Ultrafine ferrite formation through cold-rolling

and annealing of low-carbon dual-phase steel

Y. Okitsu*1, N. Takata2 and N. Tsuji3
Formation process of ultrafine grained ferrite through a simple thermomechanical route
composed of cold-rolling and annealing of dual-phase starting microstructures was investigated.
A 0?1%C steel having a ferritemartensite dual-phase microstructure was cold-rolled by 91% and
subsequently annealed below the eutectoid (A1) temperature. During the annealing, the cold-
rolled microstructure gradually changed to be equiaxed ultrafine ferrite, without preferential
growth of particular ferrite grains. Hardness of the cold-rolled specimen continuously decreased
without a significant drop. The main components of texture in the cold-rolled specimen, a-fibre
and c-fibre, did not change greatly after the formation of ultrafine grains. It was suggested that
finely subdivided region having large misorientations in the cold-rolled state grew with recovery to
form the ultrafine ferrite.
Keywords: Ultrafine grain, Carbon steels, Severe plastic deformation, Cold rolling, Dual phase steels, Martensite

Introduction Aiming for reducing the necessary plastic strain and

Global demands for reducing emission of greenhouse
gasses such as CO2 have been enhancing studies on new
high strength steels13 that can contribute to weight
reduction and improvement of fuel efficiency in auto-
mobiles. Grain refinement of ferrite or other matrix
phases in steels down to sub-micrometre sizes is thought
to be one of the important microstructure controlling
methods in such high strength steels.13 Actually, some
studies have reported improved mechanical properties
by ultra grain refinement of steels, such as high
strength at quasi-static and dynamic strain rates,48
good toughness in low temperature9 and high stretch
formability.10
Generally, severe plastic deformation (SPD) processes
such as equal channel angular extrusion,11 high pressure
torsion,12,13 and accumulative roll bonding (ARB),1416
have been applied to fabricate ultrafine grained (UFG)
materials having mean grain sizes smaller than 1 mm.
The SPD processes require very large plastic strain over
4 or 5 in logarithmic equivalent strain17 in order to
fabricate uniform UFG microstructures. Therefore, such
SPD processes do not seem adaptive to the industrial
mass-production of bulky structural sheet metals at the
present moment.
1
Automobile R&D Center, Honda R&D Co., Ltd, 4930 Shimotakanezawa,
Haga-machi, Haga-gun, Tochigi 321-3393, Japan
2
Department of Metallurgy and Ceramics Science, Graduate School of
Science and Engineering, Tokyo Institute of Technology, 2-12-1-S8-8,
Ookayama, Meguro-ku, Tokyo 152-8552, Japan
3
Department of Materials Science and Engineering, Graduate School of
Engineering, Kyoto University Elements Strategy Initiative for Structural
Materials (ESISM), Kyoto University, Yoshida-Honmachi, Sakyo-ku, Kyoto
606-8501, Japan
*Corresponding author, email yoshitaka_okitsu@n.t.rd.honda.co.jp
producing UFG microstructures with high productivity,
the present authors have proposed a new route to
fabricate UFG ferrite microstructures in low-C steels.6,18
The process is composed of conventional cold-rolling and
annealing, but characterised by the use of dual-phase
microstructures composed of ferrite and martensite as the
starting microstructure of the thermomechanical process.
In the cold-rolled microstructure, very fine lamellar
structures having various crystal orientations were
confirmed by transmission electron microscopy (TEM)
observation18 and electron backscatter diffraction
(EBSD) analysis.6 After subsequent annealing, fully
annealed and equiaxed UFG ferrite grains with sub-
micrometre grain sizes were formed. The UFG ferrite
cementite (FC) specimen showed very high yield strength,
i.e. 966 MPa, which was twice as high as that in coarse-
grained specimen.6
However, the formation process of the UFG ferrite in
the present route composed of cold-rolling and anneal-
ing of dual-phase microstructures has not yet been
clarified in detail, while the behaviours in the SPD
processes1116 have been revealed in many previous
studies. Necessary information for discussing the
mechanism of microstructural formation, such as
microstructures at low annealing temperatures, hardness
and texture, has not been shown in the previous
studies.6,18 In this paper, the formation process of the
UFG ferrite is clarified by investigating the microstruc-
ture, hardness and texture at each stage of the
thermomechanical process. Then, the mechanism of
UFG ferrite formation is discussed.
Experimental
Table 1 summarises the chemical composition of the
steel used in this study. Based on a low-C steel, small

2015 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 11 June 2014; accepted 30 August 2014
DOI 10.1179/1743284714Y.0000000660 Materials Science and Technology 2015 VOL 31 NO 6 745
Okitsu et al. Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel
amounts of Nb and B were added. Nb was added in
order to refine the starting microstructure. B was chosen
for obtaining a dual-phase structure effectively in the
starting microstructure. Typical amounts as microalloy-
ing elements in conventional steels were selected. The
roles of Nb and B will be described in detail later. The
transformation temperatures on cooling from austenite,
which were important for fabricating a dual-phase
starting microstructure, were measured by a dilatometer.
The two-phase region of ferrite and austenite at a
cooling rate of 2uC s21 was between 465 and 625uC. The
thermomechanical process consisted of conventional
hot-rolling, cold-rolling and annealing. A 30 kg ingot
of the steel prepared by vacuum melting was first hot-
rolled to a thickness of 20 mm in the austenite region.
Then the sheet was reheated to 1000uC and hot-rolled to
a thickness of 6?8 mm at a finishing temperature of
770uC in the austenite region, air-cooled to 540uC
corresponding to the intercritical region of ferrite and
austenite, and then water-cooled to room temperature to
obtain a dual-phase microstructure of ferrite and
martensite. Here, Nb in the steel was effective for
refining the microstructure by retarding recrystallisation
of deformed austenite during hot-rolling. Fine starting
microstructure seems favourable for obtaining UFG
microstructures after cold-rolling and annealing. Due to
the addition of B that retards ferrite transformation of
austenite, the austenite regions existing at 540uC (the
intercritical region) would preferentially transform to
martensite during subsequent water-cooling. The hot-
rolled sheets were cold-rolled at room temperature using
a four-high rolling mill with lubrication. Cold-rolled
sheets having 150 mm width and 0?6 mm thickness were
obtained. Total reduction in thickness through the cold-
rolling was 91%, which corresponded to an equivalent
plastic strain of 2?8 assuming plane strain compression.
The cold-rolled sheets were annealed at various tem-
peratures ranging from 550 to 680uC for 120 s in a salt
bath followed by water-cooling.
Microstructural observations were carried out for the
specimens at each stage of the thermomechanical
process. All the specimens were observed from the
transverse direction (TD) of the sheets. The samples for
optical microscopy or scanning electron microscopy
(SEM) were cut, mechanically polished and etched with
a 3% nital. Scanning electron microscopy observations
were conducted in a Hitachi S-4300E/N SEM operated
at 15 kV. For evaluating ferrite grain sizes, the mean
intersection method was employed, using SEM micro-
graphs. Lines parallel to the normal direction (ND) and
those parallel to the rolling direction (RD) of the sheets
were drawn on the micrographs, and intersection lengths
of ferrite grains on the lines along both directions
were measured and averaged. Thin foils for TEM were
prepared by twin-jet electropolishing in a 10%
HClO4z90% CH3COOH solution, and observed in a
JEOL JEM-2010HC TEM operated at 200 kV.
Electron backscatter diffraction measurements were
also carried out by using a FEI XL30S SEM equipped
Table 1 Chemical composition of low C steel used in this study/wt-%
C Si Mn P S
0.10 0.01 1.98 0.002
746 Materials Science and Technology 2015 VOL 31
1 Optical micrograph of low C steel after hot-rolling
(starting microstructure) observed from TD
with TSL (TexSEM Laboratories, Inc.) orientation
image microscope system operated at 15 kV. The
EBSD scanning was carried out at the thickness centre
on TD sections. For the cold-rolled specimen, the
mapping was carried out in a 20620 mm area at a step
size of 0?05 mm. For the annealed specimens, the
mapping was carried out in a 30650 mm area at a step
size of 0?1 mm. A hexagonal grid was applied to both
cases. Orientation data were analysed using the orienta-
tion image microscope analysis version 4.7 software. For
the cold-rolled specimen, measured points having
Confidence Index (CI) smaller than 0?1 were firstly
removed and then all the analyses were carried out. For
the subsequently annealed specimens, the data were
cleaned-up by the grain dilation method in order to
eliminate some measured points with low confidence. If
a grain consisted of one or two measured points, the
orientations of the points within the grain were modified
to that of the majority of neighbouring points. For all
the specimens, boundaries having misorientations smal-
ler than 2u were removed in order to cut off the
inaccuracy in EBSD measurement and analysis.
Vickers hardness was measured at the thickness centre
on TD sections of the specimens with a load of 1 kgf.
The hardness was measured at least three times for each
specimen, and the data were averaged.
Results
Microstructural change
An optical micrograph of the hot-rolled sheet before
cold-rolling, shown in Fig. 1, exhibited a dual-phase
microstructure composed of ferrite matrix (bright
regions) and martensite islands (dark regions).
Uniform dual-phase microstructure throughout the
specimen was obtained. Mean intersection lengths along
ND of the both regions, measured on the optical
micrograph, were 5?55 mm for ferrite and 2?47 mm for
martensite. Area fraction of martensite measured by
point-counting method was 42%. A TEM observation
confirmed that the martensite was typical lath-marten-
site including a high density of dislocations. Average
Al Nb B N
0.001 0.018 0.018 0.0015 0.0011
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 Okitsu et al. Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel

2 Scanning electron microscopy microstructures of low C steel a after cold-rolling by 91% reduction, and after annealing
at b 550uC, c 575uC, d 600uC, e 625uC and f 675uC for 120 s followed by water-cooling to room temperature

thicknesses of the martensite laths and blocks were 0?4
and 1?5 mm, respectively. Cementite particles were not
observed in the hot-rolled specimen.
Scanning electron microscopy microstructures of the
cold-rolled and annealed specimens are shown in Fig. 2.
Figure 2a shows an SEM image of the 91% cold-rolled
specimen. Ferrite matrix (dark grey regions) exhibited
wavy microstructures elongated roughly to RD and bent
around martensite islands (light grey regions). This
indicated that complex plastic flow occurred and higher
strain was introduced into the softer ferrite matrix owing
to the existence of the hard martensite phase. The
martensite regions were also deformed to some extent
during the cold-during, and exhibited diamond-like shapes
in Fig. 2a. The strains introduced into the martensite
regions would be smaller than that into the ferrite matrix,
because martensite is much harder than ferrite.
Figure 3 shows a TEM microstructure of the 91%
cold-rolled specimen. The F and M in the figure
indicate ferrite and martensite, respectively. In the ferrite
regions between martensite islands, fine lamellar struc-
tures of ferrite with mean spacing of 0?14 mm were
observed. Figure 3b shows a selected area diffraction
(SAD) pattern taken from the ferrite region indicated by
the dotted circle (b) in Fig. 3a. The SAD pattern showed
ring-like spots, indicating various orientations existing
within the selected small area. This result meant that the
lamellar structure was composed of elongated ferrite
regions with large misorientations to the neighbouring
regions. Figure 3c shows an SAD pattern taken from the
martensite region indicated by the dotted circle (c) in
Fig. 3a. The pattern was again ring-like, which sug-
gested large local misorientations in the martensite
regions as well. It was revealed that many regions with

3 a transmission electron microscopy microstructure of the low C steel after cold-rolling by 91% reduction starting from
a dual-phase structure composed of ferrite and martensite, observed from TD, b SAD pattern taken from ferrite and
c SAD pattern taken from martensite

Materials Science and Technology 2015 VOL 31 NO 6 747

Okitsu et al. Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel

4 Boundary misorientation maps for representative 20615 mm regions extracted from whole measured area in EBSD
analysis of low C steel a after cold-rolling by 91% reduction, and after subsequent annealing at b 620uC, c 635uC and
d 680uC for 120 s followed by water-cooling observed from TD: bold lines show high angle grain boundaries and nar-
row grey lines show low angle grain boundaries

different crystal orientations already existed both in the
ferrite matrix and the martensite islands in the cold-
rolled state.
Next, microstructures after subsequent annealing of
the 91% cold-rolled specimen are shown. Figure 2bf
shows SEM microstructures of the specimens after
annealing at 550, 575, 600, 625 and 675uC for 120 s,
respectively. All the annealing temperatures were below
Ac1 (700uC). After annealing at 550uC (Fig. 2b), the
wavy microstructures of ferrite remained. However,
some equiaxed fine ferrite grains were observed along
the elongated structures in the wavy shapes. At the
annealing temperature of 575uC (Fig. 2c), the equiaxed
ferrite grains grew slightly and the wavy microstructures
became less dominant. At the annealing temperature of
600uC (Fig. 2d), the microstructure was mostly filled
with equiaxed fine ferrite grains, and the wavy micro-
structures were no longer observed. In addition, fine
cementite particles (white spots in the SEM microstruc-
ture) appeared and homogeneously dispersed in the
microstructure. Mean ferrite grain size of this uniform
ferrite microstructure formed at 600uC was 0?45 mm. At
625uC (Fig. 2e), also a uniform UFG ferrite micro-
structure with mean ferrite grain size of 0?59 mm was
obtained. As the annealing temperature increased up to
675uC (Fig. 2f), mean ferrite grain size increased to be
1?23 mm. Here, large recrystallised grains, that are
commonly observed in conventional cold-rolling and
annealing of carbon steels, did not appear in the
microstructure.
Next, characteristics of grain boundaries in the cold-
rolled and subsequently annealed microstructures are
shown. Figure 4ad shows boundary misorientation
maps obtained by the EBSD measurements of the
specimens after the 91% cold-rolling, and those after
subsequent annealing at 620, 635 and 680uC for 120 s,
respectively. Representative regions with a 20615 mm
size exhibiting typical features of each specimen were
extracted from whole measured areas and are shown in
the figure. The bold lines show high angle grain
boundaries (HAGBs) of which misorientation angles
are higher than 15u, while the narrow grey lines show
low angle grain boundaries having misorientation angles
between 2 and 15u. In the cold-rolled specimen (Fig. 4a),

748 Materials Science and Technology 2015 VOL 31 NO 6

 Okitsu et al.
5 Misorientation angle distributions in low C steel specimens cold-rolled by 91% reduction and annealed at a 620uC, b
635uC and c 680uC for 120 s followed by water-cooling: fHAGB indicates fraction of high angle grain boundaries
(HAGBs) in microstructures
many bad points having small CI in the EBSD
measurement are displayed in black. Therefore quanti-
tative analyses of crystal orientations and boundary
misorientations of the cold-rolled specimen were diffi-
cult. However, some elongated ultrafine ferrite grains
are seen in Fig. 4a.
In the annealed specimens with equiaxed ferrite
microstructures (Fig. 4bd), it is shown that ferrite
grains were mostly surrounded by HAGBs, and
contained few dislocation substructures (low angle grain
boundaries) within the ferrite grains. This result
suggested that the ferrite grains in the annealed speci-
mens were equivalent to recrystallised ones. The average
grain diameters in the specimens shown in Fig. 3bd,
calculated in the EBSD analysis, were 0?49, 0?62 and
1?03 mm, respectively.
Figure 5ac shows distributions of boundary misor-
ientation angles obtained from the EBSD orientation
data for the annealed specimens shown in Fig. 4bd,
respectively. The distribution of the cold-rolled specimen
is not shown in the figure, because it may not represent
accurately the grain boundaries characteristics of the
specimen. Approximately 47% of whole measured points
having low CI values were removed before analysis. The
regions with low CI possibly contained large plastic
strain and also a large amount of HAGBs. Therefore,
the fraction of HAGBs (fHAGB) might be underestimated
when using the data after the removal of such points
6 Vickers hardness of low C specimens before cold-roll-
ing, after cold-rolling, and after annealing at various
temperatures: solid circles represent mean hardness
values of low C steel used in this study started from
DP microstructure, while open rectangles represent
hardness data for similar low C steel cold-rolled and
annealed from FC (ferrite-cementite) microstructure23
Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel
with low CI values. Here, the fHAGB of the cold-rolled
specimen was calculated for reference, to be 53%. The
fraction of HAGBs (fHAGB) of the specimen annealed at
620uC was 77?4%, and it gradually increased as the
annealing temperature rose. At the annealing tempera-
ture of 680uC, the fraction of HAGBs reached to 90%.
Other processes to obtain UFG ferrite micro-
structures without SPD, such as cold-rolling and
annealing of martensite,19,20 calibre-rolling of tempered
martensite21 and compression of ferritepearlite at
warm temperatures,22 have been proposed. However,
all the ferrite microstructures in the previous studies1922
contained some residual dislocations within the ferrite
grains, and the HAGBs fractions were lower than those
in the present study. For example, a UFG ferrite-
cementite specimen with a mean ferrite grain size of
about 1 mm in Ref 22 had approximately 60% of
HAGBs fraction. That is, those UFG microstructures
had deformed characteristics. In the present process,
fully-annealed UFG ferrite microstructures with high
HAGBs fractions were obtained through conventional
cold-rolling and annealing procedures. In addition,
required plastic strain was much lower than those in
the SPD processes.
Hardness change
Figure 6 shows Vickers hardness of the specimens before
cold-rolling (the starting microstructure), after cold-
rolling and after annealing at various temperatures for
120 s. The present data [starting microstructure: dual-
phase (DP)] are indicated by solid circles. In Fig. 6, the
data obtained by cold-rolling and annealing of an FC
microstructure which showed a typical recrystallisation
of cold-rolled ferrite are additionally shown by open
rectangles. The additional data, which have been
reported by one of the authors,23 were obtained as
follows. Using a low C steel containing 0?1%C and
2%Mn, an FC microstructure was prepared as the
starting microstructure. It was cold-rolled by 80%
reduction in thickness (equivalent strain of 1?86) and
subsequently annealed at various temperatures for
120 s.
The changes in hardness of the specimens having two
kinds of starting microstructures (DP and FC) were
quite different. In the case of the FC starting micro-
structure, the hardness after cold-rolling did not
decrease so much as the annealing temperature rose up
to 650uC, and it dropped significantly at 675700uC.
This result corresponded to the microstructural change.
Elongated large ferrite grains formed by recovery of the
Materials Science and Technology 2015 VOL 31 NO 6 749
Okitsu et al. Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel
7 ND orientation colour maps for whole measured area in EBSD measurements of low C steel a after cold-rolling by
91% reduction, and after subsequent annealing at b 620uC, c 635uC and d 680uC for 120 s followed by water-cooling
observed from TD: colours indicate crystal orientation parallel to ND, according to stereographic triangle shown in
gure
cold-rolled microstructure were seen at the annealing
temperatures below 675uC. Then, equiaxed ferrite grains
suddenly appeared in the recovered ferrite matrix at
675uC. This behaviour is similar to that in interstitial
free (IF) steels reported by Takechi et al.,24 and is typical
in recrystallisation of carbon steels.
On the other hand, in the present specimen starting
from the DP microstructure, the hardness of the cold-
rolled specimen decreased continuously as the annealing
temperature increased up to 670uC. As was shown in
Fig. 2df, the microstructures of the specimens starting
from DP only showed continuous coarsening of all
ferrite grains when the annealing temperature rose from
600 to 675uC. This result was different from that of
conventional recrystallisation in carbon steels.
Texture change
Figure 7 shows ND orientation colour maps of the
specimens after 91% cold-rolling, and after subsequent
annealing at 620, 635 and 680uC for 120 s. The colour
indicates the crystallographic orientation parallel to ND
at each region, according to the stereographic triangle
shown in the figure. The displayed regions in Fig. 7ad
correspond to the whole measured regions of each
specimen. For the cold-rolled specimen (Fig. 7a), there
are a number of black points with less accuracy because
of the strains introduced by the cold-rolling. However,
some fine ferrite grains having different colours from the
deformed matrix are observed in Fig. 7a. This meant that
ultrafine regions (grains) having various orientations
already existed in the as-cold-rolled state, as was also
suggested in Fig. 3. In the specimens annealed at 620 and
635uC (Fig. 7b and c), equiaxed ferrite grains having
crystal orientations near ,001. (coloured in red) and
,111. (coloured in blue) were dominant. They were
fully annealed grains with low dislocation densities. As
the annealing temperature increased up to 680uC
(Fig. 7d), coarse grains having orientations near ,110.
(indicated by the colours between light green and light
blue, or light grey in black and white version) increased.
750 Materials Science and Technology 2015 VOL 31
Here, textures of the specimens are shown quantitatively
using pole figures. It is well known that the cold-rolling
texture of bcc ferrite in carbon steels is composed of two
fibre components: a-fibre (,110. parallel to RD) and
c-fibre (,111. parallel to ND).2426 Generally in carbon
steels, when the cold-rolled specimens are annealed at
elevated temperatures, recrystallisation occurs and the
c-fibre texture develops.2426 Figure 8 shows (001) pole
figures constructed from the orientation data obtained by
the EBSD measurements of the 91% cold-rolled specimen
(Fig. 8a) and the subsequently annealed specimens
(Fig. 8bd). In Fig. 8e, positions of major orientations
appearing in cold-rolled and annealed bcc crystals are
indicated. As shown in Fig. 8a, the cold-rolled specimen
had a typical cold-rolling texture of carbon steels where a-
fibre and c-fibre were dominant.25 The texture after
annealing at 620uC (Fig. 8b) was still composed of the a-
fibre and c-fibre components. This feature was maintained
at the annealing temperature of 635uC (Fig. 8c). As the
annealing temperature increased up to 680uC, the two fibre
components still remained. However, the intensities of
other orientations off the fibre components seemed to
increase (Fig. 8d).
In order to evaluate the change in texture more
quantitatively, orientation distribution function (ODF)
analysis was carried out using the EBSD orientation data.
The Bunge notation, in which the crystal rotations are
described by three Euler angles, Q1, W and Q2, was
employed. Figure 9ac shows ODF maps of the speci-
mens corresponding to Fig. 8a, b and d, respectively. In
Fig. 9d, positions of major orientations appearing in
cold-rolled and annealed bcc crystals are indicated in
Q250u, 45u and 90u sections of ODFs. The two fibre
components in typical cold-rolling or recrystallisation
textures in carbon steels appear in the Q2545usection in
Fig. 9d. Figure 9a shows ODF sections at various Q2
values between 0 and 90u of the 91% cold-rolled specimen.
The ODFs showed a typical cold-rolled texture in low C
steels.26 For example, the Q2545u section showed
NO 6
 Okitsu et al.
8 (001) Pole gures obtained by EBSD measurements of low C steel a after cold-rolling by 91% reduction, and after sub-
sequent annealing at b 620uC, c 635uC and d 680uC for 120 s followed by water-cooling: e major orientations appearing
in cold-rolled and annealed bcc crystals indicated in (001) pole gure
concentrations of crystal orientations involved in the a-
fibre and c-fibre. Figure 9b shows ODFs of the specimen
cold-rolled by 91% and subsequently annealed at 620uC.
The texture was close to that of the cold-rolled specimen
(Fig. 9a). However, it was different from typical recrys-
tallisation texture of low C steels where the c-fibre is
dominant,26 even though a fully annealed equiaxed grain
structure formed. The intensity of a-fibre component was
enhanced compared with the cold-rolled specimen.
Figure 9c shows ODFs of the specimen cold-rolled by
91% and annealed at 680uC. In the Q2545u section of the
ODFs, the features of the cold-rolled texture (a-fibre and
c-fibre components) still remained. However, other
orientations off the two fibre components appeared.
For example, the Euler angles of the new orientations
were (Q50u, W555u, Q250u), (Q150u, W555u, Q2590u)
and (Q1560u, W590u,
  Q2545u), which  correspond to
(032)[100], 302 010 and 110 225 in Miller indices,
respectively. These orientations had ,110. poles close to
ND. The appearance of these new orientations in Fig. 9c
is consistent with the result of the ND orientation colour
map in Fig. 7d, showing the increase in green and light
blue grains. In summary, the equiaxed UFG ferrite
microstructures obtained in this study had textures close
to the typical cold-rolled texture of carbon steels, while
other orientations appeared by increasing the annealing
temperature.
Discussion
In this section, the UFG ferrite formation in the present
process is discussed. The microstructural analyses of the
present cold-rolled specimen revealed ultrafine lamellar
structures with large local misorientations in both ferrite
and martensite (Fig. 3), although the equivalent strain
applied to the specimen was only 2?8. Such fine lamellar
Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel
structures have been previously observed in Al27 and IF
steel28 heavily deformed to equivalent strains above 4 or
5. As was discussed in our previous studies,6,18 local
lattice rotations in ferrite in the vicinity of hard
martensite and redundant shear strain28 introduced to
ferrite matrix due to the existence of hard martensite
(wavy microstructure of ferrite in Fig. 2a) accelerated
the microstructural refinement and the development of
large misorientations. The strain substantially applied to
martensite in the present study seemed smaller than the
averaged plastic strain applied to the specimen (91%
reduction) but probably enough to introduce the fine
structures having large local misorientations in marten-
site, as Ueji et al.19 have reported similar UFG
structures having large local misorientations in a 50%
cold-rolled martensite in a 0?13%C steel.
During the subsequent annealing, as shown in
Fig. 2bf, the cold-rolled microstructure changed to be
equiaxed UFG ferrite gradually as the annealing
temperature increased up to 600uC. The process should
be naturally considered as recrystallisation. However, it
was different from typical recrystallisation characterised
by nucleation and growth, i.e. an appearance of some
recrystallised grains and their preferential growth repla-
cing the deformed matrix.29 Figure 6 revealed that the
hardness of the cold-rolled specimen continuously
decreased as the annealing temperatures increased up
to 670uC, which was quite different from the change in
hardness involving a significant drop at certain tem-
peratures during typical recrystallisation.
The main texture components observed in the cold-
rolled specimen did not change greatly during the
annealing up to 635uC. As the annealing temperature
increased to 680uC, ferrite grains having different crystal
orientations from a- and c-fibres grew preferentially
(Figs. 8d and 9c). In conventional recrystallisation of
Materials Science and Technology 2015 VOL 31 NO 6 751
Okitsu et al. Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel

9 Orientation distribution functions (in Bunge notation) of specimens after a cold-rolling by 91% reduction, b 91% cold-
rolling and subsequent annealing at 620uC for 120 s and c 91% cold-rolling and subsequent annealing at 680uC for
120 s: d major orientations typically observed in textures of cold-rolled and annealed bcc crystals indicated in Q250u,
45u and 90u sections of ODFs

carbon steels, recrystallised ferrite grains having
,111.//ND orientations preferentially develop con-
suming deformed matrix.25 The present results suggest
that the mechanism of the UFG ferrite formation in the
present study is different from typical recrystallisation in
conventionally cold-rolled and annealed ferritic steels.
Previous studies on textures of UFG steels fabricated
by plastic deformation and subsequent annealing have
shown similar behaviours. Kamikawa et al.30 have
shown that the texture of an IF steel ARB processed
by 7 cycles (equivalent strain of 5?6) did not change
greatly after subsequent annealing at 625650uC. It has
been explained in Ref. 30 that the ultrafine ferrite grains
with large misorientations to each other, which already
existed in the as-ARB processed state, grew homoge-
neously with recovery at grain interior during the
subsequent annealing. Song et al.22 have shown that
the texture of an UFG low C specimen fabricated by
warm compression and subsequent annealing still
contained strong a-fibre component. Song et al.22 have
pointed out this behaviour was due to microstructural
formation by recovery (not by conventional recrystalli-
sation). These results22,30 are consistent with the present
results.
Consequently, the process of UFG ferrite formation
observed in the present low C steel is summarised as
follows. Ultrafine regions having different crystal
orientations were introduced by the plastic deformation
(91% cold-rolling) of the ferritezmartensite dual-phase
structure. The hard martensite induced a strain con-
centration in ferrite, and the martensite was also
deformed adequately. Therefore, such ultrafine regions
with large misorientations formed in both ferrite and
martensite phases through cold-rolling. The ultrafine
regions in both phases grew continuously during
subsequent annealing accompanied by recovery at grain
interiors, and the equiaxed ultrafine grains equivalent to
recrystallised microstructures formed at 600635uC. For
the former martensite region in the starting microstruc-
ture, the ultrafine ferrite seemed to form through a
procedure of grain subdivision of the initial microstruc-
ture through cold-rolling and recovery during subse-
quent annealing, as Ueji et al.19 have pointed out in a
study on cold-rolling and annealing of a low C
martensite. For the former ferrite region, the ultrafine
ferrite grains were thought to form also through grain
subdivision and recovery, as was discussed in this
section. Therefore, the mechanism of ultrafine ferrite
formation from former martensite and former ferrite
regions are considered to be the same. There was
not clear difference in obtained ferrite grain size bet-
ween former martensite and former ferrite regions. In

752 Materials Science and Technology 2015 VOL 31 NO 6

 Okitsu et al.
addition, fine carbide particles observed in the micro-
structures after annealing (Fig. 2d and e) should
contribute to the suppression of ferrite grain growth.
As the annealing temperature increased furthermore,
further coarsening of ferrite grains occurred without
preferential growth of particular ferrite grains, and
without losing the feature of the cold-rolled texture.
There have been some studies on processes including
plastic deformation of dual-phase microstructures in low
C steels. Azizi-Alizamini et al.31 applied 50% cold-
rolling and subsequent annealing to a ferrite-martensite
dual-phase microstructure in a 0?17% C steel, aiming to
fabricate a bimodal microstructure having two peaks in
the grain size distribution profile.32 The obtained
microstructure in Ref. 31 was not a uniform UFG one
but composed of fine ferrite grains with mean grain size
of 2 mm and coarse grains with sizes of 3 to 15 mm.
Recently, Wang et al.33 prepared a ferritemartensite
dual-phase microstructure of a 0?12%C steel, and
applied 64% cold-rolling and subsequent annealing at
560uC for 90 min. The microstructure they obtained33
was a mixture of ultrafine ferrite grains with mean grain
size of 0?7 mm and coarse grains with sizes of 7 mm, not
a uniform UFG ferrite. The volume fraction of ultrafine
ferrite in the whole microstructure they33 obtained was
60%. The rolling reductions they31,33 took, which were
smaller than that in the present study (91%), seem
insufficient to get uniform UFG structures. These
results31,33 suggest that the uniformity of the UFG
microstructures obtained through the present thermo-
mechanical process is strongly affected by process
conditions, such as cold-rolling reduction and subse-
quent annealing temperature. Volume fraction and
morphology of martensite in the starting microstructure
may be also important. In other words, an optimum
condition range in order to obtain uniform UFG ferrite
microstructures may exist in the thermomechanical
process starting from ferritezmartensite dual-phase
structures. The effect of starting microstructure, rolling
reduction and annealing temperature will be clarified
and shown in our next paper.
Conclusions
By applying the simple thermomechanical process
composed of conventional cold-rolling and annealing
of ferritezmartensite dual-phase structures in low C
steels, large sheet specimens having UFG FC micro-
structures could be obtained. The formation of the UFG
ferrite microstructures during the thermomechanical
process was investigated and discussed in this paper.
The obtained results are summarised below.
1. After 91% cold-rolling, ultrafine regions having
various crystal orientations already existed in both
ferrite matrix and martensite islands. During subsequent
annealing, the cold-rolled microstructure gradually
changed to become equiaxed ultrafine ferrite grains that
were equivalent to fully recrystallised microstructures.
Uniform UFG FC microstructures having mean ferrite
grain size of 0?45 mm were formed by annealing at
600uC, and the ferrite grains continuously coarsened by
increasing the annealing temperature up to 680uC. No
particularly large recrystallised grains were observed at
any of the annealing temperatures.
2. The hardness of the cold-rolled specimen continu-
ously decreased as the annealing temperature increased
Ultrafine ferrite formation through cold-rolling and annealing of dual-phase steel
up to 670uC. A significant drop of hardness, which is
usually observed in conventional recrystallisation of
deformed metals, was not observed.
3. The cold-rolled specimen showed the typical cold-
rolling texture of carbon steels composed of a-fibre and
c-fibre orientations. The main components of texture in
the cold-rolled specimen did not change greatly after
subsequent annealing at 620uC, where a uniform UFG
microstructure formed. This feature was maintained up
to 635uC. When the annealing temperature increased up
to 680uC, the feature of the cold-rolled texture still
remained, while other orientations appeared. The
maintenance of the cold-rolled texture below 635uC
was also different from the textural characteristics in
conventional recrystallisation of carbon steels.
4. Based on these results, it was suggested that the
ultrafine regions having large misorientations to each
other in the cold-rolled specimen grew continuously
during subsequent annealing accompanied by recovery
processes, and formed the equiaxed UFG ferrite
microstructures.
Acknowledgements
One of the authors (N. Tsuji) gratefully acknowledges
the financial support from the Grant-in-Aid for
Scientific Research on Innovative Area, Bulk
Nanostructured Metals (area no. 2201), the Grant-in-
Aid for Scientific Research (A) (no. 24246114), and the
Elements Strategy Initiative for Structural Materials
(ESISM), all through the Ministry of Education,
Culture, Sports, Science and Technology (MEXT),
Japan.
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