of
14–29 mJ/m2 using different thermodynamic approaches
[23,42,44,47] (Fig. 14), which is in a good agreement with the SFE
results measured by TEM [48] and XRD [49] for an austenitic steel
with a similar composition. In addition, the martensitic transfor-
mation does not occur in the similar steel composition confirmed
by others [50] using EBSD and XRD techniques.
The work-hardening behaviour at room temperature consisted
of four distinct stages, which could be closely associated with the
microstructural changes during deformation (Fig. 3(a)). This was
demonstrated schematically in Fig. 15. The first stage reveals a
typical intense reduction in the work-hardening rate, as observed
441
1µm
111
002
[110]
0.5 µm
Fig. 6. Bright field image of 0.04 strained TWIP steel showing deformation twins.
The inset is diffraction pattern of mechanically twinned austenite with zone axis of
[110]γ. Red arrow represents the diffraction spot from the mechanical twins. (For
interpretation of the references to color in this figure legend, the reader is referred
to the web version of this article.)
in most materials regardless of their SFE (Fig. 15). This can largely
be related to the elastic strain and transition from elastic to plastic
deformation [51]. There is a minima at the end of stage (I) (i.e.
 0.025 strain) followed by an increase in the work-hardening rate
up to a strain of  0.05 (i.e. stage (II), Figs. 3(a) and 15). The work-
hardening behaviour can be associated with different micro-
structural features such as mechanical twinning [20–22,26], grain
boundaries [52], stacking faults formation [27,32], dislocation
cross slip [53] and/or DSA [4,35]. The mechanical twinning is be-
lieved to significantly influence the work-hardening as the initia-
tion of mechanical twins continuously limits the extent of the
dislocation glide by blocking their movements [20–22,26]. Indeed,
the mechanical twins propagate across the grains, progressively
reducing the dislocation mean free path during straining and in-
troducing the dynamic Hall-Petch effect. In the current study, the
mechanical twinning is, however, observed at a strain level of
 0.04, which is just below the maximum strain associated with
the end of the stage (II) of work-hardening, i.e. 0.05 (Figs. 3(a) and
442 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446

111 002
b 220
[110] 111
[112]

200 nm 100 nm 100 nm

Fig. 7. (a–b) Bright field images of stacking faults formed after 0.1 strain. The insets in (a) and (b) are diffraction patterns of austenite with a zone axis of [110]γ and [112]γ,
respectively. (c) the dark field image of (b) from (11-1)γ reflection. The red and blue arrows represent the stacking faults and the interactions of the glide dislocations with
the stacking faults, respectively. (For interpretation of the references to color in this figure legend, the reader is referred to the web version of this article.)

15). In addition, the volume fraction of mechanical twins is very
small, i.e.  0.02% (Fig. 10(a)), at this strain range. This suggests
that an increase observed at stage (II) of the work-hardening is less
likely attributed to the mechanical twinning at room temperature.
The DSA can be also rolled out here as it takes place beyond a true
strain of 0.4 at room temperature, which will be discussed in more
details further on. The current steel has a small grain size of
2.570.2 mm, having a relatively high grain boundary area, which
significantly enhances the chance of interactions between the dis-
locations and the grain boundaries [52]. These interactions can
partly contribute to the augmentation of the work-hardening rate
[52]. Another reason for an increase in the work-hardening rate at
an early stage of deformation can be attributed to the formation of
the stacking faults [32]. In the current study, the stacking faults are
frequently observed in the vicinity of grain boundaries at a strain of
0.04 at room temperature (Fig. 5). At strain level of 0.1, stacking
faults are, however, homogeneously spread inside the grains and
the gliding dislocations extensively interact with them (Fig. 7). The
stacking faults are formed as a result of the dissociation of the
perfect dislocations into Shockley partials in materials with low SFE
[27,32]. They can be widely extended and act as a source of dis-
locations production and their interaction with glide dislocations is
known to increase the work-hardening rate [32].
Interestingly, the stage (II) of the work-hardening behaviour
progressively becomes narrower with the temperature (Fig. 3).
This suggests that the elevated tensile testing temperature sig-
nificantly influences the interactions of glide dislocations with
stacking faults and grain boundaries. The stacking fault energy
increased with temperature (Fig. 14), enhancing the separation
distance of dissociated partial dislocations, which consequently
reduces the interactions of glide dislocations with stacking faults.
Similarly, the pinning of dislocations against grain boundaries
progressively becomes less effective with temperature. This is
more obvious at the temperature of 300 °C and above, where stage
(II) of the work-hardening behaviour almost disappears (Fig. 3
(d) and (e)). At this temperature regime, the stacking fault energy
is estimated beyond 60 mJ/m2, proposing that the slip is a pre-
dominant deformation mechanism (i.e. no mechanical twin for-
mation) as supported by the current result.
Stage (III) of the work-hardening behaviour is referred to the
plateau region observed at a strain range of 0.05–0.07 at room
temperature (Figs. 3(a) and 15). This could be referred to the
stacking faults and/or the formation of mechanical twins. Inter-
estingly, the volume fraction of mechanical twinning is less than
0.6% at this strain range (Fig. 10(a)), suggesting that the interac-
tions of glide dislocations with stacking faults have greater con-
tributions to the stage (III) of the work-hardening behaviour
compared with the mechanical twinning. The temperature rise
significantly reduces the strain range of stage (III), and it is almost
vanished at a temperature above 200 °C (Fig. 3(d) and (e)). The SFE

2µm 2µm
Fig. 8. Representative TEM image of austenite microstructure at different true strain levels of (a) 0.2, (b) 0.4 at room temperature. White arrows indicate the mechanical
twins.
 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446 443

500 nm 500 nm 500 nm

500 nm 500 nm

Fig. 9. SEM images of the microstructure at different true strain levels of (a) 0.1, (b) 0.2, (c) 0.3, (d) 0.4 and (e) fracture (  0.5) at room temperature.

Volume fraction of twinned grains (%)

100
RT
20
Volume fraction of twins (%)

o
100 C
o 80
200 C
15
60

10
40

5 RT
20 o
100 C
o
200 C
0 0
0.0 0.1 0.2 0.3 0.4 0.5 0.0 0.1 0.2 0.3 0.4 0.5
True strain True strain
Fig. 10. (a) Volume fraction of mechanical twins and (b) the dislocation mean free path of twinned grains as a function of true strain at different tensile testing temperatures.

500 nm 500 nm 500 nm

500 nm 500 nm

Fig. 11. SEM images of the microstructure at different true strain levels of (a) 0.1, (b) 0.2, (c) 0.3, (d) 0.4 and (e) fracture (  0.5) at 100 °C.
444 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446

500 nm 500 nm 500 nm

500 nm 500 nm

Fig. 12. SEM images of the microstructure at different true strain levels of (a) 0.2, (b) 0.25, (c) 0.3, (d) 0.35 and (e) fracture (  0.4) at 200 °C.

500 nm 500 nm

Fig. 13. SEM images of the microstructure at fracture at different tensile testing temperatures: (a) 300 °C and (b) 400 °C.

120
Work-hardening (d /d )

Allain 2004 DG GBs SFs and SFs, Twins and

Dumay et al. 2007 and SFs Twins DSA
100 Mazancova and Mazanec 2009 (i) (ii) (iii) (iv)
A.Saeed-Akbari 2009
80
SFE (mJ/m )

Slip
2

60 Low SFE
TWIP steel with fine grains

40 TWIP High SFE material

with fine grains

20
Medium to high SFE material
TRIP with coarse grains
0
0 50 100 150 200 250 300 350 400 True strain
o
Temperature ( C) Fig. 15. Schematic representation of the work-hardening behaviour of fcc materials
with different stacking fault energies (SFE) under tensile testing. Dash line curve
Fig. 14. Calculated stacking fault energy of the TWIP steel as a function of tem- represents the material with medium to high SFE having coarse grain size. Dot line
perature using different thermodynamic approaches. curve shows the material with medium to high SFE with small grain size. Solid line
curve represents the low SFE TWIP steel with fine grain. DG, GB, SF and DSA are
dislocation glide, grain boundaries, stacking faults and dynamic strain aging,
at a temperature above 200 °C enhances to such extent that sig- respectively.
nificantly reduces the effectiveness of the dislocation and stacking
faults interaction and postpones the formation of mechanical what is observed in stage (I). Interestingly, the current result re-
twins. veals a progressive augmentation in the mechanical twinning
Beyond a strain of 0.07, the work-hardening rate gradually volume fraction beyond a strain of 0.04 at room temperature
decreases at room temperature (i.e. stage (IV), Figs. 3(a) and 15), (Fig. 10(a)). It would be expected that the mechanical twinning
though the rate of work-hardening decline is much slower than enhances the work-hardening rate through dynamic Hall-Petch
 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446
effect. This suggests that the dislocation annihilation (i.e. recovery)
rate is still greater than the dislocation multiplication (i.e. hard-
ening) rate induced by the mechanical twinning and/or stacking
faults. At high strain levels, i.e. beyond 0.35 at room temperature,
the work-hardening behaviour reveals a significant oscillation as
their amplitude augmented with strain. This behaviour can be
referred to DSA effect [43,54], which is commonly observed in
high-Mn austenitic steels and is more evident in alloys with a C
concentration of more than 0.5 wt% [43]. The DSA effect is mainly
referred to the interaction of C atoms of the C-Mn bundle with the
stacking faults during straining [54], although its contribution to
work-hardening is relatively low at room temperature (  20 MPa)
[55,56]. It is worth mentioning that the initiation of DSA takes
place at a relatively late stage of straining at room temperature.
This is most likely due to the presence of Al in composition, which
significantly delays the DSA initiation [50].
Interestingly, the DSA is remarkably enhanced at a tensile
temperature of 100 °C and hardly apparent at a temperature of
200 °C and above (Fig. 1). The DSA is significantly affected by steel
composition and tends to operate in a specific temperature range
[4,35,57]. This suggests that Al shifts the DSA temperature in a
range of room temperature to 100 °C.
5. Summary
In the current study, the effect of strain on the TWIP steel
microstructure development at different deformation tempera-
tures was analysed. The microstructural changes were correlated
with the work-hardening behaviour of TWIP steel at different
deformation temperatures. The important findings of present
study were:
(1) the current TWIP steel revealed an exceptional mechanical
behaviour at room temperature, which gradually deteriorated
with an increase in the tensile testing temperature.
(2) the work-hardening behaviour revealed four distinct stages at
room temperature, though the extent of these stages was
significantly influenced by the tensile testing temperature.
(3) the work-hardening behaviour was attributed to complex
dynamic strain induced microstructural reactions consisted of
dynamic recovery, dislocation dissociation, stacking fault for-
mation, mechanical twining and dynamic strain aging.
(4) the current observation suggested that the mechanical twins
had a limited effect on the work-hardening behaviour of the
TWIP steel and its influence significantly reduced with the
temperature. The development of stacking faults and their
interactions with the glide dislocations is believed to be the
main contributor in the work-hardening enhancement of the
TWIP steel.
Acknowledgement
Prof. B.C. De Cooman is thankfully acknowledged for providing
the TWIP steel. This study was supported by grants provided by
the Australian Research Council (Grant no. FL0992361). The au-
thors would like to acknowledge the technical and scientific sup-
port of the Deakin Advanced Characterisation Facility and Monash
Centre for Electron Microscopy. VS also acknowledges Deakin
University for providing a research scholarship for this work.
References
[1] B. De Cooman, K.-g. Chin, J. Kim, High Mn TWIP steels for automotive appli-
cations, in: M. Chiaberge (Ed.), New Trends and Developments in Automotive
445
Industry, InTech, 2011.
[2] B.C. De Cooman, et al., State-of-the-Science of High Manganese TWIP Steels for
Automotive Applications, Springer, London, 2009.
[3] O. Bouaziz, et al., High manganese austenitic twinning induced plasticity
steels: A review of the microstructure properties relationships, Curr. Opin.
Solid State Mater. Sci. 15 (4) (2011) 141–168.
[4] T. Shun, C.M. Wan, J.G. Byrne, A study of work hardening in austenitic Fe—
Mn—C and Fe—Mn—Al—C alloys, Acta Metall. Mater. 40 (12) (1992) 3407–3412.
[5] L. Remy, A. Pineau, Twinning and Strain-Induced F.C.C. - H.C.P. Transforma-
tion in the FeMnCrC System, Mater. Sci. Eng. 28 (1) (1977) 99–107.
[6] O. Grässel, et al., High strength Fe-Mn-(Al, Si) TRIP/TWIP steels development –
properties – application, Int. J. Plast. 16 (10–11) (2000) 1391–1409.
[7] I. Karaman, et al., Deformation of single crystal Hadfield steel by twinning and
slip, Acta Mater. 48 (6) (2000) 1345–1359.
[8] O. Bouaziz, N. Guelton, Modelling of TWIP effect on work-hardening, Mater.
Sci. Eng.: A 319–321 (2001) 246–249.
[9] S. Allain, J.P. Chateau, O. Bouaziz, A physical model of the twinning-induced
plasticity effect in a high manganese austenitic steel, Mater. Sci. Eng.: A 387–
389 (1–2) (2004) 143–147.
[10] S. Allain, et al., Modeling of mechanical twinning in a high manganese content
austenitic steel, Mater. Sci. Eng.: A 387–389 (1–2) (2004) 272–276.
[11] O. Bouaziz, S. Allain, C. Scott, Effect of grain and twin boundaries on the
hardening mechanisms of twinning-induced plasticity steels, Scr. Mater. 58 (6)
(2008) 484–487.
[12] M. Huang, et al., Modelling the effect of carbon on deformation behaviour of
twinning induced plasticity steels, J. Mater. Sci. (2011) 1–5.
[13] D. Barbier, et al., EBSD for analysing the twinning microstructure in fine-
grained TWIP steels and its influence on work hardening, J. Microsc. 235 (1)
(2009) 67–78.
[14] J.-E. Jin, Y.-K. Lee, Strain hardening behavior of a Fe-18Mn-0.6C-1.5Al TWIP
steel, Mater. Sci. Eng.: A 527 (1–2) (2009) 157–161.
[15] R. Ueji, et al., Effect of Grain Size on the work-hardening behavior and de-
formation twinning of high-manganese austenitic steel, Mater. Charact. (2009)
4.
[16] C. Efstathiou, H. Sehitoglu, Strain hardening and heterogeneous deformation
during twinning in Hadfield steel, Acta Mater. 58 (5) (2010) 1479–1488.
[17] H. Beladi, et al., Orientation dependence of twinning and strain hardening
behaviour of a high manganese twinning induced plasticity steel with poly-
crystalline structure, Acta Mater. 59 (20) (2011) 7787–7799.
[18] O. Bouaziz, et al., Effect of chemical composition on work hardening of Fe-Mn-
C TWIP steels, Mater. Sci. Technol. 27 (3) (2011) 707–709.
[19] H. Ding, et al., Strain hardening behavior of a TRIP/TWIP steel with 18.8% Mn,
Mater. Sci. Eng.: A 528 (3) (2011) 868–873.
[20] I. Gutierrez-Urrutia, D. Raabe, Dislocation and twin substructure evolution
during strain hardening of an Fe–22 wt% Mn–0.6 wt% C TWIP steel observed
by electron channeling contrast imaging, Acta Mater. 59 (16) (2011)
6449–6462.
[21] I. Gutierrez-Urrutia, D. Raabe, Multistage strain hardening through dislocation
substructure and twinning in a high strength and ductile weight-reduced Fe–
Mn–Al–C steel, Acta Mater. 60 (16) (2012) 5791–5802.
[22] K. Renard, P.J. Jacques, On the relationship between work hardening and
twinning rate in TWIP steels, Mater. Sci. Eng.: A 542 (0) (2012) 8–14.
[23] A. Saeed-Akbari, et al., Characterization and prediction of flow behavior in
high-manganese twinning induced plasticity steels: Part I. Mechanism maps
and work-hardening behavior, Metall. Mater. Trans. A 43 (5) (2012)
1688–1704.
[24] D.R. Steinmetz, et al., Revealing the strain-hardening behavior of twinning-
induced plasticity steels: theory, simulations, experiments, Acta Mater. 61 (2)
(2013) 494–510.
[25] I. Gutierrez-Urrutia et al., Revealing the strain-hardening mechanisms of ad-
vanced high-Mn steels by multi-scale microstructure characterization, in:
Proceedings of the 8th International Conference on Processing and Manu-
facturing of Advanced Materials, THERMEC 2013, 2014, Trans Tech Publica-
tions Ltd: Las Vegas, NV, pp. 755–760.
[26] V. Shterner, I.B. Timokhina, H. Beladi, The correlation between stacking fault
energy and the work hardening behaviour of high-mn twinning induced
plasticity steel tested at various temperatures, in: Proceedings of the 8th In-
ternational Conference on Processing and Manufacturing of Advanced Mate-
rials: Processing, Fabrication, Properties, Applications, THERMEC 2013, 2014,
Trans Tech Publications: Las Vegas, NV, pp. 676–681.
[27] L. Rémy, The interaction between slip and twinning systems and the influence
of twinning on the mechanical behavior of fcc metals and alloys, Metall. Mater.
Trans. A 12 (3) (1981) 387–408.
[28] D. Barbier, et al., Analysis of the tensile behavior of a TWIP steel based on the
texture and microstructure evolutions, Mater. Sci. Eng. A 500 (1–2) (2009)
196–206.
[29] J. Kim, et al., Constitutive modeling of the tensile behavior of Al-TWIP steel,
Metall. Mater. Trans. A 43 (2) (2012) 479–490.
[30] V. Shterner, et al., A constitutive model of the deformation behaviour of
twinning induced plasticity (TWIP) steel at different temperatures, Mater. Sci.
Eng.: A 613 (0) (2014) 224–231.
[31] V. Shterner, et al., Effect of Temperature on Mechanical Behaviour of High
Manganese TWIP steel, Wollongong, NSW 2014, pp. 257–262.
[32] D. Drobnjak, J. Parr, Deformation substructure and strain-hardening char-
acteristics of metastable Fe-Mn austenites, Metall. Mater. Trans. B 1 (4) (1970)
759–765.
446 V. Shterner et al. / Materials Science & Engineering A 669 (2016) 437–446
[33] F. Hamdi, S. Asgari, Evaluation of the role of deformation twinning in work
hardening behavior of face-centered-cubic polycrystals, Metall. Mater. Trans. A
39 (2) (2008) 294–303.
[34] R.K.W. Marceau, P. Choi, D. Raabe, Understanding the detection of carbon in
austenitic high-Mn steel using atom probe tomography, Ultramicroscopy 132
(0) (2013) 239–247.
[35] Y. Dastur, W. Leslie, Mechanism of work hardening in Hadfield manganese
steel, Metall. Mater. Trans. A 12 (5) (1981) 749–759.
[36] Z.Y. Liang, Y.Z. Li, M.X. Huang, The respective hardening contributions of dis-
locations and twins to the flow stress of a twinning-induced plasticity steel,
Scr. Mater. 112 (2016) 28–31.
[37] J. Gil Sevillano, P. van Houtte, E. Aernoudt, Large strain work hardening and
textures, Prog. Mater. Sci. 25 (2) (1980) 69–134.
[38] H. Mecking, U.F. Kocks, Kinetics of flow and strain-hardening, Acta Metall. 29
(11) (1981) 1865–1875.
[39] S.R. Kalidindi, Modeling the strain hardening response of low SFE FCC alloys,
Int. J. Plast. 14 (12) (1998) 1265–1277.
[40] I. Karaman, et al., Competing mechanisms and modeling of deformation in
austenitic stainless steel single crystals with and without nitrogen, Acta Mater.
49 (19) (2001) 3919–3933.
[41] J. Gil Sevillano, An alternative model for the strain hardening of FCC alloys that
twin, validated for twinning-induced plasticity steel, Scr. Mater. 60 (5) (2009)
336–339.
[42] S. Allain, et al., Correlations between the calculated stacking fault energy and
the plasticity mechanisms in Fe–Mn–C alloys, Mater. Sci. Eng.: A 387–389 (0)
(2004) 158–162.
[43] L. Chen, et al., Localized deformation due to Portevin-LeChatelier effect in
18Mn-0.6C TWIP austenitic steel, ISIJ Int. 47 (12) (2007) 1804–1812.
[44] E. Mazancova, K. Mazanec, Stacking fault energy in high manganese alloys,
Mater. Eng. 16 (2) (2009) 6.
[45] J.C. Russ, R.T. Dehoff, Practical Stereology, 2nd ed., Plenum Press, New York, NY
1999, p. 312.
[46] A. Saeed-Akbari, et al., Derivation and variation in composition-dependent
stacking fault energy maps based on subregular solution model in high-
manganese steels, Metall. Mater. Trans. A 40 (13) (2009) 3076–3090.
[47] A. Dumay, et al., Influence of addition elements on the stacking-fault energy
and mechanical properties of an austenitic Fe–Mn–C steel, Mater. Sci. Eng.: A
483–484 (0) (2008) 184–187.
[48] J. Kim, B. De Cooman, On the stacking fault energy of Fe-18 Pct Mn-0.6 Pct
C-1.5 Pct Al twinning-induced plasticity steel, Metall. Mater. Trans. A 42 (4)
(2011) 932–936.
[49] J.S. Jeong, et al., In situ neutron diffraction study of the microstructure and
tensile deformation behavior in Al-added high manganese austenitic steels,
Acta Mater. 60 (5) (2012) 2290–2299.
[50] J.-K. Kim, et al., On the tensile behavior of high-manganese twinning-induced
plasticity steel, Metall. Mater. Trans. A 40 (13) (2009) 3147–3158.
[51] U.F. Kocks, H. Mecking, Physics and phenomenology of strain hardening: the
FCC case, Prog. Mater. Sci. 48 (3) (2003) 171–273.
[52] C.W. Sinclair, W.J. Poole, Y. Bréchet, A model for the grain size dependent work
hardening of copper, Scr. Mater. 55 (8) (2006) 739–742.
[53] W. Püschl, Models for dislocation cross-slip in close-packed crystal structures:
a critical review, Prog. Mater. Sci. 47 (4) (2002) 415–461.
[54] S.-J. Lee, et al., On the origin of dynamic strain aging in twinning-induced
plasticity steels, Acta Mater. 59 (17) (2011) 6809–6819.
[55] R.A. Mulford, U.F. Kocks, New observations on the mechanisms of dynamic
strain aging and of jerky flow, Acta Metall. 27 (7) (1979) 1125–1134.
[56] A. Wijler, M.M.A. Vrijhoef, A. Van Den Beukel, The onset of serrated yielding in
Au(Cu) alloys, Acta Metall. 22 (1) (1974) 13–19.
[57] D. Drobnjak, J.G. Parr, Deformation substructure and strain-hardening char-
acteristics of metastable Fe-Mn austenites, Metall. Trans. 1 (4) (1970) 759–765.