Effect of the Intercritical Annealing Temperature on the

Mechanical Properties of 10 Pct Mn Multi-phase Steel

SANGWON LEE and BRUNO CHARLES DE COOMAN

Intercritically annealed 10 pct Mn steel has been shown to exhibit an excellent combination of
strength and ductility due to the plasticity-enhancing mechanisms of mechanical twinning and
strain-induced martensite transformation occurring in sequence. This mechanical behavior is
only achieved for a multi-phase microstructure obtained after annealing within a specific
intercritical temperature range. A model for the selection of the optimal intercritical annealing
temperature was developed to achieve a high strength-ductility balance for 10 pct Mn multi-
phase steel. The model considers the room temperature stacking fault energy and the thermo-
dynamic stability of the retained austenite.

DOI: 10.1007/s11661-014-2449-0
 The Minerals, Metals & Materials Society and ASM International 2014

I. INTRODUCTION steel has a high Al and C content, resulting in a high SFE

STEELS with a wide range of Mn content (6 to
30 mass pct) are currently being studied as possible
advanced ultra-high strength (UTS >1 GP) materials
for automotive applications due to their superior com-
bination of strength and ductility compared to standard
low carbon formable steel grades.[1–6] These new Mn
steels can broadly be divided in three groups on the basis
of the plasticity-enhancing mechanisms which control
their mechanical properties:
The first group includes medium 4 to 8 pct Mn
transformation-induced plasticity (TRIP) steel.[1,7]
These medium Mn TRIP steels have ultra-fine grained
multi-phase microstructures consisting of ferrite and
metastable austenite. The metastable austenite trans-
forms to martensite during deformation, resulting in
high work hardening rates and total elongations of
about 30 pct.[7]
The second group includes high 12 to 22 pct Mn
twinning-induced plasticity (TWIP) steel.[8–10] TWIP
steel has a fully austenitic microstructure and a moder-
ate stacking fault energy (SFE) of approximately 20 mJ/
m2.[8] These austenitic steels exhibit mechanical twinning
which results in exceptionally high work hardening rates
and a high ductility, with total elongations of about
60 pct.
The third group of steels is characterized by a high Mn
content, 22 to 30 pct. The plasticity-enhancing mecha-
nism is microband-induced plasticity (MBIP).[11,12] MBIP
SANGWON LEE, Graduate Student, is with the Graduate Institute
of Ferrous Metallurgy, Pohang University of Science and Technology,
Pohang 790-784, South Korea, and also with the Materials Design
Laboratory, Pohang University of Science and Technology. BRUNO
C. DE COOMAN, Professor, is with Graduate Institute of Ferrous
Metallurgy, Pohang University of Science and Technology and
Director, Materials Design Laboratory, Pohang University of Science
and Technology. Contact e-mail: decooman@postech.ac.kr
Manuscript submitted October 25, 2013.
Article published online August 2, 2014
(~80 mJ/m2).[11] Micro-shear bands generated during
deformation results in a high work hardening rate and a
high ductility, with total elongations of about 60 pct.
The different plasticity-enhancing mechanisms are
critically dependent on the room temperature SFE of
the austenite, which is controlled by the phase composi-
tion and the temperature. Whereas additions of C, Mn,
and Al increase the SFE, additions of Si and Cr result in a
decrease of the SFE.[3,5,8,13–15] The TRIP effect occurs in
austenite with a SFE less than 15 mJ/m2, the TRIP and
TWIP effect occur simultaneously in the SFE range of
15 mJ/m2 < SFE < 20 mJ/m2. The TWIP effect is dom-
inant when the SFE is in the range of 20 to 35 mJ/m2.
In recently published work, the development of a Fe-
10 pct Mn-3 pct Al-2 pct Si-0.3 pct C steel which had a
duplex microstructure consisting of ferrite and austenite
after intercritical annealing was reported.[16] The room
temperature SFE and the thermodynamic stability of
the austenite phase in this steel were controlled by the
partitioning to the intercritical austenite of C and Mn
during the annealing. The austenite in the intercritically
annealed 10 pct Mn steel developed mechanical twins
during deformation at low strain. After the generation
of mechanical twins had reached a saturation point,
martensite nucleation was initiated at twin–twin inter-
sections at higher strains. This TWIP–TRIP transition
mechanism resulted in a surprisingly high work hard-
ening rate and a total elongation comparable to that of
the more highly Mn-alloyed TWIP and MBIP steels.
Due to the fact that excellent mechanical properties
were obtained with less alloying, the alloy design
concept used for the 10 pct Mn TWIP–TRIP transition
steel clearly illustrated that there were alternative alloy
designs based on intercritical annealing, for the devel-
opment of leaner steels suitable for third generation
ultra-high strength automotive steel applications.
The tensile behavior of 10 pct Mn TWIP–TRIP
transition steel is however sensitive of the choice of the
intercritical annealing temperature, as this temperature

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 45A, OCTOBER 2014—5009

determines the phase fraction and the composition of
the intercritical austenite. In the present work, a method
to predict the room temperature phase fraction, the
chemical composition, and the SFE of the austenite is
proposed. It is shown that this method can be used to
achieve an optimal strength–ductility balance.
The schematic of Figure 1 illustrates the principle of
the method. The microstructure of the cold-rolled sheet
of 10 pct Mn steel, obtained after hot rolling, consists of
ferrite, a¢-martensite and retained austenite. The mar-
tensite start temperature of the initial austenite phase,
Ms, is above room temperature. When the cold-rolled
sheet is annealed in the intercritical temperature range,
the martensite is transformed back to austenite, and the
C and Mn content of the intercritical austenite are
increased during intercritical annealing as a result of the
partitioning of C and Mn to the intercritical austenite.
The partitioning results in an enhanced room temper-
ature austenite stability, as the Ms temperature gradu-
ally decreases to a value below room temperature during
the intercritical annealing as shown schematically in
Figure 1(a). The ferrite volume fraction increases as the
intercritical annealing temperature decreases, thereby
further enhancing the partitioning of the C and Mn, as
shown in the Figures 1(b) and (c). As a consequence,
both the room temperature austenite stability and its
SFE are determined by the selection of the intercritical
annealing temperature, as this temperature determines
the equilibrium composition of the intercritical austen-
ite. In order to obtain a room temperature austenite
phase which undergoes twinning-induced plasticity, the
room temperature SFE should be controlled in the
range of 20 to 35 mJ/m2, as shown in Figure 1(d).[14]
This condition also guarantees that the Ms temperature
will be below room temperature and that the TWIP
effect and the TRIP effect will occur in succession.
Fig. 1—Schematic describing the alloy concept of intercritically annealed 10 pct Mn steel. (a) Thermal cycle showing the decrease of the Ms tem-
perature due to partitioning. (b) The influence of TIA on the ferrite and austenite phase fractions. (c) The influence of TIA on the C and Mn con-
tent of the intercritical austenite. (d) The influence of TIA on the room temperature SFE of austenite.
5010—VOLUME 45A, OCTOBER 2014
II. EXPERIMENTAL
The chemical composition of the steel used in the
present work was Fe-10 pct Mn-0.3 pct C-3 pct Al-2 pct
Si, in mass pct. Ingots were prepared by vacuum
induction melting. Slabs were hot-rolled after reheating
at 1473 K (1200 C) to produce a 2.5-mm thick sheet.
The hot-rolled sheets were pickled and cold rolled to a
50 pct reduction. The intercritical annealing tempera-
tures selected for the experimental validation of the
model were 973 K, 1073 K, and 1173 K (700 C,
800 C, 900 C). The samples were heated using a
heating rate of 4 K/s. During annealing, the samples
were held at the intercritical annealing temperature, TIA,
for 300 seconds to achieve full phase equilibrium. The
samples were cooled to room temperature using a
cooling rate of 30 K/s. ASTM-E8 subsize tensile test
samples with a gauge length of 50 mm and the tensile
axis aligned parallel to the rolling direction were
prepared from the intercritically annealed samples.
The tensile tests were carried out at a strain rate of
103 s1 using a ZWICK universal tensile testing
machine. The fraction of strain-induced martensite was
monitored during the tensile tests by means of a
portable ferrite phase analyzer.
The microstructural analysis of the deformation
microstructures was done in a ZEISS Ultra-55 Scanning
Electron Microscope equipped with a Field-Emission
electron source (FE-SEM) and an Electron-Back
Scattering Diffraction (EBSD) system. Specimens were
mechanically polished and electro-polished at room
temperature in a solution of 95 pct CH3COOH and
5 pct HClO4 to avoid preparation-related formation of
martensite.
A JEOL 2100F Transmission Electron Microscope
equipped with a Field Emission electron source
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 2—FE-SEM micrographs of Fe-10 pct Mn-x pct C-3 pct Al-
2 pct Si steel. (a) After annealing at 1273 K (1000 C) in the homo-
geneous austenite stability range. (b) After annealing at 1073 K
(800 C) in the intercritical two-phase ferrite and austenite stability
range.
Fig. 3—Retained austenite grain size in Fe-10 pct Mn-x pct C-3 pct
Al-2 pct Si steel after intercritical annealing in the 973 K to 1173 K
(700 C to 900 C) temperature range.
(FE-TEM) was used to examine the plasticity-enhancing
mechanisms by the direct observation of mechanical
twins and strain-induced a¢-martensite.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 4—True stress–strain curves of intercritically annealed Fe-10 pct
Mn-x pct C-3 pct Al-2 pct Si steel after annealing at 973 K, 1073 K,
and 1173 K (700 C, 800 C, and 900 C).
III. RESULTS
Figures 2(a) and (b) show FE-SEM micrographs of
the intercritically annealed 10 pct Mn steel after anneal-
ing at 1073 K and 1273 K (800 C and 1000 C),
respectively. The microstructure was fully austenitic at
an annealing temperature of 1273 K (1000 C) and
transformed partially to athermal a¢-martensite upon
cooling to room temperature, as shown in Figure 2(a).
A two-phase microstructure consisting of austenite and
ferrite was obtained after intercritially annealed at
1073 K (800 C). No athermal a¢-martensite was ob-
served due to the fact that the C and Mn partitioning to
the intercritical austenite resulted in a high stability
austenite phase with an Ms temperature below room
temperature.
The TIA-dependence of the average austenite grain
size, measured by means of EBSD, is shown in Figure 3.
The austenite grain size increases linearly with an
increase of TIA. The austenite grain size was very fine,
e.g., approximately 2 lm after intercritical annealing at
1173 K (900 C). This small grain size was due to the
inhibition of the austenite grain growth by the ferrite.
An increase of volume ferrite fraction leads to a
reduction of the austenite grain size to less that 1 lm
when TIA was less than 1023 K (750 C).
Tensile stress–strain curves for 10 pct Mn steel
intercritically annealed at 973 K, 1073 K, and 1173 K
(700 C, 800 C, 900 C) are shown in Figure 4. The
tensile behavior has a pronounced TIA-dependence,
which can be explained as follows.
The yield strength of intercritically annealed 10 pct
Mn steel is determined by the volume fraction, compo-
sition, and grain size of the constituent phases. The yield
strength of 10 pct Mn steel was found to increase with
decreasing TIA. The work hardening rate and the total
elongation reached their lowest value after annealing at
973 K (700 C), i.e., when the retained austenite had its
highest stability and SFE. The work hardening rate
reached its highest value after annealing at 1173 K
(900 C), i.e., when the retained austenite stability and
VOLUME 45A, OCTOBER 2014—5011
5012—VOLUME 45A, OCTOBER 2014 METALLURGICAL AND MATERIALS TRANSACTIONS A
bFig. 5—TEM micrographs of intercritically annealed Fe-10 pct Mn-
x pct C-3 pct Al-2 pct Si steel strained to 10 pct engineering strain.
The electron beam was approximately parallel to the h110ic direction
for micrographs (b) through (f). (a) Bright-field image showing the
initial ultra-fine grained microstructure [TIA = 973 K (700 C)]. (b)
Bright-field image of deformation-induced twins [TIA = 1073 K
(800 C)]. (c) Dark-field image using the (111)Twin reflection in (d).
(d) Selected area diffraction pattern of (b). (e) Bright-field image of
deformation-induced a¢-martensite [TIA = (1173 K (900 C)]. (f)
Dark-field image using the ð110Þa0 reflection in (g). (g) Selected area
diffraction pattern for (e).
SFE were the smallest. At an intermediate annealing
temperature of 1073 K (800 C), an exceptionally high
elongation was obtained due to the activation of
mechanical twinning at low strain and the strain-
induced a¢-martensite nucleation at twin–twin intersec-
tions at higher strain.[16]
Figure 5 shows the TEM micrographs of the deformed
microstructures of the 10 pct Mn steel annealed at
different TIA. The TEM samples were prepared after
tensile testing to 10 pct engineering strain. After anneal-
ing at 973 K (700 C), the microstructure had an ultra-
fine grain size. There was no evidence of mechanical
twinning or a¢-martensite formation during deformation,
as shown in Figure 5(a). The high SFE and austenite
stability clearly inhibited both the TWIP effect and the
TRIP effect. The steel annealed at 1073 K (800 C)
contained mechanical twins as shown in Figures 5(b)
through (d). No a¢-martensite was observed. The steel
annealed at 1173 K (900 C) had a high density of a¢-
martensite as shown in Figures 5(e) through (g). The
volume fraction of strain-induced a¢-martensite was
measured as a function of the applied strain. The results
are shown in Figure 6. Whereas no TRIP effect occurs
after intercritically annealed at 973 K (700 C), a¢-
martensite formation was very pronounced in the steel
intercritically annealed at 1173 K (900 C).
The TIA-dependence of the microstructure and tensile
properties of 10 pct Mn steel were investigated in detail.
The tensile properties of 10 pct Mn steel are controlled
by the kinetics of the formation of mechanical twins and
the strain-induced a¢-martensite transformation. As a
rule, the austenite stability and the SFE of retained
austenite increase when the volume fraction of the
intercritical ferrite is higher. This results in the activation
of two strain hardening-enhancing mechanisms and an
intermediate work hardening rate. When the intercritical
microstructure is fully austenitic, the kinetics of the
a¢-martensite formation is too fast, resulting in a
premature fracture. The optimal TIA should be chosen
to achieve a room temperature microstructure consisting
of ferrite and retained austenite, and athermal a¢-mar-
tensite should not be present in the initial microstructure.
The thermodynamic properties of the retained austenite
should therefore be such that athermal a¢-martensite is not
formed upon cooling to room temperature.
IV. DISCUSSION
Figure 7(a) shows a pseudo-binary Fe-C equilibrium
phase diagram for Fe-10 pct Mn-x pct C-3 pct Al-2 pct
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 6—Volume fraction of strain-induced a¢-martensite during ten-
sile testing of Fe-10 pct Mn-x pct C-3 pct Al-2 pct Si steel intercriti-
cally annealed at 973 K, 1073 K, and 1173 K (700 C, 800 C, and
900 C).
Si. The corresponding temperature dependence of the
equilibrium phase fraction is shown in Figure 7(b). The
microstructure is fully austenitic when the annealing
temperature is higher than 1098 K (825 C). Cementite
and (Fe,Mn)5C3 are formed when the annealing tem-
perature is lower than 948 K (675 C). The formation of
these carbides reduces the C and Mn content of the
retained austenite below 948 K (675 C). Figure 7(c)
shows the temperature-dependent equilibrium composi-
tion of the austenite, which reveals a temperature range
in which both C and Mn are partitioned to the
intercritical austenite with increasing volume fraction
of intercritical ferrite. As the carbide formation for
annealing temperatures lower than 948 K (675 C)
decreases the austenite stability and results in brittle
fracture of the carbides, the annealing temperature
should always be higher than 948 K (675 C). Note that
the Al and Si content of the austenite are not much
influenced by the annealing temperature.
The grain size of the room temperature retained
austenite in intercritically annealed 10 pct Mn steel must
also be taken into account, as it too influences the
austenite stability and the kinetics of the mechanical
twinning and strain-induced a¢-martensite transforma-
tion. A small austenite grain size inhibits the nucleation
of twins and martensite during deformation.[17,18] The
martensite start temperature (Ms) was obtained using
the following empirical equation which takes into
account the effect of the austenite grain size[18]:
Ms ð CÞ ¼ 545  432C  30:4Mn  60:5V1=3 : ½1
c
Here C and Mn are the C and Mn mass pct content of
the intercritical austenite, respectively. Vc is the average
austenite grain volume in lm3, which can be obtained by
using the fitting curve in Figure 3. Figure 8(a) shows the
calculated Ms temperature as a function of TIA. C and
Mn partitioning to austenite results in an increase of the
austenite stability and reduction of the Ms temperature.
VOLUME 45A, OCTOBER 2014—5013

Fig. 7—(a) Pseudo-binary Fe-C equilibrium phase diagram for Fe-
10 pct Mn-x pct C-3 pct Al-2 pct Si steel. (b) Equilibrium tempera-
ture dependence of the phase volume fraction. (c) Temperature
dependence of the equilibrium composition of the austenite.
When the grain size of retained austenite is considered,
the formation of athermal a¢-martensite is inhibited
during cooling from the intercritical temperature. The
5014—VOLUME 45A, OCTOBER 2014
Fig. 8—(a) Ms temperature of the intercritical austenite in annealed
Fe-10 pct Mn-x pct C-3 pct Al-2 pct Si steel as a function of the
annealing temperature. (b) Phase volume fractions as a function of
the temperature.
Ms temperature is higher than room temperature when
the TIA is higher than approximately 1073 K (800 C).
Figure 2 showed that whereas a high volume fraction of
athermal a¢-martensite was observed after annealing at
1273 K (1000 C), no a¢-martensite was observed after
annealing at 1073 K (800 C). The calculation results
are in good agreement with the experimental observa-
tions. The volume fraction of athermal a¢-martensite
was computed by means of the empirical equation
proposed by Koistinen and Marburger[19]:
fa0 ¼ 1  exp½aðMs  TÞb : ½2
Here fa0 is the volume fraction of athermal
a¢-martensite, T is the temperature. The unit for T and
Ms are degree Kelvin. a and b are parameters related to
the kinetics of athermal a¢-martensite formation. These
parameters can be computed by means of the following
equations[18]:
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 9—Room temperature SFE of the retained austenite in intercrit-
ically annealed Fe-10 pct Mn-x pct C-3 pct Al-2 pct Si steel as a
function of the annealing temperature.
a ¼ 0:0076  0:0182C þ 0:00014Mn; ½3
b ¼ 1:4609 þ 0:4483C  0:0545Mn: ½4
Figure 8(b) shows the room temperature volume
fraction of athermal a¢-martensite and retained austenite
calculated by using Eqs. [2], [3], and [4]. The maximum
fraction of retained austenite is obtained after intercrit-
ical annealing at 1073 K (800 C). The retained austen-
ite volume fraction decreases when TIA is higher than
1073 K (800 C) due to the formation of athermal
a¢-martensite. Athermal a¢-martensite must be absent in
the as-annealed room temperature microstructure in
order to avoid premature fracture resulting from the
brittle fracture of the a¢-martensite.
Noting that the intrinsic SFE of face-centered cubic
metals and alloys is related to the molar Gibbs energy of
the c fi e transformation, Olson and Cohen[20] pro-
posed the following equation to calculate the SFE:
SFE ¼ 2qDGc!e þ 2rc=e : ½5
Here Gc!e is the molar free energy difference between
c and e-martensite, q is the molar surface density, and
rc=e is the c/e interfacial energy. Takaki et al.[21] inves-
tigated the driving force for the c fi e transformation
and included an excess free energy DGex contribution
due to the austenite grain size in their analysis:
DGex ¼ 170:06  expðd=18:55Þ: ½6
Takaki et al.[21] reformulated Eq. [5] as follows:
SFE ¼ 2qðDGc!e þ DGex Þ þ 2rc=e : ½7
Figure 9 shows the TIA-dependence of the room
temperature SFE of the retained austenite using data
METALLURGICAL AND MATERIALS TRANSACTIONS A
from Reference 15. The room temperature SFE of the
retained austenite increases due to the partitioning effect
at lower TIA, but it decreases when TIA is less than
948 K (675 C) due to the precipitation of carbides.
The results indicate that mechanical twinning will
occur in samples intercritically annealed at a TIA higher
than 1073 K (800 C), as the SFE is in the range of 20 to
35 mJ/m2.[14] Mechanical twinning is inhibited in sam-
ples annealed at 948 K (675 C) as the SFE of the
retained austenite will be higher than 35 mJ/m2. When
the SFE is higher than 35 mJ/m2 dislocation glide is the
preferred deformation mechanism.[13] The SFE of the
retained austenite must be in the range of 20 to 35 mJ/
m2, in order to observe mechanical twinning and the
TWIP effect in the retained austenite. When TIA is
higher than 973 K (700 C), the retained austenite
exhibits mechanical twining. In addition, no strain-
induced e-martensite transformation occurs during
deformation.
The TEM observations showed that no plasticity-
enhancing mechanism was observed after annealing at
700 C while mechanical twins were observed in the
samples annealed at 1073 K and 1173 K (800 C and
900 C). None of the tested samples contained
e-martensite. The calculation of the SFE of the retained
austenite is therefore in good agreement with the TEM
observations.
The model illustrates the relation between TIA, the
room temperature SFE, and the Ms temperature of the
retained austenite, and the plasticity-enhancing mecha-
nism at low strains. Experimental observations[1] show
that the TWIP effect was followed by the TRIP effect,
which resulted from the nucleation of a¢-martensite at
twin intersections, when the conditions for mechanical
twinning and the TWIP effect were met for the retained
austenite.
The model identifies clearly the following three
conditions for the selection of an optimal TIA for
intercritically annealed 10 pct Mn steel:
1. The TIA temperature should be high enough to
avoid the formation of carbides and premature frac-
ture due to their brittle behavior.
2. The TIA temperature should be chosen such that
the Ms temperature of the C and Mn partitioned in-
tercritical austenite is below room temperature.
3. The TIA temperature should be chosen to obtain a
room temperature SFE for the intercritical austenite
which leads to mechanical twinning takes place dur-
ing deformation.
The tensile behavior of 10 pct Mn steel after anneal-
ing at 1173 K (900 C) exhibited a high work hardening
rate but a low ductility due to the presence of
a¢-martensite in the starting microstructure.
The model calculations indicate that the optimal TIA
to achieve the best mechanical properties was 1073 K
(800 C), as athermal a¢-martensite and carbides were
not present in the microstructure. The SFE of the
retained austenite is approximately 25 mJ/m2 for an
intercritical annealing at 1073 K (800 C), resulting in
mechanical twinning, the TWIP effect and the TRIP
effect in succession.
VOLUME 45A, OCTOBER 2014—5015
 V. CONCLUSIONS
A model for the selection of the intercritical annealing
temperature TIA to achieve optimal mechanical proper-
ties in multiphase 10 pct Mn steel has been proposed. It
is based on (a) the control of the Ms temperature to
obtain a microstructure without athermal a¢-martensite
upon cooling after intercritical annealing, and (b)
the control of the room temperature SFE of the
retained austenite to achieve mechanical twinning in
the austenite.
In the case of intercritically annealed Fe-10 pct Mn-
x pct C-3 pct Al-2 pct Si the model calculations indi-
cated that
1. For TIA less than 973 K (700 C), carbide forma-
tion occured during intercritical annealing and the
TWIP effect was suppressed in the austenite phase
because its SFE was too high. Both effects resulted
in premature sample fracture in uniaxial tensile
tests.
2. For TIA approximately equal to 1073 K (800 C),
the retained austenite had optimum properties in
terms of Ms temperature and SFE. Carbides and
athermal a¢-martensite were not present in the
microstructure. In addition, the steel displayed a
succession of two plasticity-enhancing mechanisms
in succession. The TWIP effect occurred at low
strains. The TRIP effect occurred at higher strains,
with the nucleation of strain-induced a¢-martensite
occurring at twin intersections.
3. For TIA higher than 1173 K (900 C), athermal
a¢-martensite was formed and the low SFE resulted
in the rapid formation of additional strain-induced
a¢-martensite. This resulted in a very limited TRIP
effect and premature sample fracture during
uniaxial tensile tests.
5016—VOLUME 45A, OCTOBER 2014
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METALLURGICAL AND MATERIALS TRANSACTIONS A