The Effect of the Initial Microstructure on Recrystallization

and Austenite Formation in a DP600 Steel

M. KULAKOV, W.J. POOLE, and M. MILITZER

The effects of initial microstructure and thermal cycle on recrystallization, austenite formation,
and their interaction were studied for intercritical annealing of a low-carbon steel that is suitable
for industrial production of DP600 grade. The initial microstructures included 50 pct cold-
rolled ferrite–pearlite, ferrite–bainite–pearlite and martensite. The latter two materials recrys-
tallized at similar rates, while slower recrystallization was observed for ferrite–pearlite. If
heating to an intercritical temperature was sufficiently slow, then recrystallization was com-
pleted before austenite formation, otherwise austenite formed in a partially recrystallized
microstructure. The same trends as for recrystallization were found for the effect of initial
microstructure on kinetics of austenite formation. The recrystallization–austenite formation
interaction accelerated austenization in all the three starting microstructures by providing
additional nucleation sites and enhancing growth rates, and drastically altered morphology and
distribution of austenite. In particular, for ferrite–bainite–pearlite and martensite, the recrys-
tallization–austenite formation interaction resulted in substantial microstructural refinement.
Recrystallization and austenite formation from a fully recrystallized state were successfully
modeled using the Johnson–Mehl–Avrami–Kolmogorov approach.

DOI: 10.1007/s11661-013-1721-z
 The Minerals, Metals & Materials Society and ASM International 2013

I. INTRODUCTION austenite might transform back into ferrite, and the

DUAL-PHASE (DP) steels were originally devel-
oped in the mid 1970s[1] but have become widely used
material for automotive manufacturers only in the last
10 years. The formability of high-strength low-alloy
(HSLA) steels is insufficient for the production of
complex shapes of automotive parts and thus limits
their applications. These limitations can be resolved by
using DP steels with a composite microstructure of hard
martensite embedded in a soft ferrite matrix. Compared
with HSLA steels at the same level of tensile strength,
DP steels possess lower yield strength, no yield point
elongation, higher work hardening rate, and higher
ductility.
DP steels for automotive sheets are primarily cold-
rolled and coated products. In this case, the DP
structure is produced through intercritical annealing
after cold rolling. Depending on cooling conditions on
the run-out table in the hot mill, various microstructures
can be produced as an input for intercritical annealing in
a continuous annealing or galvanizing line. During
heating and holding at an intercritical temperature, the
cold-rolled microstructure recrystallizes and partially
transforms into austenite. Upon cooling, a fraction of
M. KULAKOV, Ph.D. Student, W.J. POOLE, and
M. MILITZER, Professors, are with the Centre for Metallurgical
Process Engineering, The University of British Columbia, 309-6350
Stores Road, Vancouver, BC V6T 1Z4, Canada. Contact e-mail:
nkulako@gmail.com
Manuscript submitted October 23, 2012.
remaining austenite is converted into martensite. The
morphology and distribution of intercritical austenite
determines the resulting martensite distribution in the
final microstructure and this affects the mechanical
properties of intercritically annealed steels.[2–4]
If the heating rate is sufficiently low, then recrystal-
lization is completed before austenite starts to form.
Austenite formation in as-heat-treated or fully recrys-
tallized materials has been studied extensively for a
range of initial microstructures.[5–11] Microstructures
with a uniform cementite distribution and fine ferrite
grain size, e.g., tempered martensite, result in faster
austenization rates and more homogeneous austenite
distribution as opposed to coarse-grained microstruc-
tures with clusters of cementite, e.g., in pearlite.[8,9]
Modern industrial annealing lines permit heating at
rates sufficiently high to postpone recrystallization such
that it overlaps with austenite formation. The interac-
tion between recrystallization and austenite formation
has not received attention until recently. These recent
studies showed acceleration of austenite formation from
a nonrecrystallized microstructure and drastic changes
in austenite morphology and distribution.[12–18]
The purpose of the current study is to determine the
effect of initial cold-rolled microstructures on recrystal-
lization, austenite formation, and their interaction in a
low-carbon steel with a typical DP600 grade chemistry.
Three initial microstructures are included in this inves-
tigation, i.e., (1) ferrite–pearlite, (2) ferrite–bainite–
pearlite. and (3) martensite, to cover the full range of
structures which could be potentially used for cold
rolling and subsequent annealing.

METALLURGICAL AND MATERIALS TRANSACTIONS A

 II. MATERIALS AND EXPERIMENTAL
PROCEDURES
The chemical composition of the investigated steel is
shown in Table I. The industrially processed steel was
supplied by ArcelorMittal Dofasco Inc. (Hamilton, ON,
Canada) from the same heat in form of 3.6 mm thick
hot-rolled and 1.8 mm thick 50 pct cold-rolled sheets.
The hot-rolled sheets were used to create additional
starting microstructures for the intercritical annealing
studies. For this purpose, the hot-rolled material was
first re-austenized in a box furnace at 1173 K (900 C)
for 1800 seconds and then either furnace-cooled or
water-quenched to produce two different microstruc-
tures. Subsequently, these materials were cold rolled in a
single stand laboratory mill having 150 mm diameter
rolls. The cold-rolling schedule consisted of ten passes
with 5 pct reduction per pass to obtain a total reduction
of 50 pct as in the industrially cold rolled sheets. Rolling
conditions in the laboratory rolling mill were selected
such as to obtain a homogeneous strain distribution
through the sample thickness similar to that commonly
obtained in industrially cold-rolled sheets. Thus, labo-
ratory rolling was conducted with the ratio of the mean
sample thickness to the length of the sample-roll contact
being always below unity.[19]
Subsequent heat treatments were conducted under
high vacuum of 0.26 Pa using Gleeble 3500 thermo-
mechanical simulator equipped with a dilatometer
(Dynamic Systems Inc., Poestenkill, NY). From the
as-cold-rolled materials, 10 9 60 9 1.8 mm sheet sam-
ples were machined with the longitudinal axis coinciding
with the rolling direction. Temperature was controlled
through a K-type thermocouple spot welded at the
center of each sample. One test series, i.e., the heating–
holding transformation tests with 100 K/s heating rate,
was conducted with a Bähr 805A/D dilatometer using
10 9 5 9 1 mm sheet samples with the longitudinal axis
aligned with the transverse rolling direction. Equal
amounts were ground off both sides to reduce their
thickness from 1.8 to 1 mm. The microstructure was
characterized using a Nikon Epiphot 300 optical micro-
scope with image analysis software Clemex (Clemex
Technologies Inc., Longueuil, QB, Canada) and Hitachi
S2300 and S3000 scanning electron microscopes.
Recrystallization in all starting microstructures was
studied during isothermal holds at 873 K, 898 K, and
923 K (600 C, 625 C, and 650 C); the heating rate to
the holding temperature was 50 K/s. Further, recrystal-
lization was measured during continuous heating tests at
1 K/s. Partially recrystallized samples were helium-
quenched. Recrystallized volume fraction was measured
directly on secondary electron images using the point
counting method (ASTM E569-89). Vickers micro-
hardness measurements were conducted at 1 kg load
Table I. Major Alloying Elements in the Investigated Steel
(Weight Percent)
C Mn Si Cr
0.105 1.858 0.157 0.340
and 15 seconds dwell time. An average of five hardness
measurements is reported. Austenite formation was
studied during continuous heating at 1, 10 and 100 K/s
and heating–holding tests with 1200 seconds holding at
1043 K (770 C) after heating either at 1 or 100 K/s. A
dilatometer was mounted on samples either transversely
(Gleeble tests) or longitudinally (Bähr experiments) to
measure dimensional changes during austenite forma-
tion with respect to the same rolling direction. At least
two tests were conducted for each thermal path.
Austenite volume fractions were calculated from the
dilatometer data using the lever rule (ASTM A1033-10).
To validate the dilation results and obtain further
insight into the austenite formation mechanisms, par-
tially austenized samples were water-quenched at cool-
ing rates of 1000 K/s to convert all intercritical
austenite into martensite at room temperature. The
water-quenched samples were etched with LePera’s
reagent to reveal martensite.[20] The volume fraction of
martensite was measured using automatic image anal-
ysis according to ASTM E1245-03. Martensite mor-
phology and distribution were investigated with
scanning electron microscopy on samples etched with
2 pct Nital. Further, fully austenized samples were water
quenched to determine the austenite grain size resulting
from austenite formation. For these fully martensitic
samples, the prior austenite grain boundaries were
revealed by etching at 363 K (90 C) for 75 seconds in
a saturated water based solution of picric acid, 1.3 g of
sodium dodecylbenzene sulfonate and 1 mL of concen-
trated hydrochloric acid per 100 mL solution. Equiva-
lent area diameter of ferrite grains before and after
recrystallization, as well as austenite grains in fully
austenized samples were determined on at least 500
grains according to ASTM E1382-97 using the grain
area measurement technique.
III. EXPERIMENTAL RESULTS
A. Characterization of the Initial Microstructures
Three materials which had been cold rolled by 50 pct
were used for the recrystallization and austenite forma-
tion experiments in the current study. Their microstruc-
tures before and after cold rolling are shown in Figure 1
and can be described as follows:
(a) After reaustenizing at 1173 K (900 C) for
1800 seconds and slow furnace cooling of the as-
received hot-rolled material, its microstructure con-
sisted of 85 vol pct of ferrite and 15 vol pct of
pearlite (F–P), Figure 1(a). The average ferrite
grain size in the as-heat-treated condition was
11 lm. Pearlite bands were parallel to the rolling
direction with an average band spacing of 14 lm
after 50 pct cold rolling, Figure 1(d). The pearlite
band thickness characterized using the intercept
method with the test lines being aligned perpendic-
ular to the bands was equal to 5.6 and 3.4 lm
before and after cold rolling, respectively. The rela-
tive change in pearlite band thickness of 40 pct
reduction is less than the macroscopic strain of
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 1—Initial microstructures before (a) to (c) and after 50 pct cold rolling (d) to (f): (a, d) furnace cooled (ferrite–pearlite), (b, e) as-received
(ferrite–bainite–pearlite), (c, f) water-quenched (martensite) (P: pearlite, F: ferrite).
50 pct. The strain partitioning is a common feature
observed during cold rolling of ferrite–pearlite
structures.[21] After the heat treatment the hardness
was 135HV and increased by 93HV to 228HV
after cold rolling.
(b) The microstructure of the as-received material con-
sisted of 5 vol pct of pearlite, with the rest being
either ferrite or bainite (F–B–P), Figure 1(b). No
attempt was made to differentiate the latter two
constituents because of their similar appearance in
the micrographs. Grain size of the ferrite/bainite
constituents before cold rolling was equal to 3 lm.
The hardness values were equal to 189 and 272HV
before and after cold rolling, respectively, corre-
sponding to a 83HV gain in hardness due to cold
rolling, Figure 1(e).
(c) After reaustenizing at 1173 K (900 C) for
1800 seconds and water quenching of the as-re-
ceived hot-rolled material, a martensitic micro-
structure was formed, Figure 1(c), with a hardness
of 378HV. This hardness falls within the range
from 340 to 380HV expected for martensite with
0.1 wt pct carbon[22] indicating that this third start-
ing microstructure can indeed be considered as lath
martensite (M). The martensite hardness increased
by 63HV to 444HV in the course of cold rolling,
Figure 1(f).
METALLURGICAL AND MATERIALS TRANSACTIONS A
Hereafter, the initial microstructures will be desig-
nated by their abbreviations, i.e., F–P, F–B–P, and M.
B. Recrystallization
Hardness of F–P and F–B–P decreased gradually in
the course of isothermal annealing, while M softened in
two stages, Figure 2. The first, rapid softening stage,
took place in less than 10 seconds, where the micro-
structure did not show any evidence of recrystallization.
The second stage led to a more gradual hardness
decrease. When recrystallization was complete after
long annealing times, a hardness of 145HV was mea-
sured for all the initial microstructures. Figure 3 shows
the metallographically measured values for recrystalli-
zation fraction as a function of holding time at 923 K
(650 C). The F–B–P initial microstructure had the
highest rate of recrystallization, the F–P material
required the longest times for recrystallization to be
completed, while M recrystallized at intermediate rates.
Similar trends were observed for the other investigated
holding temperatures as well as for recrystallization
during continuous heating at 1 K/s, as shown in
Figure 4. After recrystallization, all the microstructures
consisted of various arrays of carbide particles in a
ferrite matrix. For the F–P, starting material pearlite
partially spheroidized in the course of annealing, and
 450 Figure 5(a). Relatively coarse carbide particles were
Ferrite-Pearlite either clustered or arranged into linear arrays in the fully
400 Ferrite-Bainite-Pearlite
Martensite
recrystallized state resulting from the F–B–P initial
structure, see Figure 5(b). The clusters were formed
Vickers hardness

350
presumably at the former bainite or pearlite areas, while
300 the linear arrays could be a result of grain boundary
carbides in the cold-deformed structure. A finer and
250 more homogeneous distribution of carbides was found
200 after recrystallization from the M initial structure,
Figure 5(c). The ferrite grain size after recrystallization
150 completion was found to be independent of the anneal-
ing temperature and equal to 7.6, 5.1, and 6.5 lm for
100 F–P, F–B–P and M, respectively. It is noteworthy that
1
0 10 100 1000
recrystallization in F–B–P and M led to a coarser grain
Time, s
size, while in F–P the final grain size was lower than the
one before recrystallization.
Fig. 2—Hardness evolution during annealing at 923 K (650 C).

C. Austenite Formation
100
Ferrite-Pearlite The fraction of austenite formed as a function of
Percentage recrystallized, pct

90 Ferrite-Bainite-Pearlite temperature for the F–B–P initial microstructure is

80 Martensite shown in Figure 6(a) for continuous heating rates of 1,
70 10, and 100 K/s. The ortho- and para-equilibrium
60 austenite fractions are also shown as calculated with
Thermo-Calc using the FE-2000 database (Thermo-Calc
50
Software, Stockholm, Sweden). The austenite fraction as
40
a function of temperature appeared to be rather
30 independent of heating rate even though in none of
20 the cases equilibrium was reached for any given tem-
10 perature. Thus, the austenite formation rates increased
0
with heating rate, and this acceleration of austenite
0
1 10 100 1000 formation scaled in a first approximation with heating
Time, s rate. There was even a slight tendency that higher
heating rates can lower the transformation tempera-
Fig. 3—Recrystallization kinetics at 923 K (650 C) (Symbols corre- tures. Similar trends were observed for the other two
spond to experimental results, error bars represent 95 pct confidence initial microstructures: Temperatures needed to achieve
interval, lines are the JMAK models). 50 pct of austenite during continuous heating were
similar for all heating rates and in some cases (M, F–B–
P) appeared to be lower by about 10 K for higher
Temperature, K heating rates, Figure 6(b). Further, the austenite forma-
913 933 953 973 993 1013 1033
100 tion start temperature was for all continuous heating
Percentage recrystallized, pct

90 cases approximately 1003 K (730 C), e.g., Figure 6(a).

80 During holding at 1043 K (770 C) after slow heating
70
at 1 K/s, the rate of austenite formation was virtually
60
the same for F–B–P and M, while the F–P starting
microstructure took longer holdtimes to achieve the
50
same austenite volume fractions, Figure 7(a). As shown
40
in Figure 7(b), the rate of austenite formation was
30
accelerated in all the three starting microstructures when
20 Ferrite-Pearlite the heating rate to the intercritical temperature was
10 Ferrite-Bainite-Pearlite
Martensite
increased from 1 to 100 K/s. After heating at a rate of
0 100 K/s, the austenite volume fraction approached the
640 660 680 700 720 740 760 paraequilibrium austenite content after 1200 seconds
0
Temperature, C long holding.
During heating at 1 K/s, recrystallization was com-
Fig. 4—Recrystallization kinetics during continuous heating at 1 K/s pleted below 993 K (720 C) for all the three starting
(Symbols correspond to experimental results, error bars represent 95
pct confidence interval, lines are the JMAK models).
microstructures (see Figure 4), i.e., before austenite
formation starts. This was confirmed by direct metallo-
graphic observations of the early stages of austenite
clusters of cementite particles in the recrystallized formation in F–B–P, Figure 8(a). Austenite nucleated at
microstructure inherited the distribution and morphol- the boundaries of recrystallized ferrite grains in this case.
ogy of the former pearlite bands, as can be observed in A faster heating rate of 10 K/s shifted recrystallization

METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 5—Fully recrystallized microstructures after annealing at 873 K
(600 C): (a) ferrite–pearlite after 4020 s, (b) ferrite–bainite–pearlite
after 3000 s, (c) martensite after 3000 s (P: intact pearlite, SP:
spheroidized pearlite).
completion into the intercritical temperature region and
resulted in concurrent processes of recrystallization and
austenite formation. It was observed that unrecrystallized
regions were found to provide additional nucleation sites
for austenite, Figure 8(b). During heating at 100 K/s
austenite formation was found to initiate before the onset
of recrystallization. As a result, a dense and relatively
uniform distribution of fine martensite particles (i.e., the
former austenite grains) was observed in an unrecrystal-
lized ferrite matrix, as shown in Figure 8(c).
The different starting microstructures and the differ-
ent scenarios for the interaction between ferrite recrys-
tallization and austenite formation resulted in a variety
METALLURGICAL AND MATERIALS TRANSACTIONS A
of austenite morphologies and distributions. Figure 9(a)
illustrates that for the fully recrystallized F–P condition,
both pearlite bands and the boundaries of recrystallized
ferrite grains provided nucleation sites for austenite
while predominantly banded austenite was found when
austenite formed in unrecrystallized F–P, Figure 9(d).
The morphology and distribution of austenite formed in
F–B–P and M was similar. After recrystallization was
completed, austenite appeared along ferrite grain
boundaries and formed a continuous boundary net-
work, Figures 9(b) and (c). In unrecrystallized F–B–P
and M, a uniform distribution of fine nearly equiaxed
austenite particles was formed, Figures 9(e) and (f). The
resulting austenite grain size decreased with increasing
heating rate, see Table II.
To provide a comparison basis for analyzing the effect
of incomplete recrystallization on austenite formation,
step-heating experiments were conducted. Here, the
samples were first heated at 1 K/s to 973 K (720 C),
which is 10 K lower than the austenite formation start
temperature (as shown in Figure 6(a)), to provide
sufficient time for recrystallization to be completed and
then the heating rate was increased to either 10 or
100 K/s. This procedure permitted to study austenite
formation from a completely recrystallized microstruc-
ture for these higher heating rates. As an example,
Figure 10(a) shows the effect of heating rate on the
austenite formation kinetics from the fully recrystallized
condition for the F–B–P starting microstructure. In
contrast to the continuous heating experiments,
Figure 6(a), the transformation curves were shifted to
higher temperatures as heating rate increased as one
might have expected. Interestingly, the austenite forma-
tion rates as measured by the temperature required to
reach an austenite fraction of 10, 50 and 90 pct were
very similar for all the three starting microstructures, see
Figure 10(b). An increase of heating rate from 1 to
100 K/s resulted in an increase of transformation
temperature by 40 K. Moreover, the final austenite
grain size was found to decrease with heating rate but
the magnitude of this decrease was lower for the step-
heating cases than for the continuous heating experi-
ments, Table II.
IV. MODELING
A. Recrystallization Model
The Johnson–Mehl–Avrami-Kolmogorov (JMAK)
model[23–25] was employed to describe the recrystalliza-
tion kinetics, i.e., for the isothermal case:
X ¼ 1  expð0:693  ðt=t50 Þn Þ ½1
where X is the recrystallized volume fraction, t is time,
t50 is time needed to achieve 50 pct of recrystallization
and n is the JMAK exponent.
The temperature dependence of the parameter t50 is
expressed in the following form:
t50 ¼ ðt50 Þ0 expðQ=R  TÞ ½2
Fig. 6—Austenite formation kinetics during continuous heating: (a) in ferrite–pearlite–bainite, (b) temperature-heating rate map for 50 pct auste-
nization.

70 70
Paraequilibrium Paraequilibrium
Austenite content, pct

Austenite content, pct

60 60
Orthoequilibrium Orthoequilibrium

50 50

40 40

30 30

Ferrite-Pearlite Ferrite-Pearlite
20 20
Ferrite-Bainite-Pearlite Ferrite-Bainite-Pearlite
Martensite Martensite
10 10
0 200 400 600 800 1000 1200 0 200 400 600 800 1000 1200
Time, s Time, s
(a) (b)

Fig. 7—Austenite formation kinetics at 1043 K (770 C) after heating at (a) 1 K/s and (b) 100 K/s (symbols correspond to experimental results,
lines—to the JMAK model).

are in close agreement with the experimentally measured

with the pre-exponential factor, (t50)0, the effective activa-
tion energy, Q, while R and T have their usual meaning.
There are three adjustable parameters n, (t50)0 and Q
in this model. Based on the isothermal recrystallization
kinetics at 873 K, 898 K, and 923 K (600 C, 625 C,
and 650 C) separate sets of the fitting parameters were
obtained for each of the three starting microstructures,
Table III. The quality of the fit is shown in Figure 3.
The JMAK model in its differential form, i.e.,
 n1
n  ð1  XÞ ln ð1=1  XÞ n
dX=dt ¼ 0:693 
t50 0:693
and the additivity principle[26,27] were then used to
predict the recrystallization kinetics during continuous
heating at 1 K/s. As shown in Figure 4, the predictions
of the model for the F–P and M initial microstructures
recrystallization kinetics for continuous heating at 1 K/s,
however for the F–B–P material the model overesti-
mates recrystallization rates at the initial stages of the
process. The experimental and modeling results, Fig-
ure 4, are within ±7 K at all times and the models are,
thus, considered as a good representation of the
recrystallization process for all initial microstructures.
The overall conformity of the experimental and model-
ing results is consistent with the additive nature of the
recrystallization process. The recrystallization models
were subsequently applied to predict temperatures of
½3 recrystallization start and finish (here indicated by 10
and 90 pct of recrystallization, respectively) for contin-
uous heating at rates between 0.1 and 100 K/s to create a
temperature-heating rate recrystallization–austenite
formation map as seen in Figure 11. As heating
rate increases, the completion of recrystallization is

METALLURGICAL AND MATERIALS TRANSACTIONS A


Fig. 8—Early stages of austenite formation in ferrite–bainite–pearlite
during continuous heating to 1013 K (740 C) at (a) 1, (b) 10, (c)
100 K/s (M: martensite, NF: nonrecrystallized ferrite).
postponed to higher temperatures. The rate of recrys-
tallization is fastest in F–B–P and slowest in F–P, while
M recrystallizes at intermediate rates. The intercept of
the austenite formation start temperature of 1003 K
(730 C) during continuous heating and temperatures
required for recrystallization to be completed gives a
critical heating rate below which austenite will form in a
fully recrystallized microstructure whereas for heating
rates above this critical value, recrystallization and
austenite formation will, at least partially, take place
simultaneously. The critical heating rate is 3 K/s for F–P
and 7 K/s for F–B–P and M. The aforementioned
agreement between experimental and modeling results
within the margin of ±7 K translates into ~20 pct
METALLURGICAL AND MATERIALS TRANSACTIONS A
relative accuracy in determination of the critical heating
rates in Figure 11.
B. Austenite Formation Model
Austenite formation is a complex multistage process
involving austenite nucleation, dissolution of individual
carbide particles or pearlite colonies and ferrite-to-
austenite transformation. Moreover, the potential inter-
action of recrystallization and austenite formation adds
further complexity as the starting microstructure also
affects austenite formation when the two processes
overlap as discussed above. In the current study,
austenite formation was modeled for the fully recrystal-
lized microstructures by fitting the JMAK model to the
results of the step-heating experiments assuming addi-
tivity. Real austenite volume fractions were normalized
by the orthoequilibrium fractions, Eq. [4], for the
intercritical temperature region between 963 K and
1085 K (690 C and 812 C), i.e.,
feq
c ¼ 50  0:1033  T þ 0:0000536  T
2
½4
where T is temperature in K; the coefficients were
obtained from fitting to the Thermo-Calc predictions
shown in Figures 6(a) and 10(a).
The austenite formation start temperature (defined as
when fc/feq
c = 0.05 is reached) was expressed as a
function of heating rate using:
Ts ¼ A  qB ½5
where q is the heating rate; A and B are empirical fitting
parameters, Table IV.
The JMAK model parameters, Table IV, were
deduced from the results of the step-heating experiments
using the Rios method.[28] The JMAK model fit is in
excellent agreement with the results of the step-heating
experiments at 10 and 100 K/s, Figure 10(a), while for
heating at 1 K/s the model provides a good description
for the first 50 pct transformed but then overestimates
the austenite content for higher fractions. However, it is
worth noting that for intercritical annealing, the initial
portion of austenite formation (i.e., up to 50 pct) is
primarily of interest. The model predictions for austen-
ite formation after heating at 1 K/s and holding at 1043
K (770 C) for the three starting microstructures had
similar trends as the experimental results: austenite
formed at higher rates in F–B–P and M, than in F–P,
Figure 7(a). However, the model overestimates the
austenite content for the F–B–P and underestimates it
for the F–P initial microstructures, respectively. Never-
theless, the predicted austenite content is at all holding
times within ±5 pct of that measured in the experiments.
V. DISCUSSION
The three starting microstructures have different grain
sizes and different distributions of carbon. In F–P, carbon is
clustered in pearlite bands, and for M, carbon is uni-
formly distributed, while the F–B–P initial microstructure
Fig. 9—Austenite morphology after continuous heating to ~1033 K (760 C) at (a) to (c) 1 and (d) to (f) 100 K/s in (a, d) ferrite–pearlite, (b, e)
ferrite–bainite–pearlite, (c, f) martensite (M: martensite, F: ferrite).

Table II. Austenite Grain Sizes (lm)

Continuous Heating (K/s) Step Heating (K/s)

Material 1 10 100 1 to 10 1 to 100

Ferrite–Pearlite 9.2 5.8 5.5 7.1 5.4
Ferrite–Bainite–Pearlite 6.8 4.2 3.4 6.8 6.2
Martensite 8.3 6.3 3.5 6.4 5.4

represents an intermediate case in terms of carbon distri-
bution. These three materials cover the full spectrum of
structures which could be potentially used for cold rolling
and subsequent annealing.
For the ideal site-saturated nucleation and constant
three-dimensional growth conditions, the exponent n in
the JMAK model is equal to 3. The exponents found in
this study for recrystallization of the F–P and F–B–P
initial microstructures are equal to 1.4 and 1.7, respec-
tively, Table III, and close to the values typically
obtained for recrystallization of cold-deformed iron
and steels.[14,29,30] The difference in the ideal and
measured exponents is because the simplifying assump-
tions of the JMAK model (homogeneous nuclei distri-
bution, site saturation or constant nucleation rate,
constant and isotropic growth rate) are not fulfilled
during recrystallization due to the time- or spatial
dependence of the nucleation and growth rates, see
Reference 31. However, the exponent for M is the
highest among the three microstructures studied here
and approaches the ideal value of 3; this indicates a
more homogeneous structure of M compared with the
other two initial microstructures. The activation energy,
Q, representing in a first approximation the average
activation energy for the migration of high-angle grain
boundaries, Table III, was found to be nearly constant
for the three starting microstructures with the average of
375 kJ/mol being similar to 330 kJ/mol found for
another steel with a typical DP 600 chemistry (Fe-
0.06C-1.86Mn-0.16Mo).[14]
The following simple physical model is proposed to
explain the observed recrystallization rates in different

METALLURGICAL AND MATERIALS TRANSACTIONS A

Fig. 10—Austenite formation kinetics during the step-heating experiments (a) in ferrite–bainite–pearlite (symbols correspond to experimental re-
sults, lines—to the JMAK model), (b) temperature-heating rate austenization map (dashed lines are trendlines).

Table III. Recrystallization Model Parameters  1

p  d3
Microstructure n (t50)0 (s) Q (kJ/mol) N¼ ½7
6
18
Ferrite–Pearlite 1.7 6.7 9 10 342
Ferrite–Bainite–Pearlite 1.4 2.9 9 1020 377 where d is the average ferrite grain size after recrystal-
Martensite 2.5 2.7 9 1021 398 lization completion.
The growth rate of a recrystallizing grain is equal to
the product of grain boundary mobility, M, and driving
pressure, P:
V¼MP ½8

The mobility of high-angle grain boundaries can be

assumed to be the same for all the three initial
microstructures. While the driving pressure for recrys-
tallization is the stored energy having two components:
the energy stored during phase transformations before
cold rolling, PTransformation, and the stored energy due to
the deformation, PDeformation:
P ¼ PTransformation þ PDeformation ½9

To estimate the driving pressure, the relative softening

Fig. 11—Temperature-heating rate recrystallization–austenite forma-
tion map.
starting microstructures. Recrystallization proceeds
through nucleation and growth. Assuming site satura-
tion conditions and three-dimensional growth, the
recrystallized volume fraction is equal to:
X ¼ 1  expðN  ðV  tÞ3 Þ
where N is the nuclei density and V is the growth rate.
Since annealing temperatures are comparatively low
[£923 K (650 C)], no substantial ferrite grain coarsen-
ing is expected such that the nuclei density can be
assumed to be equal to:
during annealing in all the three initial microstructures
was considered:
H0  H
S¼ ½10
H0  HRex
where H0, H, and HRex are the microhardness values of
the as-deformed, partially recrystallized, and fully
recrystallized materials, respectively.
For the F–B–P initial microstructure, the relative
½6 softening was in a close agreement with the recrystal-
lization percentage as shown in Figure 12. Therefore,
the total hardness change in the course of annealing can
be assumed to be due to the dislocation density decrease,
Dqdis, neglecting all other possible factors affecting
hardness, e.g., grain size, different inherent hardness of
different microconstituents, etc.:

METALLURGICAL AND MATERIALS TRANSACTIONS A

 Table IV. Austenite Formation Model Parameters

Transformation Start
Temperature (K) (Eq. [5]) JMAK Parameters
1B B
Microstructure A (K Æs ) B n (t50)0 (s) Q (kJ/mol)
56
Ferrite–Pearlite 1008 0.0087 0.29 1.4 9 10 1155
Ferrite–Bainite–Pearlite 1008 0.0104 0.44 1.3 9 1041 843
Martensite 1015 0.0090 0.42 2.8 9 1045 921

100 fragmentation of cementite lamellas thereby promoting

pearlite spheroidization upon subsequent anneal-
90
ing.[13,17] Even in the fully recrystallized microstructure
80 of F–P, unspheroidized areas can still be found, as
70
shown in Figure 5(a). Spheroidization took place con-
currently with recrystallization, and therefore, it is
Softening, pct

60 rather challenging to discriminate their individual effects

50 on hardness changes. However, for 0.1C (wt pct) plain
carbon steel complete spheroidization of fine pearlite
40
leads to ~20HV hardness decrease,[32] while total soft-
30 ening for the F–P initial microstructure during isother-
20
mal annealing was 82HV in the current study.
Ferrite-Pearlite
Therefore, the hardness changes are primarily due to
10 Ferrite-Bainite-Pearlite
recrystallization, and Eq. [14] can still be applied for an
Martensite
0 order of magnitude estimate of the stored energy for
0 10 20 30 40 50 60 70 80 90 100 F–P. Finally, turning to the case of M, during cold
Recrystallized percentage, pct deformation of a low-carbon martensite, laths are
replaced with dislocation cell structures.[33,34] Upon
Fig. 12—Comparison of relative softening estimated using hardness subsequent annealing, the hardness of M dropped by
changes and recrystallized percentage quantified through metallo- ~150HV within the first 10 seconds without any evi-
graphic measurements.
dence of recrystallization, Figure 2. This initial soften-
ing was ascribed to the martensite tempering. Greater
annealing times result in a gradual hardness decrease
P  0:5  G  b2  Dqdis ½11 through recrystallization of tempered M. Typically high
temperature anneals, such as those used for the recrys-
where G is the shear modulus of iron, equal to 83 GPa; b
tallization experiments in the current study, lead to
is the magnitude of Burger’s vector, equal to 0.25 nm.
extremely rapid tempering. For instance, Caron and
The dislocation density decrease is related to the yield
Krauss[35] found, in Fe-0.2C martensite, a hardness drop
strength change, Dry:
of 50 pct due to carbide precipitation after a 0.26-second
pffiffiffiffiffiffiffiffiffiffiffi
Dry  0:5  G  b Dqdis ½12 heat treatment at 923 K (650 C). Thus, tempering was
assumed to take place first, followed by recrystallization
for the M initial microstructure. The hardness achieved
In a first approximation, the yield strength change (in after the first 10 seconds of annealing is assumed to be
MPa) is equal to one third of the Vickers hardness drop, the initial hardness for the estimates of the stored energy
DH (in MPa): to separate this from the tempering effect. Based on
Dry  DH=3 ½13 these arguments, the estimated values for the nuclei
density and stored energy are summarized in Table V.
They are the lowest for the F–P initial microstructure.
The stored energy is thus proportional to the square The M microstructure possessed the highest stored
of the hardness change for the F–B–P initial micro- energy, while the highest number of nuclei formed
structure: during recrystallization of F–B–P.
The average nuclei density and stored energy repre-
2
P DH2 ½14 senting an average microstructural compartment were
9G used to estimate ratios of characteristic times required
for 50 pct recrystallization, t50, for different initial
Only a fraction of the softening for F–P and M can be microstructures using Eqs. [6], [7], [14]:
attributed to recrystallization, as other processes also
lowering hardness took place in these materials, Fig- d
ure 12. In F–P, the additional softening mechanism is t50 / ½15
pearlite spheroidization. Cold-deformation leads to DH2

METALLURGICAL AND MATERIALS TRANSACTIONS A

Table V. Nuclei Density and Stored Energy for Recrystalli- the nuclei density at the beginning of the transforma-
zation tion, more nuclei were formed during faster heating in
the step-heating experiments, Table II. Nucleation and
Nuclei growth are competing phenomena. Higher heating rates
Density Stored Energy
Initial (1015 m3) (MPa)
lead to less growth of nuclei at any given temperature
Microstructure (Eq. [7]) (Eq. [14]) and promote additional nucleation at higher superheat-
ing.
Ferrite–Pearlite 4.4 1.8 As shown in Figure 11, for continuous heating
Ferrite–Bainite–Pearlite 14.4 4.2 experiments at a rate above the critical value, austenite
Martensite 7.0 5.3 forms in a partially recrystallized microstructure. Con-
sidering that during continuous heating at 1 and 100 K/s
austenite forms within the same temperature range of
1003 K to 1123 K (730 C to 850 C) and taking into
Table VI. Ranking of the Initial Microstructures Based on
Recrystallization Rates account the hundredfold difference in time available for
the transformation, Figure 6(a), the rate of austenite
Ratios of Times for formation in unrecrystallized material is accelerated by
50 Pct Recrystallization more than one hundred times. Comparison of austenite
formation kinetics during continuous and the step-
Based on heating experiments reveals that the presence of unre-
Hardness JMAK crystallized regions lowers the transformation start
Ratio of Change and Models temperatures during heating at 10 and 100 K/s for all
Initial Grain Size [T = 973 K
initial microstructures by approximately 20 and 40 K,
Microstructures (Eq. [15]) (700 C)]
respectively, e.g., compare Figures 6(a) and 10(b). The
M/FBP 1.0 1.3 recrystallization–austenite formation interaction also
M/FP 0.3 0.4 affects austenite nuclei distribution and density as can
FBP/FP 0.3 0.3 be seen in Figures 8 and 9. Employing the final austenite
grain size as a measure of the nuclei density, as much as
six times more nuclei were formed during the continuous
heating than during the step-heating experiments for a
given heating rate (see Table II). These observations are
The obtained ratios of annealing times needed to consistent with previous studies on the recrystallization–
reach 50 pct of recrystallization for different initial austenite formation interaction, where preferential
microstructures, Table VI, replicate the experimentally nucleation of austenite in unrecrystallized regions was
observed trends suggesting similar recrystallization rates reported.[13,15–17]
for F–B–P and M initial microstructures, and longer The higher austenite nuclei densities in partially
times required for F–P recrystallization. Moreover, the recrystallized microstructures can be explained with
ratios of times for 50 pct recrystallization are similar to the aid of the classical nucleation theory. The activation
those calculated using the JMAK models, i.e., Eq. [2] barrier for nucleation, DG*, is lowered by increasing the
and Table III. driving pressure for austenite formation, DgV, by the
To rationalize the observed trends for austenite magnitude of the stored energy, P, otherwise released in
formation, nucleation and growth also need to be the course of recrystallization:
considered. Two conditions must be met for the
nucleation to take place. First of all, according to the SðhÞ
DG / ½16
iron–carbon phase diagram, carbon solubility in aus- ðDgV þ PÞ2
tenite is much higher than in ferrite, and austenite nuclei
will form at carbon rich sites. Second, classical nucle- where S(h) is the shape factor (0 < S < 1) that is related
ation theory predicts preferred nucleation at high-energy to the benefits of heterogeneous nucleation sites in
nonequilibrium defects, which lower the activation lowering the activation barrier.
barrier for nucleation, i.e., heterogeneous nucleation. For instance, at the austenite formation temperature
For a distribution of cementites in ferrite matrix, such as of 1003 K (730 C), the chemical driving pressure for
fully recrystallized F–B–P and M, Figures 5(b) and (c), the nucleation is equal to 82 MPa under orthoequilib-
both conditions are met for cementite particles located rium conditions based on the Thermo-Calc prediction,
at ferrite grain boundaries as observed experimentally, while the stored energy varies between 1.7 MPa for the
Figure 8(a). In fully recrystallized F–P, preferable F–P initial microstructure and 5.3 MPa for M, Table V.
nucleation sites for austenite are F–P interfaces at the An additional contribution of 5 MPa is equivalent to a
beginning of the transformation, while ferrite grain 10 K temperature drop for the same magnitude of
boundaries become active nucleation sites at later driving pressure of 82 MPa for the nucleation. Local
transformation stages, this being observed in as- variations in the stored energy could also magnify the
quenched samples with different contents of martensite, effect of the stored energy on the austenite nucleation.
i.e., austenite at an intercritical temperature. Assuming Moreover, the quality of nucleation sites as quantified
that the density of austenite grains after the transfor- by the shape factor in Eq. [16] is also improved in
mation completion provides some indication of trends in deformed material thereby lowering the energy barrier

METALLURGICAL AND MATERIALS TRANSACTIONS A

for the nucleation even further. The combination of the
lower activation energy for the nucleation and the
higher density of potential nucleation sites increases the
nucleation rate in partially recrystallized or unrecrystal-
lized material.
However, the enhanced nucleation alone cannot
account for the observed increase in the transformation
rate, i.e., the growth rate changed dramatically as well.
Considering again the case of austenite formation
during continuous heating at 1 or 100 K/s between
1003 K and 1123 K (730 C and 850 C), Figure 6(a),
the ratio of the final austenite grain sizes was approx-
imately equal to two, see Table II. Taking into account
the hundredfold difference in the transformation time,
the average velocity of austenite–ferrite interface during
the fast heating is estimated to be accelerated by at least
50 times. Further, austenite grain coarsening may have
taken place and its extent will be more pronounced
during slow heating. Then, the growth rate increase
would be even greater than 50 times. One possible
explanation for the fast austenite growth in non-recrys-
tallized microstructures may be related to the presence
of fast diffusion paths for substitutional alloying ele-
ments in the deformed ferrite. The enhanced diffusion of
austenite stabilizing elements such as manganese toward
the ferrite–austenite interface may accelerate austenite
formation. The fast growth rate could be even further
amplified by reduced solute drag.[36–38] Solutes exert
lower pressures on a boundary moving rapidly, this
leading to its apparent mobility increase.
Another consequence of the fast austenite formation
during rapid continuous heating is an inhomogeneous
carbon distribution after complete austenization. For
heating at a constant rate, the carbon diffusion distance
can be estimated from:
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
T2  T1
L ¼ DcC  ½17
q
where T1 = 1003 K and T2 = 1223 K (730 C and
850 C, respectively) are temperatures for the austenite
formation initiation and completion during heating at a
rate q = 1 or 100 K/s, DcC is the average carbon
diffusion coefficient in austenite for this temperature
range.[39] The carbon diffusion distance in austenite
decreases from 14 to 1.4 lm when the heating rate is
increased from 1 to 100 K/s, i.e., the diffusion distance
in the latter case is smaller than the radius of the
austenite grain, Table II.
The through-thickness manganese distribution is not
uniform in the industrially produced steel sheets as
evidenced by the banded structure of pearlite in F–P,
Figure 1(a). The variation of manganese content is
typically inherited from casting and remains unaffected
by the laboratory reaustenitization heat treatment at
1173 K (900 C) for 1800 seconds in the current study,
as much higher soaking times and temperatures for the
homogenization treatment are typically employed. The
nonuniform distribution of manganese leads to pearlite
banding in F–P, whereas there are no obvious signs of
banding in the other two initial microstructures (F–B–P,
and M). As a result, intercritical annealing of the F–P
initial microstructure leads to the development of the
banded austenite, Figures 9(a) and (d). Primarily
because of its higher carbon concentration, pearlite
serves as a preferential site for austenite nucleation and
growth. In the F–B–P and M materials, carbon is more
uniformly distributed, and manganese segregation, in
the current case, does not have any major effect on
austenite nucleation and morphology.
VI. CONCLUSIONS
It was found that the 50 pct cold-rolled ferrite–
bainite–pearlite (F–B–P) and martensite (M) initial
microstructures recrystallized at nearly the same rates,
while slower recrystallization was observed in ferrite–
pearlite (F–P) microstructure. The effect of initial
microstructure on austenite formation kinetics was
nearly completely eliminated when recrystallization
was completed before austenite formation starts. Upon
heating to an intercritical temperature at a rate higher
than a critical value (3 to 7 K/s for the initial micro-
structures examined here), the interaction of recrystal-
lization and austenite formation was observed. Shorter
holding times are needed after faster heating (provided
heating rate exceeds the critical value) to reach the
desired austenite content. Martensite morphology in DP
steels can be controlled by variation of either the initial
microstructure or through the interaction of recrystal-
lization and austenite formation. Moreover, substantial
microstructural refinement can be achieved by forming
austenite in unrecrystallized F–B–P and M initial
microstructures.
Recrystallization and austenite formation in fully
recrystallized microstructures were successfully de-
scribed by means of the JMAK model. Limitations of
this approach were found for conditions when recrys-
tallization was not fully completed before austenite
formation and starting microstructures were essentially
a function of heating rate, thereby affecting austenite
nucleation and growth rates. A more advanced model,
for example, based on the phase-field approach, needs to
be developed for an accurate description of the recrys-
tallization–austenite formation interaction and the
observed variety of austenite morphologies.
ACKNOWLEDGMENTS
The authors acknowledge the financial support
received from the Natural Sciences and Engineering
Research Council of Canada (NSERC) and Arcelor-
Mittal Dofasco Inc. (Hamilton, ON, Canada). The au-
thors further wish to thank CanmetMATERIALS
(Hamilton, ON, Canada) and personally Fateh Fazeli
for the opportunity to use the Bähr dilatometer. Stim-
ulating discussions with Benqiang Zhu are greatly
acknowledged.
METALLURGICAL AND MATERIALS TRANSACTIONS A
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