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Acta Materialia 61 (2013) 558578


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Inuence of carbon content on the microstructure,


martensitic transformation and mechanical properties
in austenite/e-martensite dual-phase FeMnC steels
Jae-Bok Seol a,b, J.E. Jung b, Y.W. Jang b, C.G. Park b,c,
a
Max-Planck-Insititut fur Eisenforschung, Max-Planck-Str. 1, 40237 Dusseldorf, Germany
b
Department of Materials Science and Engineering, Pohang University of Science and Technology (POSTECH), 790-784 Pohang, Republic of Korea
c
National Center for Nanomaterials Technology (NCNT), POSTECH, 790-784 Pohang, Republic of Korea

Received 2 September 2012; received in revised form 27 September 2012; accepted 29 September 2012
Available online 7 November 2012

Abstract

We report on the eects of carbon content on the martensitic transformation and its contribution to the work-hardening behavior of
FeMnC steels during tensile deformation based on analysis by X-ray diraction, electron backscatter diraction and transmission elec-
tron microscopy. Austenite/e-martensite dual-phase Fe17MnC (wt.%) steels containing dierent carbon contents (0.01, 0.10, 0.20
wt.%) were investigated before, during and after tensile deformation. Before deformation, the transformation of austenite to thermally
induced e-martensite on cooling was suppressed as the carbon content increases. To precisely monitor microstructural changes during
deformation, stepwise loading experiments were carried out in combination with electron backscatter diraction analysis. This approach
revealed that with increasing carbon content, the kinetics of transformation of c phase to deformation stimulated e-martensite became
faster, while that of e-martensite to a-martensite was sluggish. We attribute this controversial eect to an increased c grain size by the
microstructural renement of thermally induced e-martensite and the reduction of solid solution strengthening eects by the redistribu-
tion of solute carbon. In addition, the dependence of deformation-induced e-martensite on the loading direction diered from that of a-
martensite, and the evolution of a morphology was controlled by achieving appropriate levels of strain during stepwise loading. Based
on the observations at the surface and inside the bulk after deformation, insights into various deformation-driven displacive phenomena,
such as the formation of a-martensite at the nonintersecting parts of two einitial bands, the presence of nanotwinned bundles inside aus-
tenite, cementite precipitation inside a-martensite, and the origin of the serrated ow in strainstress curves, were obtained. Therefore,
the present study is able assist in identifying whether the deformation-induced martensitic transformation varied as a function of carbon
content and the resulting fracture behavior, thereby enabling us to understand the work-hardening behavior of these steels.
Crown Copyright 2012 Published by Elsevier Ltd. on behalf of Acta Materialia Inc. All rights reserved.

Keywords: High manganese steels; Deformation-induced e-martensite; Stepwise tensile loading experiment; Transmission electron microscopy; Electron
backscatter diraction

1. Introduction nation of strength and elongation of materials. Recently,


research on high-manganese (Mn) steels, which are consid-
Design for the automotive industry and for a range of ered a highly attractive material, has dramatically
structural applications aims to achieve an excellent combi- increased. The high strain-hardening rate of the alloys,
which varies with the Mn content, depends on the austenite
stability, and hence is controlled either by deformation-
Corresponding author at: Department of Materials Science and induced martensitic transformation (DIMT) of austenite
Engineering, Pohang University of Science and Technology (POSTECH), (c) into e-martensite and a-martensite or by mechanical
790-784 Pohang, Republic of Korea. Tel.: +82 54 279 2139 (C.G. Park).
twinning [116]. The former plasticity mechanism is termed
E-mail address: cgpark@postech.ac.kr (C.G. Park).

1359-6454/$36.00 Crown Copyright 2012 Published by Elsevier Ltd. on behalf of Acta Materialia Inc. All rights reserved.
http://dx.doi.org/10.1016/j.actamat.2012.09.078
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 559

transformation-induced plasticity (TRIP), and the latter The deformation behavior of high-Mn steels containing
twinning-driven plasticity (TWIP). Deformation bands considerable numbers of C atoms is complicated. Besides
associated with the accumulated motion of planar defects the SFE, the C content plays a substantial role in strain
may be formed due to the overlapping of stacking faults hardening. It was shown that for the FeMnC TWIP
on {1 1 1}c planes during deformation. Such bands can be steels, the work-hardening rate depended strongly on the
in the form of martensitic constituents, mechanical twins C content [27]. Recently, a TEM study of an FeMnC
or dense stacking fault bundles, depending on the stacking alloy revealed that C content can aect the dislocation
fault energy (SFE) and Mn content [1719]. structure dispersed inside the stacking faults of austenite
In binary FeMn alloy systems, the interpretation of phase [28]. Indeed, an atom probe tomography study of
deformation-induced phase transformation is based on Fe17Mn0.18C (wt.%) alloys demonstrated the segrega-
the two modes of austenite to martensite transformation, tion of C atoms at the crystal defects, such as stacking
which include hexagonal e-martensite and nearly cubic faults, c/e phase boundaries and c grain boundaries [29].
a-martensite. The e-martensite was discovered by Schmidt Although numerous reports describe the SFE and the char-
[20] in FeMn alloys in which the Mn content ranges from acterization of microstructural changes in fully austenitic
12 to 29 wt.%. In addition, Schumann [17] proposed that FeMn or FeMnC TWIP steels, very few studies have
FeMn alloys containing 1014 wt.% Mn had e-martensite identied the eects of C on the work-hardening rate and
and a-martensite at room temperature and Fe(1427)Mn the deformation-induced martensitic transformation of
steels exhibited e-martensite without a-martensite; in par- austenite/e-martensite dual-phase FeMnC steels [30].
ticular an Fe17Mn alloy had the maximum volume frac- Furthermore, an unambiguously detailed characterization
tion of thermally induced e-martensite on cooling. The of the eects of C on the microstructural evolution before,
DIMT is commonly found in austenitic steels with a low during and after the tensile deformation of dual-phase Fe
SFE [27]. The DIMT is related to the heterogeneous MnC alloys has not previously been reported [31].
nucleation of martensite embryos at new defect sites intro- The current study aims at identifying the eects of the C
duced by plastic strain, and the kinetics of the transforma- content on the microstructure, the DIMT and the
tion of c-austenite to a-martensite have been reported in work-hardening behavior in medium- or high-Mn steels
the previous studies [2,3,8,9]. According to these studies, consisting of c and pre-existing e (the so-called thermally
the strain- or deformation-induced a-martensite was corresponding displacive transformation products formed
formed at the intersection of two initial e-bands during on cooling). In this context, Fe17Mn alloys with C con-
tensile loading, and their growth was controlled by the tent ranging from 0.01 to 0.20 wt.% were investigated.
movement of the phase boundaries between c phase and For these alloys, the theoretically calculated SFEs exhibit
thermally introduced e. Therefore, the calculation of SFE a large variation in transitions that occur by TRIP and
is required for understanding the magnitude of dissocia- TWIP [2327]. Hence, the present study also aims to eluci-
tions into Shockley partials which lead to dislocation reac- date the type of displacive deformation behavior (deforma-
tions and the resultant work-hardening rate. Indeed, tion-induced transformation or mechanical twinning) that
several authors have predicted the SFE of high-Mn steels prevailed. In particular, we used stepwise tensile loading
as a function of Mn content. For instance, Lee et al. [21] tests in combination with electron backscatter diraction
used a regular solution model to describe the dierence (EBSD), which has been found to be suitable for the study
in the chemical Gibbs energy between the face-centered of TRIP steels [32]. By this approach, the deformation-
cubic (fcc) and hexagonal close-packed (hcp) phases. induced transformation sequence occurring at identical
Saeed-Akbari et al. [22] proposed a model based on the surface regions of the samples during deformation, prior
collection of thermodynamic parameters reported by dif- to fracture, can be monitored. To draw parallels with the
ferent authors [21,23]. Recently, Abbasi et al. [24] con- EBSD observations, the microstructural features within
ducted ab initio calculations on binary FeMn alloys. the bulk of the samples were characterized by X-ray dirac-
Nakano et al. [25] also evaluated the SFEs of FeMnC tion (XRD) and transmission electron microscopy (TEM).
ternary systems by proposing new thermodynamic descrip-
tions linking the experimental values of enthalpy and the 2. Experimental
thermodynamic equilibrium temperature (To). On the
other hand, the characteristic correlations between The Fe17Mn alloys were melted by means of a high-
mechanical properties and microstructural evolution in frequency vacuum induction furnace and cast into Cu
FeMn systems have been experimentally discussed as a molds. The chemical composition of the alloys used in this
function of Mn content [26]. From transmission electron study was analyzed by inductively coupled plasma mass
microscopy (TEM) studies of Fe22Mn0.6C (wt.%), spectroscopy and is listed in Table 1. The 15 mm diameter
Allain et al. [23] stated that the mechanical transformation cast ingot was reheated and homogenized in a protective
of c- to e-martensite or a-martensite (by TRIP) occurs Ar atmosphere at 1200 C for 24 h and hot-rolled to 75%
when the SFE is smaller than 18 mJ m2, whereas mechan- thickness reduction at 1050 C. A solution treatment was
ical twins were formed if the SFE was the range 12 performed in Ar atmosphere at 1150 C for 7 h, followed
35 mJ m2. by cooling to room temperature in air. The grain sizes of
560 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

Table 1
Chemical composition (wt.%) of the alloys used in the study and the
transformation temperatures. The temperatures of M fcc!hcp
s and Ashcp!fcc
were determined by dilatometry.
Samples C Mn Si + P Fe Ms (C) As (C)
0.01 C steel 0.012 17.0 0.008 balance 130 187
0.10 C steel 0.131 17.2 0.009 balance 80 160
0.20 C steel 0.185 16.8 0.012 balance 47 150

austenite were measured by the mean linear intercept. All


the samples exhibited a constant average grain size value
of 37.5 8.8 lm. The starting temperatures required for
the transformation from c phase to the thermally activated
e-martensitic phase M fcc!hcp
s and that for the reverse
transformation Ahcp!fcc
s were determined by dilatometry
with heating and cooling rates of 1, 25 and 50 K s1. In Fig. 1. Representative engineering stressstrain curves obtained from
total, 27 samples were tested for the dilatometry measure- stepwise tensile loading experiments. A curve obtained from the contin-
ments. The transformation temperatures are included in uous loading test is provided for comparison.
Table 1. In this context, we expressed the temperatures
for M fcc!hcp
s and Ahcp!fcc
s as the carbon content [C] increased During the interrupted loading experiments, the micro-
from 0 to 0.5 wt.% according to the following experimen- structural changes in the central gauge region of the
tally obtained empirical equations. deformed tensile samples were characterized by EBSD

M s C 133:7  744:5  C 1527:7  C
2
1 analysis at each level of strain. The EBSD scans were car-
 2
ried out at 10 kV. An area of 40  18 lm2 of the sample
As C 191:5  405:0  C 983:7  C 2 surface was detected with a step size of 50 nm. The raw
The correlation factors (R2) for Ms and As were 0.970 and data obtained in this study were processed using TSL-
0.990, respectively. The formulated equations for M fcc!hcp OIM software. A condence index (CI) value of 0.20 was
s
and Ahcp!fcc are consistent with the experimental data re- selected. Details of the EBSD data processing have been
s
ported by Kim et al. [33] and Koyama et al. [34]. An in- published elsewhere [15]. The volume fractions of the
crease in the C content leads to a reduction of Ms constituent phases before and after the tensile tests were
temperature due to the eect of the addition of C on the measured by XRD and EBSD. To prevent the deformation-
T0 between c and e phases [35]. With increasing C content, induced transformation during mechanical polishing, all
the decrease in Ms is greater when compared to that of As the specimens for XRD and EBSD measurements were
for the as-annealed alloys. This indicates that an increase in prepared using electropolishing and chemical etching
the C content leads to a decrease in the driving force for the (Lectropol-5, StruersTM) with a solution of acetic acid (90
transformation of c phase to thermally induced e-martens- vol.%) and perchloric acid (10 vol.%). The XRD experi-
ite on cooling [33]. ments were performed using Cu Ka radiation generated
Specimens of ASTM E8 standard for the continuous at 40 kV and 20 mA. Due to considerable peak overlaps
tensile tests were obtained from the quarter through-thick- between (0 0 0 2)e and (1 1 0)a at 44.5, (2 2 0)c and (1 1 
2 0)e
ness position of the hot-rolled sheets. All the samples used at 74.9, and (3 1 1)c and (1 1 2 2)e at 91.2, the fractions
for tensile tests were prepared along the rolling direction. of each phase can be either overestimated or underesti-
The samples for the stepwise tensile loading experiments mated. To overcome this, we used a Rietveld method in
were mechanically polished and subsequently electropo- combination with the General Structure Analysis System

lished in the central gauge region by Lectropol 5 (Stru- (GSAS ) software at a chi-squared value of 3.0. The aver-
ersTM) using a solution of acetic acid (90%) and age phase fractions were determined using ve or more
perchloric acid (10%) at 15 V and 5 C for 10 s. Next, XRD scan data sets for each sample. Moreover, the micro-
the electropolished samples were etched with an aqueous structure of the deformed specimens was examined by
K2S2O5 (1.2%) solution for microstructure characteriza- TEM using a JEOL 2010F microscope operated at
tion. Uniaxial interrupted and continuous tensile tests were 200 kV. Additional high-resolution TEM (HRTEM)
performed (Instron 5582 Tester) with a 100 kN load cell micrographs were acquired with a JEOL 2200FS micro-
operated at an initial strain rate of 104 s1 at room tem- scope equipped with an aberration corrector. The sample
perature. The data points were averaged with the values foils used for TEM were thinned by mechanical polishing
obtained from three tests. The representative stressstrain and subsequently by electropolishing with a double elec-
curves produced by the interrupted and continuous tensile tropolisher (Tenupol-5, StruersTM) at 0 C using an electro-
loading experiments for an Fe17Mn0.01C (wt.%) alloy lyte solution containing of CH3COOH (90 vol.%) and
are shown in Fig. 1. HClO4 (10 vol.%). For a thorough understanding of the
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 561

orientation dependence of deformation-induced martens- in the UTS. The changes in the 0.2% oset stress with
itic phases on the tensile loading direction, TEM samples increasing C content were not as prominent. Surprisingly,
were also prepared by focused ion beam (FIB, FEI Helios the uniform elongation signicantly decreased from 40%
Nano-LabTM). Subsequently, a low-energy ion milling sys- to 16% with increasing C concentration. It is important
tem (Linda IV8, GentleMillTM) at 0.5 kV and 4 of beam to note that serrations associated with dynamic strain aging
incidence was used to eliminate the surface penetration of (DSA) [36] were visible in steels containing 0.10 and 0.20
Ga+ ions during FIB milling. wt.% C at 23 C, as shown in Fig. 2a. Clear serrations were
identied at room temperature with increasing C content.
3. Results In addition, we observed that the value of critical strain
(ecritical) for the serrations decreased with increasing con-
3.1. Tensile properties tent of C. On the other hand, the work-hardening rates
(dr/de) were derived from the continuous true stressstrain
The tensile properties of the alloys used in the present curves shown in Fig. 2b. The work-hardening rate and
study are shown in Fig. 2. The mechanical properties vary deformation characteristics of the alloys depended on the
signicantly with the C content. The material with 0.01 amount of C added. All the specimens exhibited a steep
wt.% C showed an ultimate tensile strength (UTS) of decrease in the work-hardening rate below a true plastic
610 MPa, 0.2% oset stress of 380 MPa and an elongation strain of 0.08 due to an elasticplastic transition. Beyond
to fracture of 40%. When the C content increased up to the elasticplastic transition point, the work-hardening rate
0.10 wt.%, the UTS increased marginally to 710 MPa, of steels containing 0.01 wt.% C decreased linearly with
and C addition beyond 0.10 wt.% resulted in a decrease further strains, after which the plastic instability condition
was attained at a true strain of 0.35. Consequently, the Fe
17Mn0.01C (wt.%) sample showed a ductile fracture
behavior. The samples with 0.10 wt.% C showed a wide ser-
rated ow behavior above 0.11 until fracture. For the 0.20
wt.% C steels, the work-hardening rate at the onset of plas-
tic deformation below strains of 0.10 was higher than
shown by the steel samples containing 0.01 and 0.10
wt.% C, and reaches a level of about 2800 MPa. Subse-
quently, the work-hardening rate decreased steeply with
further increase in true strain. Premature fracture occurred
in the steels containing 0.10 and 0.20 wt.% C; thus, these
alloys were more brittle than the steel samples with 0.01
wt.% C. We hence conclude that controlling C content in
the FeMnC alloy system plays a signicant role in
strain-hardening at room temperature. Supposing that
the highest temperature (Md) for stress-induced e-martens-
itic transformation of all samples was 100 C [37], the
plastic deformation could be controlled mainly by defor-
mation-induced e-martensite rather than by slip
deformation.

3.2. Microstructure of the as-annealed samples before


deformation

The microstructure of the as-annealed samples contain-


ing dierent amounts of C was characterized by means of
EBSD and XRD. The EBSD maps revealed the absence
of anisotropic textures in the microstructure with variation
in the rolling direction (RD), as shown in Fig. S1 (Supple-
mentary information). These observations conrmed that
the as-annealed samples were composed of a mixture of
retained austenite (cR) and thermally induced e-martensite
on cooling. In this context, thermally induced e-martensite
Fig. 2. (a) Engineering stressstrain curves and (b) work-hardening rates
implies pre-existing e-martensite formed prior to deforma-
of steels with dierent amounts of C. The initial strain rate used was
104 s1 at room temperature. The blank rectangles, triangles and circles tion. We do not observe ferrite and a-martensite in the
represent the values observed in steels with 0.01, 0.10 and 0.20 wt.% C, nal microstructure. Moreoever, there were no carbides
respectively. in the as-annealed samples by TEM, either in diraction
562 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

Table 2 although strains increased around the point of fracture.


Volume fractions (absolute) (%) of the thermally induced e-martensite in This indicates that the deformation-induced a-martensite
the as-annealed samples determined by EBSD and XRD.
is formed from thermally induced einitial plates and not
Samples EBSD XRD from cR phase during the global tensile loading tests.
0.01 C steel 72.2 7.5 76.0 2.3 On the other hand, we conrmed that the nucleation of
0.10 C steel 43.5 6.5 52.0 1.7 a-martensite occurred at the einitial/einitial boundaries
0.20 C steel 35.7 4.8 40.1 2.0
(intersections of two e bands), where the nucleation sites
are known to exist [3,5,6,10,15,39]. Subsequently, the
mode (as appearance of extra spots) or in the imaging growth of a-martensite took place along the einitial bound-
mode at high magnications. The volume fractions of the aries, irrespective of the loading direction at an earlier stage
pre-existing e-martensite as a function of C content, as of deformation. Further a growth stopped at the c/einitial
determined by EBSD and XRD, are listed in Table 2. boundaries. With further straining, the thickness or width
The measured volume fraction of c phase increased with of a-martensite increased in parallel to the tensile direc-
decreasing pre-existing e fraction, as the C content tion. This implies that a-martensite exhibited a lm-type
increased. This trend was consistent with the results morphology in the earlier stage of deformation, which sub-
obtained from the dilatometry experiments given by empir- sequently attained a block-type morphology at later stages
ical Eqs. (1) and (2). These observations suggest that before of deformation due to an increase in width. Another
deformation, the transformation of austenite to thermally important point observed in this study was that the e/e
induced e-martensite on cooling is controlled by the boundaries were newly aligned inside a single einitial grain
amount of C added to these steels. at the strains between 7% and 12%, as marked by rectan-
gles in Fig. 3a. Upon further straining, the resultant phase
3.3. Evolution of martensitic grains present at the surface at this region was gradually indexed as a-martensite (red)
during deformation along the new boundaries.
Fig. 4 shows the EBSD phase maps monitored during
The microstructural changes in the steel with 0.01 wt.% stepwise loading tests carried out on the steels containing
C subjected to interrupted straining tests were monitored 0.10 wt.% C. The einitial to a transformation was primarily
by EBSD, as shown in Fig. 3. It should be noted that the present as a DIMT when compared with the transforma-
EBSD scan data were taken from identical regions of the tion of c to eD. Nonetheless, similar trends of the DIMT,
sample surface at each strain level. In the phase maps, a- such as the nucleation-growth procedure of eD and a,
martensite, e-martensite and metastable austenite (cR) the absence of cR- to a-martensite, the morphology of
phases are identied as red, yellow and blue regions, a, and the formation of new e/e boundaries aligned, were
respectively. The yellow region represents both thermally observed in the steel with 0.01 wt.% C as well. In particular,
introduced e-martensite on cooling (pre-existing e) and a local fraction with a poor CI value was observed within
newly formed e-martensite during deformation. For clarity, the einitial grains, which was attributed to the combined
it is necessary to dierentiate between the thermally intro- eects of high dislocation density and surface relief, as
duced e-martensite that pre-existed before deformation and marked by circles in Fig. 4a. Subsequently, the deforma-
the deformation-induced e-martensite, which are hence tion bands were indexed as the resultant a-martensite at
assigned as einitial and eD, respectively. Due to the poor higher strains. We used the tapping mode of atomic force
strength of the Kikuchi patterns, the phase or grain bound- microscopy (AFM) to reveal the plasticity mechanisms of
aries with highly concentrated stress driven by the this region. Fig. 4b shows the AFM image of the strained
employed straining could not be indexed with the software. specimens after EBSD observation. It can be seen that
Beyond plastic strains of 7%, the DIMT occurred in the the surface regions observed by EBSD and AFM were
two ways, which included the transformations of c to eD identical. From the height prole along the region of inter-
phase and that of the einitial to a-martensite. The eD plates est (indicated by the arrow shown in Fig. 4b), a-martensite
nucleated mainly at the phase boundaries between c and formed inside the einitial can be clearly attributed to a phase
einitial, and then grew in association with the movement transformation-induced stress relaxation. Consequently, a
of the c/einitial interface depending on the tensile loading phases inside an individual pre-existing einitial plate were
direction. This is consistent with the results observed by formed by plastic deformation. In addition, when the
Lee et al. [38]. The inverse pole gure (IPF) maps of e- strains increased from 12% to 20%, the density of deforma-
phase (as shown in Fig. 3b) revealed that when the eD tion bands increased, as indicated by rectangles in Fig. 4a.
plates grew, their orientation was aligned with that of the With further straining, the bands could not be clearly iden-
adjoining einitial grains. With further straining, the volume tied. This region could also be observed in the AFM
fraction of eD began to saturate when a eD plate collided image, which indicates that the deformation bands con-
either against a einitial phase with a dierent {1 1 1}c habit sisted of nely dispersed eD and several slip bands inside
plane or with the c/einitial phase boundaries. Beyond this einitial plate. In addition to conrming that the e-martensite
point, further transformation of eD to a ceased to occur, was intersected by parallel and multiple slip dislocations
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 563

Fig. 3. (a) EBSD phase maps and (b) the corresponding IPF maps taken from e-martensite in the steel sample containing 0.01 wt.% C during a stepwise
loading test prior to fracture. (RD: rolling direction, TD: transverse direction). The cyan circles in the maps represent the deformation-induced e-
martensite. Note that the images were acquired from identical regions. (For interpretation of the references to colour in this gure legend, the reader is
referred to the web version of this article.)

[40], the average interspacing between slip dislocations was ogy, two dierent types of c/einitial interfaces can be dier-
found to be about 1 lm (Fig. 4b). entiated depending on the einitial growth direction: the
The phase identication and IPF maps obtained from transverse interface perpendicular to the einitial growth
the EBSD scan of the steels containing 0.20 wt.% C during direction was denoted as interface A, whereas the longi-
the stepwise loading tests are displayed in Fig. 5a and b, tudinal interface, interface B, is parallel to its growth
respectively. As observed in the case of steels with 0.01 direction as shown in Fig. 5a. It has been reported that
wt.% C, during the growth of eD phases the orientation due to the higher elastic stress eld of interface A as com-
of a majority of the eD plates was maintained along that pared to that of interface B, the movement of interface A
of the pre-existing einitial grains. Given that the pre-existing was mainly responsible for the formation of deformation-
einitial grains typically exhibit an elongated plate morphol- induced eD phase during tensile loading [38]. However,
564 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

Fig. 4. (a) EBSD phase maps of the Fe17Mn0.10C (wt.%) alloy strained up to 20% during interrupted loading tests. (b) AFM image of the sample
surface after applying a strain of 20% and (c) its height prole along the arrows. The phase map and AFM image were taken from identical regions of the
deformed sample.

we revealed that irrespective of the dierent stress elds of at the einitial/einitial boundary and underwent growth (as
the two interfaces, the movement of either interface A or shown in the regions enclosed by rectangles in Fig. 5b).
interface B was controlled by the tensile direction during Interestingly, the orientation of the indexed e plates inside
deformation (see Fig. 5a). This could be due to the fact that the new boundaries was dierent from that of the adjoining
all the c/einitial interfaces in the as-annealed steels are high- pre-existing einitial grains. With further straining, the
angle grain boundaries of 1590. This indicates that when boundaries could not be indexed as a-martensite. The
the e-martensite was newly formed by deformation, the dis- gray-colored boundary map in combination with the IPF
location motion at the c/einitial interface was governed by a map given by Fig. 5b conrmed the formation of hcp ten-
critical resolved shear stress (CRSS), which is determined sile {1 0 1 2} twin boundaries. Hence, the absence of phase
by geometrical considerations, including the tensile axis. transformations from einitial to a-martensite in this region
Additionally, we found that the new boundaries nucleated could be due to the presence of deformation-induced hcp
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 565

Fig. 5. (a) EBSD phase maps of the steel sample containing 0.20 wt.% C during stepwise loading tests and (b) the corresponding IPF maps acquired from
e-martensite. The circles and rectangles in the maps represent the deformation-induced e-martensite and the hcp tensile twins formed at the intersection of
the deformation bands, respectively. The boundary map reveals the characteristics of the hcp twin plane.

twins at the intersection of two einitial plates. The {1 0 1 2} 14Mn9Cr5Ni alloy [41] and in an Fe17Mn0.3C steel
hcp twins have also been detected at the intersection of [37]. This means that the formation of hcp twins at the
two einitial plates upon tensile deformation in an Fe intersection of einitial phases can retard the transformation
566 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

of einitial to a-martensite for the steels containing 0.20 wt.% tensite, corresponding to the combined fractions of pre-
C. On the other hand, we observed that the IPF map mon- existing e and the newly formed eD, increased from
itored beyond 12% straining presented a local distribution 58.0 3.2 vol.% in steels with 0.01 wt.% C to 68.7 2.8
of the high-stress concentrated regions with a poor CI vol.% in steels with 0.20 wt.% C. These results concurred
value. In this case, in comparison to the block-type a- with the results obtained from the EBSD studies shown
laths, the c/einitial and eD/eD boundaries were the regions in Figs. 35. However, the trend was reverse for the as-
at which higher levels of stress were concentrated at the annealed steels. As mentioned earlier, the transformation
later stages of deformation. This indicates that the fracture of c to thermally introduced einitial on cooling was retarded
behavior of the alloys with 0.20 wt.% C could be controlled by higher C content (Table 2). Therefore, we suggest that
by the einitial boundary area rather than by the blocky-type the eect of C content on deformation induced e-martensite
a. These observations suggest that the fractions of c/einitial diers from that of thermally induced transformation eini-
and eD/eD boundaries are the origins of intergranular frac- tial. When the e-martensite (einitial) is formed from c phase
ture for the present steels, in good agreement with the below Ms temperature as a result of elastic strain energy
results of Koyama et al. [37]. We hence conclude that on cooling, all the partials of 1=62 1 1, 1=61 2 
1 and
block-type a phase plays no substantial role in the brittle 1=61 1 2 on the {1 1 1}c planes are responsible for the
fracture of the dual-phase high-Mn steels containing con- fcchcp transformation, whereas preferred slip direction
siderable amounts of C. This can be attributed to the exists and hence is favorable for plastic deformation-
higher prevalence of slip systems in the cubic a phase induced transformation [38,42]. This will be discussed later.
rather than in fcc and hcp crystals [26].
3.5. Morphology of the deformed samples observed by TEM
3.4. Volume fractions of deformation-induced martensitic
phases inside the bulk of the samples A TEM micrograph of the steel with 0.01 wt.% C after
plastic straining to 37% and the corresponding selected-
XRD results of the steels containing 0.01, 0.10 and 0.20 area diraction patterns (SADPs) of [0 1 1]c and [1 1 1]a
wt.% C after nal fracture are presented in Fig. S2 (Supple- zone axes are presented in Fig. 6. Extensive stacking faults
mentary information). It can be seen that all the peaks were are displayed inside one einitial bundle (denoted as eA) and
clearly resolved. From a more general point of view, the their direction was parallel to the growth direction of einitial.
detected body-centered cubic (bcc) peaks correspond to Typically, the faulted morphology of the einitial plate has
deformation-induced a-martensite. The volume fractions been attributed to high internal stresses driven by quench-
(Vf) of constituent phases after deformation were calcu- ing [43]. a-martensite was observed to grow inside an indi-
lated from the XRD results by applying the Rietveld vidual eA grain. Given that a-martensite is transformed
method. The fractional changes in the corresponding from thermally induced einitial as shown in Figs. 35, eA
phases before and after deformation are shown in and eB are thermally induced einitial plates formed on cool-
Fig. S3. The dierence in the fraction of each phase before ing before deformation. The orientation relations observed,
and after deformation can be quantied in terms of a as shown in Fig. 6b and c, were (1 1 1)c//(0 0 0 1)e//(1 1 0)a
DV = Vf (vol.% in deformed sample)  Vi (vol.% in as- and h1 1 0ic//h1 1 2 0ie//h1 1 1ia or h1 1 2ic//h1 1 0 0ie//h1 1 0ia.
annealed sample). The Vf and DV values for the steels are The orientation relation between c and e corresponded to
listed in Table 3. The DIMT kinetics depended signicantly the ShojiNishiyama (S-N) type [44,45] and the relation-
on the C content for both c ! eD and pre-existing einitial - ship between c and a was characterized as Kurdjumov
! a. Higher C content leads to a decrease in the fraction Sachs (K-S) or NishiyamaWassermann (N-W) types
of deformed-induced a, while accelerating the transforma- [46,47]. The habit plane between c and einitial belonged to
tion of c to eD. In other words, steels with high C content the {1 1 1}c type and the formation of deformation-induced
showed a strong tendency for the transformation of c to a depended on both relationships. That is, the presence of
deformation-induced eD, while the transformation of pre- the {0 1 1}a plane parallel to both the {1 1 1}c and {0 0 0 2}e
existing e to a-phase was prevalent in the Fe17Mn planes was found to be energetically favorable for the for-
0.01C alloys. Indeed, the total volume fraction of e-mar- mation of a-martensite, which is in good agreement with
the reports on 304 stainless steels [48]. The SADP along
the [1 1 1]a zone axis (shown in Fig. 6c), which showed
Table 3 diraction spots only from hcp-eA and body-centered
Volume fractions (Vf) of each phase after deformation and the dierence tetragonal (bct)-a, demonstrated that the a was newly
(DV) between the fractions before and after deformation. The Vf and DV
transformed from a single pre-existing eA. In other words,
indicate absolute (%) values, which were determined by XRD.
deformation-induced a-martensite can occur at a single
Samples austenite e-martensite a-martensite
einitial plate as well as at the intersection of two einitial bands.
Vf |DV| Vf |DV| |DV| We referred to a-martensite which emerged at one einitial
0.01 C steel 16.9 7.1 58.0 18.0 25.1 phase as a-martensite formed at the nonintersecting
0.10 C steel 34.0 14.0 48.5 3.5 17.5 parts of two einitial bands. As observed in Fig. 4, the growth
0.20 C steel 18.5 41.0 68.7 30.6 12.8
of a within a single einitial plate was induced by a stress
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 567

Fig. 6. (a) TEM micrograph of the Fe17Mn0.01C (wt.%) alloy after being strained to 37% and the corresponding SADPs taken from (b) two e-
martensite plates and (c) a-martensite. The corresponding schematic illustrations are also displayed. The pink, yellow, green and purple circles indicate the
diraction spots for austenite, eA, eB and a-martensite, respectively. (For interpretation of the references to colour in this gure legend, the reader is
referred to the web version of this article.)

concentration, resulting from the slip dislocations piled up einitial grains. The mechanism of the a formed at noninter-
at the new e/e interface. Recently, Koyama et al. [37] secting einitial plates will be discussed in the following
showed that a-martensite was not observed at intersec- section.
tions of einitial bands, but rather at nonintersecting einitial Fig. 7 shows dark-eld TEM images of the deformed
bands. Hence, we conclude that the new nucleation site sample containing 0.10 wt.% C and the corresponding
for a-martensite is a single pre-existing e-plate and hence SADP along the [1 1 3]a//[1 2 1 3]e zone axis. In the SADP,
grows while maintaining the S-N relation with the abutting the diraction spots corresponding to hcp-e and bct-a
568 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

Fig. 7. Dark-eld TEM images of the steels containing 0.10 wt.% C after being strained to 20% was obtained from the (1 1 0) reection for a-martensite
and (b) was acquired from the 1 1 0 1 spot of e-martensite. (c) SADP of a [1 1 3]a zone axis; (d) represents the corresponding schematic illustration. The
purple and yellow circles represent the diraction spots for a-martensite and e-martensite, respectively. The growth direction of a-martensite was due to a
stress relaxation mechanism. (For interpretation of the references to colour in this gure legend, the reader is referred to the web version of this article.)

were detected. The images taken from (1 1 0)a reections varied from 1 to 8 nm and the twin boundary spacing
and (1  1 0 1)e reections revealed that the growth direction was within the range 550 nm. The twins originated the
of blocky-type a depended on achieving distinct orienta- formation and development as n-layer twins of intrinsic
tion relationships of ( 1 2 1)a//(1 0 
1 0)e and [
1 1 3]a// stacking faults on every {1 1 1}c plane of the close-packed
[1 
2 1 3]e with the einitial. From the SADP and the fcc lattice, as shown in Fig. 8b. In particular, an intrinsic
corresponding schematic illustration, the formation of SF serves as the nucleus of the mechanical twins because
a-martensite inside a single einitial grain at the two nonin- the energy associated with an intrinsic SF is about 1.5 times
tersecting einitial plates was unambiguously attributed to a lower than that of an extrinsic SF [49,50]. While the defor-
stress-relaxation mechanism. This agrees with the results mation twinning was also detected in steel samples with
obtained from a joint EBSD and AFM analysis, as shown 0.20 wt.% C, mechanical twinning was absent in steels with
in Fig. 4. 0.01 wt.% C. Hence, the deformation mode of the presently
Additional characterization by HRTEM (the results of discussed FeMnC alloys was determined by the amount
which are shown in Fig. 8) revealed the occurrence of extre- of C addition, which contributed to an embryo of either
mely thin deformation twins (referred to as nanotwinned hcp stacking or a twin. Therefore, the eD-martensite
bundles) inside the c phase for steels with 0.10 wt.% C. appears only when the Fe17Mn steel contains 0.01 wt.%
In the SADP acquired along the [0 1 1]c zone axis, the dif- C, while mechanical twins can be locally formed in addition
fraction spots corresponding to the c and to the twins were to eD-martensite for the steels containing 0.10 and 0.20
detected and further spots that were neither e plates nor wt.% C.
a-martensite were present. The nanotwinned bundles were TEM images obtained from the deformed steels contain-
of the order of several micrometers in diameter, with ing 0.20 wt.% C and the corresponding SADP acquired
lengths of a few micrometers. This was attributed to the along the [0 0 1]a zone axis are shown in Fig. 9. As men-
intersecting of the parallel slip bands, as indicated by the tioned earlier, the microstructure of the deformed steel
arrows in Fig. 8a. An inverse fast Fourier transform samples containing high C content was mainly governed
(IFFT) study revealed that the thickness of the twin layer by the transformation of c to eD. The blocky-type a laths
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 569

Fig. 8. (a) Dark-eld TEM images of the steels containing 0.10 wt.% C after being strained to 20% and its inverse fast Fourier transform image showing
the formation of nanotwinned bundles. The diraction spots originating from the twins are indicated by arrows. (b) Schematic illustration of the
mechanical twin formation associated with the intrinsic stacking faults in austenite.

Fig. 9. TEM micrographs of the blocky type a-martensite at later stages of deformation, acquired in (a) bright-eld and (b) dark-eld, which was
obtained from the (1 1 0)a reection.

were clearly present in the later stages of deformation. strain-induced precipitates were formed inside the blocky-
Based on the results obtained from EBSD (shown in type a, which is the deformation-induced product phase
Figs. 35), the shape of a was attributed to an increase of the pre-existing einitial. The particles were nely dispersed
in width, depending on the tensile direction. Additionally, depending on the specic orientation relationships with the
many variants of the deformation-driven cementite, includ- tensile direction. The following transformation sequence
ing orthorhombic (Fe,Mn)3C or Fe3C, were observed in the can be inferred from the results.thermally activated pre-
deformed FeMn0.20%C alloy. Fig. 10 shows the TEM existing einitial ! deformation-induced a ! a + strain-
and HRTEM images of the cementite particles. The induced cementite
570 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

Fig. 10. (a) Typical TEM and HRTEM images of steels containing 0.20 wt.% C after being strained to 12% along with the SADP and NBD pattern
acquired along the [0 1 1]a zone axis showing the precipitation of strain-induced cementite inside a-martensite. The purple and green circles represent the
diraction spots from a-martensite and cementite, respectively. (b) Inverse fast Fourier transform image taken from a/cementite interface and the
corresponding atomic height prole along the arrow. (For interpretation of the references to colour in this gure legend, the reader is referred to the web
version of this article.)
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 571

The average size of the strain-induced cementite was esti- untransformed c, respectively; x denotes the applied engi-
mated as 130 20 nm in length and 16 5 nm in width, neering strain and A is a tting parameter. Hence, A repre-
indicating a remarkably anisotropic shape. This is thought sents the kinetics of the transformation of cR to eD during
to be due to the rapid pace of the nucleation process for car- deformation, and the equation suggests that a higher A
bide precipitation during deformation at room tempera- value corresponds to an increase in the rate of transforma-
ture, whereas their growth rates are relatively sluggish. tion of c to eD [53].
The SADP and nanobeam diraction (NBD) pattern We used the empirical equation to describe the eect of
acquired along the [0 1 1]a zone axis shown in Fig. 10a stepwise straining on the c fractions. The c fractions at the
revealed the occurrence of ( 211)a//(1 0 0)cem and [0 1 1]a// employed strain level were determined by EBSD, and the
[0 0 1]cem as the predominant orientation relationship, which calculated relative kinetics of the transformation of cR
corresponds to the Bagaryatski relationship between a- for all the alloys is listed in Table 4. The A values of the
martensite and cementite. From the diraction spots of steels varied signicantly with the amount of C addition.
a-matrix and cementite, the planar spacing of the (2 1 1)a Fig. 11 presents the calculated kinetics and the correspond-
planes was found to be almost three times that of the ing curve ts. It is important to note that the kinetics of the
(1 0 0)h planes. The growth of the nanometer-sized cement- transformation of cR to eD for steels with 0.10 wt.% C
ite occurred along the h0 1 1ia or h1 1 1ia direction to reduce began to saturate at a true strain of about 0.18, as shown
mist strains. Considering the orientation relationship, an in Fig. 2b and Fig. 11. This implies that the strain-harden-
IFFT technique conrmed that the lattice parameter of ing behavior at low strain levels was mainly controlled by
the particles with orthorhombic crystal structure was about the c to e transformation rather than by the transformation
0.459 nm, as shown in Fig. 10b. In general, various transi- of pre-existing einitial to a or by the dislocation substruc-
tion metal carbides, such as hexagonal-e, orthorhombic-g ture evolution.
M2C, orthorhombic M7C3, fcc M6C, and fcc M23C6, are Matsumura et al. [54] proposed that an increase in the
widely known to precipitate readily in the early stages of applied engineering strain (e) leads to a reduction in the rel-
tempering or quenching (the so-called autotempering) of ative fractions of cR (FcR). This reduction was reported to
austenitic high-Mn or stainless steels [41,51,52]. However, follow an inverse relationship (shown below) and the tting
as mentioned previously, the formation of cementite or parameters A and B were obtained by the least-squares
metal carbides could not be observed in the as-annealed method:
samples before deformation, either during TEM analysis
F cR A  e B1=2 : 3
in the diraction mode or in the imaging mode at high mag-
nications of TEM. Hence, the autotempering eect cannot The values of A and B were determined by EBSD to be
account for the formation mechanism of strain-induced 0.1870 and 0.9522 for steel with 0.01 wt.% C and as 0.2959
cementite observed here. The detailed mechanism of this and 0.9204, respectively, for steels containing 0.20 wt.% C.
cementite precipitation will be discussed later. According to the calculations, a remarkable decrease in the
kinetics of the transformation of cR to eD-martensite was
4. Discussion observed with an increase in the amount of C. However,
the cR fractions measured by EBSD could not be directly
4.1. Transformation kinetics of retained austenite compared with those of the bulk specimens due to the
limited area subjected to the EBSD analysis. In recent
The deformation-induced martensitic transformation in
the alloys considered in this study can be identied from
the kinetics of the transformation of cR to eD whilst being
subjected to interrupted tensile loading tests. Thus, the
kinetics can be quantied in terms of an empirical equa-
tion, y = 1  eAx, as suggested by Shi et al. [53]. The y rep-
resents DV/V = (V0  V)V0 = 1  V/V0, where the V0 and
V indicate the volume fractions of the initial c and the

Table 4
Calculated empirical equations for the kinetics of the transformation from
austenite to deformation-induced e-martensite. The volume fraction of
austenite was determined by EBSD. A higher A value corresponds to an
increase in the rate of the kinetics.
Samples Fitting function A R2 (correlation)
Fig. 11. Calculated kinetics of the transformation from austenite to e-
0.01 C steel y = 1  exp(0.05) 0.05 0.91
martensite as a function of applied engineering strain. The triangles,
0.10 C steel y = 1  exp(0.71) 0.71 0.95
rectangles, and circles represent steels with 0.01, 0.10 and 0.20 wt.% C,
0.20 C steel y = 1  exp(0.92) 0.92 0.92
respectively.
572 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

XRD and EBSD analyses carried out on an FeMnSiC c ! eD ! a martensite. As previously considered in
TRIP steel [32], the relative trend of the cR fraction austenitic or duplex stainless steels, the intersections of
obtained from EBSD showed a more marked decrease two e bands or the crossover of e bands with the grain
compared to the XRD results. It was suggested that the dif- boundaries and regions in proximity to these have been
ferences in the transformation behavior could be due to the known to function as nucleation sites for a-martensite
spatial freedom of the austenite grains at the surface, tak- [16,55,56]. However, the presently studied alloys followed
ing into account the depth resolutions of the XRD and the global kinetic path involving c ! eD and thermally
EBSD measurements [14,32]. Hence, we used the afore- induced einitial ! a transformations. From the results of
mentioned equations to identify the relative trends in the the EBSD analysis shown in Figs. 35, it was conrmed
transformation kinetics of austenite, instead of obtaining that the einitial acted as a precursor to the deformation
absolute quantitative values. The relative trends obtained induced a transformation. Hence, the einitial volume frac-
in combination with the results of EBSD analysis are con- tion in the as-annealed samples played an important role
sistent with the XRD data, as shown in Table 3 and in determining the fraction of the newly formed a during
Fig. S2. Therefore, the deformation-induced transforma- deformation. Furthermore, the formation of new boundary
tion of c to e was better promoted in the alloys containing arrays within the einitial plates assisted in the nucleation of
a higher C content, which delayed the transformation of e deformation-induced a, as shown in Figs. 3 and 4, which
to a. Therefore, it is the amount of C that determines the was also conrmed by the TEM studies shown by Figs. 6
DIMT in high Mn-containing steels. and 7. Therefore, we propose that the new phase bound-
aries formed within einitial plates during tensile deformation
4.2. Transformation behavior of deformation induced e- acts as additional nucleation sites for a-martensite. There
martensite and a-martensite are two possible explanations for such a transformations,
as mentioned below. (i) As the previous section shows, the
The sequence of deformation-induced transformation transformation could be induced by a stress concentration
observed in this context did not follow the kinetic path: resulting from the slip dislocations piled at the newly

Fig. 12. TEM images of the undeformed samples showing the high density of dislocation bundles dispersed inside the e-martensite zones. (a) Bright-eld
image and the corresponding dark-eld image acquired from the (1 0 1 0)e reection of the SADP along the 2 4 2 3e zone axis. (b) Dark-eld image taken
from the (0 0 0 1)e reection of the SADP along the [0 0 1]c zone axis. (c) The motion of the partial dislocations piled at the e interface.
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 573

formed e/e interface. Typically, the formation of a-mar-


tensite is facilitated by the interaction of various deforma-
tion bands with the e-martensite zones [3]. (ii) Upon
deformation, the local recombination of the thermally acti-
vated mobile dislocations inside the einitial phase could also
induce these transformations, i.e. the interaction of the pre-
existing dislocations dispersed inside the einitial zones may
promote the nucleation of a-martensite. Fig. 12 shows
the representative TEM images of the dislocation motion
in the undeformed samples. Indeed, the dark-eld images
acquired under the two-beam diraction conditions con-
rmed that before deformation, the highly dense disloca-
tion bundles were distributed selectively in the einitial
zones. Fig. 12c distinctly displays the continuous piling
Fig. 13. The variation of the thickness of pre-existing e-plates in the
up of partials in the einitial plate at the e interface, until undeformed samples as a function of C content, as determined by EBSD
the shear packet was suciently thick to nucleate a. It and TEM. For comparison, the volume fraction of the e-phase in the as-
has been suggested that the dislocation motion of einitial annealed steels is provided. The blank rectangles and circles represent the
plates can aect the strain-hardening rate [57]. Details with average width and volume fraction of the pre-existing e plates,
respectively.
regard to the origin of the dislocations are described exten-
sively elsewhere [28]. Therefore, with the driving force for
the interactions between partial dislocations being lower C redistribution [14]. (ii) This could be due to an initial
than that for the transformation of eD to a, it is plausible microstructure of the pre-existing einitial at room tempera-
that the kinetic path of the transformations in the steels ture, namely an increased grain size of retained c (cR)
studied here follows c ! eD and einitial ! a. phase by the microstructural renement of einitial plates
before deformation. Larger cR grains were transformed
4.3. Eect of carbon content on the deformation-induced more easily during tensile loading, compared to smaller
transformation, microstructure and mechanical properties cR grains that were found to be mechanically better stable
[14]. Indeed, an increase in C content resulted in the pro-
The DIMT behavior in the deformed samples at dier- duction of ner einitial phases in the as-annealed steels, as
ent strains was monitored by XRD and EBSD analyses shown in Figs. 13 and S1. The average thickness or width
and the corresponding results were found to concur. We of the pre-existing einitial was determined by EBSD and
also observed that the C content is a parameter controlling TEM. The ner morphology of pre-existing einitial could
the work-hardening rate. It is known that when the amount be attributed to an increase in the C content, which segre-
of added C increases, the c phase is better stabilized and gated at prior c grain boundaries. A higher C content at
hence its shear strength is improved due to solid-solution grain boundaries that acted as nucleation sites for the
strengthening eects [14]. However, a stepwise tensile test pre-existing einitial can interrupt the movement of 1/
combined with the EBSD analysis considered here reveals 6h1 1 2i partials that were nuclei for the pre-existing einitial.
that with increasing carbon content, the transformation Accordingly, the microstructural renement of einitial plates
kinetics of c phase to deformation-stimulated e-martensite leads to a gradual increase in the cR grain size, and
became faster, while that of pre-existing e- martensite to a- mechanical stabilization of c phase deteriorated with defor-
martensite was sluggish. From a general thermodynamic mation (the so-called constraining eect). In other
point of view, this observation seems controversial. The words, the integral transformation of cR phase into eD
trend observed in our study, which is opposite to the usu- occurring during global tensile tests is controlled mainly
ally observed tendencies, can be explained as follows. (i) by the mechanical stabilization of c phase. We propose that
This could be due to the distribution of C being inhomoge- the c phase in Fe17Mn0.20C steels is transformed more
neous in the as-annealed samples. Indeed, Petrov et al. [58] easily compared to smaller cR grains in Fe17Mn0.01C
showed the presence of C enrichments at c grain bound- alloys, and hence the steel containing high C content exhib-
aries and the stacking faults inside c phase for an austenitic its an accelerated transformation of c to eD during defor-
Fe22%Mn alloy. Recently, for the Fe17Mn0.2C alloys mation. Moreover, as previously mentioned, the e/e
(wt.%), we revealed the segregation of C to the crystal boundary fractions associated with ner einitial plates may
defects by means of atom probe tomography (APT) [29]. play an important role in the formation of deformation-
This means that the redistribution of interstitial solute C induced a. Hence, we also suggest that the ner einitial
atoms at either c/einitial interfaces or grain boundaries can plates could act as formidable obstacles to plastic ow,
lead to a depleted C content in the c grain interiors as com- showing extremely steep work-hardening behavior.
pared to the usually assumed nominal compositions. Con- Another possible obstacle to a formation are deforma-
sequently, the associated solid-solution strengthening tion-induced {1 0 1 2} hcp twins at the intersection of two
eects contributing to the strength can be deteriorated by einitial plates, as shown in Fig. 5b.
574 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

An increase in the C content leads to an accelerated reported [27], the friction stress r0 in high-Mn steels, which
transformation of pre-existing e to a with suppressing depends on the C and Mn content, is mathematically ex-
transformation of c phase to eD, resulting in a deteriorated pressed by the following equation:
elongation and an improved ultimate tensile strength
r0 MPa 228 187wt:%C  2wt:%Mn 5
(UTS). Bearing in mind the evolution of the mechanical
properties, the corresponding plasticity mechanism was The tted values of r0 and jy were 200 MPa and
not observable in the alloys considered in the present study. 1.3 GPa lm1/2, respectively, for the alloy containing 0.01
This indicates that even though the deformation-induced wt.% C, and 227 MPa and 1.2 GPa lm1/2 for the samples
transformation of c- to e-martensite occurred in the present with 0.20 wt.% C. This indicates that YS is independent
FeMnC alloys, the resulting TRIP eect was insucient. of the C content of these alloys. Moreover, the prior c
There are two possible explanations for this. (i) This could grain size of 37.5 8.8 lm was also found to be invariant
be due to a low C content in the steels studied here. It with C content. Hence, the changes in YS are not likely
seems that there is a critical value of C content that is to be prominently observed with increasing C content
required to achieve plasticity. This trend has also been below 0.20 wt.%.
reported in the FeNiC system [7], and it was shown that Meanwhile, we observed the deformation-driven forma-
when the amount of C addition was below 0.3 wt.%, strain- tion of cementite inside a-martensite during the tensile
induced martensitic transformation was absent. Above this deformation at room temperature, as shown in Fig. 10.
critical value, the alloys showed higher UTS due to the Previous theoretical studies using DICTRA [62] and
occurrence of an ecient TRIP eect. Indeed, it was mixed-mode [63,64] simulations have reported an improve-
reported that this triggering eect associated with C addi- ment in the mobility (by a factor of 45) of all alloying ele-
tion could support the idea of the existence of a critical ments in a-martensite when compared to that in ferrite
resolved shear stress for twinning or for martensitic trans- [65]. The activation energy for cementite precipitation
formations [5961]. (ii) This could be owing to the presence inside a-martensite is low (7.7 kJ mol1). As mentioned
of a-martensite with a low density of dislocations. Typi- above, a-martensite formed from einitial phase contains a
cally, the TRIP eect exploits the deformation-stimulated low density of mist dislocations in the Fe17Mn0.20C
transformation of metastable retained c-martensite to hard steels. Hence, the dislocation density introduced through
a-martensite and the resulting plasticity required to the transformation of einitial to a is insucient to explain
accommodate the transformation mist [15]. Accordingly, such an enhanced C diusion in a-martensite. As has been
the a-martensite shown in conventional low-C bearing suggested by Raabe et al. [66,67], pipe diusion could be
TRIP and duplex stainless steels cannot be identied as a one reason for the enhanced C diusion in martensite.
separate phase when using EBSD because of the extremely We speculate that the mechanism of cementite formation
low image quality factors below 0.05 [11,32]. This is associ- is due to the pipe diusion of C, associated with the defor-
ated with a high density of dislocations induced by the lat- mation-activated local heating occurring within the central
tice distortion [11]. However, the deformation-induced a gauge region of the tensile samples. This local heating leads
observed in our study was clearly detected to be close to to strong kinetic deviations from the material behavior
the ferrite lattice, with a CI value > 0.5 (Figs. 35). This observed at room temperature, which could be expected
indicates that the transformation of a in the case of the to be the nominal temperature at which a global test takes
steels employed in the present study diers from that in place [68]. Local heating during tensile loading is plausible,
TRIP steels or duplex stainless steels. In other words, the as many thermally activated processes, such as dislocation
transformation of einitial to a can lead to a low density of motion, interface motion, nucleation and strain hardening
dislocations due to their simple displacive mechanism, depend exponentially on the temperature [69]. Further
which was characterized by TEM (Fig. 10a). As a result, analysis combined with digital image correlation (DIC)
the Fe17Mn0.01C steel, in which the transformation of revealed that the strain rate of the central gauge region
einitial to a was prevalent, shows a ductile fracture behavior of samples was 35 times higher than a global initial strain
when compared to samples containing higher concentra- rate of 104 s1. This is due to the localized nature of
tions of C, as shown in Fig. 2b. It seems that the transfor- deformation. This indicates that the local heating at the
mation of einitial to a can soften the steels. We therefore central gauge region of tensile samples can be attributed
conclude that the deformation-induced transformation of to the strain rate localization. It is plausible that the local
einitial to a is benecial to the elongation, while the trans- dissipative heating at the center of tensile samples exerted
formation of c to eD leads to an increase in the strength. a remarkable acceleration eect on the kinetics of carbide
To evaluate the yield strength (YS), the standard Hall precipitation inside a-martensite. Therefore, we propose
Petch-type relation is considered. that for a dual-phase Fe17Mn0.2C alloy, the cementite
can be formed inside deformation-induced a-martensite,
YS r0 jy  d 1=2 ; 4
although the tensile test here was performed at room tem-
where r0 is the lattice friction stress, jy is the strengthening perature. As a result, the deformation-driven cementite
coecient, and d is the prior c grain size. As previously precipitation can improve the strength, and hence is an
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 575

additional factor responsible for reducing the ductility of be reoriented C atoms driven by stress elds at the core
the steel samples containing 0.20 wt.% C. of dislocations, as suggested by Dastur and Leslie [80].
As mentioned in Fig. 2a, a clear dependence of the ser- However, we do not observe any enrichment of Mn atoms.
rated ow on C content, which was associated with DSA, More detailed experiments and discussion will be presented
was observed in the stressstrain curves of the current elsewhere [81]. Even though direct TEM observations of
FeMnC alloys at room temperature. Additionally, we the atom probe samples are required [82], the APT results
found the presence of serrations in the stressstrain curves show the C content at the enriched regions, thus enabling
operated with an initial strain rate of 104 s1 at 430 K us to give a strong hint as to the origin of serrations in
below Ahcp!fcc
s temperature. The volume fractions of e the present steels. Among the dierent mechanisms of ser-
and a phases at 430 K are the same as those of martensitic rations, we hence propose that the origin of the modied
phases at 293 K, since no phase transformation occurs in type A serrations observed here is thought to be attributed
the steels during tensile tests at 430 K. A signicant point to a strong interaction between the dislocations and the
is that the diusivity of C atoms is accelerated at 430 K, redistribution of C, especially Cvacancy pairs. Cuddy
as compared to at 293 K. We therefore conclude that the et al. [83] proposed empirical equations available for esti-
martensitic transformation occurring during deformation mating activation energy (Q) for the pipe diusion of C
plays no substantial role in serrations. In this study, the atoms as given below.
propagation of a PortevinLe Chatelier (PLC) band, which
e_ Aemb
c eQ=RT ; 6
resulted from a microscopic DSA process, was detected by
means of a DIC method available for detecting PLC bands where e_ is the strain rate, ec is the critical strain of serra-
in tensile samples. We estimated that the PLC bands were tions, m and b are constants related to the vacancy concen-
inclined at an angle of 40 to the tensile axis for the Fe tration and mobile dislocation density, respectively, A is a
17Mn0.2C (wt.%) alloy. This value was constant during constant, R is the gas constant, and T is the absolute tem-
the global tensile tests. Based on these observations, we perature. Using the enhanced diusion coecient due to
believe that the serrations observed in the stressstrain vacancies forming during plastic ow [84], we calculated
curves of the 0.10C and 0.20C samples belong to be mod- the activation energy (Q) for the pipe diusion of C. The
ied type A [13,70]. Extensive studies have reported the experimentally calculated Q for type A serrations in
role of DSA on the strain-hardening rate of high-Mn steels the steels considered in this context is 37.1 kJ mol1,
and stainless steels [7077], focusing specically on the which is close to the reported Q of 4080 kJ mol1 [83].
presence of serrated ow. According to the van den Beukel This estimated value is higher than the activation energy
model [78], mobile dislocations are locally arrested and for deformation-induced cementite precipitation
their movement is blocked during deformation by means (7.7 kJ mol1), as mentioned earlier. It may also be inter-
of solute clusters that were driven by the bulk diusion. esting to investigate the eects of deformation-driven
Next, further straining causes atomistic jumps of solute cementite particles on the serrated ow in the high-Mn
atoms from the dislocations. Mulford and Kocks [79] also steels. Overall, given that the dependency of mechanical
suggested a new DSA model in which the enhanced diu- properties on C content (Fig. 2), we expect that an en-
sion of solute atoms to dislocations was attributed to pipe hanced DSA due to higher C content might be one factor
diusion. Dastur and Leslie [80] argued that the formation contributing to strain hardening.
of dynamic MnC solute clustering with the strain eld of
dislocations might be one reason for the room-temperature 4.4. Stacking fault energy and deformation mode
serrations in the stressstrain curves of FeMnC-based
Hadeld steels. Recently, Saeed-Akbari et al. [22] stated As mentioned earlier, mechanical twins of austenite
the eects of short-range ordering (SRO) on the strain were locally formed in addition to eD-martensite in steels
hardening of high-Mn steels. These authors proposed that containing 0.10 and 0.20 wt.% C, conrming that the
a strain-hardening parameter contributed to the SRO SFE depends on the C content. Remy suggested that in
strengthening mechanism. In order to identify the origin Fe20Mn4Cr0.5C (wt.%), deformation-induced e-mar-
of room-temperature serrations in the Fe17Mn0.2C tensite is formed when the SFE is smaller than
(wt.%) steels, stepwise loading tests combined with APT 18 mJ m2, while twins are formed when the SFE is in
analysis were applied. More specically, the steels were the range of 1848 mJ m2 [85]. Allain et al. [23] proposed
strained until a local increase in the gradient of the from TEM studies of Fe22Mn0.6C (wt.%) that the for-
stressstrain curve was observed, indicating the onset of mation of deformation-induced e-martensite occurs if the
serrations (indicated by the arrows at the section between SFE is lesser than 18 mJ m2, whereas mechanical twins
A1 and B1 or between A2 and B2 in Fig. 14a). Subse- are shown when the SFE takes a value between 12 and
quently, the deformed samples were considered for APT 35 mJ m2. More recently, Saeed-Akabari et al. [22]
measurement. Using APT, we mapped the redistribution observed that a higher C content leads to an increase in
of C atoms in an Fe17Mn0.2C (wt.%) steel during defor- the SFE of the deformed samples with deteriorating
mation, as shown in Fig. 14b. Judging from the recon- DIMT, and as a result of this the twinning occurs as plastic
structed C map, the C-enriched regions are presumed to deformation. From our TEM observations, the value of the
576 J.-B. Seol et al. / Acta Materialia 61 (2013) 558578

Fig. 14. (a) An enlarged engineering stressstrain curve showing type A serrations in the steel with 0.20 wt.% C after being strained to the onset of
serrations (arrows at section between A and B) and the corresponding strain distribution maps obtained from B1 and B2 points as detected by digital
image correlation. (b) APT map of C (red) and one-dimensional concentration prole of C. (For interpretation of the references to colour in this gure
legend, the reader is referred to the web version of this article.)

SFE for alloys with 0.10 and 0.20 wt.% C, consisting of cR Eqs. (1) and (2)), T0 values for diusionless (martensitic)
and einitial existing in the transition between mechanical transformation can be determined [27]. According to this
twinning and deformation-induced e, was consistent with estimate, the SFE was calculated as 16 mJ m2 for the
the thermodynamic calculations of SFE proposed by Nak- Fe17Mn0.01C (wt.%) alloy and as 22 mJ m2 for the
ano et al. [27]. According to their calculations, the SFE of Fe17Mn0.20C (wt.%) steels. We did not consider mag-
the Fe17Mn alloy without C at room temperature was netic eects, as austenite is paramagnetic in this context
about 19 mJ m2, whereas for an Fe17Mn0.2C alloy at room temperature [86]. This value agrees with the exper-
the SFE value was less than 24 mJ m2. Hence, we used imentally obtained SFE by Volosevich et al. [87] and Pet-
the model derived by Nakano et al. [27] to estimate the rov et al. [58]. Hence, steels containing high levels of C
SFEs of the present alloys in terms of the experimentally (either 0.10 or 0.20 wt.% C) can improve the eciency of
obtained T0 values. Using the undercooling the local nanotwinned bundles functioning as obstacles to
DT Ahcp!fcc
s  M fcc!hcp
s formulated in this study (in gliding dislocations. Thus, the ease of twin nucleation
J.-B. Seol et al. / Acta Materialia 61 (2013) 558578 577

seemed to result from the increased partial dislocation sep- e-martensite was nucleated mainly at the phase
aration occurring upon straining. Details of the contribu- boundaries between c and pre-existing e. At lower
tion of twinning to work hardening have been described strains, the new e plates which showed orientation iden-
[88,89]. However, the contribution of the nanotwinned tical to that of the adjoining pre-existing e grains grew
bundles to global ow stress, i.e. strengthening due to assisted by the movement of the c/e interface depending
nanotwin bundles [90], would be negligible because their on the loading direction. When the external stress was
volume fractions are considerably lower than that of the increased further, the growth ceased when a deforma-
deformation-induced martensitic phases (e and a). As a tion-induced e plate collided against either a pre-existing
result, the fraction of the deformation-induced transforma- e phase with a dierent {1 1 1}c habit plane or against a
tion, especially the transformation of cR-martensite to e- c/e phase boundary.
martensite, is an important factor even though the mechan-  The deformation-induced transformation of pre-existing
ical twins were formed in Fe17Mn steels containing high e to a was found to be benecial for the elongation,
amounts of C. So far, systematic methods for measuring while the transformation of c to e led to an increase in
the twin volume fraction are unavailable [31] and only rel- the strength. Even though the deformation-induced
ative values of the trend in twinning kinetics can be deter- transformation of c to e occurs, the resulting TRIP eect
mined by high-energy XRD [91] or EBSD [92]. was insucient. In this context, the material was soften
by the deformation-induced a transformation. There-
5. Conclusions fore, the elongation reduction in sample containing high
levels of C could be attributed to both the delayed trans-
The mechanical properties, DIMT and microstructural formation of the pre-existing e to a and the deforma-
changes in dual-phase FeMnC alloys were investigated tion-driven precipitation of nanosized cementite.
as a function of C content by using stepwise tensile loading
tests in combination with EBSD obtained from the surface
of the samples. These experiments revealed that the overall Acknowledgements
transformation sequence in the alloys studied herein
occurred in two ways, which included the transformation The authors acknowledge the fruitful comments of Prof.
of c-martensite to e-martensite and the transformation of D. Raabe, Dr. M. Koyama, Dr. P. Choi, MPIE. We also
pre-existing e-martensite to a-martensite. The amount of thank Dr. S.G. Lee and Dr. S.G. Hong, POSCO, and
C added was an important factor that determined whether Dr. J.E. Jin and Prof. Y.K. Lee, Yonsei University. This
a deformation-stimulated transformation was prevalent, work was nancially supported by BK21 Program of
which aected the mechanical properties. The main results KOREA.
and conclusions derived from our study are summarized
below. Appendix A. Supplementary material

 Before deformation, with increasing C content (i) ther- Supplementary data associated with this article can be
mally-induced phase transformation from austenite into found, in the online version, at http://dx.doi.org/10.1016/
e-martensite was retarded, (ii) the width of e-martensite j.actamat.2012.09.078.
became ner, and (iii) SFE increased.
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