mechanism of plastic behavior (TWIP vs TRIP) has
Communication
Processing and Properties of Medium-
Mn TRIP Steel to Obtain a Two-Stage
TRIP Behavior
D.M. FIELD, L.G. GARZA-MARTINEZ, and
D.C. VAN AKEN
Two medium-Mn steels of nominal composition 0.15C-
2.0Si-10.5Mn-(0.75, 1.5) Al-0.04Nb-balFe (wt pct) were
processed to produce sub-micron grain sizes of 0.65 and
0.80 lm. Mechanical testing was performed in three
successive conditions: hot rolled, intercritically
annealed, and cold rolled with subsequent intercritical
annealing. Intercritical annealing was performed at
923 K for 20 hours. Electron-backscattered diffraction
and X-ray diffraction were utilized to characterize the
microstructure, consisting of a-ferrite, a-martensite,
e-martensite, and c-austenite. Microstructural con-
stituents were tracked during tensile deformation and
it was found that both steels exhibited two-stage TRIP
with c-austenite martensitically transforming first to
e-martensite and as strain increased e-martensite trans-
formed to a-martensite.
https://doi.org/10.1007/s11661-020-05901-2
 The Minerals, Metals & Materials Society and ASM
International 2020
Twinning-induced plasticity (TWIP) and transforma-
tion-induced plasticity (TRIP) steels with 10 to 15 wt pct
Mn have demonstrated properties desirable for auto-
motive applications with ultimate tensile strengths of
1200 to 1500 MPa and total ductility of 30 to 25 pct.
These manganese bearing steels obtain their elevated
strengths and ductility either through the formation of
deformation twins (TWIP steels), single-stage TRIP
(cfia), or two consecutive martensitic transformations
(c fi e fi a) leading to a two-stage TRIP behavior.[1–6]
To date, the most successful method of predicting the
D.M. FIELD is with the US Army Combat Capabilities Development
Command Army Research Laboratory, Aberdeen Proving Ground, MD
21005. Contact e-mail: Daniel.m.field6.civ@mail.mil L.G. GARZA-
MARTINEZ is with AK Steel, Middletown, OH, 45005. D.C. VAN
AKEN is with the Department of Materials Science and Engineering,
Missouri University of Science and Technology, Rolla, MO 65409.
Manuscript submitted January 28, 2020.
Article published online July 6, 2020
METALLURGICAL AND MATERIALS TRANSACTIONS A
been by calculation of the intrinsic stacking fault energy
(ISFE).[5,7–10] It has been well established that deforma-
tion twinning will occur if the c-austenite ISFE is in the
range of 20 to 45 mJ/m2.[7–10] A TWIP-TRIP response,
where c-austenite will mechanically twin followed by a-
martensite formation at twin intersections, can be
obtained if the ISFE is 11 to 20 mJ/m2 and the two-
stage TRIP behavior is observed when the ISFE of the c-
austenite <10 mJ/m2. Field et al.[5] recently showed that
in dual-phase microstructures it is important to calculate
the ISFE based on the composition of the c-austenite
after annealing due to the enrichment of the c-austenite
with Mn and C leading to a change in the ISFE.
In two-stage TRIP alloys, McGrath et al.[1] quantified
the microstructure of a steel with a composition of
0.07C-2.85Si-15.3Mn-2.4Al-0.017N-balFe in wt pct and
showed that the steel had two distinct work hardening
rates associated with each TRIP stage. Work hardening
during cfie TRIP was lowest with K  2500 MPa and n
 0.2, whereas a maximum in work hardening was
reached as efia TRIP occurred with K = 8,065 MPa
and n = 1.3. Grässel observed that when TRIP is
activated, the tensile strength and total elongation were
increased due to the delayed necking from mobile
dislocation generation.[2]
Dynamic strain aging (DSA) is a significant concern
for implementation of these Mn steels due to the
negative strain-rate dependence on ultimate strength.
Early onset of necking was observed in two-stage TRIP
alloys due to DSA[5] as well as alloys where twinning is
observed.[11,12] Field and Van Aken[4] showed that
introducing chromium of sufficient quantity to produce
M23(C,N)6 precipitates reduces the concentration of
dissolved interstitials in the c-austenite and this leads to
the dynamic strain aging mechanism transitioning from
an interstitial defect interaction to the trapping of Mn at
the stacking fault. This work attempts to elucidate the
effect of aluminum on the microstructure of two-stage
TRIP steels, and how the developed microstructure
influences the work hardening capability of the alloys.
Two steels of nominal composition 0.15C-2.0Si-
10.5Mn-(0.75, 1.5)Al-0.04Nb-balFe (compositions given
in wt pct) were induction melted using iron, ferrosilicon,
electrolytic manganese, pure aluminum, ferroniobium,
and carbon in the form of graphite. An argon cover gas
was used to shield the melt and calcium wire was added
to modify oxide inclusions and remove sulfur. Before
tapping a synthetic vermiculite, slag was added to the
surface of the melt and an argon lance with a porous
plug was submerged into the melt to inject gas bubbles
for inclusion flotation and slag entrapment; this was
performed for 60 seconds prior to tapping into the ladle.
Alloys were tapped into a ladle with a 150 K (150 C)
superheat and cast into a phenolic no-bake sand mold to
form a Y-block with dimensions measuring 176 9 178 9
60 mm3. Chemical analyses were obtained by inductively
VOLUME 51A, SEPTEMBER 2020—4427
coupled plasma (ICP) spectrometry after sample disso- annealing with a cool down of typically ~24 hours, and
lution in hydrochloric and nitric acid. Carbon and this material will be designated as the ICA condition.
nitrogen contents were determined using Leco CS600 The main purpose of the ICA treatment was to permit
and TC500 analyzers, respectively. Alloy composition, greater reductions during cold rolling. A Stanat TA 315
ISFE, and martensite start temperatures are listed in in a 4-high roll configuration was used to cold roll the
Table I. Alloys are designated by their nominal alu- ICA material to a reduction of 50 pct in thickness. Cold
minum concentration. Mse and ISFE were calculated rolled alloys were heated to 923 K (650 C) for 20 hours
according to the method of Olson and Cohen[13] using in chemically treated stainless steel bags and furnace
Eq. [1] with an updated regular solution model as cooled to 298 K to simulate an industrial batch anneal-
described by Pisarik and Van Aken.[14] ing process and are designated as BA. A schematic of
  the processing is shown in Figure 1.
ISFE mJ=m2 ¼ nqðDGc!e Þ þ 2rc=e ½1 Tensile bars were milled from the HB, ICA, and BA
strip according to ASTM E8[16] standard for testing
where n is the number of (0001)e layers within the par-
sheet product. All tensile bars had a gage length of 50
ent austenite and q is the molar surface density of the
mm and gage width of 12.5 mm with tensile loading
{111}c for the steel composition using Vegard’s law.
conducted parallel to the rolling direction. The sheet
DGcfie is the driving force for the transformation of c-
surface was not machined nor chemically milled prior to
austenite to e-martensite, and rc/e is the interfacial
testing. Interrupted tensile tests were conducted on the
energy between the c-austenite and e-martensite and
final processed BA condition using displacement control
was held constant at 10 mJ/m2. The martensite start
rate of 0.01 mm/sec with a 245 kN servo-hydraulic test
temperature, MaS , was calculated according to the work
frame with strain measured using a contact extensome-
by Field and Van Aken,[15] where the strain energy of ter. For samples strained to failure, a non-contact laser
transformation, ( DGc!astr ) was balanced against the extensometer was utilized to capture the entire strain to
chemical driving force ( DGc!a
Chem ) according to Eqs. [2] failure.
and [3]. X-ray diffraction (XRD) samples were obtained for
DGc!a c!a all conditions to investigate the microstructural evolu-
Chem þ DGStr ¼ 0 ½2
tion throughout processing. XRD samples were
  mechanically polished to 0.1 lm using a diamond paste
DGc!a
Str
J=mol ¼ EXd2 ð14:8  0:013TÞ ½3 in the Longitudinal-Transverse plane (Rolling Plane
Normal). Diffraction patterns were obtained with a
where DGc!aChem is calculated according to a modified Philips X-pert diffractometer using a Cu Ka radiation
regular solution model, X is the molar volume for iron
of 7.15 9 106 (m3/mol), d is the lattice misfit between
the c-austenite and a-martensite with an approximate
strain of 1.11 9 102 (m/m), T is the temperature in
Kelvin, and E is the modulus in units of Pa calculated
in accordance with Reference 12. The start tempera-
ture for the a-martensite was calculated by determining
the temperature where Eq. [2] is true. It should be
noted that the values calculated in Table I assume a
fully austenitic microstructure with the listed
chemistry.
Castings were milled to a parallelepiped block of
dimensions 173 9 150 9 58 mm3, hot rolled at 1523 K
(1250 C) to a thickness of 2.0 mm, and cooled between
two insulating blankets. Finish roll temperature was 990
± 30 K (717 ± 30 C). Alloys in this condition are
termed hot band (HB) steels. Intercritical annealing Fig. 1—Schematic of the processing history of the alloys under
(ICA) was performed at 923 K (650 C) for 20 hours and investigation.
furnace cooled to room temperature to simulate a batch

Table I. Composition and Calculated Parameters of the Alloys Under Investigation

Composition (Wt Pct) Calculated Parameters*

Mse Msa
Alloy C Mn Si Al Nb N ISFE (mJ/m2) K (C) K (C)
0.75Al 0.15 10.2 2.07 0.71 0.040 0.026 3.0 346 (73) 453 (180)
1.5Al 0.17 10.6 2.08 1.54 0.042 0.013 11.5 286 (13) 360 (87)
*Assuming single phase c-austenite.

4428—VOLUME 51A, SEPTEMBER 2020 METALLURGICAL AND MATERIALS TRANSACTIONS A

source with a Ni filter and equipped with a flat graphite
monochrometer. Phase quantification, including e-
martensite, was calculated using the Rietveld refinement
method as described by Martin et al.[17] for an Fe-16Cr-
6.8Mn-6.1Ni steel and modified accordingly for the steel
chemistry investigated in this study.
Specimens for electron-backscattered diffraction
(EBSD) were also mechanically polished and finished
using a vibratory polisher with a 0.02 lm colloidal silica
solution. EBSD samples were examined in the Longitu-
dinal-Short plane (perpendicular to both the rolling
plane normal and rolling direction). Phase image map-
ping via pattern analysis was performed on a Helios
Nanolab 600 using an accelerating voltage of 20.0 kV
and emission current of 11 nA. Phase identification was
performed using a Nordlys detector and the AZTEC
software package. Degree of recrystallization was deter-
mined according to the work described by Field et al.[5]
and using the post-processing software Channel 5 on
multiple EBSD maps to analyze at least 1000 grains.
Grains containing internal misorientation greater than
5 deg were considered deformed, and grains with
misorientation less than 1 deg were considered fully
recovered. Grain size was measured according to the
ASTM E112–13[18] using the Heyn–Lineal Intercept
method.
Stress vs strain plots for the two alloys in all three
conditions are shown in Figure 2. Hot band and
intercritically annealed alloys exhibit rapid work hard-
ening immediately after yielding and reached ultimate
tensile strengths greater than 1400 MPa with total
strains to failure ranging from 12 to 25 pct. Cold rolled
and batch-annealed alloys demonstrate strains to failure
greater than 38 pct. All specimens exhibited post
necking ductility despite observing dynamic strain aging
in the BA condition for both alloys as well as the 0.75Al-
ICA condition. A summary of tensile properties is
provided in Table II.
EBSD phase maps of the two alloys in the various
processed conditions are shown in Figure 3 which
illustrates the distribution of three phases: c-austenite
is shown in green, e-martensite is shown in red, and a-
ferrite/martensite is shown as blue. The mean linear
intercept (L3) of the BA alloys was measured to be 0.65
± 0.05 lm for the 0.75Al alloy and 0.80 ± 0.02 lm for
the 1.5Al alloy. Instantaneous work hardening rate and
work hardening exponents were calculated according to
Eqs. [4] and [5] and graphed for the BA alloys with the
phase quantities as measured according to XRD in
Figure 4. Logarithmic smoothing was applied to the
curve. Tabulated XRD volume fractions of the three
conditions are shown in Table III. The highest rate of

Fig. 2—Stress-strain plot of the (a) 0.75 Al and (b) 1.5Al alloys under investigation throughout processing.

Table II. Mechanical Properties of the Alloys in the Three Conditions and the Measured Degree of Deformation According to
EBSD Analysis with a 95 Pct Confidence Level Shown

YS Recrystallized
Alloy Condition (MPa) UTS (MPa) Total Strain (Pct) Deformed (Vol Pct) (Vol Pct)
0.75Al HB 490 1690 13.0 74 ± 6 26 ± 4
ICA 385 1490 24.6 54 ± 10 46 ± 11
BA 770 1280 38.0 31 ± 3 69 ± 8
1.5Al HB 670 1600 12.1 69 ± 11 31 ± 5
ICA 610 1390 19.5 68 ± 6 32 ± 7
BA 875 1200 47.5 28 ± 1 72 ± 1

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 51A, SEPTEMBER 2020—4429

Fig. 3—EBSD phase maps of the 0.75Al alloy in the (a) HB, (b) ICA, and (c) BA conditions and the 1.5Al steel in the (d) HB, (e) ICA, and (f)
BA conditions. c-austenite is shown in green, e-martensite is red, and a-ferrite/martensite is shown in blue (Color figure online).

Fig. 4—Instantaneous work hardening rate (K), exponent (n), and microstructural components as a function of true plastic tensile strain of the
0.75Al-BA (a), (b). 1.5Al-BA (c) and (d).

work hardening was obtained during the second stage of

ei
TRIP with e-martensite transforming to a- martensite. n¼K ½5
ri
dr
K¼ ½4
de Previous researchers work on two-stage TRIP steels
have shown that there are two distinct martensitic
reactions that occur during straining. McGrath et al.[1]

4430—VOLUME 51A, SEPTEMBER 2020 METALLURGICAL AND MATERIALS TRANSACTIONS A

and Field and Van Aken[4] showed that for the initial
transformation, Stage I, a low initial work hardening
rate (~2700 MPa) is observed for the two-stage TRIP
steel; and is observed in the current study where both
alloys exhibit a work hardening rate (K) of 1200 to 1600
MPa in the initial Stage I regime. The higher initial work
hardening rate reported by McGrath et al. is potentially
due to a very low initial yield strength associated with a
prior austenite grain size of 30 lm and the starting
microstructure containing a higher fraction of c-austen-
ite and e-martensite. The high volume fraction of e-
martensite contributes to TRIP induced refinement of
the microstructure during work hardening. McGrath
et al. reports properties in a hot band condition that was
rolled to gauge thickness, reheated to 1173 K (900 C)
for 10 minutes, and quenched to room temperature in
water. The developed microstructure was reported to be
a mixture of c-austenite (27 pct), e-martensite (60 pct),
and a-martensite (13 pct). The BA alloys in this work
contain c-austenite (< 40 vol pct), e-martensite, and a-
martensite/ferrite (> 45 vol pct) due to processing by
cold rolling and intercritical annealing. The a-phase will
not TRIP and reduces the work hardening capability of
these alloys. The total content of transformable product,
the volume fraction of c-austenite, and e-martensite is
much lower (44 ± 11 vs87 vol pct) in the alloys
contained within this study compared to the work by
McGrath et al. The maximum work hardening rate and
exponent (K  6000 MPa, n  0.90 in Figures 4(a) and
(b)) for the 0.75Al-BA alloy was observed at true plastic
strain value of 0.20 and this corresponds to the final e-
martensite transforming to a-martensite. A lower work
hardening rate and exponent (K  3700 MPa and n 
0.70) is observed for the 1.5Al-BA steel at a true plastic
strain value of 0.30. A maximum in the strain hardening
occurs when the final e-martensite is exhausted and e-
martensite transform to a-martensite: at true plastic
strains of 0.07 for 0.75Al and 0.12 for 1.5Al. It is well
documented[5,11,19] that aluminum will lower the work
hardening behavior of both TRIP and TWIP steels. The
primary difference between the two alloys being inves-
tigated here is the aluminum content and the lower work
hardening rate of the 1.5Al alloy appears to be related to
the slower rate of a-martensite formation, since both
steels produced an equivalent amount of transformable
e-martensite prior to the onset of Stage II TRIP.
In the hot bands microstructure, a fraction of grains
appeared to be not fully recrystallized or unrecovered.
The increase in aluminum concentration leads to an
increased volume of recovered grains in the hot band
samples. Prior observations by Field et al.[5] on two-
stage TRIP steels has demonstrated that the stored
deformation from hot rolling exhibits a non-linear
relationship to the Si:Al ratio, where a Si:Al > 1 leads
to a primarily unrecovered steel in the hot rolled product
(HB).
The 0.75Al alloy also has a higher concentration of e-
martensite in both conditions (10 vol pct HB and 23
vol pct ICA) compared to the 1.5Al alloy which has a
higher volume fraction of c-austenite (18 vol pct HB and
22 vol pct ICA). The increased e-martensite content
leads to a consistently lower yield strength during tensile
testing (ry 0.75Al < ry 1.5Al), and this is rationalized
due to the volume change associated with the competing
martensitic reactions. The cfie-martensite transforma-
tion is a volume contraction of  0.74 pct as reported
for both two-stage TRIP alloys and shape memory
steels.[5,20,21] Upon straining, the e-martensitefia trans-
formation is a volume expansion of +2.1 pct. as
reported in Reference 5 and this volume change is
larger than the direct cfia reaction (+1.4 pct.). A
volume expansion (e fi a, DV>0) will accommodate an
imposed tensile strain, whereas a volume contraction
(cfie, DV<0) will resist the imposed tensile strain. Thus,
alloys with higher concentrations of e-martensite tend to
have lower yield strengths whereas alloys with high c-

Table III. Phase Quantities of the Hot Band, Intercritical Annealed, and Batch-Annealed Processed Alloys Utilizing XRD

c-Austenite e-Martensite a-Martensite/Ferrite

Alloy Condition (Vol Pct)
0.75Al HB 2 4 94
ICA 9 24 67
BA 22 11 67
1.5Al HB 8 1 91
ICA 21 6 73
BA 40 16 44

Table IV. Composition and Calculated Thermodynamic Parameters of the c-Austenite from Multiphase Equilibria Simulation
Using ThermoCalc 2018a

Composition (Wt Pct) Calculated Parameters

SFE Mse
Alloy C Mn Si Al N NbC (mJ/m2) K (C)
0.75Al-BA 0.20 19.8 2.35 0.21 0.026 0.046 4.6 341 (68)
1.5Al-BA 0.23 16.2 2.40 0.90 0.013 0.048 7.6 317 (44)

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 51A, SEPTEMBER 2020—4431

 Table V. Calculated Mechanical Properties of the Developed Alloys According to Equations Referenced from Ref. 5
Calculated Values
Alloy YS (MPa) UTS (MPa)
0.75Al-BA 665 1315
1.5Al-BA 620 1270
austenite that first TRIPs to e-martensite will have
higher yield strengths assuming each has the same
content of a-phases.
To better replicate the composition of the a-ferrite
and c-austenite using the thermodynamic software, a
temperature was determined to reproduce the measured
a-ferrite volume fraction. ThermoCalc 2018b was
utilized to calculate the thermodynamic equilibrium
composition of the c-austenite using the TCFE9
database and this chemistry is shown in Table IV with
an equilibrium temperature chosen to replicate the
quantity of measured a-ferrite. Precipitation of
Nb(C,N), partitioning of Al to the a-ferrite, and Mn
and C to the c-austenite significantly alters the ISFE
and e-martensite stability of the alloy. The loss of Al
and increase in Mn and C into the c-austenite decrease
the ISFE and raises the e-martensite start temperature
of both alloys. This effect is most significant in the
1.5Al steel with a decrease of 4 mJ/m2 compared to the
bulk composition leading to an increase in the Mse of
31 K (31 C) and translates to an Mse > 298 K (25 C).
This explains the higher volume fraction of e-martensite
observed in BA vs both the ICA and HB conditions.
This translates to greater total elongation and a
reduced work hardening rate.
Field et al.[5] report a compositionally based empir-
ical equation to calculate the ultimate tensile strength
and total elongation of two-stage TRIP steels and are
shown in Eqs. [6] and [7] where xi represents the weight
percent alloying element ‘‘i’’; they also showed that for
the sub-micron grain structure an inverse root rela-
tionship to the yield strength was obtained for the
mean linear intercept distance (L3) calculated according
to Eq. [8].
UTS ðMPaÞ ¼ 2580ðxC Þ þ 13ðxMn Þ  42ðxSi Þ
 30ðxAl Þ þ 72ðxCr Þ þ 7820ðxN Þ þ 750
Tot:eðpct:Þ ¼ 77ðxC Þ  2ðxMn Þ  5ðxSi Þ
þ 20ðxAl Þ þ 6ðxCr Þ  115ðxN Þ þ 51
 pffiffiffiffiffiffiffi
390 MPa lm
ry ðMPaÞ ¼ pffiffiffiffiffiffi þ 185ðMPaÞ
L3
The calculated values and their relative error are
shown in Table V. A high relative error is calculated for
4432—VOLUME 51A, SEPTEMBER 2020
Rel. Error (Pct)
Pct etot YS UTS Pct etot
40  13 3 5
50  29 4 5
the yield strength of the alloys compared to the
relationship reported by Field et al.; however, it should
be noted that the alloys under investigation are modified
with Nb to promote NbC formation during hot rolling.
A Nb contribution was not included in the previously
proposed empirical equation and more work needs to be
performed to determine where these carbides reside: at
grain boundaries to provide grain size stability or grain
interiors leading to Orowan strengthening. It has been
reported that NbC as a micro-alloying addition can lead
to significant increases in strength of Mn TWIP
alloys.[22, 23] Bai et al.[22] showed that with a moderate
addition of niobium (0.09 wt pct) a strength increase of
up to 160 MPa could be obtained. Scott et al. however
showed that Nb had a moderate effect (~60 MPa) on
increasing the strength of high Mn (‡ 18 wt pct) TWIP
steels[23] after accounting for grain size. If an average
increase of 100 MPa is added to the strengths of the steel
in this investigation a relative error of  6 and  18 pct
is obtained. The UTS and total elongation show a good
agreement with the calculated properties exhibiting a
relative error less than 5 pct.
Two 10.5 wt pct manganese steels have been pro-
cessed to obtain a two-stage TRIP response during
tensile testing. A high ultimate tensile strength >1220
MPa and an increased total elongation >38 pct was
obtained after hot rolling, intercritical annealing at
923 K (650 C), and cold rolling 50 pct and annealing at
923 K (650 C). A sub-micron grain structure comprised
of c-austenite, e-martensite, and a-ferrite was developed
after processing. Strength and ductility were shown to
exceed the DOE targets for future 3rd generation
advanced high-strength steels after processing to obtain
a dual-phase microstructure.
½6
This work was supported by the Peaslee Steel
Manufacturing Research Center (PSMRC). Companies
directly involved in this work include AK Steel,
ArcelorMittal, Nucor Steel, and US Steel. The FEI
½7 Helios NanoLab dual-beam FIB was obtained with a
Major Research Instrumentation grant from the Na-
tional Science Foundation under Contract DMR-
½8 0723128. The authors also acknowledge the support of
the Materials Research Center and in particular Dr.
Clarissa Wisner and Dr. Eric Bohannan for guidance
and training in using the FIB and performing the
XRD work.
METALLURGICAL AND MATERIALS TRANSACTIONS A
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Publisher’s Note Springer Nature remains neutral with regard to
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