Effect of Composition and Deformation on Coarse-Grained

Austenite Transformation in Nb-Mo Microalloyed Steels

N. ISASTI, D. JORGE-BADIOLA, M.L. TAHERI, B. LÓPEZ, and P. URANGA

Thermomechanical processing of microalloyed steels containing niobium can be performed to

obtain deformed austenite prior to transformation. Accelerated cooling can be employed to
refine the final microstructure and, consequently, to improve both strength and toughness. This
general rule is fulfilled if the transformation occurs on a quite homogeneous austenite micro-
structure. Nevertheless, the presence of coarse austenite grains before transformation in dif-
ferent industrial processes is a usual source of concern, and regarding toughness, the coarsest
high-angle boundary units would determine its final value. Sets of deformation dilatometry tests
were carried out using three 0.06 pct Nb microalloyed steels to evaluate the effect of Mo alloying
additions (0, 0.16, and 0.31 pct Mo) on final transformation from both recrystallized and
unrecrystallized coarse-grained austenite. Continuous cooling transformation (CCT) diagrams
were created, and detailed microstructural characterization was achieved through the use of
optical microscopy (OM), field emission gun scanning electron microscopy (FEGSEM), and
electron backscattered diffraction (EBSD). The resultant microstructures ranged from polygo-
nal ferrite (PF) and pearlite (P) at slow cooling ranges to bainitic ferrite (BF) accompanied by
martensite (M) for fast cooling rates. Plastic deformation of the parent austenite accelerated
both ferrite and bainite transformation, moving the CCT curves to higher temperatures and
shorter times. However, an increase in the final heterogeneity was observed when BF packets
were formed, creating coarse high-angle grain boundary units.

DOI: 10.1007/s11661-011-0624-0
Ó The Minerals, Metals & Materials Society and ASM International 2011

I. INTRODUCTION ical processes to microalloyed grades. When controlled

VALUE-ADDED applications of microalloyed steels
continue to be developed to meet the increasing material
demands of a variety of structural applications. Most of
the required properties can be obtained via two main
strategies: chemical alloying and optimization of the
processing parameters. Suitable combinations of alloy-
ing element additions, such as Nb, Ti, Mo, or B,
contribute to an increase in strength directly through
microstructural refinement, solid solution strengthening,
and precipitation hardening, as well as, indirectly,
through enhanced hardenability and associated modifi-
cation of the resultant microstructure.[1] Nevertheless,
toughness may be impaired depending on the selected
processing strategy followed to achieving the strength
requirements. Nowadays, combinations of high resis-
tance and high toughness are required for applications
such as gas and oil transportation pipes, offshore
facilities, and naval technologies.[2–4]
Reducing grain size improves both strength and
toughness, and the best way to obtain fine microstruc-
tures in the final product is by applying thermomechan-
N. ISASTI, Graduate Student, and D. JORGE-BADIOLA,
B. LÓPEZ and P. URANGA, Researchers, are with CEIT and
TECNUN (University of Navarra), Donostia-San Sebastian, 20018,
Basque Country, Spain. Contact e-mail: puranga@ceit.es M.L.
TAHERI, Hoeganaes Assistant Professor of Metallurgy, is with
Materials Department, Drexel University, Philadelphia, PA 19104.
Manuscript submitted November 16, 2010.
Article published online February 12, 2011
rolling is applied to Nb microalloyed steels, the austenite
is rolled at temperatures low enough to produce strain-
induced precipitation of carbonitrides during deforma-
tion to inhibit recrystallization.[5] As is well known, the
addition of Nb as an alloying element can retard or
inhibit recrystallization due to two mechanisms: the
solute drag effect owed to Nb atoms in solid solution
and the pinning effect due to strain-induced precipita-
tion, the latter usually exerting the strongest effect.[6,7]
Some authors reported that the reduction of austenite
grain size and an increase in retained strain provide a
higher density of nucleation sites, which leads to a
refinement of the final transformed microstructure[8,9]
and a modification of the balance between the different
ferrite morphologies.
Occasionally, rolled products show heterogeneous
austenite structure prior to transformation. For exam-
ple, the presence of microstructural banding in rolled
plates was reported as an origin for final heterogeneities
in the microstructure in low-carbon microalloyed
steels.[10] The microstructural bands are coarse bainitic
phases formed in a uniform matrix of ferrite and are
transformed from coarse austenite grains, which are
developed when conditions favor abnormal grain
growth or strain-induced grain boundary migration in
the rolling passes.[11,12] It is also possible to have
inappropriate austenite refinement before strain begins
accumulating, in some cases, as a consequence of a low
soaking temperature[13] or in others due to microalloy-
ing segregation.[14] Also, in thin slab direct rolling

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 42A, DECEMBER 2011—3729

technologies, the refinement and conditioning of aus-
tenite prior to transformation may be limited. The initial
as-cast coarse grain sizes are present at the entry of the
first stand. Together with the small total reductions, it
makes it difficult to reach enough refinement before
transformation;[15] this problem is most notorious when
final gages thicker than 10 mm are produced. In all these
cases, the transformation behavior of these coarse grains
will be completely different from those corresponding to
the surrounding finer grains. In a recent work, it was
observed that a higher fraction of coarse grain sizes in
the microstructure increases the chance of finding those
grains at the cleavage origin, leading to a wider scatter in
fracture stress in comparison to more homogeneous
grain size distributions.[14]
Various terms were proposed to name the transfor-
mation microstructures. Those terms mostly used are by
Bramfitt and Speer[16] and the ISIJ Bainite Commit-
tee.[17] In the present article, the ISIJ Bainite Committee
notation will be adopted, as phases observed fit better to
proposed ones. The phases are identified as polygonal
ferrite (PF), lamellar pearlite (P), degenerated pearlite
(DP), quasi-polygonal ferrite (QF), granular ferrite
(GF), bainitic ferrite (BF), and martensite (M).
PF nucleates as grain boundary allotriomorphs and is
characterized by very low dislocation densities and the
absence of substructure. Growth of polygonal equiaxed
ferrite is controlled by rapid substitutional atom transfer
across partially coherent boundaries and long-range
diffusion of carbon atoms, which are rejected from the
growing ferrite.[18–20]
QF grains have irregular grain boundaries and often
show etching evidence of substructure. Similar to PF,
QF nucleates heterogeneously at the boundaries of the
austenite grains. The transformation can be accom-
plished by short-range diffusion across transformation
interfaces.[21] However, interstitial or substitutional
atom partitioning may occur at the migrating interfaces,
causing irregular growth and jagged boundaries of
massive ferrite crystals.[22] QF also contains high dislo-
cation densities, dislocation sub-boundaries, and even
martensite-austenite (M/A) constituents.[23,24]
GF, or granular bainite, consists of sheaves of
elongated ferrite crystals with low misorientations and
a high dislocation density,[25] generally containing
roughly equiaxed islands of M/A microconstituent.
The carbon that is partitioned from the BF stabilizes
the residual austenite so that the final microstructure
contains both retained austenite and some high carbon
M;[26] the dispersed particles have granular or equiaxed
morphology. There is evidence that the GF crystals
grow by a diffusion-controlled ledge mechanism.[27] The
formation of different second phases is directly con-
nected with the effect of alloying elements on the ferrite
reaction, which in turn determines the size and carbon
content of the last transformed austenite. M/A constit-
uents are the most common feature of granular bai-
nite.[28] M/A either forms small islands, distributed
between ferrite grains, or covers the surfaces of larger
bainitic grains, which develop a steep carbon gradient.
Similar to lamellar P, degenerated P is formed at low
cooling rates by diffusion processes, and because of its
3730—VOLUME 42A, DECEMBER 2011
morphology, the difference is attributed to the insuffi-
cient diffusion of carbon to develop continuous lamel-
lae. Also, when degenerated P is formed during
continuous cooling, it involves transformation of M/A
island to degenerated P along with massive ferrite
transformation.
The transformation temperatures for the formation of
BF, which consists of packets of parallel ferrite laths or
plates separated by low-angle boundaries and contain-
ing very high dislocation densities, are in the interme-
diate temperature range. Although the austenite
decomposition is only to ferrite, coexisting with retained
austenite or M/A constituent, the microstructural
arrangement of acicular-shaped ferrite crystals in groups
of parallel laths is included in bainite classification. The
most prominent features of the microstructure are the
aligned, elongated, parallel islands of retained austenite
or M/A constituent within the prior austenite grains and
the conservation of the austenite grain boundary. The
structure consists of many fine, elongated ferritic crys-
tals with a high dislocation density.[25]
Dilatometry tests have been widely used in order to
obtain in-situ information concerning austenite decom-
position kinetics in steels.[29,30] Dilatometry registers
length changes that occur during heat treatment of a
sample. This information combined with microstruc-
tural analysis is the basis for CCT diagram determina-
tion. Taking into account all the information gathered
from dilatometry tests and microstructural character-
ization, this article undertakes a detailed study of the
transformation products in coarse austenite grains,
analyzing the effect of composition and austenite defor-
mation in low carbon niobium microalloyed steels
containing different levels of molybdenum.
II. MATERIALS AND EXPERIMENTAL
PROCEDURE
The chemical compositions of the steels studied are
listed in Table I. Uniaxial compression tests were
performed in a Bähr DIL805A/D quenching and defor-
mation dilatometer (Bähr-Thermoanalyse GmbH, Hull-
horst, Germany), where solid cylinders (5-mm diameter,
10-mm long) were employed. The steels were subjected
to simulated recrystallization (cycle A) and nonrecrys-
tallization (cycle B) deformation schedules depicted
schematically in Figure 1, followed by controlled cool-
ing at constant rates in the range 0.1 K/s to a maximum
cooling of 200 K/s. Both schedules (cycles A and B)
included a simulated roughing step performed at a
temperature of 1423 K (1150 °C) using a strain of 0.30
and a strain rate of 1 s1, followed by postdeformation
holding at the same temperature for 12 seconds to
ensure complete recrystallization. Furthermore, the
simulated nonrecrystallization schedule (cycle B) con-
tained an additional finishing step performed at a
temperature of 1173 K (900 °C), which was applied in
the nonrecrystallization temperature region using a
strain of 0.4 at 1 s1.
The microstructures generated at the end of the cycles
were characterized after etching in 2 pct Nital by optical
METALLURGICAL AND MATERIALS TRANSACTIONS A
 Table I. Chemical Compositions of Steels (Weight Percent)
Steel C Mn Si
6NbMo0 0.05 1.56 0.05
6NbMol6 0.05 1.6 0.05
6NbMo31 0.05 1.57 0.05
Fig. 1—Schematics of thermomechanical schedules performed at the
dilatometer for both cycle A (transformation from recrystallized aus-
tenite) and cycle B (transformation from deformed austenite).
microscopy (OM, Olympus IX2-UCB, Olympus Cor-
poration, Tokyo, Japan), SEM (PHILIPS* XL30CP),
*PHILIPS is a trademark of FEI Company, Hillsboro, OR.
and field emission gun scanning electron microscopy
(FEGSEM, JEOL** JSM-7000F). The dilatometry
**JEOL is a trademark of Japan Electron Optics Ltd.
samples were sectioned along their longitudinal axis,
selecting the region corresponding to a maximum area
fraction of nominal strain and reduced strain gradient.
Figure 2 shows the equivalent strain distribution in
the central cross section calculated using Abaqus/
Explicit[31] for a dilatometry sample deformed 0.3 at
1 s1, under the same conditions as for the cycle A
schedule. The observation plane is also drawn on the
image.
Selected samples were prepared for electron backscat-
tered diffraction (EBSD) observations. The specimens
were polished down to 1 lm and the final polishing was
with colloidal silica. Orientation imaging was carried
out on the PHILIPS XL30CP scanning electron micro-
scope with W-filament, using TSL (TexSEM Laborato-
ries, Provo, UT) equipment. For some specific samples,
higher resolution orientation imaging analysis was
carried out on the JEOL JSM-7000F FEGSEM using
HKL Channel5 EBSD. Different scan step sizes were
defined depending on the resolution needed, varying
from 0.2 lm for high resolution scans to 2 lm for
general microstructural characterization. Vickers hard-
ness measurements were made using a 1-kg load and are
reported as an average of 10 measurements.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Nb Mo Al N
0.06 0.01 0.028 0.004
0.061 0.16 0.03 0.005
0.059 0.31 0.031 0.005
Fig. 2—Equivalent strain distribution in the central cross section of
the dilatometry sample for the cycle A deformation pass
(T = 1423 K (1150 °C), e = 0.3, and e_ ¼ 1 s1 ). The section at
which the microstructural observation and hardness tests were per-
formed is also marked.
Austenite grain structure was analyzed in samples
quenched at 1173 K (900 °C). Samples were etched
using saturated picric acid and HCl. Average recrystal-
lized austenite grain size prior to transformation was
measured using the mean intercepted length method.
Recrystallized austenite mean grain sizes of Dc =
119 ± 8 lm, Dc = 125 ± 8 lm, and Dc = 84.8 ±
5 lm were obtained for steels 6NbMo0, 6NbMo16,
and 6NbMo31, respectively.
III. RESULTS
A. Microstructures
The microstructures of the specimens cooled at every
cooling rate were analyzed by OM for both schedules
and three steels. As an example, and for the case of steel
6NbMo0, the optical micrographs of the specimens
cooled at 0.1, 0.5, 10, and 100 K/s are shown in Figure 3
for both recrystallized (schedule A) and unrecrystallized
(schedule B) conditions of the parent austenite phase
prior to transformation.
A gradual shift from low cooling rate phases such as
PF and P (0.1 K/s) to high rate phases such as BF and
M (100 K/s) is observed with a transition through
microstructures composed by QF and GF (10 K/s). For
the slowest cooling rate of 0.1 K/s, the microstructure is
formed by PF and P. The significant refinement of the
VOLUME 42A, DECEMBER 2011—3731
Fig. 3—Light micrographs of the microstructures transformed from (a) through (d) recrystallized and (e) through (h) deformed austenite at steel
6NbMo0. 0.1 K/s: (a) PF + GF and (e) PF + P. 0.5 K/s: (b) PF + QF + GF and (f) PF + GF. 10 K/s: (c) QF + GF and (g) QF + GF. 100 K/s:
(d) BF + M and (h) BF + M + QF + GF.

3732—VOLUME 42A, DECEMBER 2011 METALLURGICAL AND MATERIALS TRANSACTIONS A

ferrite grain size when transformation has occurred from
unrecrystallized austenite should be noted. The opposite
condition corresponds to the highest cooling rate of
100 K/s, where a mixture of bainite and M is obtained in
both conditions, although the amount of M formed
from the recrystallized austenite is larger. For interme-
diate cooling rates, 0.5 K/s, for example, the micro-
structure is a mixture of PF and GF in the
unrecrystallized austenite; an important fraction of
GF, together with an increase in quasi-polygonal ferrite
fraction, is formed in the recrystallized condition.
After a 10 K/s cooling rate, the microstructure is
constituted by QF and GF, for both schedules. The
morphology of bainite is changed as a function of the
cooling rate. By increasing the cooling rate, the domi-
nant morphology of bainitic structures progressively
changes from granular ferrite (GF) to BF. It should be
noted that, in the deformed austenite, the GF morphol-
ogy predominates over the BF and that the grains are
distributed in a more random manner; i.e., the prior
austenite grain boundary networks are less evident
compared to recrystallized austenite.
Figure 4 shows several FEGSEM micrographs of
some microstructural features, which cannot be cor-
rectly shown using optical microscopic images. In
Figure 4(a), which corresponds to deformed austenite
cooled at 0.5 K/s, a mixture of PF and GF is shown.
The characteristic equiaxed shape of ferrite crystals and
a mixture of M/A islands in GF and cementite carbides
are observed. Degenerated P is also detected in some of
the PF/GF interphases. Figure 4(b) shows a mixture of
quasi-polygonal ferrite and GF in a sample correspond-
ing to deformed austenite cooled at 10 K/s. The
presence of M/A islands, instead of carbides, has been
confirmed by means of diffraction patterns using EBSD
technique. In Figure 4(c), cooled at 100 K/s, a mixture
of M and bainite (mainly BF but still with an important
fraction of GF) is represented. This BF microstructure
shows the characteristic elongated ferrite laths separated
by elongated M/A islands.

B. Dilatometry Tests
For the dilation curves to be interpreted, a careful and
systematic analysis of resulting data is needed. This
analysis has to be made in conjunction with optical
micrographs and detailed scanning electron microscopic
pictures. Figure 5(a) depicts the measured dilation
curves, represented as DL/L0 vs temperature, for several
cooling rates (0.1, 0.5, 10, and 100 K/s) obtained from
cycle B tests performed with steel 6NbMo31. Fig- Fig. 4—FEGSEM micrographs of microstructures corresponding to
ure 5(b) shows the evolution of the transformed fraction steel 6NbMo0 and schedule B: (a) 0.5 K/s, (b) 10 K/s, and (c)
derived from dilatometry curves in Figure 5(a) once the 100 K/s.
lever rule is applied.[32] This rule is based on extrapo-
lating the linear expansion behavior from the temper-
ature regions where no transformation occurs, and cooling rate, the transformed fraction curve exhibits
subsequently assuming proportionality between the several slope changes related to transitions from PF to
fraction of decomposed austenite and the observed GF and DP phases. For other cooling rates, and even if
length change. Depending on the cooling rate, the shape the optical micrographs show that the microstructures
of the curve and the transformation temperatures vary, are composed by a mixture of different phases, the
lowering the transformation start temperature as the evolution of the transformed fraction does not show
cooling rate increases. For the particular case of 0.5 K/s clearly the beginning and end of each transformation.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 42A, DECEMBER 2011—3733

Fig. 5—(a) Dilatometry curves and (b) evolution of transformed
fraction in steel 6NbMo31, cycle B (deformed austenite) and selected
cooling rates.
Therefore, for the temperature range and fraction of
each phase formation to be determined, additional
information can be extracted if the slope of the
transformed fraction (dftrans/dt) is analyzed. Figures 6(a)
and (b) show transformation rates as a function of the
temperature for the tests plotted in Figure 5. At a
cooling rate of 0.1 K/s (Figure 6(a)), the transformation
rate curve has a single peak related to the formation of
PF. For the 0.5 K/s cooling rate, two different peaks
corresponding to the formation of PF and GF are
detected. In the case of 10 K/s, the curve has a single
peak corresponding to the formation of the mixture of
QF and GF. Comparing these four curves, similar start
temperatures are observed for PF formation (0.1 and
0.5 K/s curves) and GF formation (0.5 and 10 K/s
cooling rates). For higher cooling rates (e.g., 100 K/s,
Figure 6(b)), the transformation rate curve shows
a sharp peak corresponding to the bainite and M
formations. This peak increases in value, i.e., higher
transformation rates, shifts to lower temperatures, and
3734—VOLUME 42A, DECEMBER 2011
Fig. 6—(a) and (b) Transformation rate as a function of temperature
calculated from tests in Fig. 5 for steel 6NbMo31, cycle B (deformed
austenite) and selected cooling rates.
reduces the transformation start-finish range as the
cooling rate increases. The transformation rate is much
lower for PF than for BF, which indicates the higher
growth rate of the bainitic laths, characteristic for
displacive transformations.
C. Hardness Measurements
Measurements of the bulk Vickers hardness of each
specimen were made and each value is the average of 10
individual measurements performed in the longitudinal
section marked in Figure 2. These data are summarized
in Figure 7, where hardness values are plotted for each
steel and the deformation schedule studied as a function
of the transformation start temperature. As expected,
the lowest hardness values correspond to the micro-
structures composed by PF, which are formed at
the highest transformation temperatures. Conversely,
the highest hardness values were displayed by the
microstructures composed by BF and M, formed at
METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 7—Vickers hardness values plotted as a function of the trans-
formation temperature for the three steels studied. Open and filled
symbols correspond to the transformation products formed from the
recrystallized and unrecrystallized austenite, respectively.
the lowest transformation temperatures. The hard-
ness data obtained for QF and GF combinations,
characterized by intermediate transformation tempera-
tures, lay between the aforementioned limits. For the
three steels examined, there is no significant influence of
steel composition when similar microstructures are
compared.
The comparison of hardness values plotted as a
function of the cooling rate is not always evident as
different microstructures are being compared. Based on
this reasoning, values in Figure 7 are plotted using
transformation temperatures, where comparable micro-
structures are roughly approximated by similar trans-
formation start temperatures. Hardness values for
samples produced from deformed austenite are reported
to be systematically higher than those from recrystal-
lized austenite.[33] Analyzing the data in Figure 7 (filled
symbols for deformed austenite and open symbols for
recrystallized austenite), this conclusion is not valid for
the entire range of microstructures generated.
Three different ranges can be defined depending on
transformation start temperature and hardness values.
For the highest transformation start temperatures
(>973 K (700 °C), i.e., low cooling rates), most of the
points in the graph are from samples of deformed
austenite, full symbols. This fact implies that ferritic
structures are formed mainly in deformed samples and
not in the ones transforming from recrystallized austenite.
Various effects of the deformation of austenite, such as
austenite grain refinement, increase in grain boundary
area per unit volume, Sv, presence of microalloy precip-
itates, and loss of microalloying elements due to precip-
itation in austenite, ultimately result in promoting the
austenite/ferrite transformation and a decrease in harde-
nability. As a consequence, the hardness of the deformed
samples is found to be lower than that of the undeformed
samples when the structure is mainly ferritic.[34] For
intermediate transformation start temperatures, 823 K
to 973 K (550 °C to 700 °C), phases are mainly QF and
METALLURGICAL AND MATERIALS TRANSACTIONS A
GF. For these structures, the hardness in samples of cycle
B is higher than for samples of cycle A. Finally, for the
highest cooling rates, samples transformed from recrys-
tallized austenite show higher hardness values due to the
higher M fractions present.
IV. DISCUSSION
A. CCT Diagrams
The information obtained from dilatometry tests,
micrographs, and hardness measurements was used to
build continuous cooling transformation (CCT) dia-
grams for both schedules and three steels. In addition to
phase stability regions, cooling rates and Vickers hard-
ness values are presented in those CCT diagrams
(Figure 8). The transformation start and finish temper-
atures were determined as the 5 and 95 pct transformed
fractions, defined from curves such as the ones shown in
Figure 5(b).
In all CCT diagrams, similar phases are observed. At
the lowest cooling rates, the transformed microstruc-
tures are composed by PF, GF, and P. At intermediate
cooling rates, a mixture of QF and GF is formed; and
the transformation sequence during continuous cooling
is QF formation followed by GF. Finally, at the highest
cooling rates, the transformed microstructures are
composed by BF and M.
In the case of 6NbMo0 and transformation from
undeformed austenite (cycle A), Figure 8(a), cooling
rates lower than 0.5 K/s promote the formation of a
mixture of PF and GF. The transformed microstruc-
tures containing GF and QF could be achieved at a
cooling rate range from 1 to 10 K/s. BF is formed at
cooling rates higher than 20 K/s simultaneously with M.
For steel 6NbMo0, the austenite deformation causes an
expansion of the transformation field for PF in the CCT
diagram (Figure 8(b)) and causes the formation of
lamellar P at the lowest cooling rate (0.1 K/s). Defor-
mation in the austenite causes a shifting in the trans-
formation to higher temperatures. The PF formation
occurs at 1080 K (807 °C) at 0.1 K/s (Ar3 displaced
34 K compared to undeformed austenite). On the other
hand, the formation of GF + QF increases until 20 K/s.
A mixture of BF, GF, QF, and M is obtained at the
cooling rates from 20 to 200 K/s.
The CCT diagram from recrystallized austenite of
steel 6NbMo16 (Figure 8(c)) shows some similarities
compared to the CCT of 6NbMo0 from the same
thermomechanical process. In that case, PF ceases to be
formed from 1 K/s. The addition of Mo causes a
shifting in the transformation to lower temperatures and
shorter times. CCT corresponding to 6NbMo16 from
deformed austenite (Figure 8(d)) also shows an increase
in PF field at the cooling range from 0.1 to 5 K/s.
Moreover, Ar3 shifts to higher temperatures (is displaced
5 to 15 K). At the cooling rate of 0.1 K/s, DP appears
instead of lamellar P and the first is favored by coarse-
grained austenite.[34] For intermediate cooling rates
corresponding to the formation of GF, QF, and BF,
the diagram exhibits shifting in Bs temperature to higher
VOLUME 42A, DECEMBER 2011—3735
Fig. 8—CCT diagrams for the (a), (c), and (e) recrystallized and (b), (d), and (f) deformed austenite for the three steels studied: (a) and (b) steel
6NbMo0, (c) and (d) steel 6NbMo16, and (e) and (f) steel 6NbMo31.

temperatures compared to the case of recrystallized
austenite (Bs is displaced 10 to 50 K).
For steel 6NbMo31, the transformed phases and CCT
diagram shape are similar compared to the previously
analyzed diagrams. For the case of undeformed
austenite (Figure 8(e)), PF formation along austenite
grain boundaries is limited at lower cooling rates
(0.1 K/s and 0.5 K/s) and GF is also formed. The
mixture of GF, QF, and BF could be achieved at cooling
rates ranging from 10 to 50 K/s. Finally, the formation

3736—VOLUME 42A, DECEMBER 2011 METALLURGICAL AND MATERIALS TRANSACTIONS A

of M is observed at cooling rates higher than 50 K/s. In
the case of 6NbMo31 and deformed austenite (Fig-
ure 8(f)), the diagram shows the same trend previously
mentioned. Deformation increases the transformation
start and finish temperatures, as well as accelerating
bainitic and ferritic transformations.
Comparing both CCT diagrams, in the case of
recrystallized austenite, both the transformation start
and finish temperatures were clearly lower than in the
case of deformed austenite. In the same way, deforma-
tion accelerates bainitic and ferritic transformation.
There is no significant change in morphology of the
transformation products derived from deformed aus-
tenite compared to the microstructures formed from the
recrystallized austenite except for the observed refine-
ment of the PF and QF grains (Figure 2) and the GF
and BF assemblies. The effect of the strain accumulation
on the ferrite refinement is related to the increase of the
specific grain boundary area and is attributed to a
significant increase in the density of ferrite nucleation
sites introduced by deformation.[35–38]
B. Effect of Composition
The effect of molybdenum on the transformed phases
and temperatures can be evaluated by comparing the
CCT diagrams shown in Figure 8. On one hand, it can
be affirmed that there is no clear effect on Ar3, Bs, or Ms
temperature, even if a decrease in Ms is observed for the
two steels containing Mo. On the other hand, a slight
shift of the PF formation region to lower cooling rates is
observed when Mo is added, due to the increase in
hardenability. Cizek et al.[33] also observe a relatively
weak contribution of molybdenum to the hardenability
enhancement. The authors suggest that the static recrys-
tallization occurring after deformation at a high tem-
perature of 1423 K (1150 °C) for the tests reported in
the present article and accompanied by the movement of
the austenite grain boundaries might prevent molybde-
num from segregating to these boundaries. In addition
to this effect, the steels analyzed in the current study
have bigger austenite grain sizes and higher levels of
niobium. Therefore, the total grain boundary area per
unit volume, Sv, is reduced and the niobium in solution
may have reached an important hardenability effect,
saturating any further effect attributable to molybde-
num.
Nevertheless, an important effect of Mo addition on
the ferritic structure size distribution is observed for the
low cooling rates. Figure 9 shows three image quality
maps obtained after the application of schedule B for
the three steels studied and the same cooling rate of
0.1 K/s. PF is the predominant phase in the three
microstructures with a banded secondary phase. This
secondary phase is lamellar P for the 6NbMo0 steel and
degenerated P for the steels containing Mo. A decrease
in the banding is also noticed as Mo content increases.
As shown in Figure 9(d), a considerable coarsening is
measured as Mo content increases. The mean ferritic
grain sizes are 16.4, 16.8, and 19.1 lm for 6NbMo0,
6NbMo16, and 6NbMo31 steels, respectively. Addition-
ally, the homogeneity of the final structure is clearly
METALLURGICAL AND MATERIALS TRANSACTIONS A
affected if the Mo level is increased. A useful parameter
to evaluate the length of the tail of a distribution is to
calculate a critical grain size for a fixed area fraction.
The grain sizes for which 10 pct of the area fraction of
grains have a size greater than that value (denoted as
Dc10 pct) are 65, 67, and 77 lm 6NbMo0, 6NbMo16,
and 6NbMo31 steels, respectively. Alloying elements are
reported to decrease the nucleation rates of all the ferrite
morphological types nucleating heterogeneously on the
austenite grain or deformation-induced boundaries.[33]
C. Effect of Deformation
In Figure 10, the CCT diagrams developed for steel
6NbMo31 for both recrystallized and deformed austen-
ite are plotted together for comparison; the cooling rates
are also indicated. The deformation of the prior
austenite forces an expansion of the ferrite transforma-
tion field in the CCT diagram. An increase in the ferrite
transformation start temperature was observed (Ar3).
Similarly, an increase of the bainite transformation start
temperature was also observed in the range of high
cooling rates.
While the increase of Ar3 temperature with deforma-
tion is well documented, the behavior of Bs is more
complex. It has been widely accepted that the enhanced
PF formation, brought about by the deformation of
austenite, may be largely attributed to an increase in the
ferrite nucleation rate, while the ferrite growth rate
seems to be less affected. This suggestion leads to a
significantly finer PF grain size obtained in the present
study after transformation from the deformed austenite,
compared to the case of the recrystallized austenite.[33]
In contrast to what occurred with ‘‘reconstructive’’
type transformations, such as allotriomorph ferrite, for
displacive transformations such as bainite and M,
plastic deformation retards the decomposition of the
austenite; this effect is known as ‘‘mechanical stabiliza-
tion.’’[39] The mechanism appears to be that the growth
of bainite/M laths is retarded by the deformation in the
austenite. The transformation of deformed austenite
might be accelerated at initial stages, although the
overall rate of transformation would be reduced com-
pared to nondeformed austenite. As a consequence, a
smaller quantity of bainite may be formed in the former
case, although this behavior seems to depend on the
degree of deformation. Lightly deformed austenite
transforms more rapidly relative to undeformed austen-
ite because of the increase in the defect density (nucle-
ation sites, higher Sv). However, although the nucleation
rate will be larger in heavily deformed austenite, the
overall rate of transformation will be reduced; the
growth will be retarded.
Similarly to what is observed in the present study,
Kazimierz and Lis recently observed that bainitic trans-
formation was also accelerated in deformed austenite in
the range of high cooling rates.[40] These authors sug-
gested that a higher dislocation density in the deformed
austenite leads to a faster nucleation of the bainite laths.
In contrast, at slower cooling rates, they observed a
retardation of the bainitic transformation compared to
the kinetics found in nondeformed austenite.
VOLUME 42A, DECEMBER 2011—3737
Fig. 9—Microstructural details obtained by EBSD for a cooling rate of 0.1 K/s and cycle B: image quality maps for (a) steel 6NbMo0, (b) steel
6NbMo16, and (c) steel 6NbMo31. (d) Unit size distributions (defined using the 15 deg misorientation criterion) plotted in terms of accumulated
area fraction for the three steels.
Fig. 10—Comparison between the CCT diagrams obtained for re-
crystallized and deformed austenite in steel 6NbMo31.
In order to better characterize the effect of stored
deformation in austenite on transformed structures,
EBSD scans were performed for different cooling rates
3738—VOLUME 42A, DECEMBER 2011
and both schedules in steel 6NbMo16. Different imaging
options were used to define parameters that can be
related to the microstructure, among others, the 4 and
15 deg misorientation crystallographic unit sizes. The
first one is related to the strength level of the resulting
microstructure, while the second defines toughness
properties related to microstructural homogeneity.
Figure 11 shows the influence of cooling rates on the
mean unit size for the microstructures transformed from
recrystallized (schedule A) and deformed (schedule B)
austenite in steel 6NbMo16, considering both the afore-
mentioned misorientation criteria of 4 and 15 deg. As
expected, using a 15 deg threshold misorientation, larger
unit sizes are quantified at all conditions. On the other
hand, it is found that, as a general trend, the average
unit size decreases with increasing the cooling rate. For
mainly ferritic structures, this fact is related to an
increase in the nucleation rate and a decrease in grain
growth with increasing the cooling rate.[41–43] If the
4 deg criterion is chosen, the average unit size decreases
from 16.9 to 8.5 lm in the case of recrystallized
austenite and from 13.8 to 8.1 lm in the case of
unrecrystallized austenite. Meanwhile, in the case of
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 11—Influence of cooling rate on the average unit size for both
recrystallized (schedule A) and unrecrystallized (schedule B) austenite
using 4 and 15 deg threshold misorientation criteria in steel
6NbMo16.
the 15 deg criterion, mean unit sizes decrease from 25.4
to 11.8 lm and from 17.6 to 12 lm for recrystallized
and deformed austenite, respectively.
In contrast to mainly ferritic structures, a different
behavior is observed when the microstructures show an
important fraction of BF. An increase in the mean unit
size value is observed for the 15 deg criterion, and the
increase is more important in the case of schedule A (5
and 10 K/s cooling rates). For schedule B, this increase
shifts to higher cooling rates (20 K/s). The further
reduction in mean unit size at higher cooling rates is
related to the formation of M. This variation is not
observed for the 4 deg criterion, due to the fact that only
high-angle grain boundary density is affected when the
bainite fraction increases; the low-angle boundary den-
sity remains approximately constant.
The results shown in Figure 9 define the evolution of
the mean values of several microstructural features, but
they do not provide information concerning the influ-
ence of accumulated strain and cooling rate on micro-
structural heterogeneity that could affect the toughness
behavior. In order to take this into account, the 15 deg
unit size distributions obtained at different cooling rates
are represented in Figure 12. Grain area fractions were
considered in order to better identify the presence of
coarse grains.
In the case of schedule A (Figure 12(a)), different
trends may be highlighted for the 15 deg crystallo-
graphic grain distributions. For the lowest cooling rates
of 0.1 and 0.5 K/s, the mainly ferritic structures lead to
homogeneous distributions. As the cooling rate is
increased to the 1 to 10 K/s range, an increase in
heterogeneity is observed and the cooling rate of 10 K/s
is the one with the widest unit size distribution.
Nevertheless, for the 20 and 50 K/s cooling rates, tied
to M formation, an improvement in homogeneity is
reached obtaining the finest and most homogeneous
distribution for the 50 K/s cooling rate.
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 12—Grain size (15 deg) distributions plotted in terms of accu-
mulated area fraction for steel 6NbMo16 and cycles (a) A and (b) B.
For schedule B (Figure 12(b)), a gradual increase in
heterogeneity is measured as the cooling rate increases.
Relatively fine-grained and homogeneous distributions
are obtained for mainly ferritic structures (0.1 to 1 K/s
range). When GF becomes the main phase, an increase
in heterogeneity is clearly noticed, reaching a maximum
level of heterogeneity for the 20 and 50 K/s cooling rate,
exactly where BF appears. For the highest cooling rate
measured, 100 K/s, a slight increase in homogeneity is
observed as the M fraction is increased.
Previously published studies suggest that, to quantify
the ductile-brittle transition, instead of the mean unit
size, a parameter able to properly catch the relevance of
coarse grain fractions is required.[44,45] Following that,
the unit size for which 10 pct of the area fraction of
grains have a size greater than that value was selected
(denoted as Dc10 pct).
The corresponding Dc10 pct values have been drawn
in Figure 13 as a function of the cooling rate. A similar
trend in Dc10 pct is observed for microstructures
transformed from recrystallized and deformed austenite.
Dc10 pct values increase as the cooling rate increases up
to a maximum located at 10 K/s for cycle A and 50 K/s
for cycle B. For higher cooling rates, the Dc10 pct value
decreases sharply in both cases.
At the lowest cooling rates, with mainly ferritic
structures, the accumulation of strain provides a higher
VOLUME 42A, DECEMBER 2011—3739

Fig. 13—Change of Dc10 pct value as a function of the cooling rate
in steel 6NbMo16 and both cycles A and B. The crystallographic
grains with misorientations of 15 deg were considered.
density of nucleation sites resulting in a refined and
more homogeneous microstructure compared to the
nondeformed material, following a tendency similar to
that observed for the mean unit size (Figure 11). At
these cooling conditions, nucleation density is high
enough to achieve a refinement in the entire unit size
distribution and, therefore, results in low Dc10 pct
values.
However, in the case of higher cooling rates (>1 K/s),
where the microstructure is constituted mainly by QF
and GF, the increase in the cooling rate seems not to
have an important effect on the refinement of the tail of
the unit size distribution given by high-angle grain
boundaries. The increase in heterogeneity, reflected in
the peak in the Dc10 pct, is tied to the maximum
fraction of BF in the microstructure. For the case of
high-temperature bainite transformations, Furuhara
et al.[46,47] observed that a small undercooling promotes
variant selection leading to coarse bainite packet sizes,
and Lambert-Perlade et al.,[48] also in conditions corre-
sponding to initial coarse austenite grains, confirmed
that the austenite grain size can play an important role
in the nucleation of bainite variants. The formation of
M at high cooling rates promotes an important micro-
structural homogenization reflected in the Dc10 pct
value drop and general refinement (distributions in
Figure 12), for structures transformed from both re-
crystallized and unrecrystallized austenite. This refine-
ment, related to M formation and bainite packet size
reduction, is also observed for normal austenite grain
sizes and high undercooling.[49,50]
The influence of deformed austenite in microstruc-
tural heterogeneities at high cooling rates must be taken
into account. The beneficial effect observed in ferritic
microstructures, and also for QF and GF combinations,
completely disappears when BF becomes the main
phase. In contrast to what happens with ferrite, results
suggest that, for coarse austenite grains, bainite packet
refinement is not enhanced by the accumulated strain. In
the present case, probably the limited accumulated
3740—VOLUME 42A, DECEMBER 2011
strain was not sufficient to promote additional intra-
granular bainite nucleation on austenite defects.[51]
For a better understanding of the transition in
homogeneity between mainly bainitic structures and
the formation of some M, additional EBSD scans were
performed using the FEGSEM with a 0.2-lm step and
for a 140 9 140 lm2. Figure 14 shows two scans relative
to the 6NbMo16 steel and two cooling rates of 20 and
100 K/s transformed from deformed austenite (cycle B).
The first one is composed by a mixture of GF and BF,
while in the latter, some M is formed together with the
previous phases. Misorientation angle maps (Fig-
ures 14(c) and (d)) are plotted considering 4 and
15 deg criteria using gray and black colors, respectively.
Even if image quality maps suggest that the structure
in Figure 14(a) is finer and more homogeneous when
compared to the one in Figure 14(b), misorientation
image maps show that the high-angle boundary density
in the first one is low (Figure 14(c)), and therefore the
toughness properties of this microstructure would be
affected by the coarse units formed. Analysis of the
100 K/s phases (Figures 14(b) and (d)) shows that BF
packets are formed in parent austenite grain bound-
aries. Areas with phases such as BF and GF (left side
of the image) show a low high-angle grain boundary
density, while regions with M formation (right side of
the image) reflect an important refinement in the
15 deg unit sizes.
V. CONCLUSIONS
The transformed microstructures for the three Nb-Mo
microalloyed steels contain PF, QF, and P, bainite with
different morphologies such as GF or BF, and M. The
accumulation of strain in the austenite accelerates both
the ferritic and bainitic transformations, displacing the
CCT diagrams to higher temperatures and shorter
times.
A slight effect of molybdenum is observed in the
ferrite stability region shifting it to longer times when
the alloying level is increased. Additionally, microstruc-
tural coarsening was quantified for low cooling rates
(0.1 K/s) when Mo content increases.
Mean unit size, measured by means of 4 or 15 deg
misorientation criteria using EBSD scans, decreases as
the cooling rate increases; the refining effect is more
notorious in the range of low cooling rates where the
microstructures are mainly formed by ferrite. Similarly,
the accumulation of strain in the austenite results in
smaller mean unit sizes. Nevertheless, this general trend
is not valid for cooling rates where BF fraction becomes
important, and an increase in the 15 deg mean unit size
is observed until M is formed at higher cooling rates.
Structure homogeneity varies depending on the cool-
ing rate and the phases formed. In the range of low
cooling rates, the microstructure is relatively finely
grained and homogeneous. As the cooling rate increases
and the GF fraction becomes the major constituent, a
coarsening in the structure together with a more
heterogeneous distribution is measured, reflected in the
15 deg mean unit size, unit distribution, and Dc10 pct
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 14—Microstructural details obtained in steel 6NbMo16 and cycle B using FEGSEM EBSD. Image quality maps: (a) 20 K/s, (b) 100 K/s
and misorientation angle maps (4 deg units: gray; 15 deg units: black), (c) 20 K/s, and (d) 100 K/s.

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the austenite grain size may play an important role in
the nucleation of bainite variants. The formation of M
promotes a refined and more homogeneous structure;
this homogenization is more important as the M
fraction increases.
ACKNOWLEDGMENTS
Financial support of this work by the Spanish Sci-
ence and Innovation Department (MAT2009-09250
project) is gratefully acknowledged. One of the authors
(NI) acknowledges a research grant from the Univer-
sity of Navarra. PU is grateful to NSF and TMS for
the MS&T’10 Conference registration fee funding.
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