Materials Science & Engineering A 767 (2019) 138406

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Materials Science & Engineering A

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

The effect of reduced temperatures on microstructure development in tensile T

tested high-manganese steel
Joanna Kowalskaa,∗, Janusz Ryśa, Grzegorz Ciosb, Wiktor Bednarczyka
a
AGH University of Science and Technology, Faculty of Metals Engineering and Industrial Computer Science, Cracow, Poland
b
AGH University of Science and Technology, Academic Centre for Materials and Nanotechnology, Cracow, Poland

A R T I C LE I N FO A B S T R A C T

Keywords: The current research is part of a project covering several grades of high-manganese steels (20–26 wt% Mn) with
High-manganese steel different chemical compositions, which were deformed at room and reduced temperatures. In the present paper,
Stacking fault energy the microstructure development is analyzed at the onset of plastic deformation in Fe–Mn–Al–Si steel containing
Tensile deformation 21.2 wt% Mn. The examination was conducted under conditions of lowering the deformation temperature and
Microstructure
aimed to show the influence of reduced temperatures on the occurrence of strain induced phase (martensitic)
Phase transformation
Martensite
transformation.
The steel samples were subjected to uniaxial deformation in a tensile test at gradually reduced temperatures,
starting from 20 °C and then applying the temperatures 0 °C, −50 °C and −150 °C. The present paper includes
the analysis of microstructure development and orientation relationships as well as determination of operating
deformation mechanisms for samples after 10% of tensile strain. The main part of the research was carried out by
means of scanning electron microscopy (SEM), using the method of electron back-scatter diffraction (EBSD).
The carried out analysis indicates that within the range of small strains the mechanism controlling de-
formation behavior of high-manganese steel Fe–21Mn–3Al–3Si was slip of partial dislocations. This was im-
mediately followed by the occurrence of strain induced phase transformation γ (fcc) → ε (hcp) and then locally ε
(hcp) → α' (bcc). With decreasing deformation temperature a noticeable increase of the volume fraction of the
martensitic phases was observed, first of all the ε-phase and to a much lesser extent α′-martensite. The ε-mar-
tensite appeared on the background of a deformed austenite initially in the form of relatively narrow bands. The
α′-martensite was formed predominantly at the intersections of the ε-bands. An interesting result, however, is
the fact that numerous places were also found where α′-martensite was formed in single set of parallel ε-phase
bands. The preferential crystallographic orientation relations (ORs) between the γ-austenite and the strain in-
duced ε- and α′- phases were successively followed, showing first of all the appearance of Shoji-Nishiyama (S–N)
and Kurdjumov-Sachs (K–S) ORs respectively.

1. Introduction heavy loads. High-manganese steels show an advantageous combina-

Austenitic steels with a higher manganese contents have attracted
attention and remained at the centre of interest practically since the end
of the 19th century. Discovered by Hadfield in 1882, manganese steels
are regarded as one of the first alloy steels. These materials show ra-
dically higher mechanical properties in comparison to plain carbon
steels and first of all have no equal in their ability to work-harden and
to absorb impact energy.
Over the last few decades, an increasing scientific and technological
interest in high-manganese steels was observed [1–6]. Currently, these
materials are the next generation of steels for the automotive structural
parts as well as a number of other structural applications exposed to
tion of strength and plastic properties which is related to the mechan-
isms of plastic deformation. Depending on chemical composition and
temperature, they exhibit different values of stacking fault energy (SFE)
which strongly influences deformation mechanisms, and as a result
final mechanical properties [1,3,7–11]. Together with changes in the
SFE value, the required toughness and strength are usually achieved by
the combined operation of three different deformation mechanisms.
First of all this is the mechanism of dislocation slip and more specifi-
cally, the slip of Shockley partials separated by stacking faults. The
second mechanism is mechanical twinning, which should increase the
total elongation and ensure the pronounced hardening rate. While the
third one, is the strain-induced phase transformation, resulting in the

∗
Corresponding author.
E-mail address: joannak@agh.edu.pl (J. Kowalska).

https://doi.org/10.1016/j.msea.2019.138406
Received 25 July 2019; Received in revised form 28 August 2019; Accepted 8 September 2019
Available online 09 September 2019
0921-5093/ © 2019 Elsevier B.V. All rights reserved.
J. Kowalska, et al.
appearance of the ε- and/or α′-martensite within the microstructure.
This mechanism is supposed to increase the yield strength and hard-
ening rate of the steel.
Taking the above into account, the high-manganese steels are called
steels with the TWIP effect, if the mechanical twinning is the me-
chanism controlling plastic flow (TWIP - twinning induced plasticity) or
steels with the TRIP effect, if the martensitic phase transformations
occur during deformation (TRIP - transformation induced plasticity)
[7–11]. In general, both effects improve work hardening rate and delay
the necking before fracture, resulting in a very good combination of
strength and ductility. It should be emphasized however, that the
analysis of strain induced phase transformations usually appears a
complex problem because of a diversity of nucleation sites, formation
mechanisms and transformation sequences, including the most fre-
quently reported: γ (fcc) → ε (hcp) → α' (bcc) or γ (fcc) → twin → α'
(bcc) as well as direct γ (fcc) → α' (bcc).
Numerous hitherto studies indicate that SFE value is the basic factor
determining the occurrence of mechanisms that control the plastic flow
of high-manganese steels. At this point it should be noted, that in low
stacking fault energy fcc alloys, perfect (or unit) dislocations are dis-
sociated into two Shockley partials, which are separated by ribbons of
stacking faults. Hence, the appearance of SFs results from the passage of
partial dislocations with Burgers vectors a/6 < 112 > on {111} slip
planes and in consequence the sequence of close packed planes across
the associated stacking fault becomes effectively hcp [12]. The forma-
tion of the ε-phase and twins results from different spatial arrangement
of stacking faults, i.e. the character of their overlapping. The ε-phase is
formed if overlapping of SFs proceeds on alternate {111} planes (i.e.
every second close-packed plane), while deformation twins are pro-
duced when SFs overlap on successive {111} planes (e.g. Refs.
[13–15]).
According to Dumay et al. [16] for the SFE values above 18 mJ/m2
the alloys show tendency to mechanical twinning, whereas for smaller
SFE values the TRIP effect dominates upon plastic deformation of these
steels. Also Grässel et al. [1] published the work concerning the TRIP/
TWIP effect in high-manganese steels. They examined the influence of
alloying elements on mechanical properties of the austenitic steels Fe
(15–30 wt%) Mn with Al and Si additions. The authors found that alloys
show the TRIP effect if the content of Mn was below 20 wt%, whereas
the effect of TWIP dominated in the case of manganese content higher
than 25 wt% [1]. On the other hand Bouaziz et al. [3] found that if the
content of manganese is between 15 and 25 wt%, the structural effects
of both types of transformations co-exist within the microstructure of
the steel after deformation. Addition of silicon into the high-manganese
steel reduces SFE and favors the γ (fcc) → ε (hcp) transformation, both
during cooling and deformation [7]. On the contrary, it was shown that
aluminum causes an increase in SFE value, and therefore strongly
suppresses the γ (fcc) → ε (hcp) transformation [8,17]. Increasing the
carbon content in high-manganese steel raises SFE and stabilizes the
austenite. Ghasri-Khouzani and McDermid [9] investigated the effect of
carbon content on the properties and deformation structure of the
Fe–22Mn–C steel. During deformation of the steel with a lower carbon
content, the transformation of γ-austenite into ε-martensite dominated,
whereas the mechanical twinning controlled plastic flow in the alloy
with a higher carbon content, about 0.6 wt % C. In turn, Shen et al. [18]
examined the steel Fe–20Mn-0,6C with similar chemical composition,
which also showed the TWIP effect during deformation. However, the
essence of the study was the analysis of the influence of grain size and
strain rate on the course of twinning process and the resulting combi-
nation of plastic and strength properties [18].
A well-known experimental result is that the temperature sig-
nificantly influences the SFE value of alloys and in consequence affects
mechanisms operating upon deformation [11]. Lowering the tempera-
ture leads to a decrease in SFE and thus martensite should form during
plastic deformation of austenitic steels. In turn, the increase of the
deformation temperature results in the increase of SFE, so the dominant
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Materials Science & Engineering A 767 (2019) 138406
deformation mechanism should be twinning.
Most of the investigations conducted so far on high-manganese
steels concerned the influence of higher or elevated temperatures on
microstructure development and consequently the resulting TWIP effect
(e.g. Refs. [19–26]). On the other hand, much less research was devoted
to the plastic deformation of austenitic steels at lower temperatures
[4,17,27]. That is why, the purpose of this study was to examine the
influence of reduced temperatures on deformation behaviour, micro-
structure development and mechanical properties of high-manganese
steel containing 21.2 wt% Mn. The focus was on the initial stage of
plastic deformation, because the very beginning of the process clearly
indicated at structural instability of austenite and thus the γ (fcc) → ε
(hcp) phase transformation as a mechanisms controlling deformation.
Attention was also paid to the formation mechanism and nucleation
sites of α′-martensite in the initial stages of deformation.
2. Material and experimental procedure
The starting material for the experiment was high-manganese steel
Fe–Mn–Al–Si after hot-rolling and subsequent solution treatment. The
model steel was obtained by laboratory melting in vacuum induction
furnace VSG-100PVA TePla AG. Casting was carried out in argon at-
mosphere. Analysis of the chemical composition of the steel (given in
Table 1) was determined by the ICP-OES method (Inductively Coupled
Plasma - Optical Emission Spectroscopy) using Ultima 2 spectrometer
by Jobin-Yvon. After casting, steel homogenization at the temperature
1150 °C and then hot-rolling were conducted. Finally the steel was
annealed in argon atmosphere at the same temperature 1150 °C for 1 h
followed by water quenching.
Steel samples suitable for tensile testing were cut from the material
after the preliminary treatment. Tensile tests were carried out at four
temperatures, i.e. 20 °C, 0 °C, −50 °C and −150 °C, on test gauge bars
having a diameter of 5.0 mm and a gauge length of 50.0 mm. The
tensile machine used was an Instron 5982 apparatus and the applied
strain rate was 10−3s−1. For the examination presented in this paper,
the material was taken in the initial state (0%) and after a deformation
of 10% for each of the selected test temperatures. It is to note, that
tensile curves were not corrected from view point of machine com-
pliance and each temperature variant was performed to sample fracture
and carefully up to 10%.
X-ray phase analysis was carried out on a Siemens D500 dif-
fractometer using a lamp with a copper anode. Diffraction analysis was
performed on a longitudinal-section, parallel to the direction of
straining, in a middle part of the gauge length. The samples were pre-
viously ground on abrasive papers, polished on diamond pastes and
electro-polished to remove the deformed layer.
Samples for the metallographic examination were also taken from a
longitudinal section parallel to the direction of straining.
Microstructure observations and analysis were performed using the FEI
QUANTA 3D FEGSEM scanning electron microscope. A method of
backscattered electron diffraction (EBSD) was applied, using EDAX
Hikari camera with the following system parameters: beam current
20 nA, acceleration voltage 20 kV, binning 4 × 4 (120 × 120 effective
pixel resolution), step size of 100 nm and acquisition time of approxi-
mately 5 ms.
Table 1
The chemical composition of high-manganese steel under examination, in wt.%.
Mn Si Al C P S Fe
21.2 2.99 2.73 0.02 0.005 0.014 balance
J. Kowalska, et al. Materials Science & Engineering A 767 (2019) 138406

Fig. 1. Stress-strain curves for the Fe-Mn-Al-Si steel samples tensile tested at
reduced temperatures.
3. Results and discussion
3.1. Mechanical testing
Stress-strain curves for the Fe–Mn–Al–Si steel under examination,
obtained at reduced deformation temperatures, are shown in Fig. 1. The
results regarding ultimate tensile strength, total elongation and ad-
ditionally Vickers micro-hardness, are juxtaposed for each test tem-
perature in Table 2. It is evident that the values of ultimate tensile
strength increase significantly as the temperature decreases, starting
from 680 MPa at the temperature 20 °C up to 845 MPa and 1017 MPa at
−50 °C and −150 °C respectively. Simultaneously a parameter char-
acterizing plastic properties, i.e. the total elongation, decreases its value
from 65% at the temperature 0 °C to 58% and 54% at −50 °C and
−150 °C respectively. It should be noted, that the values of both
parameters remain very high for each of the test temperatures (Table 2)
compared to plain carbon steels. This comparison indicates at a very
good combination of plastic and strength properties of investigated
steel. Similarly, a value of another quantity that characterizes strength
properties, i.e. Vickers micro-hardness, also increases markedly with a
decrease in test temperature (244–294 HV0.1).
The microstructure analysis undertaken in this paper concerns
samples deformed up to 10% of tensile strain. It is necessary therefore,
to compare the rate of work hardening at different test temperatures for
this level of deformation. The stress-strain curves in Fig. 1 indicate that,
in the range of small deformations, differences in hardening rates be-
tween samples deformed at the temperatures 20 °C and 0 °C were rather
small. In both cases, the stress values achieved after 10% strain were
within a relatively narrow range of 480–500 MPa. Only the reduction of
deformation temperatures to −50 °C and then to −150 °C caused a
significant increase in stress up to about 560 MPa and 620 MPa re-
spectively.
3.2. X-ray analysis
X-ray diffraction patterns registered for the examined steel in the
Table 2
Mechanical properties of Fe-Mn-Al-Si steel at different deformation tempera-
tures.
Temperature of tensile test UTS Total elongation Microhardness, HV0.1
MPa % After 10% of tensile strain the structural effects of deformation
20 °C 680 57 244
0 °C 742 65 256
−50 °C 845 58 270
−150 °C 1017 54 294
initial state (0%) and after the tensile strain of 10% at different test
temperatures are shown in Fig. 2a and b. The diffraction pattern of the
starting material (0%) shows only lines originating essentially from
austenite, first of all (111)γ and (200)γ, as well as (220)γ, (311)γ and
(222)γ. It should be emphasized however, that the small contribution of
the α-ferrite was also detected after the preliminary treatment, reaching
roughly up to about 3% of volume fraction. After 10% of tensile strain,
clear and strong peaks appeared on diffraction patterns coming from
the ε-martensite having the hexagonal structure, namely the (10‾ 1 0) ε
and (10‾ 1 1) ε, as well as the weaker ones (10‾1 2) ε and (20‾
2 1) ε. These
peaks began to appear at reduced temperatures, starting from 0 °C. A
similar result was obtained by Koyama et al. [28] in the case of cold
deformed high-manganese steel Fe–17Mn-0.6C with increased carbon
content. The authors also observed the phase transformation induced
by strain γ (fcc) → ε (hcp) at deformation temperature of 0 °C, although
at ambient temperature of 20 °C the austenite remained essentially a
stable phase.
In addition to the initial α-ferrite, clear diffraction lines coming
from the strain-induced bcc phase were also detected in deformed
material, it means peaks from the α′-martensite. In general the intensity
of the martensite diffraction lines (ε and α′) increased with decreasing
deformation temperature. For deformation temperature of −150 °C, a
certain decrease in the intensity of the lines originating from the ε-
phase at the expense of the α′-martensite can be observed. It should be
noted however, that the X-ray phase analysis of the steel under ex-
amination faces certain difficulties, because some diffraction lines
coming from the analyzed phases overlap for given values of 2θ angle,
for example (111)γ and (0002)ε, (220)γ and (11‾ 2 0)ε as well as (222)γ
and (0004)ε.
Very significant influence of temperature on the occurrence of strain
induced martensitic transformation and twining was also found in the
research of Fang et al. [27]. The authors examined high manganese
(26 wt% Mn) steel Fe–Mn–Al–Si with low carbon content, tensile tested
within the temperature range 500 °C to −70 °C. On the diffractogram of
the sample in the initial state only the austenite was identified, whereas
after deformation at 20 °C and −70 °C the austenite turned out to be a
metastable phase during deformation and partially transformed into the
ε-martensite. Also in this case the X-ray phase analysis clearly in-
dicated, that the reduction of deformation temperature favored a par-
tial phase transformation γ (fcc) → ε (hcp) [27].
3.3. Microstructure examination
Fig. 3a shows the SEM microstructure of Fe–21Mn–3Al–3Si steel in
the initial state. Nearly equiaxed austenite grains of various size, fre-
quently exceeding even 100 μm, with numerous annealing twins are
visible. As may be seen from Fig. 3b, i.e. the inverse pole figure (IPF)
map, austenite grains showed almost random orientation distribution
after the preliminary treatment. It should be noted however, based on
the EBSD map in Fig. 3c, that the applied heat treatment resulted in the
appearance of some amount of the α-ferrite within the microstructure
of the initial material. A selective quantitative assessment showed, that
the average amount of ferrite (α) is approximately up to about 3% of
the volume fraction. The α-ferrite grains had much smaller size in
comparison to austenite, reaching only occasionally up to about 30 μm
in diameter, and were rather non-uniformly distributed within the
austenitic matrix. The crystallographic orientation relationship of
Kurdjumov-Sachs (K–S) was found to dominate between the austenite
(γ) and ferrite (α) grains, {111}γ‖{101}α and < 101 > γ‖ < 111 > α,
which in Fig. 3c is marked with a thin white line.
appeard in austenite grains for all the temperature variants (Figs. 4–7).
These effects are in the form of thin deformation bands from at least one
slip system. Taking into account the calculated SFE value of the steel
(14.26 mJ/m2 - see section 3.4) this should be a slip of dissociated
partial dislocations. At the temperature 20 °C a slight proportion of the

3
J. Kowalska, et al.
Fig. 2. X-ray diffractograms for Fe-Mn-Si-Al steel samples in the initial state (0%) and after 10% of tensile strain at four deformation temperatures (a), the expanded
plot the (111) and (200) for austenite and the (0002) and (10‾ 1 1) for ε-martensite peaks (b).
ε-martensite with a hexagonal close-packed structure appeared within
the microstructure of examined steel (Fig. 4, Table 3). However the
average fraction of this phase was very small and almost inconsiderable
in some places. As the temperature of deformation was reduced, to 0 °C,
−50 °C and finally −150 °C, the stability of austenite gradually de-
creased and the martensitic transformation took place to a much greater
extent. Starting from the temperature 0 °C, the contribution of strain
induced ε-phase has considerably increased after 10% of tensile strain,
reaching in places about 10.5% of the volume fraction.
Afterwards, the amount of the ε-phase exceeded 16% at the tem-
perature −50 °C, and then increased to about 20% of volume fraction at
the temperature −150 °C (Table 3 and Figs. 4c–7c). These results
4
Materials Science & Engineering A 767 (2019) 138406
clearly indicate at the reduction of austenite stability together with the
fall of deformation temperature, and are in agreement with a well-
known experimental fact, that lowering the temperature results in a
decrease in the SFE value [4,17,27]. In general it should be noted, that
in the steel under examination the strain induced γ (fcc) → ε (hcp)
transformation was initiated at low strains, regardless of the applied
deformation temperature.
In the case of the α′-martensite, it was difficult to determine the
exact mean values of its volume fractions, because of the selective
character of the measurements, which differed considerably depending
on the place of measurement. Within the range of small strains, diverse
results were obtained due to the low contents of α′-martensite and first
Fig. 3. Microstructure of Fe-Mn-Al-Si steel in the
initial state: band contrast image (a), IPF map (b),
EBSD phase map (red colour - γ-austenite, blue
colour - α-ferrite), the K-S relationship is marked
with a white line (c). (For interpretation of the re-
ferences to colour in this figure legend, the reader is
referred to the Web version of this article.)
J. Kowalska, et al.
of all its local occurrence, mainly at the intersections of ε-phase bands.
At this point it should be emphasized that, according to a number of
observations (e.g. Bracke et al. [29]), the α′-phase embryos do not
expand beyond the relatively small intersection areas of the ε-phase
bands, where they are usually formed. This may be one of the
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Materials Science & Engineering A 767 (2019) 138406
Fig. 4. Microstructure of Fe-Mn-Al-Si steel after
10% of deformation at temperature 20 °C: band
contrast image (a), IPF map (b), EBSD phase map
(red colour - γ-austenite, blue - α-ferrite, yellow - ε-
martensite), the K-S and S-N relationships are
marked with a white and black lines respectively
(c). (For interpretation of the references to colour in
this figure legend, the reader is referred to the Web
version of this article.)
explanations of relatively very low volume fraction of α′-martensite at
this level of deformation. Additionally, the places were also found,
where the α′-martensite was formed within a single set of parallel bands
of the ε-phase (Fig. 6c). In general, this observation is consistent with
the results of Olson and Cohen [13,30,31], who showed that the
Fig. 5. Microstructure of Fe-Mn-Al-Si steel after
10% of deformation at temperature 0 °C: band
contrast image (a), IPF map (b), EBSD phase map
(red colour - γ-austenite, blue - α-ferrite, yellow - ε-
martensite), the S-N relationship is marked with a
black line (c). (For interpretation of the references
to colour in this figure legend, the reader is referred
to the Web version of this article.)
J. Kowalska, et al. Materials Science & Engineering A 767 (2019) 138406

Fig. 6. Microstructure of Fe-Mn-Al-Si steel after 10% of deformation at temperature −50 °C: band contrast image (a), IPF map (b), EBSD phase map (red colour - γ-
austenite, blue - α′-martensite, yellow - ε-martensite), the K-S, S-N and B relationships are marked with a white, black and green line respectively (c), pole figures
from the area marked with a rectangle on Fig. 6c for FCC, HCP and BCC phase (d). (For interpretation of the references to colour in this figure legend, the reader is
referred to the Web version of this article.)

nucleation of the α′-martensite may proceed within the areas con-
taining bundles or packets of stacking faults, the ε-phase or deformation
twins. However, an exact explanation of this result will be given later in
this chapter.
Another complication in determining the real amount of this phase
resulted from the difficulty in distinguishing between the α′-martensite
and α-ferrite. Because of the very low carbon contents (0.02 wt%C) α′-
martensite had almost the same structure as α-ferrite, i.e. the body
centered cubic structure (bcc), instead of the body centered tetragonal
(bct) as in high-carbon steels. Thus, the only major differences between
both phases consisted in the morphology as well as nucleation sites and
the resulting places of α′-martensite formation.
As far as the ε-martensite is concerned, its contents within the range
of small strains is much larger and even the local character of the
measurements indicates at clear upward trend of its volume fraction
with decreasing temperature. This is especially well visible in
Figs. 5c–7c, i.e. on EBSD phase maps, where the increasing number of ε-
martensite bands (yellow colour) appeared on the background of un-
stable austenite (red colour). The lower deformation temperature, the
higher density of ε-bands, and the more frequent their mutual
intersections, which lead to the formation of α′-martensite embryos and
then small islands.
Fig. 6c shows the formation of α′-martensite in austenite grains,
where only a single system of the ε-bands was visible. According to
Olson and Cohen [13,31], two shear displacements are required to form
the α′-martensite. This principle was based on the model for the (fcc→
bcc) lattice transition, originally suggested by Bogers and Burgers [32].
It indicates that the shear necessary for this transition should be divided
between two invariant plain strains that can take place sequentially or
simultaneously. Hence, attempts to explain the formation of α′-mar-
tensite in cases of adjacent and non-intersecting bands always use ad-
ditional sources of stresses operating in non-parallel systems (e.g. Ryś
and Cempura [33], Fujita and Katayama [14], etc.).
The explanation proposed in this case indicates at the onset of a
secondary compatibility slip within the austenite grains. Therefore, in
spite of the fact that only a single deformation system of the ε-bands
was detected, there are sufficient stresses acting in still non-operating
(not revealed) secondary systems capable to induce nucleation and then
formation of the α′-martensite. It should be emphasized that the shapes
of the just formed α′-areas are extended parallel to the traces of planes

6
J. Kowalska, et al. Materials Science & Engineering A 767 (2019) 138406

orientation relationship between ε-martensite and α′-martensite, which

obeys the Burgers relationship i.e. {0001}ε‖{110}α′ and < 1120 >
ε‖ < 111 > α′, is marked with a thin green line (see Fig. 6c and d and
7c,d).
Fig. 7b and c displays the EBSD and IPF maps together with the
enlarged fragments for samples deformed at −150 °C. It is well visible
that α′-martensite formed islands exactly at the intersecting regions of
the ε-bands. Similarly the enlarged fragment of the EBSD map for
sample deformed at −50 °C indicates, that α′-martensite areas were
located exactly inside the bands of ε-phase (Fig. 6c). From these ob-
servations unambiguously results, that in examined steel austenite was
transformed into α′-martensite according to the sequence γ (fcc) → ε
(hcp) → α' (bcc).

4. Summary

The chemical composition of the steel under examination is a ty-

pical example of currently applied compositions for high-manganese
steels (e.g. Fe–Mn–Al–Si, Fe–Mn–C, Fe–Mn–Al–C, etc.). It includes high
contents of manganese with smaller additions of silicon and aluminum,
and a low amount of carbon, namely; Mn (21.2 wt%), Si (< 3 wt%), Al
(< 3 wt%) and C (0.02 wt%). In general, these steels have low stacking
fault energy at ambient temperature with SFE typically within the range
up to about 40 mJ/m2 [35,36]. Due to the chemical composition their
microstructure usually consist of single-phase austenite, which should
be a stable phase at room temperature and during further plastic de-
formation. In the case of the investigated steel the calculated SFE value
is 14,26 mJ/m2 [36,37]. Nevertheless, the microstructure of examined
steel contained small amount (roughly up to 3%) of bcc α-ferrite in the
initial state, i.e. after the preliminary treatment. Similar initial micro-
structure, i.e. containing small amount of bcc-phase (about 7%),
showed the 20Mn-3Si-3 Al-0.045C steel studied by Shen et al. [38]. The
chemical composition of that steel was very similar to the steel under
examination, except the carbon content which was more than twice as
high. Carbon is a very effective austenite stabilizer, and this fact might
Fig. 7. Microstructure of Fe-Mn-Al-Si steel after 10% of deformation at tem-
explain the occurrence of both mechanisms during deformation of that
perature −150 °C: band contrast image (a), IPF map (b), EBSD phase map (red
steel, i.e. twinning and strain induced phase transformation γ (fcc) → ε
colour - γ-austenite, blue - α-ferrite and α′-martensite, yellow - ε-martensite),
and IPF map from the area marked with a rectangle on Fig. 7b, the K-S, S-N and (hcp) → α' (bcc). On the other hand, the results of X-ray diffraction
B relationships are marked with a white, black and green line respectively (c), analysis and microstructure observations indicate that during de-
pole figures from the area marked with a rectangle on Fig. 7c for FCC, HCP and formation the austenite in examined 21Mn-3Si-3Al-0.02C steel turned
BCC phase (d). (For interpretation of the references to colour in this figure out to be metastable and underwent a strain-induced phase transfor-
legend, the reader is referred to the Web version of this article.) mation into martensite. The interpretation of strain-induced martensitic
transformation is based on the two ways of austenite to martensite
Table 3 transition, which concern hcp ε-martensite and bcc (or bct) α′-mar-
Phase composition of Fe-Mn-Al-Si steel in the initial state and after tensile tensite. The observed austenite instability refers not only to deforma-
deformation of 10% at reduced temperatures, estimated based on several local tion carried out at reduced temperatures, since a certain amount of ε-
EBSD measurements. martensite appeared within the microstructure of the steel already after
10% of tensile strain at ambient temperature of 20 °C. With the re-
Deformation FCC (γ) HCP (ε) BCC (α/α′) Non indexed
temperature phase [%] phase [%] phase [%] points [%] duction of deformation temperature, a gradual increase in the volume
fraction of the ε-phase was observed (Figs. 5c–7c and Table 3), up to
Initial state 97 – 3.0 – about 20% at −150 °C. It should be emphasized, that in the range up to
20 °C 96 0.8 3.1 0.1
10% of tensile strain, the amount of the α′-martensite was at the same
0 °C 86.8 10.4 2.4 0.6
−50 °C 80.8 16.4 2.5 0.3 time rather small. Despite the fact, that although in the steel under
−150 °C 74.6 20.0 4.9 0.5 examination the γ (fcc) → ε (hcp) → α' (bcc) transformation sequence
was observed, a deformation behaviour of the steel within the range of
small strains was dominated by strain-induced γ (fcc) → ε (hcp) mar-
of potential secondary systems. tensitic transformation. The lower the deformation temperature, the
It is well known from the literature, that hexagonal martensite is larger the amount of austenite transformed into ε-martensite and in
preferentially formed in the {111} planes of fcc austenite [34]. It is consequence, the higher degree of strain hardening was found. There-
obvious that the arrangement of atoms in {111}γ and (0001)ε planes of fore, the observed difference in strain-hardening is supposed to be first
both structures as well as along the respective directions < 110 > γ of all the result of the amount of strain-induced ε-martensite. The close-
and < 1120 > ε is identical. packed hexagonal structure is highly anisotropic and the easy slip is
Thus, the orientation relationship found between γ-austenite and ε- essentially possible only on the basal planes (0001) in three slip di-
martensite obeyed the Shoji-Nishiyama (S–N) relationship rections < 11‾ 2 0 > . As a result the number of slip systems showing low
{111}γ‖{0001}ε and < 110 > γ‖ < 1120 > ε, which is marked with a values of critical resolved shear stresses (CRSS) is the least in the ε-
thin black line on enlarged fragments in Figs. 6c and 7c. In turn the martensite and the remaining potential slip planes are characterized by

7
J. Kowalska, et al.
much higher values of CRSS. That is why, the ε-phase is usually re-
ported as a strong barrier for further plastic flow.
As mentioned before, the formation mechanism of deformation
bands in this type of alloys is associated with the accumulated motion
of planar defects in the form of so called extended dislocations, i.e.
dissociated dislocations coupled by the SF ribbons. Depending on the
SFE value and the resulting manner of stacking fault overlapping (in
other words, SF spatial arrangement) the bands of ε-martensite or twin
bands may be formed, or simply dense stacking fault packets
[13,15,29,39]. The deformation behavior of high-manganese steels may
considerably change depending on the applied temperature range and
the exact chemical composition. It follows from the fact that both fac-
tors, i.e. the temperature and the chemical composition, determine the
SFE value and in consequence the operating deformation mechanisms,
which result in a specific microstructure and final mechanical proper-
ties.
For example, Choi et al. [10] examined the microstructure of the
austenitic steel Fe–24Mn-0.12C tensile tested at various temperatures
within the range 7 °C–277 °C. In the case of samples deformed at tem-
peratures ranging from 7 °C to 57 °C, both, the strain induced ε-mar-
tensite as well as deformation twins were found within the micro-
structure of the steel. On the other hand, in the case of tensile tests
conducted at higher temperatures, i.e. between 127 °C and 227 °C, the
twinning mechanism prevailed resulting in domination of deformation
twins within the microstructure. In turn Huang et al. [19] investigated
mechanical properties of an austenitic Fe–23Mn–2Si–2Al (wt.%) steel,
with small addition of niobium, as a function of deformation tem-
perature, within the range 20 °C to −75 °C. The microstructure ob-
servations revealed a large number of twins induced by deformation
above −60 °C. As a result the steel achieved a relatively high total
elongations of about 80% and the increase of the ultimate tensile
strength from 660 to 750 MPa, which was the effect of twinning-in-
duced plasticity (TWIP). At temperatures below −60 °C, the stability of
the austenite decreased and martensitic transformations occurred, γ
(fcc) → ε (hcp) → α' (bcc), as a result of TRIP effect. Due to transfor-
mation-induced plasticity, total elongations attained 87% and ultimate
tensile strength reached up to 810 MPa.
During lowering of deformation temperature the rate of transfor-
mation in the steel under examination and the resulting volume fraction
of ε-martensite bands considerably increased. Therefore, it should be
assumed that the SFE value of the examined steel significantly de-
creased, despite the relatively high Mn contents (about 21 wt%). The
results obtained by Li et al. [40] indicate that suitable content of Mn
increased the stability of austenite as well as the ε-martensite, because
the SFE value of austenite increases with Mn content. The authors found
that α′-martensitic transformation was rather difficult in steel having
~19 wt% of Mn because of the high stability of ε-martensite.
Simultaneously, it was frequently observed, that the intersecting
bands of ε-martensite lead to strong local distortion of the austenite
lattice. According to a number of authors, such a situation may be a
source of driving force for the formation of the α′-martensite
[12,19,29,34,41]. Therefore the deformation behaviour in the course of
strain induced transformations, which are engaging the three phases
(i.e. γ-austenite, ε- and α′-martensite), is frequently explained in the
following way. The γ (fcc)→ε (hcp) transformation is considered to
increase the strength of deformed steel and, on the other hand, the
occurrence of the ε (hcp) → α’ (bcc) transformation is supposed to
decrease the local internal stresses resulting from the intersection of ε-
bands (Li et al. [40]). It is assumed that intersections of ε-bands with
non-parallel secondary slip systems, often observed in the examined
steel at the initial stage of deformation, may also have the same effect.
In general, martensitic transformation taking place during deformation
of the examined high manganese steel affected in a very significant way
the work hardening behaviour and mechanical properties through the
TRIP effect, starting from the range of relatively small strains.
8
Materials Science & Engineering A 767 (2019) 138406
5. Concluding remarks
During reduction of deformation temperature in tensile tested high-
manganese Fe–Mn–Si–Al steel, a marked increase in the ultimate tensile
strength was observed and simultaneously a relatively small decrease in
total elongation. It should be emphasized that the steel showed a very
good combination of strength and plastic properties for each of the
applied test temperatures from the range 20 °C to −150 °C.
Due to the small SFE value of the steel, the dominant deformation
mechanism at the onset of yielding was slip of dissociated dislocations.
Just afterwards, still within the range of small strains, the strain-in-
duced phase transformation γ (fcc) → ε (hcp) was increasingly occur-
ring during lowering of the deformation temperature.
The carried out analysis indicates that in the steel under examina-
tion the deformation-induced phase transformations occurred at low
temperatures in accordance with the following sequence γ (fcc) → ε
(hcp) → α' (bcc). In the range of small strains a considerable increase in
work hardening with decreasing temperature corresponded to a sig-
nificant increase in the amount of ε-martensite within the micro-
structure of the steel.
Lowering of the deformation temperature had a very significant
influence on increasing the volume fraction of ε-martensite with a
hexagonal structure. This effect was a consequence of the decrease in
the SFE value and the reduction of austenite stability at low tempera-
tures.
After 10% of tensile strain the volume fractions of ε-phase increased
up to about 16% and 20% at the temperatures reduced to −50 °C and
−150 °C respectively. On the other hand the volume fraction of α′-
martensite was rather slight and it was frequently formed at the in-
tersections of the ε-phase bands from two non-parallel sets.
Additionally, formation of α′-martensite was also observed at the in-
tersections of ε-bands with non-parallel secondary slip systems.
Preferential crystallographic orientation relations were detected,
dominating between γ-austenite and the strain induced ε- and α′-
phases, i.e.: Shoji-Nishiyama (S–N) - {111}γ‖{0001}ε
and < 110 > γ‖ < 1120 > ε and Kurdjumov-Sachs (K–S) -
{111}γ‖{110}α′ and < 110 > γ‖ < 111 > α′ respectively. In con-
sequence, between ε-martensite and α′-martensite, the Burgers re-
lationship i.e. {0001}ε‖{110})α′ and < 1120 > ε‖ < 111 > α′ was
observed.
Acknowledgements
This work was sponsored by the National Science Centre, Poland
under Contract no 2011/01/D/ST8/03905.
The authors wish to thank Professor Piotr Bała for offering facilities
in AGH-UST Academic Centre for Materials and Nanotechnology, which
made possible to conduct a significant part of the presented research.
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