Author’s Accepted Manuscript

Accumulative Roll Bonding (ARB)-Processed

High-Manganese Twinning Induced Plasticity
(TWIP) Steel with Extraordinary Strength and
Reasonable Ductility

A. Etemad, G. Dini, S. Schwarz

www.elsevier.com/locate/msea

PII: S0921-5093(18)31512-0
DOI: https://doi.org/10.1016/j.msea.2018.10.119
Reference: MSA37114
To appear in: Materials Science & Engineering A
Received date: 9 August 2018
Revised date: 25 October 2018
Accepted date: 29 October 2018
Cite this article as: A. Etemad, G. Dini and S. Schwarz, Accumulative Roll
Bonding (ARB)-Processed High-Manganese Twinning Induced Plasticity
(TWIP) Steel with Extraordinary Strength and Reasonable Ductility, Materials
Science & Engineering A, https://doi.org/10.1016/j.msea.2018.10.119
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 Accumulative Roll Bonding (ARB)-Processed High-Manganese Twinning Induced Plasticity
(TWIP) Steel with Extraordinary Strength and Reasonable Ductility

A. Etemad1, G. Dini1*, S. Schwarz2

1
Department of Nanotechnology Engineering, Faculty of Advanced Sciences and Technologies,
University of Isfahan, Isfahan 81746-73441, Iran
2
University Service Centre for Transmission Electron Microscopy, Technische Universität Wien,
Wiedner Hauptstrasse 8-10, 1040 Wien, Austria

*
Corresponding author. Ghasem Dini (Assistant Professor). Tel.: +93-31-37932607; fax: +98-31-
37934242. g.dini@sci.ui.ac.ir,

Abstract
Accumulative roll bonding (ARB) process at room temperature was used to fabricate a
nanostructured twinning-induced plasticity (TWIP) steel. The effect of the number of ARB cycles
from 1 to 3 on the microstructure and mechanical properties of Fe-31Mn-3Al-3Si (wt. %) TWIP
steel was investigated. The results showed that the microstructure of the 1-cycle ARB-processed
sample mainly contained the primary and secondary mechanical twins. However, in the
microstructure of 2-cycle ARB-processed sample, new configurations of small nanotwins which
they are known as the hierarchical nanotwinned (HNT) structures were observed between the
secondary mechanical twins. In the microstructure of 3-cycle ARB-processed sample, new
subdivided grains with a mean size of about 100 nm were produced. Additionally, the 3-cycle ARB-
processed TWIP steel sample exhibited extraordinary strength (about 1.2 GPa) and reasonable
ductility (about 15 %). The mechanical behavior of ARB-processed TWIP steel was interpreted as
the evidence for microstructural features such as the mechanical twins (especially, the HNT
structures) and nano/ultrafine grains.

Keywords: Accumulative roll bonding (ARB) process; twinning-induced plasticity (TWIP) steel;
hierarchical nanotwinned (HNT) structures; nano/ultrafine grains; mechanical properties
1. Introduction
In new decades, the issue of safety standards and energy utilization in the automotive industry has
been attracted a great attention. Therefore, the development of new materials to meet these
requirements is always essential. High-manganese twinning-induced plasticity (TWIP) steels are
prospective candidates for next-generation automotive steels, because of their superior combination
of strength and ductility due to extensive mechanical twinning during deformation at room
temperature [1-6].
The value of stacking fault energy (SFE) of TWIP steels is relatively low and their alloying systems
are high solid solution Fe-Mn-Al-Si-C alloys. In these steel, the simultaneous occurrence of some
special phenomena during deformation such as the limited dynamic recovery, mechanical twinning,
and dynamic strain aging leads to achieving a high tensile strength (about 800 MPa) and an
extraordinary elongation (about 100 %) [7-9].
During the two past decades, several different compositions of high-manganese TWIP steels have
been deeply investigated [9-12]. The investigations focused mainly on the mechanical properties as
a function of microstructural evolutions, dislocation structure, and mechanical twinning. For
example, some studies show that the grain refinement has a significant effect on the strength of
these steels [10, 12]. Nevertheless, achieving a nano/ultrafine grained TWIP steels with
conventional methods such as the cold rolling and subsequent annealing is very difficult.
On the other hand, the development of nano/ultrafine grained bulk metallic materials by means of
techniques that are mainly based on the imposing extremely large plastic strain on metallic
materials have been expanded. Today, these techniques are well-known as severe plastic
deformation (SPD) methods. The research activities in the field of SPD processing have continued
to develop novel nanostructured bulk metallic materials up to the present day. Among various
techniques of SPD, the accumulative roll bonding (ARB) process has been widely used to fabricate
bulk nanostructured metallic materials [13-18].
In the ARB process, two strips of similar or dissimilar metallic materials are fitted together and
repeatedly rolled to the 50 % thickness reduction. The final structure of ARB-processed materials
consists of multilayers, which refines progressively with the continuation of the ARB process [19-
20]. The microstructural evolutions and related mechanical properties during ARB cycles at room
temperature were studied for several metals and alloys such as commercially pure aluminum [16,
21], and interstitial free (IF) steels [16].
Generally, it is believed that the ARB process similar to other SPD techniques leads to a grain
refinement by the formation of incidental dislocation boundaries and geometrically necessary
boundaries. This leads to a nano/ultrafine grained structure and equilibrium and non-equilibrium
grain boundaries [22-24]. However, the final structure of deformed material depends strongly on: 1)
processing regimes including the deformation temperature, the degree of strain, pressure, and
deformation route [25-27] and 2) the type of material including the atomic structure, chemical
composition, and SFE of the material processed [13, 28].
Although many studies on the ARB-processed metallic materials are published, only a few of them
are related to the ARB-processing of steel sheets including interstitial free (IF) steels and austenitic
stainless steels [4, 17, 19, 29-34]. In this study, therefore, the effect of ARB process at room
temperature on the microstructure and mechanical properties of a high-manganese austenitic TWIP
steel sheet has been investigated.

2. Experimental procedures
A 90 % cold-rolled TWIP steel sheet with the chemical composition of Fe-31Mn-3Al-3Si (in wt. %)
in as-received condition was cut into strips of dimensions 100 × 20 × 1 mm3 parallel to the rolling
direction (RD). Before ARB processing, the strips were annealed at 850 ◦C for 1 h in an electric
furnace to obtain a fully recrystallized structure. The mean grain size of the annealed strips was
around 18 µm [6].
To obtain a good bonding in the ARB process, before each cycle any contaminant especially oxides
must be removed from surfaces of two strips to be bonded. To do this, the preparation procedure
including degreasing the strips for 5 min in an acetone bath followed by scratch-brushing with a
stainless steel brush wire was applied to all the strips. To prevent the reformation of the oxides on
the surfaces of the strips, the ARB process was performed immediately after scratch brushing.
Briefly, the brushed surfaces of the two strips were fitted together and fixed with three spots of
resistance welding at the first, middle and end of the strips. In each cycle, the ARB process was
performed to achieve a reduction in thickness of 50 % (an equivalent strain of 0.8) using an
industrial rolling machine with a capacity of 40 tons. The roll diameters were 220 mm, and the
rolling speed was about 7 m/min. After each cycle, the ARB-processed strips were cut in half and
the procedure was repeated up to 3 cycles at room temperature [35].
Microstructural features were investigated on the rolling direction-transverse direction plane of all
the ARB-processed samples by a transmission electron microscope (TEM, 200 kV FEI TECNAI
F20 S-Twin). The TEM samples were prepared by cutting, grinding and ion polishing with a Gatan
precision ion polishing system.
Tensile test specimens were cut from the cold-rolled, annealed and ARB-processed strips along the
rolling direction according to the ASTM E8-04 standard. All Tensile tests with a strain rate of 10-3
s-1 were carried out at room temperature by a servo-hydraulic testing machine (Gotech, 2T)
equipped with a laser extensometer. All the tensile tests were replicated three times to find the
average values. Also, micro-hardness values of all the samples were obtained at a load of 15 N
using a Vickers hardness tester (Buehler, Micromet 5101). The presented hardness values are an
average of at least 5 measurements.
X-ray diffraction (XRD) patterns of all the samples were recorded between 30 and 100 o at room
temperature using a diffractometer (Bruker D8 Advance) with a Cu target and a step size of 0.05o.

3. Results and discussion

The XRD patterns of annealed, 1-, 2-, and 3-cycle ARB-processed TWIP steel samples are given in
Fig. 1. From this figure, it can be seen that the structure of the annealed sample is austenite. After
the third cycle of the ARB process, where a true strain of 2.4 was applied to the sample, the
structure is still austenitic. Moreover, no evidence of phase transformation (i.e., martensitic
transformation) is observed in the XRD patterns of other ARB-processed TWIP steel samples.

Fig. 1. The XRD patterns of annealed, 1-, 2-, and 3-cycle ARB-processed TWIP steel samples.

In Figs. 2a to 2c, the different TEM micrographs of 1-cycle ARB-processed TWIP steel sample are
shown. After the first cycle, the microstructure is highly deformed and the primary mechanical
twins are found in throughout the microstructure (Fig. 2a). The corresponding selected area electron
diffraction pattern in Fig. 2a confirms the presence of mechanical twins at this sample. The
occurrence of extensive mechanical twins is the main microstructural feature of TWIP steels during
cold deformation and it is related to the low SFE of TWIP steels [1-2]. Actually, TWIP steels
deform plastically by both the dislocation slip and mechanical twinning mechanisms [12]. As can
be seen from Fig. 2a, the primary mechanical twins are in the form of narrow strips with the
thickness of about a few ten nanometers.
Since the applied strain in the first cycle is relatively high (the true strain of 0.8), it can be expected
that the secondary twin system is observed in some area of the deformed microstructure (Fig. 2b).
Also, shear banding is activated in some local areas to accommodate deformation (Fig. 2c). This
microstructure is similar to the microstructure of cold-rolled TWIP steel [36]. However, the
ultrafine-grained microstructure is not observed in this strain level.

Fig. 2. The different TEM micrographs of 1-cycle ARB-processed TWIP steel sample showing, a)
primary mechanical twins, b) primary and secondary mechanical twins, and c) shear bands.

The microstructural features of 2-cycle ARB-processed TWIP steel in most areas are similar to the
1-cycle ARB-processed TWIP steel. Although the ultrafine-grained microstructure is not found in
this sample yet, a special kind of nanotwins was formed between the secondary mechanical twins
(Fig. 3). These nanotwins are completely different from the secondary mechanical twins. In other
words, the secondary mechanical twins are similar to primary ones and they cut the primary
mechanical twins (Fig. 2b). However, in Fig. 3 it can be seen that the new formed small nanotwins
are located between the secondary mechanical twins.

Fig. 3. The TEM micrograph of 2-cycle ARB-processed TWIP steel sample showing the HNT
structures (the dashed box region).

This kind of microstructures is called the hierarchical nanotwinned (HNT) structures, which leads to
unique mechanical properties (a good combination of strength and ductility) [37]. The HNT
structures are complete twin systems. It means the primary, secondary, tertiary mechanical twins or
even higher ordered nanotwinned structures coexist in a single grain. The HNT structures have
already been observed during martensitic transformation [38], equal-channel angular pressing
(ECAP)-processed ultrafine/nanocrystalline Cu and Cu alloys [39], and TWIP steels during the
process of surface mechanical attrition treatment and subsequent tensile deformation [37]. In a very
recent study [40], a complete review of experimental, computational and theoretical efforts on
metals with the HNT structures is given.
Finally, as shown in Fig. 4 the subdivided microstructure is formed in the 3-cycle ARB-processed
TWIP steel, where a true strain of 2.4 was imposed on the sample. However, new subdivided areas
are not homogenous. The average size of the subdivided grains is about 100 nm.
 Fig. 4. The TEM micrograph of 3-cycle ARB-processed TWIP steel sample.

Interestingly, the new nano/ultrafine grains were formed in the current TWIP steel at the strain level
much lower than the values required for many other SPD-processed metallic materials. Generally,
in order to form a nano/ultrafine-grained microstructure, the degree of the true strain during
deformation process should exceed 4-5. These high values of applied strain lead to accumulate high
density of dislocations [13].
The formation of ultrafine grained microstructure in TWIP steels at a low value of applied strain
may be associated with the low SFE of TWIP steels. Indeed, the rate of dislocation accumulation of
metallic materials during deformation increases with decreasing the value of SFE [6]. With
decreasing the SFE, the distance of two partial dislocations dissociated from a perfect dislocation
will be extended, and thus the frequency of cross slip of partial dislocations which is essential for
the dynamic recovery will be reduced. Therefore, decreasing in the value of SFE causes an increase
in the rate of dislocation accumulation with strain. Namely, a higher density of dislocations will be
stored in deformed TWIP steels in comparison with other high SFE metals at a given applied true
strain. Consequently, the enhancement of accumulated dislocation density in TWIP steels leads to
considerably reduce in a minimum true strain required to form an ultrafine-grained microstructure.
Additionally, the subdivided grains do not contain any mechanical twins. This might be related to
an inverse grain-size effect on the mechanical twinning. Generally, in coarse-grained metals, the
formation of mechanical twins became more difficult by reducing the grain size below a critical
size. The previous studies showed that this critical limit of grain size for the current TWIP steel is
approximately near to 1 μm [10, 12].
Figs. 5a and 5b show the engineering and true stress-strain curves obtained from the tensile test of
TWIP steel samples subjected to different ARB cycles, as well as cold-rolled and annealed samples.
For better comparison, the mechanical properties such as 0.2 % offset yield strength (YS), ultimate
tensile strength (UTS), total elongation (etot), and micro-hardness values are given in Table 1.

1400 (a)
Cold-rolled sample
Engineering stress (MPa) 1200 3 cycles

1000 2 cycles

800 1 cycle
Anealed sample
600

400

200

0
0 10 20 30 40 50 60 70 80 90
Engineering strain (%)

1600
Cold-rolled sample (b)
1400 3 cycles

1200 2 cycles
True strength (MPa)

1000 Anealed sample

1 cycle

800

600

400

200

0
0 0.1 0.2 0.3 0.4 0.5 0.6
True strain

Fig. 5. a) Engineering and, b) true strain-stress curves of cold-rolled, annealed, 1-, 2-, and 3-cycle
ARB- processed TWIP steel samples.

Table 1. Mechanical properties of cold-rolled, annealed, 1-, 2-, and 3-cycle ARB-processed TWIP
steel samples
TWIP steel Total elongation Yield strength Tensile strength Micro-hardness
sheet (%) (MPa) (MPa) (Vickers)
Annealed 81 ± 0.7 282 ± 4 622 ± 3 182 ± 5
Cold-rolled 3 ± 0.3 1308 ± 5 1308 ± 5 617 ± 7
1 cycle 11.6 ± 0.4 723 ± 4 893 ± 7 367 ± 4
2 cycles 13.1 ± 0.6 911 ± 7 1114 ± 6 402 ± 4
3 cycles 15.2 ± 0.3 1211 ± 5 1225 ± 5 456 ± 3
As expected, among all the samples, the annealed one has the minimum strength values and the
highest percentage of elongation. After the first cycle of the ARB process, both the YS and UTS
increase and the etot decreases in comparison with the annealed sample. But, in the second and third
cycles, both the strength and elongation are increased in comparison with the first cycle. However,
the reductions in elongation of ARB-processed samples with the conventional cold-rolled sample
are very different. As can be seen from Table 1, the etot of 90 % cold-rolled TWIP steel sample is
just a few percents and the stress-strain curve obtained does not have a uniform plastic deformation
region (Fig. 5). It should be noted that the cold-rolled sample has the maximum strength but the
minimum elongation among all the samples. By contrast, as shown in Fig. 5, all the ARB-processed
TWIP steel samples have an appropriate uniform elongation after applying different ARB cycles.
Other studies showed that although the SPD process leads to a reduction in ductility, the retention
of ductility is usually greater than the conventional cold rolling [41-42].
From Table 1, it can be seen that the values of YS and UTS increase with increasing the number of
ARB processing cycles. Surprisingly, the value of UTS increases up to 1225 ± 5 MPa after the third
cycle. This value is about two times greater than that of the annealed sample (622 ± 3 MPa). The
same trend is observed for the values of micro-hardness (Table 1). After the third cycle, there is a
significant increase in the hardness and this value increased from about 182 ± 5 Hv in the annealed
sample to 456 ± 3 Hv in the 3-cycle ARB-processed sample. This strength enhancement in the
ARB-processed TWIP steel is mainly related to the direct effect (the Hall-Petch strengthening
mechanism) of nanostructuring of TWIP steel via the ARB processing [43-45].
On the other hand, the value of etot decreases sharply from about 81± 0.7 % for the annealed sample
to 11.6 ± 0.4 % for the 1-cycle ARB-processed sample. After the second cycle, the value of etot is
13.1 ± 0.6 % and then this value increases slightly to 15.2 ± 0.3 % at the end of the third cycle. The
significant initial reduction of etot in all materials subjected to a high strain is a common practice,
independent of the process of plastic deformation. However, in the conventional cold rolling the
ductility decreases by a similar magnitude initially, and thereafter, the ductility continues to
decrease with increasing rolling strain although at a slower rate [41-42].
By contrast, the SPD processing of an alloy leads ultimately to a greater retention of ductility than
conventional cold rolling. As can be seen from Table 1, the values of etot of ARB-processed samples
are still satisfying and the ARB process leads to reasonable ductility in comparison with
conventional cold rolling. Additionally, straining of TWIP steel to 3 cycles of the ARB process
simultaneously increases both the strength and ductility in comparison with 1-cycle of ARB-
processed TWIP steel sample. This enhancement of strength, as well as ductility with accumulated
deformation due to an increase in the number of cycles, is termed as the “paradox of strength and
ductility in SPD-processed metals” in the literature [46-50].
Concerning to the origin of this phenomena, several approaches have been proposed such as an
increase in the fraction of high angle grain boundaries with increasing straining, a bimodal
distribution of grain size, a higher strain rate sensitivity, and introducing high density of mechanical
twins as an effective approach to accumulate dislocations inside the grains [46-52].
Among them, the last one could play an important role in the case of SPD-processed TWIP steels in
achieving extraordinary strength and reasonable ductility. Mechanical twin boundaries act as
effective barriers to dislocation movement inside the grains. Therefore, the presence of mechanical
twin boundaries is important to the strengthening of bulk nanostructured metallic materials.
As shown in the TEM micrographs (Figs. 2 to 4), the deformed microstructures of all ARB-
processed TWIP steel samples in this study contain the extensive content of mechanical twins. Also,
the HNT structures were clearly observed after the second cycle of the ARB process. The formation
of HNT structures in crystalline materials could be a novel strategy to maintain higher strength and
better ductility. Since the HNT structures lead to a finer twin network, they are more beneficial to
the improvement of strength in comparison with the conventional mechanical twin boundaries. The
researchers demonstrate that HNT structures can contribute to the fantastic improvement of strength
without sacrifice of ductility. Experimentally, however, the fabrication of HNT structures in metals
is still a challenging topic [40]. Besides, after the third cycle of the ABR process, the nano/ultrafine-
grained microstructure is formed in TWIP steel.
In summary, it can be concluded that the dislocation hardening mechanism (i.e., dislocation-
dislocation and dislocation-mechanical twin boundary interactions) is surely responsible for the
increase of the strength in the 1-cycle ARB-processed TWIP steel. In the second cycle, in addition
to the contribution of the HNT structures formed on the improvement of strength and ductility, the
formation of the subgrain structure also contributes to this improvement via the dislocation
hardening mechanism. After the third cycle, the more subgrain boundaries changed into high angle
grain boundaries and the strength enhancement can be well interpreted by the Hall-Petch relation.
However, as mentioned before, an increase in the strain rate sensitivity which is well-known to be
dependent on the grain boundary character could lead to an increase in the ductility. Although, this
effect was not investigated in this work, the positive effect of the increased strain rate sensitivity on
the ductility was well investigated in other studies [4, 31, 50]. For example, Ruppert et al. [31]
concluded that the increased strain rate sensitivity, martensitic transformation as well as twinning
appear to contribute to a satisfactory ductility during tensile testing of two different austenitic
stainless steels after two ARB cycles.
Conclusion
In this study, the microstructural evolutions and mechanical properties of Fe-31Mn-3Al-3Si TWIP
steel have been investigated during the ARB process up to three cycles at room temperature. The
results showed that the 3-cycle ARB-processed sample exhibited the extraordinary tensile strength
of about 1.2 GPa and the reasonable total elongation of about 15 %. The formation of some
microstructural features such as the mechanical twins (especially, HNT structures) and
nano/ultrafine grains may be responsible for the enhanced mechanical properties of ARB-processed
TWIP steel. Therefore, it can be concluded that the applying of the relatively small value of strain
(of about 2.4) via the ARB process is enough to manufacture the nano/ultrafine grained TWIP steel
with a unique combination of strength and ductility. However, other studies including the strain rate
sensitivity, and detailed microstructural investigations of ARB-processed TWIP steel are suggested
to a better explanation of how these mechanical properties are obtained.

Acknowledgments
The transmission electron microscope images were obtained using facilities at the University
Service Centre for Transmission Electron Microscopy, Vienna, University of Technology, Austria.

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