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A Study of the Batch Annealing of Cold-Rolled HSLA Steels Containing

Niobium or Titanium

Article  in  Metallurgical and Materials Transactions A · August 2015

DOI: 10.1007/s11661-015-2949-6

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A Study of the Batch Annealing of Cold-Rolled HSLA
Steels Containing Niobium or Titanium
CHAO FANG, C. ISAAC GARCIA, SHI-HOON CHOI, and ANTHONY J. DEARDO

The batch annealing behavior of two cold-rolled, microalloyed HSLA steels has been studied in
this program. One steel was microalloyed with niobium while the other with titanium. A suc-
cessfully batch annealed steel will exhibit minimum variation in properties along the length of
the coil, even though the inner and outer wraps experience faster heating and cooling rates and
lower soaking temperatures, i.e., the so-called ‘‘cold spot’’ areas, than the mid-length portion of
the coil, i.e., the so-called ‘‘hot spot’’ areas. The variation in strength and ductility is caused by
differences in the extent of annealing in the different areas. It has been known for 30 years that
titanium-bearing HSLA steels show more variability after batch annealing than do the niobium-
bearing steels. One of the goals of this study was to try to explain this observation. In this study,
the annealing kinetics of the surface and center layers of the cold-rolled sheet were compared.
The surface and center layers of the niobium steel and the surface layer of the titanium steel all
showed similar annealing kinetics, while the center layer of the titanium steel exhibited much
slower kinetics. Metallographic results indicate that the stored energy of the cold-rolled con-
dition, as revealed by grain center sub-grain boundary density, appeared to strongly influence
the annealing kinetics. The kinetics were followed by the Kernel Average Misorientation re-
construction of the microstructure at different stages on annealing. Possible pinning effects
caused by microalloy precipitates were also considered. Methods of improving uniformity and
increasing kinetics, involving optimizing both hot-rolled and cold-rolled microstructure, are
suggested.

DOI: 10.1007/s11661-015-2949-6
 The Minerals, Metals & Materials Society and ASM International 2015

I. INTRODUCTION
PRODUCT uniformity is an important attribute for
steel in a highly competitive market. In the production of
annealed cold-rolled gages of microalloyed HSLA steels
using the batch annealing process, minimum variation of
properties along the coil length is important. For cold-
rolled and annealed steels, one of the principal sources of
strength in partially recrystallized steels is the non-
recrystallized regions, where high dislocation densities
survive through the anneal. The larger the amount of
these regions of high retained strain or stored energy, the
higher will be the strength. The variation in heating rate
and annealing temperature between the ‘‘cold’’ spot (mid-
coil length) and ‘‘hot’’ spot (coil ends) in large coils is
largely responsible for the variation in strength and other
mechanical properties along the coil length after batch
CHAO FANG, is with the Global Foundries Inc., Malta, New
York 12020. C. ISAAC GARCIA, Professor, is with the Department
of Mechanical Engineering and Materials Science, University of
Pittsburgh, Pittsburgh, PA 15261. SHI-HOON CHOI, Professor, is
with the School of Applied Materials Engineering, Sunchon National
University, 413 Jungangno (315 Maegok) Suncheon, Jeonnam 540-
742, South Korea. ANTHONY J. DEARDO, is with the Basic Metals
Processing Research Institute (BAMPRI), Department of Mechanical
Engineering and Materials Science, University of Pittsburgh, Pittsburgh,
PA 15261, and Finland Distinguished Professor with the Oulu
University, Centre for Advanced Steels Research, Oulu, Finland.
Contact e-mail: ajdeardo.pitt@gmail.com
Manuscript submitted July 2, 2014.
Article published online May 19, 2015
annealing. The alloy design of the steel also plays a role in
the property variation. For example, it has been known
since the early 1980s that titanium microalloyed steels
were more difficult to recrystallize and had larger
property variations than did niobium steels, even when
annealed to the same cold spot strength and with
reasonably equal atom pct additions.[1] For example,
for steels annealed to the 350 MPa (50 KSi) strength
level, the Ti grade showed approximately twice the
strength variation along the coil length as did the Nb
grade, even when annealed to the same cold spot
temperature. Interestingly, these observations on batch
annealing are opposite to those found in numerous
studies of both the recovery and recrystallization of
austenite during hot rolling, and in the later line anneal-
ing studies of cold-rolled ferrite in ultra-low carbon or IF
steels. In the cases of hot rolling of austenite[2,3] and line
annealing of ferrite in IF steels,[4,5] it is now accepted that
Nb additions retard recovery and recrystallization more
strongly than do Ti additions. One of the goals of this
study was to investigate the reasons for this behavior,
especially the differences in annealing behavior between
steels containing either Nb or Ti in a batch annealing
simulation.[6]
It is well known that the kinetics of annealing are
controlled by diffusivity, driving forces and retarding
forces. The driving force for recovery and recrystalliza-
tion in annealing is the retained strain or stored energy
of cold work, while the retarding force is caused by
solute drag and/or precipitate pinning of sub-grain and

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 46A, AUGUST 2015—3635

grain boundaries. In this study, both the driving force
and the retarding force for static recovery and recrys-
tallization have been investigated.
The stored energy[7] in cold-rolled metals is associated
with various lattice defects generated during deforma-
tion and provides the initial driving force for recovery
and recrystallization during the annealing process. The
total amount and distribution of the stored energy will
dramatically affect the annealing behavior. In cold-
rolled metals of high stacking fault energy such as
ferrite, the stored energy can be considered to be the
sum of (i) the grain center dislocation density present in
sub-grain boundaries after cold rolling, and (ii) the extra
grain boundary energy resulting from the grain shape
change that occurs during cold rolling. The average
dislocation density has been estimated in the past by
both indirect methods, e.g., calorimetry, X-ray line
broadening, changes in strength,[8] and direct means,
e.g., etch pits[9] and transmission TEM.[10]
Electron back-scattered diffraction (EBSD)[11] is a
relatively new analytical technique, which has evolved
into a powerful tool for the crystallographic analysis of
steels and other engineering materials using the scanning
electron microscopy (SEM). The automatic analysis of
these EBSD patterns yields the crystallographic orien-
tation, the phase present and the value indicating the
quality of the diffraction pattern for every scan point.
From these data, the microstructure and texture of the
scanned area can be reconstructed, as well as informa-
tion gained concerning the presence or absence of lattice
perfection through elastic distortion of the Kikuchi
bands and its resulting diffraction distortions.[12,13]
Taylor factors calculated from EBSD scanning data
were also used in early applications as a measurement of
an orientation-dependent stored energy in cold-rolled
steels.[14,15] However, the assumption of the upper
bound or full constraint method (stress and strain rate
are assumed uniform in each grain) is not appropriate to
simulate the heterogeneous distribution of stored energy
found in the deformed grains.
In the current study, the EBSD data have been
analyzed to determine the summation of sub-grain
boundary energy in the investigated steels. This has led
to what is now referred to as Stored Energy Maps,
which attempt to measure the effect of the elastic strain
in the matrix caused by dislocation density and solute
atoms.[16,17] To this grain-center stored energy was
added the extra grain boundary energy resulting from
the grain shape change associated with the cold rolling.
The resulting sum was taken as the total stored energy.
The stored energies of the hot band, cold-rolled, and
annealed conditions of the two steels were determined
using this approach. These results were then related to
the observed annealing kinetics of the two steels.
Table I. Nominal Compositions of the Steels Used in this Study (Weight Percent)
C Mn Si
Ti-bearing 0.046 0.730 0.191
Nb-bearing 0.053 1.068 0.194
3636—VOLUME 46A, AUGUST 2015
II. EXPERIMENTAL PROCEDURE
The chemical compositions of the 350 Grade HSLA
steels (nominal YS 350 MPa, 50 KSi) used in this study
are listed in Table I. Commercial hot band and full-hard
(cold rolled) samples were supplied from a thin slab
casting steel company. The cold reductions used were
approximately 58 pct for the Ti-bearing steel and 55 pct
for the Nb-bearing steel, respectively. The final thick-
nesses were approximately 1.25 mm for the Ti steel and
1.40 mm for the Nb steel. The difference in cold
reduction was not considered important since they were
similar. Also, the differences in final gage were not
thought to be important during annealing since the
annealing temperatures were subcritical and the heating
and cooling rates were very slow.
Small samples were sectioned from these conditions
and reheated from room temperature to 943 K (670 C)
at a heating rate of about 16 K/h (16 C/h). All samples
were put into the furnace at the same time and
individual specimens were removed at every 20 K
(20 C) interval from 873 K to 933 K (600 C to
660 C) and at different soaking times ranging from 2
to 8 hours, then water quenched to room temperature.
These quenched samples were cut along the rolling
direction into smaller pieces, about 10 mm in length and
5 mm in width, and thermo-mounted using bakelite for
optical metallography or copper powder for SEM/
EBSD metallography. Then, they were ground on
400 to 2400 grit silicon carbide abrasive paper and
polished with 0.05 lm alumina power on abrasive
cloths. The vibratory polishing machine and 0.05 lm
alumina power were used for the final polishing step.
These samples could then be used for EBSD analysis. In
addition, the samples were etched with 2 pct Nital to
observe the microstructures in the SEM. A TSL EBSD
system attached to a Philips XL30 FEG SEM was used
for scanning the desired areas. The original raw data
were collected using the TSL OIM data collector
software. The SEM was operated at 20 kV voltage and
the beam spot size used was 6 or 5. The scanning step
size was about 0.2 lm.
For further analysis of small precipitates and to
obtain additional crystallographic data, transmission
electron microscopy (TEM) utilizing a JEOL 200CX
and a JEOL 2100F was used. The TEM studies were
conducted at 200 kV, 118 lA, and a beam spot size of 2.
Thin foil sample preparation involved sectioning the
samples, mechanical or chemical thinning, and elec-
tropolishing. After thinning, the foils were then punched
into 3 mm disks and electropolished until perforation
using a Fischione twinjet electropolisher with an elec-
trolyte solution of Na2CrO3 (20 pct by weight) and
acetic acid (80 pct). Finally, the samples were cleaned
Cu Nb V Ti N
0.127 0.003 0.004 0.058 0.009
0.148 0.032 0.002 0.010 0.007
METALLURGICAL AND MATERIALS TRANSACTIONS A
using a three step ethanol cleaning process to remove all
residues from the specimens.
Since it is common for the microstructure to vary
through the thickness, each specimen was observed at
five different depths. Figure 1 illustrates schematically
the five different layers or depths through the thickness
where measurements and observations were made.
Unless stated otherwise, the measurements and obser-
vations presented below were taken from the center or
mid-thickness region. Figure 1 also shows the orienta-
tion of the observed regions with respect to the original
hot band rolling direction. The microhardness values
were measured using the Vickers test on a Leco M-400-
G Hardness Tester, employing a 500 g load and a
15 seconds dwell time. The results were plotted as the
average value of three layers (surface, quarter point,
center) and with 10 measurements per layer. The
standard deviation of the mean value for any group of
measurements was less than 4 pct.
To access the total stored energy of the cold-rolled
condition going into the anneal, two sets of measure-
ments were made. The first was the sum of the stored
energy of the sub-grain boundaries found in the ferrite
grain centers. The second was the contribution from the
ferrite grain boundaries which became elongated during
the cold rolling. These two were added to estimate the
total stored energy of cold work available to drive the
recovery and recrystallization in the anneal.
The sub-grain method[17] was used in this study to
construct stored energy distribution maps. The sub-
grain structure in the grain centers of the deformed
microstructure was used in the calculation of the
dislocation-related stored energy, since the plastic de-
formation of polycrystalline steels normally shows the
dislocations in a sub-grain boundary network, typical of
high stacking fault alloys. If the dislocation substructure
can be simplified in the form of sub-grains of diameter,
D, and boundary energy, c, then the stored energy, Si of
each lattice site, can be given by Eq. [1]:
c each pixel equal to the average misorientation of that
Si ¼ a ;
D particular pixel with its neighbors
where a is the geometric constant ~3. If it is assumed
that the boundary energy of a sub-grain is only a func-
tion of the boundary misorientation (Dh) and not de-
pendent on the boundary types (tilt and twist), the
R
Surface Quarter Center
D the recovery and recrystallization processes in both hot
layer Point layer layer
T rolling of austenite and cold rolling and annealing of
D
Fig. 1—Schematic illustration of areas examined in each specimen.
METALLURGICAL AND MATERIALS TRANSACTIONS A
boundary energy from the Read–Shockley[18] relation
can be expressed in Eq. [2]:
( 0
h  0 i
cm hh 1  ln hh ; h0 < h
cðDhÞ ¼ ½2
cm ; h0  h
where h¢ = |Dh| for 0 £ |Dh| £ p and h¢ = 2p  |Dh|
for p £ |Dh| £ 2p. In this approach, Dh is the boundary
misorientation between two neighboring sub-grains, h*
is the misorientation limit for low-angle grain bound-
aries, which was chosen as 15 deg, and cm is the specific
energy of high-angle grain boundaries which was taken
to be 0.756 J/m2.
The grain boundary contribution to stored energy was
estimated through the use of Eq. [3].
Total high angle GB Energy
½3
¼ SvðGBÞ  7:56  105 J=cm2
In this equation, the grain boundary area per unit
volume, SV in cm2/cm3, was measured for the various
conditions using Eq. [4].[19]
SvðGBÞ ¼ 0:429ðNL Þk þ 1:571ðNL Þ? ; ½4
where (NL)k and (NL)^ are the intercept numbers per
unit length along the rolling and thickness directions,
respectively.
However, it will be shown later that the energy stored
in the grain boundaries is much lower than that stored in
the sub-grain boundaries. It is estimated that about
10 pct of the total stored energy resides in the high-angle
ferrite grain boundaries, while the balance is related to
the dislocations and sub-grain boundaries. Another
method of measuring and displaying the amount and
distribution of stored energy is by determining Kernel
Average Misorientation (KAM) maps.[20] This tech-
nique is based on the point-to-point lattice rotation
within a grain or specimen. These data have a value for
½1
As the internal strain and lattice imperfection varies,
the disparity is depicted by changes in value of the
KAM. In the standard representation, the magnitude of
the KAM representing a near-perfect lattice region is
given a small value, whereas areas of larger elastic strain
are assigned larger values. In this study, the color blue is
assigned to very small KAM values (recrystallized
areas), while the color red to very large ones (high
stored energy). This color representation permits a
highly visible summary of the local elastic strain
N distribution in the specimen, including stored energy in
recrystallization studies and transformation strains in
D
phase transformation studies
Niobium and titanium are known to be very effective
as microalloying additions in steels. They can influence
ferrite. It is well known that they do so by solute drag
and/or pinning of sub-grain boundaries by nitride and
carbide precipitates, thereby influencing the final mi-
VOLUME 46A, AUGUST 2015—3637
crostructure and properties. There have been some
interesting recent studies of the effects of niobium and/
or titanium additions in steels. Belyakov et al., studied
the development of primary recrystallization in ferrite in
a steel containing 0.4 pct of volume of fine TiC
precipitations with an average particle size of
12 nm.[21] After sufficiently large cold strains, the
recrystallization developed readily upon annealing at
temperatures above 873 K (600 C). Not surprisingly,
an increase in the cold strain as well as the annealing
temperature resulted in the acceleration of recrystalliza-
tion kinetics. However, a certain amount of the cold
worked microstructure, about 15 pct of volume, re-
mained unrecrystallized even after annealing at a rather
high temperature of 973 K (700 C). The unrecrystal-
lized portions were composed of grains with the h0 0 1i
crystallographic direction parallel to the compression
axis. Both the low stored energies in these grains after
cold deformation and the pinning of recrystallizing grain
boundaries by the dispersed carbides were discussed as
crucial factors that resulted in the incomplete recrystal-
lization. On the other hand, small amounts of niobium
in steels have also been known to affect both the
microstructure and properties. The topic of niobium in
steels has been covered extensively in a review paper by
DeArdo.[22] Recent research by Hutchinson et al., illus-
trated the comparative effectiveness of solute Nb and
NbC particles in impeding grain boundary motion with
a theoretical treatment.[23] The Nb can be present both
as solute in solution, where it is thought to exhibit a
strong solute drag effect, or as NbC precipitates, which
are thought to be effective at pinning sub-grain and
grain boundaries. It was shown that, for a steel
containing ~0.05 at pct Nb (~0.1 wt pct Nb), under
typical recrystallization conditions, solute Nb is more
effective in the ferrite, whereas in the austenite, depend-
ing on the exact recrystallization temperature, either
solute Nb or NbC precipitates may be more effective.
The goal of this current study was to determine the
annealing kinetics of two cold-rolled microalloyed
HSLA steels during a batch annealing simulation, and
to determine the operative driving and retarding forces.
The driving force was to be followed using the EBSD
Stored Energy approach, while the retarding force was
to be evaluated by precipitate observations using thin
foil electron microscopy. A better understanding of
these forces would then be the basis for understanding
how to both improve property uniformity and shorten
the required process time.
III. RESULTS AND DISCUSSION
The changes in microhardness (VHN-500 g) values,
measured at the mid-thickness location, from the cold
rolled to the annealed conditions up to 933 K (660 C) for
both steels are shown in Figure 2. A significant drop in
hardness occurred between 853 K and 873 K (580 C and
600 C), meaning that significant softening by advanced
recovery or polygonization or the onset of recrystalliza-
tion had started there for both steels. But the hardness of
Nb-bearing steel decreased much faster than did the Ti-
3638—VOLUME 46A, AUGUST 2015
Microhardness (VHN)
300
Ti-based
Nb-based
250
200
150
CR 350 540 560 580 600 620 640 660
Quench Temperature (°C)
Fig. 2—Comparison of average through thickness microhardness
values in specimens quenched from different annealing temperatures.
bearing steel, and it seems to reach a lower plateau at
around 903 K (630 C), while the hardness of Ti-bearing
steel was still continuing to drop up to 933 K (660 C).
Therefore, the Nb steel had a faster rate of softening, i.e.,
recrystallization, than the Ti-bearing steel. The higher
annealing kinetics exhibited by the Nb steel are important
since they would help minimize the difference in mi-
crostructure generated during the annealing process. The
sluggish annealing kinetics shown by the Ti steel means
that the final microstructure would be more sensitive to
variations within the process, i.e., annealing near the hot
spot versus cold spot.
This difference in annealing behavior could also be
observed by the microstructural changes observed in the
SEM and shown in Figure 3, using secondary electron
diffraction imaging. This figure shows the microstructure
evolution at the centerline of the Nb-bearing steel from
Figures 3(a) through (e), while Figures 3(f) through (j)
show the Ti-bearing steel. This same evolution is present-
ed in Figure 4 based on the KAM approach. In Figure 4,
only the center region of the Nb steel was shown because
the surface and center regions showed similar kinetics.
Both the surface and center regions of the Ti steel were
used, since they exhibited such different kinetics. Clearly,
the Nb-bearing steel recrystallized much faster than the
Ti-bearing steel, based on grain shape or aspect ratio, and
the KAM results, all of which corresponded well with the
hardness drops.[6]
Kernel average misorientation maps shown in Fig-
ure 4 calculated from EBSD data are used in this study
to evaluate the fraction of recrystallized area in each
condition. As mentioned above, in the KAM data
representation, the red or orange colored regions denote
high lattice distortion or high dislocation density, while
the blue colored regions denote a relatively undistorted
lattice, i.e., full recrystallization. The fractions of re-
crystallized area were compared in Figure 5. The first
thing to note in the data of Figure 5 is that the kinetics
are faster in the surface regions than the center for each
steel. The kinetic curves can be compared with regard to
rates in the sequence from high to low: Nb(Surface),
Nb(Center), Ti(Surface), and Ti(Center), where the first
three are similar, but the fourth is much slower. A
comparison of the surface to center behavior revealed
that the Nb-bearing steel had a more uniform annealing
behavior than did the Ti-bearing steel, since the surface
and center recrystallization kinetics in the Nb steel were
very similar. It should also be noted that the surface and
center curves indicated that annealing was nearly
METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 3—Microstructure evolution of Nb-bearing steel: (a) cold rolled, (b) 873 K (600 C), (c) 893 K (620 C), (d) 913 K (640 C), (e) 933 K
(660 C); and Ti-bearing steel: (f) cold rolled, (g) 873 K (600 C), (h) 893 K (620 C), (i) 913 K (640 C), (j) 933 K (660 C). Centerline observa-
tions.

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 46A, AUGUST 2015—3639

Fig. 4—Kernel average misorientation maps of Nb-bearing steel at center layer: (a) 873 K (600 C), (b) 893 K (620 C), (c) 913 K (640 C), (d)
933 K (660 C); and Ti-bearing steel at surface layer: (e) 873 K (600 C), (f) 893 K (620 C), (g) 913 K (640 C), (h) 933 K (660 C); and
Ti-bearing steel at center layer: (i) 873 K (600 C), (j) 893 K (620 C), (k) 913 K (640 C), (l) 933 K (660 C).

completed throughout the Nb steel at 898 K (620 C),
whereas the annealing of the Ti steel was still evolving
up to 948 K (670 C), especially at the mid-thickness.
These different features from surface to center and in the
time scale are very likely the cause of the difference in
property level variation frequently observed between the
two steels in batch annealing.
The grain boundary misorientation distributions for
both steels were also measured using EBSD. The
fraction of low-angle grain boundaries (<15 deg) is high

3640—VOLUME 46A, AUGUST 2015 METALLURGICAL AND MATERIALS TRANSACTIONS A


Fraconof recrystallized area (%)
Fig. 5—Comparison of the fraction of recrystallized area during an-
nealing based on KAM measurements.
0.45
0.35
Fraction
100 Stored energy distribution maps and changing trends
calculated from the EBSD scanning data from the
90
centerline location using the grain center sub-grain
80 method are shown in Figures 7 and 8. Since the starting
hot band grain sizes are different, it was decided that the
70
total stored energy should be used, as it comprised
60 contributions from both the grain boundaries and grain
center sub-grain boundaries. The total stored energy in
50
the surface and centerline regions of both hot rolled and
40 cold rolled, including contributions from both grain
Ti-bearing Surface center sub-grain boundaries and ferrite grain bound-
30 aries, is presented in Figures 9 and 10, and summarized
Ti-bearing Center
20 in Tables II, III, and IV. Figures 7, 8, and 10 were
Nb-bearing Surface reconstructured from data taken at 10009 with a step
10 Nb-bearing Center size of 0.2 lm.
0
The data of Table II, calculated based on the average
CR 580 600 620 640 660 670 670-1 670-2 670-4 670-6 grain size and assuming no variation in ferrite grain size
Annealing Stages or Temperature (°C) through the thickness in the hot-rolled condition, reveal
that the GB contribution is about 10 pct of the grain
center sub-grain contribution for both steels, and
furthermore comprises about 10.3 pct (Ti steel) to
11.4 pct (Nb steel) of the total stored energy. The stored
energy in the Nb steel is 87 pct higher than for the Ti
steel at the surface and 34 pct higher in the centerline
0.4 regions. Clearly, the hot band of the Nb steel has a much
larger stored energy than the Ti steel.
Table III, for the cold-rolled conditions, shows that
0.3
the total stored energy for the Nb steel is 11.4 pct higher
than for the Ti steel in both the surface and centerline

0.25 regions. However, the total stored energy of the cold

0.2
0.15
0.1
0.05
0 Therefore, based on the data of Table III, the Nb steel
0 5 10 15 20
Misorientation (Degree)
Cold Rolled
Fig. 6—Misorientation distribution changing trend during annealing.
Centerline area-Ti steel.
in the fully hard cold-rolled samples, since the very high
dislocation density resides mainly in the sub-grain, i.e.,
low-angle boundaries. As annealing progresses and
recrystallization commences, these low-angle boundaries
are replaced by high-angle grain boundaries. Therefore,
as annealing progresses, the amount or fraction of low-
angle boundaries will diminish, while the high-angle
boundaries (>15 deg) increases, as presented in Figure 6
for the centerline region of the Ti steel. The transition
from low-angle to high-angle boundaries is another
indication of the consumption of the stored energy as
recrystallization progresses. Both steels exhibited similar
trends, but at different annealing stages.
band for each location agrees well with the observed
recrystallization kinetics as presented in Figure 5, and
therefore can help explain the observed variation in
annealing behavior at different locations in the two
steels. Higher stored energy in the starting cold-rolled
state supplies higher initial driving force for recrystal-
lization which led to a higher rate of recrystallization.
25 30 35 40 45 50 55 60 65
surface would be expected to have the highest recrys-
tallization kinetics, followed by the Nb steel centerline,
Ti steel surface, and then Ti steel centerline. This is what
Partially Recrystallized
is observed, in fact. The data of Table IV illustrate the
Nearly Fully Recrystallized increase in total stored energy when the hot band
undergoes cold rolling. Again, the increase in total
stored energy resulting from cold rolling correlates well
with the variation of annealing kinetics with steel and
location, i.e., Nb steel surface the highest and Ti steel
center the lowest.
Figure 10 reveals that there is a certain amount of
deformed areas and grains that have rather little stored
energy, even after cold rolling. A similar observation
was also made in the Belyakov et al. study discussed
earlier.[21] There can be two interpretations of this
observation. First, that there can be a change in grain
shape in cold rolling with little accumulation of stored
energy, and second, that the dislocations generated
during cold rolling were very rapidly incorporated into
the sub-grain boundaries, i.e., either dynamic or rapid
static recovery. A similar phenomenon has been ob-
served before in the cold deformation of iron single
crystals.[24]

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 46A, AUGUST 2015—3641

 (a) (e)

Min: 0.503, Max: 17.956 Min: 0.487, Max: 17.978

(b) (f)

Min: 0.319, Max: 18.527 Min: 0.418, Max: 18.202

(c) (g)

Min: 0.303, Max: 16.304 Min: 0.475, Max: 18.016

(d) (h)

Min: 0.309, Max: 13.473 Min: 0.338, Max: 18.111

Fig. 7—Stored energy distribution maps of Nb-bearing steel at center layer: (a) 873 K (600 C), (b) 893 K (620 C), (c) 913 K (640 C), (d)
933 K (660 C); and Ti-bearing steel at center layer: (e) 873 K (600 C), (f) 893 K (620 C), (g) 913 K (640 C), (h) 933 K (660 C).

3642—VOLUME 46A, AUGUST 2015 METALLURGICAL AND MATERIALS TRANSACTIONS A

 Ti-bearing Fr Nb-bearing Fr Ti-bearing SE Nb-bearing SE

100.00 6.00

Fraction of Recrystallized Area (%)

5.68

Average Stored Energy (J/cm3)

90.00
5.15 5.12 5.00
80.00 4.88
70.00 4.00
60.00 3.73

50.00 3.08 3.00

40.00
2.00
30.00
1.64
20.00 1.27
0.92 1.00
10.00 0.71

0.00 0.00
Cold Rolled 600°C 620°C 640°C 660°C
Stage

Fig. 8—The change in average grain center stored energy (SE) and the fraction of recrystallized area (Fr) during annealing.

(a) (b) (c) (d)

Min: 0.453, Max: 16.694 Min: 0.328, Max: 16.366 Min: 0.282, Max: 16.126 Min: 0.265, Max: 16.483

Fig. 9—Stored energy distribution maps for hot band samples of (a) Nb steel at surface layer, (b) Nb steel at center layer, (c) Ti steel at surface
layer, (d) Ti steel at center layer.

(a) (b) (c) (d)

Min: 0.724, Max: 18.059 Min: 0.810, Max: 18.141 Min: 0.384, Max: 18.515 Min: 0.377, Max: 18.274

Fig. 10—Stored energy distribution maps for cold-rolled samples of (a) Nb steel at surface layer, (b) Nb steel at center layer, (c) Ti steel at sur-
face layer, (d) Ti steel at center layer.

Since the lattices of the microalloyed precipitates they form on grain or sub-grain boundaries, they can
(NaCl type) do not fit well with either the austenite hinder the motion of these defects leading to the
(FCC) or ferrite (BCC) lattices, the particles must suppression of recovery and recrystallization. Palmiere
form heterogeneously on pre-existing crystalline de- et al. showed that the local pinning force exerted by
fects such as grain or sub-grain boundaries, interphase particles on a flexible sub-grain boundary can be
interfaces or even individual dislocations.[22] When expressed in Eq. [3]:

METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 46A, AUGUST 2015—3643

 Table II. Comparison of the Stored Energy (J/cm3) in the Hot Band Before Cold Rolling

Ti Steel Nb Steel
Steel/Location
S. E. Region GB Matrix Total GB Matrix Total
Surface 0.280 0.750 1.03 0.493 1.40 1.893
Centerline 0.242 0.651 0.893 0.323 0.87 1.193

Table III. Comparison of Stored Energy (J/cm3) with Location in Cold Band Before Anneal

Ti Steel Nb Steel
Steel/Location
S. E. Region GB Matrix Total GB Matrix Total
Surface 0.470 5.52 5.99 0.582 6.09 6.672
Centerline 0.470 5.15 5.62 0.582 5.68 6.262

Table IV. Total Change in Stored Energy (J/cm3) Hot Rolled to Cold Rolled

Steel/Location CR Total HB Total Difference

Ti surface 5.99 1.03 4.96
Ti center 5.62 0.893 4.729
Nb surface 6.672 1.893 5.479
Nb center 6.262 1.193 5.069

FP ¼ 3cfl=ð2pr2 Þ; ½3
where c is the surface energy between the particle and
the matrix, f is the local volume fraction of particles, l is
the sub-grain diameter, and r is the particle radius.[25]
Therefore, for an array of particles to exert a large
pinning force on a boundary, the ratio of f/r2 must be
high. In this investigation, several types of particles were
observed in annealed specimens, TiN, Ti4C2S2 and TiC
in the titanium steel and Fe3C in the niobium steel.
These particles were identified by selected area diffrac-
tion and EDS.[6] Although there were fine particles
observed in both steels, very few exhibited a f/r2 ratio
high enough to cause possible pinning effects that would
be expected to retard the observed annealing kinetics.
The role of particle pinning was, therefore, disregarded.
It should be mentioned that the small amount of TiC
precipitates found in the titanium steel exhibited the
Kurdjumov–Sachs orientation relationship, which
means the particles precipitated in the prior austen-
ite.[6,22] The absence of fine TiC or TiN with large f/r2 in
the Ti steel during annealing might be caused by
annealing well below the nose of the TTT curve for
precipitation of TiC in ferrite,[26] or by particle coars-
ening during the very slow heating rate and long
annealing times at the subcritical temperatures.[27] Jang
et al., have shown that the TiC particle size can
approach 3000 lm in radius at 928 K (700 C) in steels
that are hyper-stoichiometric with respect to Ti/C ratio
and held 1 hour at temperature.[27] This might be
another reason why particles fine enough to retard
recovery and recrystallization were not observed in the
Ti steel, which is also hyper-stoichiometric.
IV. CONCLUSIONS
1. The Batch Annealing Simulation used in this study
can be useful in programs to reduce property vari-
ability along the length of annealed coils and to un-
derstand how to accelerate the process.
2. The KAM and stored energy maps are valuable
methods of studying the formation and elimination
of retained strain or stored energy during cold roll-
ing and annealing. They are also helpful in follow-
ing the progress of softening during annealing.
3. The two steels used in this study exhibited different
recrystallization kinetics principally because of dif-
ferent levels of stored energy in the cold-rolled con-
dition. At similar cold reductions, the difference in
stored energy was caused by different hot band
stored energy and also possibly by variations in
work hardening during the cold rolling.
4. The Ti steel would be expected to have a larger var-
iation in properties along the coil because of the
large difference between hot spot and cold spot an-
nealing behavior. The large difference observed be-
tween surface and center regions observed in these
experiments for the Ti steel is a predictor of varia-
tion in properties along the coil length. The smaller
difference for the Nb steel means more uniform
properties.
5. The hot band microstructure plays an important
role in the behavior during cold rolling and anneal-
ing. Increasing the stored energy of the hot band
using higher cooling rates on the runout table, and
lowering the coiling temperature, or using larger
cold reductions, would be expected to increase the
hot band stored energy, shorten the annealing time,

3644—VOLUME 46A, AUGUST 2015 METALLURGICAL AND MATERIALS TRANSACTIONS A

 and increase property uniformity along the coil
length.
ACKNOWLEDGMENTS
The authors would like to thank the steel companies
that form part of the BAMPRI-Thin Slab Casting and
Rolling Consortium for providing the steel samples
and for their financial support for this program. In ad-
dition, the authors would like to thank the Basic Me-
tals Processing Research Institute (BAMPRI) and the
Mechanical Engineering and Materials Science Depart-
ment, University of Pittsburgh for providing the fa-
cilities to conduct this work. Special thanks are
extended to Dr. Kengun Cho, Dr. Xiaojun Liang, and
Professor Mingjian Hua as well as to Hoe-Seok Yang,
Long Li, Albert Stewart, Cole Van Ormer and Dr.
Ken Goldman, for their generous and constant help.
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