evidence the correlation of grain size and properties of
dual phase steels. A finer grained microstructure improves
New Thermomechanical Hot Rolling
Schedule for The Processing of High
Strength Fine Grained Multiphase Steels
A. Schmitz, J. Neutjens*, J.C. Herman, and V. Leroy
CRM, Rue E. Solvay, 11, B-4000 Liège, Belgium,
*
currently at RDCS, Bvd de Colonster, B57,
B-4000 Liège, Belgium
+32-4-254.62.97
ABSTRACT
The present paper deals with the metallurgical
aspects of microstructural evolution of austenite prior to
its transformation to ferrite during continuous cooling.
The optimization of the processing route in terms of
chemistry and rolling schedule is carried out by means of
hot compression and torsion tests. The control of austenite
recrystallization during the multipass deformation and the
subsequent phase transformation provides fine grained
ferrite-martensite microstructure. The combined use of a
new thermomechanical rolling schedule with an
appropriate continuous cooling down to martensite start
temperature allows to produce a high strength level (750
MPa) based on a C-Mn-Nb steel chemistry which exhibits
a very attractive resistance-ductility balance, a high
toughness as well as interesting fatigue properties in the
as hot-rolled condition.
1. INTRODUCTION
Fuel economy and safety considerations constitute
the driving force for the increasing demand of higher
strength steels in the automotive industry. Concurrently
with the use of microalloyed strip and sheet, dual phase
steels whose microstructure is a mixture of ferrite and
martensite are known to provide a good combination of
strength and ductility(1). As hot-rolled, dual phase steels
are now accepted for automotive wheel disks because
their cost and property performances are superior to those
of heat treated dual phase steels. Maid et al(2) have put in
the elongation and tensile properties. As shown by Sudo
et al(3), the grain refinement is also beneficial for better
hole expansivity, sufficient for application. Furthermore,
wheel disks produced from fine grained dual phase steels
exhibit superior fatigue life when compared to the
microalloyed pearlite reduced steel grades of the same
tensile strength level(4).
Different rolling schedules have been developed to
produce microalloyed steels with ultrafine grain size, each
of them being characterized by the way the austenite is
prepared before the phase transformation to ferrite on the
run-out table. The addition of Mo, Nb or Ti influences
both static and dynamic recrystallization during hot
deformation of austenite. Static recrystallization occurs
in all steels with low alloying levels and high
temperatures, and the austenite grain size is reduced
through repeated static recrystallization between the
different stands of a finishing train. This leads to the
recrystallization controlled rolling process (RCR). If there
is sufficient strain-induced precipitation of the micro-
alloying elements, neither static nor dynamic recrystalli-
zation can take place and the austenite grains become
pancaked through the finishing process. The pancaked
austenite grain structure is the basis for conventional
controlled rolling (CCR). When Mo, Nb or Ti are in
solution in steels, static recrystallization is retarded. If the
interpass times are short enough, the strain is accumulated
from pass to pass in the absence of large amount of strain-
induced precipitation up to the initiation of dynamic
recrystallization. In their study of dynamic recrystal-
lization controlled rolling (DRCR) of strips, Samuel et
al(5) have observed that this process produces fine grained
austenite (below 5µm) and ferrite grain sizes of about
3µm when cooling rate is 10°C/s. On the other hand, the
pancaked austenite obtained by the CCR route leads to ~
7µm ferrite grain size after cooling.
From the similar results of Kaspar et al(6), the
dynamic recrystallization controlled rolling seems thus the
most performant route to refine the ferrite grain size.
Bowden et al(7) have subsequently studied the effect of
interpass time on austenite grain refinement in presence of
dynamic recrystallization. The possible metadynamic
recrystallization which is expected to take place after
initiation of dynamic recrystallization during the
subsequent interpass times has been analyzed and
modelled by Roucoules et al(8), and extended later to
other alloying elements(9).
ISS Technical Paper, A. Schmitz Page 1 of 14
 To achieve an appropriate microstructure in hot- 2. EXPERIMENTAL PROCEDURE
rolled dual phase steels, first alloy concepts were based on
Mn, Si, Cr and Mo alloyed steels(10). Owing to the rather Experiments were conducted in three phases. First,
high alloy content, these steels were expensive and static recrystallization kinetics was analyzed by compres-
alternative grades have been proposed with an optimized sion tests which simulate the critical interstand of a
stepwise cooling down to a low coiling temperature(11). finishing train. Next, the dynamic recrystallization
The principal disadvantage of these complex thermal behaviour of the different steels was evaluated up to large
paths on the run-out table lies in the regulation of the deformation by means of torsion tests. Finally, an
cooling system to ensure a constant thermal profile along optimized rolling schedule was tested at the laboratory
the length of the coil. Without any coil-box prior to scale.
finishing, this problem is amplified by the speed-up which
is necessary to obtain a constant temperature at the exit of
the finishing train. Non homogeneous microstructure with 2.1. Materials
varying amounts of ferrite along the length of the coil
results from the sensitivity of this rolling schedule to the The chemical compositions of the grades chosen to
process parameters. Another rolling procedure has been carry out this study are presented in Table I.
put forward by Mizui and Takahashi(4) in which low-
carbon Si-Mn steels containing no other alloying elements Table I Chemical composition (10-3wt.%) of the
are hot-rolled at temperatures slightly below the Ar3 experimental Nb-containing steels
transformation temperature. This helps to accelerate the
ferrite formation and a continuous rapid cooling leads to Steel C Si Mn P S Ti Al Nb N
a fine grained dual phase steel. However, this solution 1 87 75 1570 16 7 18 37 4 5
suffers from the loss of ductility related to the fact that 2 81 121 1378 14 5 17 44 17 5
ferrite is slightly strain hardened. 3 82 123 1533 15 6 21 45 34 5
4 87 130 1533 16 6 22 34 53 5
The key idea of the present work combines the grain 5 82 124 1410 15 6 22 49 83 4
refinement of austenite by means of dynamic
recrystallization with the resulting enhanced transfor- To promote the initiation of dynamic recrystal-
mation kinetics in order to produce a dual phase steel by lization, the finishing rolling must be performed below a
a continuous cooling to room temperature. Some results temperature Tnr for which no static recrystallization is
of Kaspar et al.(12) seem indeed to indicate the presence of expected to occur between the interstands, and above the
high-carbon constituent in the microstructure as well as transformation temperature Ar3 to ensure deformation in
the absence of a sharp yield point, the both effects being the austenitic temperature range. From a practical point of
characteristic of a dual phase steel. view, the temperature range between Tnr and Ar3 must be
sufficient to enable a rolling schedule on an industrial
The aim of this work is the optimization of the line. This range is spread by means of an addition of Mn
process in terms of chemistry and rolling schedule to to lower Ar3 and different levels of Nb to increase Tnr.
achieve a fine grained dual phase steel by a continuous From the different atoms which retard static
cooling. A systematic study of the effect of different recrystallization by the solute drag effect, Nb constitutes
amounts of microalloying element on the kinetics of the best candidate in the austenitic temperature range(13).
static and dynamic recrystallization is carried out in Its effect on final refinement of ferrite grain size is
parallel with the influence of rolling parameters such as systematically analyzed for different contents ranging
the rolling temperature, the amount of cumulative strain from 0 to 83 10-3wt.%. Finally, Ti is added to remove N
and the interpass time. An optimized process is proposed in solution by the formation of TiN precipitates which
and the mechanical properties are evaluated on an as hot- also inhibit grain growth at high reheating temperatures.
rolled strip elaborated in laboratory. The steels were cast and hot-rolled to plates of 25mm and
12.5mm final thicknesses at the CRM pilot line plant.
Compression samples of 20mm in diameter and 20mm in
height were machined out of the 25mm plates. Torsion
test specimens with a gage length of 24mm and a diameter
of 6mm were machined from the 12.5mm hot-rolled plate
with the orientation along the transverse direction.

ISS Technical Paper, A. Schmitz Page 2 of 14

2.2. Double-hit compression tests
To study the progress of static recrystallization
during finishing rolling, several sets of double-hit
compression tests were conducted on the CRM
computerized MTS servohydraulic press. The specimens
were austenitized at 1250°C for 20 min which ensures
complete dissolution of Nb precipitates, and then slowly
cooled (~1-2°C/s) to the testing temperature (850, 900,
950, 1000 and 1050°C). They were subsequently hot
compressed to a true strain of 0.5 at a strain rate of 1/s.
After a constant unloading time of 5s, the specimens were
reloaded at the same strain rate. The load-contraction data
were converted into true stress σ and true strain ε, and the
degree of softening X during the unloading period was
fitted with the help of the first σ1 and second σ2 loading
curves on the basis of the mixture low :
σ2 (ε) = X . σ1 (ε - 0.5) + (1 - X) . σ1 (ε)
2.3. Hot torsion tests
To investigate the softening behaviour up to large
deformation and the resulting refinement of ferrite grain
size, torsion tests were carried out on the CRM hot-
torsion machine equiped with an induction heating. After
austenitization at 1250°C for 300s, the specimens were
cooled down at 5°C/s to 1100°C and subjected to a first
roughing strain of 0.5 at 1/s to refine the austenitic grain
size. They were subsequently cooled to the test tempera-
ture at 5°C/s. True stress and true strain were derived
from the torque-twist data using the method of Gräber and
Pöhland(14) at the critical radius for a solid specimen.
Isothermal torsion tests were performed at strain rate of
1/s and at temperatures ranging from 1000°C down to
850°C. Different types of torsion tests were carried out :
(a) The dynamic recrystallization behaviour was obtained
for different Nb content from continuous curves up to
a strain of 3 which is representative of the cumulative
strains observed on industrial lines.
b) The effect of interpass time was evaluated for the 83
10-3wt.% Nb steel for which strain-induced precipi-
tation is expected to take place.
c) Interrupted torsion tests at various strain levels were
performed to examine the influence on ferrite grain
size.
The influence of the different austenite
microstructures generated by the various rolling schedules
on the ferrite grain refinement was analyzed after the
austenite to ferrite transformation during continuous
cooling to room temperature at a cooling rate of 20°C/s
characteristic of most laminar cooling systems on the run-
out table. Metallographic samples were polished and
etched in a Marshall solution to reveal the ferrite grain
boundaries or in a Lepera solution to put high-carbon
constituents in evidence. The retained austenite was
detected by X-ray diffraction using Mo-K
radiation.
2.4. Laboratory scale hot-rolling simulation
From the above process analysis, an optimized
chemistry and rolling schedule was proposed and tested
on the instrumented CRM pilot scale rolling mill.
Mechanical properties were determined from flat tensile
specimens (5 x 20 x 150 mm³) and low temperature
toughness was evaluated from Charpy specimens (5 x 10
mm² fracture section) machined out of the strip. The
fatigue properties of this dual phase steel were measured
by means of strain controlled fatigue tests. The tests were
performed on a MTS closed loop system at a strain ratio
of R = -1, and at a frequency of 0.3 Hz with specimens of
20mm in gauge length and 6mm in width.
3. RESULTS
3.1. Static softening during interpass time
Figure 1 shows the thermal profile computed by the
STRIPCAM program(15) which simulates the rolling of a
transfer bar of 28mm thickness down to 3mm on an
industrial finishing train. The corresponding equivalent
strain reaches 2.9 value in this case. Due to the natural
heat losses by convection and radiation between the
stands, the mean temperature of the strip continuously
decreases throughout the train. In parallel, a decreasing
interpass time IPT translates the mass flow continuity
which is characteristic of the plastic deformation of
metals.
From the point of view of kinetics of static
recrystallization, the most critical interstand is located
between stands 1 and 2 where the highest temperatures
and the longest interpass times are observed.
ISS Technical Paper, A. Schmitz Page 3 of 14
 TEMPERATURE PROFILE IN ROLLING (°C)
recrystallization is only initiated in the Nb free steel at the
highest temperature (1050°C). While in that case
1000 metadynamic recrystallization is supposed to take place,
the other Nb steels never exhibit dynamic recrystallization
under the simulated conditions.
960

Mean
1/2 thick.
The softening curves as function of the temperature
920 1/4 thick. of pre-deformation are illustrated in figure 3 for the
1/8 thick.
1/16 thick. different Nb content.
880
IPT = 5.4 s IPT = 3.3 s IPT = 2.1 s IPT = 1.4 s IPT = 1.0 s
STATIC RECRYSTALLIZATION KINETICS

840 1
370 375 380 385
Strain=0.5
Time since exit of furnace (s) 1/s
0.8
IPT=5 s
Fig.1. Thermal profile through the strip thickness

Relative softening X
simulated for an industrial finishing train 0.6
0
17
34
One can assume that static recrystallization will become 53
0.4
more and more difficult downwards in the train, and only 83

the thermomechanical conditions prevailing in the

0.2
interstand 1-2 will be retained here for the softening study
by means of compression tests. A first strain of 0.5 is
0
applied to the samples, which corresponds to the mean 800 850 900 950 1000 1050 1100
strain value observed at the stand 1 of the train. An Temperature (°C)
interpass time of 5s is adopted in this study. Fig.3. Softening curves of the C-Mn and Nb steels
corresponding to 5s unloading time (Nb content
The static recrystallization behaviour of the different in 10-3 wt.%)
Nb content steels are compared at 950°C in figure 2.
Below 850°C, recrystallization is essentially arrested in
DOUBLE HIT COMPRESSION TEST
all steels and strain accumulation is thus expected to take
950 °C - IPT = 5 s place under strip rolling conditions even for Nb free steel.
200
While some softening is observed at 900°C for the C-Mn
steel, the addition of 0.017 percent of Nb is enough to
160
prevent static recrystallization to appear between the two
first stands. The increase of the entry temperature to
Stress (MPa)

0
120
17 950°C necessitates a Nb level of more than 0.034 percent
34
53
to ensure complete strain accumulation while static re-
80
83 crystallization is complete for C-Mn steel. At 1000°C,
1/s only the 0.083%Nb steel is able to cumulate the defor-
40
mation whereas for temperatures higher than 1050°C,
static recrystallization seems unavoidable for all the steels
0
0.00 0.20 0.40 0.60 0.80 1.00 tested in the work.
Strain

Fig.2. Double-hit compression tests on Nb-containing

steels for the critical interpass time of 5s (Nb 3.2. Dynamic softening up to large deformation
content in 10-3wt.%)
The torsion curves for the different Nb steels
During the prestrain, only positive slopes are observed at deformed at 950°C are presented in figure 4.
950°C, and this corresponds to the dynamic recovery
regime on which Nb has a slight effect by solid solution
(around 83 percent increase of the flow stress per added
weight percent of Nb). After a prestrain of 0.5, dynamic

ISS Technical Paper, A. Schmitz Page 4 of 14

 TORSION TEST
levels while it seems to saturate for higher alloying levels,
950 °C especially at the low temperature (850°C).
200

The figure 6 illustrates the effect of the interpass

160
time on the softening behaviour during multipass
deformation at 900°C of steels with three levels of Nb
Stress (MPa)

120 0 Nb
17 Nb content.
34 Nb
80 83 Nb TORSION TEST
1/s 900 °C - IPT=10s
200
40
1/s
0 160
0.00 1.00 2.00 3.00 4.00

Stress (MPa)
Strain 120
0 Nb
Fig.4 Torsion flow curves for different Nb steels 17 Nb
83 Nb
80
tested at 950°C and a strain rate of 1/s (Nb
content in 10-3 wt.%)
40
All the steels work harden to a maximum at the peak
strain εp and then soften to eventually reach a plateau with 0
an approximatively constant flow stress. This softening is 0.00 1.00 2.00 3.00 4.00

attributed to the dynamic recrystallization which spreads Strain

during straining up to completion at the steady-state
stress. Nb addition has a marked retarding effect on the
kinetics of dynamic recrystallization by shifting the peak
strain to larger values. In the case of the 0.083%Nb steel,
the importance of the peak strain shift is such that no
complete dynamic recrystallization is seen even up to a
strain of 3. On the other hand, Nb slightly influences the
level of the steady state stress once it is reached.
DYNAMIC RECRYSTALLIZATION KINETICS
2.4
1/s
2 envelope of the individual curves is noticed, which can be
Peak strain
Fig.6 Interrupted stress-strain curves at 900°C for
different Nb content with an interpass time of
10s (in 10-3 wt.%)
The C-Mn flow curve exhibits a rounded shape for the
individual curves which remain at approximatively the
same level. This can be explained from the compression
tests (fig.3) since an interpass time of 10s should be
enough for complete static recrystallization of a C-Mn
steel at 900°C. In sharp contrast to Nb free steel, complete
strain accumulation from pass to pass is observed for the
0.083%Nb steel. Furthermore, no softening of the
translated into a complete pancaking of the microstruc-

0
17
ture. Such an amount of Nb thus prevents static and
1.6
34 dynamic recrystallization by solid solution and probably
83
also by strain-induced precipitation of Nb that can take
1.2 place during the 10s delay for this high alloying content.
An intermediate situation is given by the 0.017%Nb steel
for which the overall stress level for the first two passes is
0.8
800 850 900 950 1000 1050
the same than for the 0.083%Nb case, but followed by a
Temperature (°C) decrease of the mean stress for the subsequent deforma-
Fig.5 Dependence of the peak strain on the tempe- tion steps. After the first pass, the holding period is too
rature for different Nb content (in 10 -3 wt.%) short for static recrystallization in agreement with the
compression test (Fig.3) of the 0.017% Nb steel.
The strains corresponding to the peak stress are reported
in figure 5 as function of the temperature of deformation.
Despite the decrease of the peak strain with the tempe-
rature, a lower bound of strain of 0.8 has to be obtained to
observe dynamic softening in any steel under 1000°C.
The retarding sensitivity to Nb is pronounced at low

ISS Technical Paper, A. Schmitz Page 5 of 14

Consequently, the strain accumulates up to the initiation
of dynamic recrystallization. This is possible since Nb
certainly does not precipitate at this Nb level and retards
dynamic recrystallization by the solid solution effect. The
subsequent softenings have to be related to the fast
metadynamic recrystallization which takes place within
10s after initiation of dynamic recrystallization.
T O R S IO N T E S T
9 0 0 °C - 1 /s
200
160
S tress (M P a)
120
80
40
0
0 .0 0 1 .0 0
S train
Fig.7 Influence of the Nb content after straining at 900°C and on the as-cooled microstructure
(Marshall etchant)
3.3. Influence of the rolling parameters on the
microstructure
The effect of Nb content on the grain refinement is
displayed in figure 7 in which the flow curves at 900°C
are presented with the corresponding ferrite micro-
structure after cooling down to room temperature at
20°C/s. The sensitivity of ferrite grain size to the Nb
content is already marked for low Nb level such as
0.017%. While complete dynamic recrystallization is
noticed for the C-Mn and 0.017% Nb steels, the finest
grain size of around 2-3µm is obtained in the case of the
0.083%Nb steel which does not recrystallize completely
after a strain of 3.
As shown in figure 8, the addition of 0.017% of Nb
still allows dynamic recrystallization for any temperature
of deformation ranging from 850°C to 1000°C. After ha-
ving been cooled down to room temperature, the metal-
lographic specimens present a transition from acicular to
fine equiaxed ferrite when the temperature of deformation
is decreased from 1000°C to 850°C.
T8/5 = 1 5 s
CR = 2 0 °C/s
0 Nb
1 7 Nb
8 3 Nb
20 µm
2 .0 0 3 .0 0 4 .0 0
However, no great differences are observed for the
lower temperatures at 850°C and 900°C. For the
interpretation of the influence of the temperature of
deformation, care must be taken over the time that the
austenitic microstructure spend at high temperature during
cooling down to 20°C. As a matter of fact, some
metadynamic recrystallization is expected to take place at
the higher temperatures after complete dynamic
recrystallization. Indeed, the kinetics of metadynamic
recrystallization is known to be faster than for static
recrystallization, and this latter is already active after 5s
above 900°C for the 0.017% Nb steel.
ISS Technical Paper, A. Schmitz Page 6 of 14
 T O R S IO N T E S T
1 7 N b - 1 /s
2 00
1 60
S tress (M P a)
1 20
80
40
0
0 .0 0 1 .0 0 2 .0 0
S train
Fig.8. Temperature effect on the dynamic softening of the 0.017% Nb steel and on the resulting
microstructure after cooling down to room temperature (Marshall etchant)
Consequently, some metadynamic softening should
appear for deformation above 950°C where sufficient time
(a few seconds) is spent between deformation and
transformation with a cooling rate of 20°C/s.
The evolution of ferrite microstructure with the
amount of continuous deformation at 900°C is illustrated
in figure 9 in the case of 0.083% Nb. By straining up the
austenite, the as-cooled microstructure transforms
gradually from a pure bainitic state to a polygonal ferrite.
The additional strain leads to the nucleation of small
grains of ferrite along the grain boundary of parent
austenite, and the volume fraction of these fine grains
increases with prior deformation. A mixed ferrite-bainite
microstructure is observed up to a strain of 3 where fine
grained ferrite prevails throughout the sample. From a
practical point of view, the above results confirm that a
sufficient amount of strain has to be cumulated within the
finishing train in order to enable the formation of ferrite
with a fine equiaxed grain size, and this necessitates an
entry temperature lower than Tnr.
The effect of the interpass time (fig.10) has been
more particularly studied for the 0.083% Nb steel which
8 5 0 °C
9 0 0 °C
9 5 0 °C
1 0 0 0 °C
T8/5 = 1 5 s
CR = 2 0 °C/s
20 µm
3 .0 0 4 .0 0
presents the higher level of Nb supersaturation. This steel
is able to pancake easily through copious strain-induced
precipitation which should occur during straining at
900°C. An interpass time of 0s corresponds to a conti-
nuous deformation and leads to a nearly complete dyna-
mic recrystallization after a strain of 3. The corresponding
grain size of ferrite is very fine (2-3µm). For all the other
values of the interpass time, the mechanical behaviour is
characteristic of full pancaking of the austenitic micro-
structures, even for interpass time as low as 0.6s.
However, the ferrite grain size after austenite pancaking
increases from 2-3 µm for an interpass time of 0.6s
towards a rougher value around 6-7 µm in the case of 10s
interpass time. This experimental fact does not match the
interpretation of other searchers(6,7) which identify a clear
relationship between the fine ferrite and the occurrence of
dynamic recrystallization of austenite prior to its
transformation. Some complementary comments on the
fine grained ferrite formation will be presented later in
the discussion part of this paper.
ISS Technical Paper, A. Schmitz Page 7 of 14
 T O R S IO N T E S T
8 3 N b - 9 0 0 °C
2 00

1 /s

1 60

T8/5 = 1 5 s
CR = 2 0 °C/s
S tress (M P a)

1 20

80

40

20 µm
0
0 .0 0 1 .0 0 2 .0 0 3 .0 0 4 .0 0
S train

Fig.9. Microstructural evolution of the as-cooled 0.083% Nb steel as function of the amount of
strain applied at 900°C (Marshall echant)

The etching of the metallographic samples with Lepera
etchant reveals a fine distribution of small white islets
which correspond either to martensite or to austenite. As
a matter of fact, X-ray diffraction has put in evidence the
presence of some retained austenite at room temperature
which amounts to 4.3% volume fraction. The shift of the
(220) austenite peak allows the determination of the
carbon concentration in the retained austenite with the
help of the extrapolation method of the austenite lattice
parameter. By means of the Ridley's expression(16) for the
austenite lattice parameter a as a function of the carbon
concentration C,
a (Å) = 3.573 + 0.033 wt.%C
a carbon content around 0.9 wt.% is estimated for the
retained austenite. The micrographs also show that a
refinement of the ferrite grain size leads to a more
widespread distribution of smaller martensite-austenite
islets. This refining effect should be beneficial for the
mechanical properties, especially for what concerns
ductility and toughness.
3.4. Optimized chemistry and rolling schedule
From the previous results, it appears that the
formation of a fine grained dual phase steel implies a
cumulative deformation of austenite above a strain value
around 2 (see fig.9) which corresponds to a minimum
thickness reduction of 85%. On the other hand, the strain
accumulation necessitates the absence of any static
recrystallization within the finishing grain. To avoid static
recrystallization of steels, the rolling temperature can be
decreased below 850°C (Nb free steel in fig.3) but this is
accompanied by an important rise of the rolling forces and
powers. To increase the temperature at the entry of the
finishing grain, the kinetics of static recrystallization can
be slowed down by means of Nb addition through its
retarding effect by solute drag. This temperature increase
does not affect too much the ferrite grain refinement if it
is limited to 950°C (see fig.8) to avoid any post softening
during a subsequent cooling. A minimum of 0.030 wt.%
of Nb has to be added to steels in order to reach an entry
temperature of 950°C (fig.3) and below which static
recrystallization is prevented. Furthermore, Nb addition
favours a fine grain size (fig.7), even at a low level.

ISS Technical Paper, A. Schmitz Page 8 of 14


2 00
1 /s
1 60
S tress (M P a)
1 20
80
40
0
0 .0 0 0 .5 0 1 .0 0
Fig.10 Effect of interpass time on pancaking and microstructure of the 0.083%Nb steel cooled to
room temperature (Lepera etchant)
Taking into account the temperature loss which takes
place throughout an industrial finishing train (fig.1), it is
necessary to extend the temperature range between Tnr
and Ar3 in order to avoid phase transformation within the
train. A temperature loss around 100°C is commonly ob-
served on the lines for a strip of 3mm thickness, which
leads to a maximum Ar3 value around 800°C. This can be
achieved by Mn addition which is also beneficial by its
solid solution strengthening of ferrite. According to the
Ouchi formula(17) of Ar3 temperature for strain-hardened
austenite, an Ar3 of 800°C requires a minimum Mn
addition of 1.4 wt.% on a basis of 0.07 wt.% of C. This C
content should provide sufficient volume fraction of finely
dispersed second phase particles in order to ensure
performant mechanical properties.
During the continuous cooling at a cooling rate of
20°C/s, strain-hardened austenite transforms into a fine
grained ferrite (fig.10) which rejects its carbon into the
residual austenite. The cooling rate must not be too high
T O R S IO N T E S T
8 3 N b - 9 0 0 °C
T8/5 = 15 s
C R = 2 0 °C /s
IP T =0 s
IP T =0 .6 s
IP T =2 s
IP T =1 0 s
30 µm
1 .5 0 2 .0 0 2 .5 0 3 .0 0 3 .5 0 4 .0 0
S train
to enable complete ferrite transformation and a good
carbon enrichment of residual austenite, but also not to
low to prevent the austenite transformation into bainite or
pearlite.
The nature and hardness of the second phase issued
from the transformation of enriched austenite are defined
by the coiling temperature. To produce a ferrite-
martensite microstructure, the coiling temperature must be
below the martensite start (Ms) temperature. The previous
evaluation of 0.9 wt.%C in the retained austenite allows
to estimate an Ms temperature around 170°C according
Kunitake(18). It is therefore advised here to continuously
cool the strips down to room temperature to ensure
sufficient transformation of residual austenite into
martensite. Some retained austenite is however
unavoidable but it can be beneficial for the mechanical
properties through the Transformation Induced Plasticity
(TRIP effect) during the tensile test at room temperature.
ISS Technical Paper, A. Schmitz Page 9 of 14
 From the above considerations, the laboratory
rolling trial has been carried out on a steel whose
chemical composition is given in table II. The optimized
rolling schedule is summarized in table III. The interpass
time does not exceed 10s for any pass. The cooling of the
strip was performed by quenching in still water at room
temperature.The objective was thus the production of a
Dual Phase Continuous Cooling (DPCC) steel.
The chemical composition and the optimized rolling
schedule proposed hereabove are subjected to an Euro-
pean Patent(19) which is currently under examination.
Table III Thermomechanical processing parameters of
the laboratory hot-rolling trial
Reheating temperature 1150°C (1h)

Table II Chemical composition of the experimental Finishing pass schedule 30
20
11
5 mm

steel (10-3wt.%) Start rolling temperature 940°C

C Mn P S Nb Al N Finish rolling temperature 840°C

70 1400 27 25 27 50 10 Cooling rate ~ 80°C/s

The innovative aspect of this process of thermo- Coiling temperature ~ 20°C

mechanical rolling is two-fold. First, it allows to produce
dual phase steels from a lean chemical composition which
is quite cheap. Second, the production schedule is based 3.5. Mechanical properties of the laboratory strip
on a continuous cooling of the hot-strip on the run-out
table down to room temperature.This way to process the The results of the tensile test as well as the
hot-strip avoids the problems akin to heterogeneous microstructure of the experimental steel processed by the
microstructures along the length of the coil that result optimized process are presented in figure 11.
from the stepwise cooling paths proposed in the past for
the elaboration of dual phase steels.

T E N S IL E T E S T

800

YS = 4 5 0 MP a
T S = 7 5 3 MP a
A 50 = 2 3 %
600
S tre s s (M P a )

400

200

10 µm

0
0 .0 0 5 .0 0 1 0 .0 0 1 5 .0 0 2 0 .0 0 2 5 .0 0

S tra in (%)

Fig.11 Tensile stress-strain curve and optical micrograph of the laboratory multiphase steel hot-
rolled according the optimized schedule (Lepera etchant)

ISS Technical Paper, A. Schmitz Page 10 of 14

The laboratory strip gives a yield strength of 450 MPa and
a tensile strength of 753 MPa associated with an
important total elongation of 23%. This steel thus
provides a good combination of strength and ductility
with a product TS x A50 value which amounts to 17,300
Mpa. %. The stress-strain curve of such a steel does not
exhibit any yield point, which results in a low YS/TS
yield ratio of 0.6. The absence of sharp yield point is
typical of dual phase microstructures where the presence
of high-carbon constituents leads to a less effective
locking of the increased dislocation population. This is
confirmed by the Lepera etching of the metallographic
sample which puts in evidence a fine distribution of white
martensite-austenite particles dispersed in a fine grained
ferrite of 4-5 µm. The interface between these martensite
particles and the ferrite grain is particularly rich in
dislocations that were created by the volume expansion
accompanying the martensitic transformation of residual
austenite during cooling below the Ms temperature. The
unlocked dislocations are considered to the origin of the
stress-strain curve free from any yield point elongation.
The market benefit of fine grained ferrite can also be
observed by the measurement of the low temperature
toughness (figure 12).
Charpy test - subsize (5mm)
200
Energy (J/cm2)
150
100
50
0 recrystallization
-150 -100 -50 0 50
Temperature (°C)
Fig.12. Low temperature toughness curve by Charpy
test on the laboratory multiphase steel
While the impact energy at room temperature saturates to
200J/cm², the impact transition temperature ITT
determined at half the upper shelf energy is as low as
-130°C. This excellent result may be attributed to the
microstructure since it is well known that the resistance to
brittle fracture is greatly enhanced by grain refinement.
But an additional reason seems to be the scale of the
high-carbon constituent whose fine homogeneous
distribution is probably less damaging to fracture
initiation and propagation despite its high hardness.
In figure 13, the cyclic response curve at 0.25%
strain shows an initial cyclic hardening followed by cyclic
softening. The peak stress amplitude (420 MPa) is
attained at around 1 percent of the number of cycles to
failure which amounts to 50000.
OLIGOCYCLIC PLASTIC FATIGUE
500
400
Stress amplitude (MPa)
Strain = 0.25%
300
200
Strain = 0.1 %
100
0
1 10 100 1000 10000 100000
N Cycles
Fig.13. Stress response curves at low cycle fatigue test
on the laboratory multiphase steel
The subsquent softening around 15% at the moment of
failure demonstrates the relative stability of this steel.
4. DISCUSSION
4.1. Retardation effect of Nb on static and dynamic
The kinetics of recrystallization are retarded by Nb
addition either by solid solution or under the form of
precipitates. Different modes of precipitation can be
distinguished depending on the state of austenite prior to
precipitation. In a recrystallized austenite, the static
precipitation is characterized by a sparse nucleation of
precipitates on grain boundaries and around undissolved
particles. On the other hand, strain-induced precipitation
is considerably accelerated by a prestrain and is still
further accelerated during a continuous deformation
which generates dynamic precipitates. The rate increase
ISS Technical Paper, A. Schmitz Page 11 of 14
can be attributed to the relatively dense nucleation of
precipitates on dislocations and the enhanced growth rate
by the increased Nb diffusion in the presence of excess
vacancies(20).
In their investigation of the progress of precipitation
in a 0.035%Nb steel containing 0.050% of C and 0.42%
of Mn, Weiss and Jonas(21) have determined the kinetics
of the different precipitation mode by means of a
mechanical method based on the determination of the
peak stress of dynamic recrystallization during constant
strain rate compression tests. Whereas static precipitation
only takes place after 100s at 900°C, the imposition of 5
percent prestrain considerably speeds up the precipitation
rate by about one order of magnitude and initiates strain-
induced precipitation after 10s at 900°C. The rate of dy-
namic precipitation is again one order of magnitude faster
than strain-induced precipitation and already appears after
1s at the temperature nose which lies at 900°C.
After a prestrain of 0.5 at 900°C, no important
amount of strain-induced precipitation should occur
within 5s for the Nb steels investigated by compression in
this work (see fig.3), except perhaps for the 0.083%Nb for
which the high level of supersaturation is supposed to
enhance precipitation. Consequently, Nb is assumed here
to interact with static recrystallization after a single pass
by the solute drag effect.
While solute Nb certainly delays dynamic
recrystallization during continuous deformation, some
dynamic precipitation is possible after a strain of more
than 1 since it corresponds to a deformation time of 1s
with a 1/s strain rate. This precipitation should be more
pronounced in presence of high Nb supersaturation and
could eventually affect dynamic recrystallization. This is
indeed put in evidence in figure 4 where the stress-strain
curve of the 0.083%Nb steel displays a plateau around a
strain of 1 before softening. More complex situations are
encountered in the case of multipass deformations
separated by varying interpass times. In the case of long
interpass times and a high degree of supersaturation (such
as 10s and 0.083%Nb) strain-induced precipitation delays
both static and dynamic recrystallization, so that meta-
dynamic recrystallization is also prevented and a full
pancaking is observed (fig.6). As mentioned by
Roucoules et al.(9), the introduction of fresh precipitates
that nucleate during the successive interpass times
compensates the coarsening which takes place in the
subsequent passes and renders ineffective the retarding
effect on the recrystallization. When lower levels of
supersaturation or shorter interpass times are used (as in
continuous mills), the density of fresh precipitates is
apparently not high enough to prevent dynamic
recrystallization which leads in turn to metadynamic
recrystallization (see 0.017%Nb in fig.6). The rate of the
latter mechanism increases with accumulated strain
because the amount of dynamic precipitate coarsening
increases with deformation(22). However, it should be
remarked that at high supersaturation contents such as
0.083%Nb, interpass times as short as 0.6s ensure a
complete pancaking of austenite (fig.10). This can be
explained by the solute drag effect of Nb on both static
and dynamic recrystallization up to the peak strain
(around 1.8 at 900°C), associated with a fine dynamic
precipitation which is expected to take place during the
corresponding 4s cumulative time.
4.2. Refinement of ferrite grain size by Nb
In agreement with some authors(5,7), the analysis of
the effect of the interpass time on the microstructure
(fig.10) for continuous (IPT = 0s) and long interruption
time (IPT = 10s) would lead to conclude that it is dynamic
recrystallization which is at the basis of ferrite grain
refinement through the generation of fine recrystallized
grains more efficient than pancaked grains. Nevertheless,
this interpretation does not explain how the interrupted
torsion test with 0.6s interpass time also provides a very
fine ferrite grain although full pancaking is observed.
Another explanation is given here where the accent
is put on the effect of Nb in solid solution on the grain
refinement of ferrite during the phase transformation. As
shown in figure 7, the ferrite grain size is quite sensitive
to the addition of Nb after direct cooling of the
dynamically recrystallized austenite in which Nb has
mainly remained in solid solution. Furthermore, Fujioka
et al(23) have shown that retardation of ferrite
transformation is weakened by the progress of strain-
induced precipitation in austenite and they concluded that
ferrite transformation is significantly restrained by Nb in
solution but unsubstantially as precipitates. As a
consequence of these observations, it results that only Nb
in solution plays an important role in the refinement of the
ferrite grain size, probably by its effect on carbon
diffusivity. On the other hand, Herman et al(24) have
determined the isothermal kinetics of strain-induced
precipitation after a single pass deformation by selective
eletrolytic dissolution of a 0.080%Nb steel with 1.5% of
Mn. Their analysis revealed that strain-induced
precipitation starts at 10s, in agreement with previous
works(21), and that 0.040%Nb has precipitated after 100s.
ISS Technical Paper, A. Schmitz Page 12 of 14
This situation should be amplified during multipass
deformation where fresh precipitates are continuously
nucleated and one can expect a monotonic decrease of the
Nb solute content with the interpass time. Although the
dynamic recrystallization of austenite is very beneficial to
obtain a fine grained ferrite, the effect of the interpass
time on the grain refinement has to be translated more in
terms of Nb solute depletion of the austenitic matrix than
due to dynamic recrystallization of austenite.
4.3. Effect of austenite hot-deformation on the kinetics
of austenite to ferrite transformation
As mentioned above, in itself Nb in solution in steels
slows down the isothermal kinetics of transformation.
Despite of that, the addition of Nb generally leads to a
faster transformation given that it prevents from
recrystallization and allows to retain work-hardened
austenite up to the start of transformation. Umemoto et
al(25) have found that the ferrite nucleation rate was
substantially increased by the work-hardening of austenite
which refines considerably the ferrite grain size. The
mechanism of enhanced nucleation was formulated
considering the ledge formation at grain boundaries, the
increase in dislocation density within austenite grains,
etc... Furthermore, the work-hardened austenite is rich in
dislocations which favour the carbon diffusion ahead the
front of transformation and thus increase the ferrite
growth rate. The acceleration of transformation due to
work-hardening of austenite is important in ferrite and
pearlite transformations, whereas the bainite
transformation is not much affected by austenite defor-
mation(26).
The enhanced kinetics of ferrite transformation from
a work-hardened austenite allows the formation of a dual
phase steel by continuous cooling since the ferrite rejects
is carbon content into austenite. As a consequence, the
mean carbon content of residual austenite increases with
the volume fraction of polygonal ferrite, and this carbon
enrichment slows down the kinetics of austenite
transformation up to an extent where only martensite
transformation remains possible. The enhanced ferrite
kinetics thus avoids any stepwise cooling to allow
sufficient volume fraction of ferrite to appear in the
austenite microstructure.
5. CONCLUSIONS
The influence of the chemical composition and
rolling schedule parameters on the ferrite microstructure
after continuous cooling have been investigated in this
work. From the mechanical and metallographic results,
the following conclusions can be drawn :
1. During multipass deformation in a finishing mill, the
addition of 0.030 wt.%Nb prevents the occurrence
of static recrystallization for an entry temperature
below 950°C.
2. During continuous deformation, the Nb addition
retards considerably the initiation of dynamic
recrystallization and a cumulative strain of more
than 2 has to be applied below 950°C on a 0.030
wt.%Nb steel in order to induce complete dynamic
recrystallization.
3. After continuous cooling down to room temperature
at 20°C/s, a polygonal fine grained ferrite is
obtained in the absence of any static recrystal-
lization by a prior deformation below 950°C up to a
cumulative strain of 3. In these conditions, the Nb
content in solid solution has a marked effect on
refinement of ferrite grain size leading to 2-3µm
ferrite grains with 0.083 wt.%Nb addition.
4. In the case of multipass deformation in the presence
of Nb, an increase of the interpass times gives more
time for strain-induced precipitation to take place
and thereby delays dynamic recrystallization. Long
interpass times higher than 10s and high levels of
Nb supersaturation such as 0.083 wt.% prevent
dynamic recrystallization and lead to full pancaking
of austenite microstructure. However, lower super-
saturation and shorter interpass times allow meta-
dynamic recrystallization to occur once dynamic
recrystallization is initiated.
5. Longer interpass times provide rougher ferrite grain
sizes after continuous cooling to room temperature.
This fact is interpreted as a result of the loss of
solute Nb due to strain-induced precipitation during
the hot-deformation of austenite.
6. After the application of the optimized rolling
schedule proposed in this work, a continuous
cooling to room temperature provides a strip with a
fine grained ferrite (4-5µm) in which small high-
carbon constituents are homogeneously dispersed.
The resulting dual phase steel exhibits excellent
tensile properties (TS = 750MPa, A50 = 23%) aswell
as improved toughness and fatigue resistance.
ISS Technical Paper, A. Schmitz Page 13 of 14
 ACKNOWLEDGMENTS
Grateful acknowledgments is made to the Belgian Public
Authorities for financial support.
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