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JOURNAL OF IRON AND STEEL RESEARCH, INTERNATIONAL. 2013, 20(5): 42-49

Structure and Texture Formation During Single and Double Cold Rolling
and Annealing Processes for Nb+Ti Added Interstitial-Free Steels
FENG Yan-qing"' , WANG Fu-ming'*Z, T A O Su-fen'.' ,
ZHAO Dian-qing3, ZHANG Xiao-yan3
[l. State Key Laboratory of Advanced Metallurgy, University of Science and Technology Beijing, Beijing
100083, China; 2. School of Metallurgical and Ecological Engineering, University of Science and
Technology Beijing, Beijing 100083, China; 3. Baotou Iron and Steel (Group) Co. , Ltd. ,
Baotou 014010, Inner Mongolia, China]

Abstract: The structure and texture formation for single cold rolling (SCR) with annealing and double cold rolling
(DCR) with annealing were investigated based on optical microscope and X-ray diffraction (XRD) with a Nb+ Ti
bearing interstitial free (IF) steel. The results indicated that DCR recrystallization grain was smaller than that of
SCR sample and double cold rolling process resulted in better mechanical properties than those resulted from single
cold rolling process with the same total reduction conducted. The plastic strain ratio increases from 2. 23 for single
cold rolling process to 3. 2 for double rolling process. The fish-bone structure was observed in all SCR and DCR sam-
ples. DCR annealed sample is made up of equiaxed grains of almost uniform size, whereas SCR annealed sample
shows a duplex grain structure, consisting of both large and small-sized grains. ( T i f N b ) C and Fe(Ti+Nb)P type
precipitates were very rarely observed in SCR annealed and DCR annealed steels. The intensity of { 111) //ND for the
DCR annealing was higher than that for SCR annealing.
Key words: single cold rolling; double cold rolling; Nb; Ti; IF steel; structure; texture

Interstitial-free (IF) steels constitute one of the
major groups of formable steels used in automobile
industry worldwide. T h e main advantage with this
grade of steels is their excellent deep drawability,
which enables automobile body panels to be made in
intricate shapes. The formation of { 111} < uvw>
recrystallization texture in I F steel sheet continues
to be the subject of many detailed
Conventionally, the subsequent process following
hot rolling is large cold reduction with proper annea-
ling. Among the factors influencing the evolution of
the texture in I F steel, cold rolling and annealing
processes are the most important of all. Although
numerous investigations on texture formation during
single cold rolling (SCR) and subsequent recrystalli-
zation have been carried out with a view to produce
deep-drawing cold rolled steel sheets, there is still
research stage during double cold rolling (DCR) now,
particularly on the { 111} texture development. T h e
aim of this work is to compare the difference of the
structure and texture in Nb-kTi-IF steel between single
cold rolling with annealing and multiple cold rolling
with annealing along two cold rolling processes.
1 Experimental Method
Samples were taken from a hot rolled ( H R ) plate
of Nb+Ti-IF steel, which was produced at an indus-
trial mill with good lubrication. Finish rolling was
carried out in the ferrite zone at 800 'C followed by
coiling at 700 'C. Their chemical compositions are
given in Table 1. T h e hot rolled samples were cut
into pieces and divided into two parts for two kinds
of cold rolling processes. Cold rolling processes were in-
vestigated using four-high reversing cold strip mill.
T h e tensile strength, yield strength, elongation and
value of work hardening coefficient n for as-annealed

Foundation Item: Item Sponsored by National Natural Science Foundation of China (51174020) ; Fundamental Research Funds for Central
Universities of China (FRF-SD12-OlOA)
Biography:FENG Yan-qing(l977-), Female, Doctor Candidate, Engineer4 E-mail: fyq588B126. com; Received Date: September 28, 2012
Issue 5 Structure and Texture Formation for Nb+Ti Added Interstitial-Free Steels 43 '

Table 1 Chemical composition of tested samples (mass percent, %)

C Si Mn P S Al, Alt Nb Ti N
~~ ~

0.005 0.020 0.14 0.008 0.003 0.033 0.039 0.022 0.068 0.0034

specimens vary little with or without lubrication, Table 3 Schematic of double cold rolling process
whereas the value of the plastic strain ratio Y increa- Pass
Thickness/ Reduction Reduction/ Total reduction
mm ratio/ % mm ratio/%
ses with the decrease of friction coefficientC4'. So lu- Stage 1 1 5. 0 24. 6 1. 73
bricated cold rolling conditions were selected by using 2 3. 3 36. 6 1. 19
the same lubricant oil. One process is single cold 3 2. 1 32. 3 0. 67
4 1.4 26. 6
rolling with annealing which was carried out to 90% 0. 38
1. 0 4. 8 0.03 80
reduction in a single pass at the experimental mill Annealing at 720 T: for 7200 s
Stage 2
and then annealed at 720 "C for 7200 s in a furnace Stage 3 1 1. 0 20. 0 0. 20
with hydrogen protection. Another process is double 2 0. 8 25.0 0. 20
cold rolling with annealing, namely, the SCR an- 3 0. 6 17.0 0. 10
n. s 50
nealed samples were cold rolled again and annealed ~~ ~

Stage 4 Annealing at 720 T: for 7200 s 90

for the second time. T h e annealing temperature was
also 720 'C. Performances and textures of samples
for single cold rolling with annealing and for multi-
ple cold rolling and annealing in Nb 4-Ti-IF steels
which have the same total reduction, lubricant and
annealing temperature. were compared. T h e key fac-
tor affecting the drawability of the steel dealt with
single cold rolling is cold rolling reduction. The rvalue
reaches maximum when the cold rolled reduction is
about 75%--80%. For DCR, the main factors that
influence the drawability are the total cold rolled re-
duction and the distribution of the total reduction.
Drawability improved remarkably when the total re-
duction is above 80% and the distribution of SCR is
above 50%c5-81. T h e basic rolling schedules were
shown in Table 2 and Table 3.
Tensile tests were performed to measure strength
properties, ductility property and r-value according
to JIS13A. Microstructures and precipitates of the
as-received samples were studied with a microscope
and TEM. Texture measurements were carried out
on samples at the 1/4 thickness sections using X-ray
diffraction (XRD). Orientation distribution functions
(ODFs) were calculated using the X-pert texture
software and ( l l o ) , (200) and (112) pole figures were
determined. T h e ODFs were then calculated from
these pole figures using the method of Bunge.
2 Results and Analysis
2.1 Microstructure and precipitation
T h e microstructures of samples for the hot roll-
ing, cold rolling (SCR and DCR) and recrystalliza-
tion annealing are shown in Fig. 1, Fig. 2 and Fig. 3 ,
respectively. T h e main metallographic feature of the
deformed state in the present samples was the pres-
ence of intracrystalline shear bands. Among the
present cold rolled samples with shear bands, shear
bands for stage 1 of SCR are finer than those for
stage 1 of DCR. Shear bands have been mentioned
by the name of fish-bone s t r u c t ~ r e ~ ~T-h~e~fish-
.
bone structure was observed in stage 1 of SCR,
stage 1 and stage 3 of DCR. And the fish-bone struc-
tures are found to appear on the whole thickness di-
rection. For stage 2 of SCR, stage 2 and stage 4 of
DCR, the fish-bone structure of sample was replaced

Table 2 Schematic of single cold rolling process

Thickness/ Reduction Reduction/ Total reduction
Pass
mm ratio/% mm ratio/%
Stage 1 1 5.00 39. 0 1. 95
2 3. 05 38. 1 1. 16
3 1. 89 38. 3 0. 72
4 1. 17 37. 9 0. 44
5 0. 73 31. 5 0. 23
0. so 90
~ ~ ~~

Stage 2 Annealing at 720 C for 7200 s

Fig. 1 Microstructure for hot rolling
 ' 44 ' Journal of Iron and Steel Research, International VOl. 20

(a) Stage 1; (b) Stage 2.

Fig. 2 Microstructures of SCR annealed samples

(a) Stage 1; (b) Stage 2; ( c ) Stage 3 ; (d) Stage 4.

Fig. 3 Microstructures of DCR annealed samples

by small and equiaxial recrystallization grains. Com-
pared with the grain size of hot rolling process, the
grain size of cold rolling and annealing becomes
smaller. T h e sizes of annealed grains for stage 2 of
SCR, stage 2 and stage 4 of DCR are 15-20, 15-
22 and 10-17 pm, respectively. Although all the
samples are in an annealing condition and show re-
crystallized grains only, sample for stage 4 of DCR
is made up of equiaxed grains with almost uniform
size, whereas sample for stage 2 of SCR shows a du-
plex grain structure, consisting of both large and
small-sized grains.
The precipitates of TiN, MnS, Ti4 C, S, c71 , Ti(CN)
and Fe(Ti,Nb)P commonly presented in stage 2 of SCR
and stage 4 of DCR are shown in Fig. 4. However, the
sizes of precipitates are perceptibly larger in stage 4
of DCR as compared to stage 2 of SCR. This may be
due to the precipitates grow up continually during the
second annealing process. The frequency of Fe (Ti, Nb)P
precipitates is perceptibly higher in double annealing.
Issue 5 Structure and Texture Formation for N b f Ti Added Interstitial-Free Steels 45

Fe
I

* 488-
2 326- S
Ti

0 1 2 3 4 6 6 7 8 9 1 0

lloot Fe

0 1 2 3 4 6 6 7 8 9 1 0
1 100
0
Ti
I

1 2 3 4 6 6 7 8 9 1 0

ilA-
Al
I

Fe
A . , I

1 2 3 4 5 6 7 8 9 1 0
7400 Lci) Ti
6600

2 3700 -
c)

A l
V
1900
Fe
I , I , ,

0 1 2 3 4 6 6 7 8 9 1 0
EnergykeV

Fig. 4 TEM extraction replica micrographs showing presence of different types of precipitates and
spectra for stage 2 of SCR and stage 4 of DCR
 46 Journal of Iron and Steel Research, International Vol. 20

However, ( T i , N b ) C and F e ( T i , N b ) P type precipi-
tates were very rarely observed in stage 2 of SCR
and stage 4 of DCR.
2.2 Performance
Yield strength, tensile strength, elongation,
values of the plastic strain ratio and work hardening
coefficient of samples with the same total reduction
suffered from SCR annealing and DCR annealing are
summarized in Fig. 5 , respectively. Yield strengths
are in the range of 140 - 150 MPa for SCR annealing
400
(a)
Tensile strength
process and 100- 125 MPa for DCR annealing process,
respectively. Tensile strengths are in the range of
315 -325 MPa for single cold rolling and 290- 320 MPa
for DCR annealing process, respectively. The varia-
tion of the plastic strain ratio was always less than
1. 2 while the variation of the work hardening coeffi-
cient is less than 0.04. For the DCR annealing
process, the elongation was more than 45% and r can
reach 3.2. The above results demonstrate that double
cold rolling process resulted in better mechanical
properties than those resulted from single cold rolling
0.48 A A
(b) A
A

$ ' ; A $ A 0.441 A A A Stage 2 of SCR I

I I
f
300 X
X X Stage 4 of DCR
* Stage 2 of SCR
0 Stage 4 of DCR
A Stage 2 of SCR
Yield strength x Stage 4 of DCR
r/i
4 * * * * *
0 .
100 O . 0

0.36 3.6
(d)
O.*W 0 0
0
3.2 - 0
0

0
0

m 0 0
B 0 yi

'id 0.25
0
f 2.8 - n Stage 2 of SCR
t 0 0
Q 0
0
0

I
i Stage 4 of DCR
0.20 0 Stage 2 of SCR 2.4 -
Stage 4 of DCR (1
Q
D
0.16 I I I I 2.0 I I P I I I

process with the same total reduction.
2.3 Texture
Fig. 6 shows whole ODF sections obtained from
X-ray diffraction analysis of SCR and DCR. T h e
main texture components are a-fibre ( R D / < l l O > )
and y-fibre ( N D / < l l l > ) texture components, as
shown in Fig. 7.
For SCR annealing and DCR annealing, the ma-
jor texture components were (yl = O " - 9 O 0 , @=55",
p = 45") orientations. Especially, ( y1 = 50°, @ =
55", p = 4 5 " ) and (yll=55", @=55", ylz=45") ori-
entation function values reach 7.64 and 11.00 in stage 2
of SCR and stage 4 of DCR, respectively (as shown in
Fig. 6).
T h e hot rolled samples were cold rolled to a re-
duction of 90% and then annealed at 720 "C. As shown
in Fig. 7 (a), the intensity for { 111}<110> texture of
sample for stage 4 of DCR is much higher than those of
others. It can be seen from Fig. 6 that the hump in-
tensities are different in various processes. T h e in-
tensity of sample for stage 2 of SCR is lower than
that for stage 4 of DCR. It is noted that I F steels
with a fine ferrite grain are favorable to develop y-fi-
bre (ND/ (111 >) texture components with large
r, after cold rolling and annealing process. T h e
mean r-value, r, = ( r, 27-45 + + ) / 4 , where the
subscripts represent angles between tensile direction
and rolling direction, is generally used to evaluate deep
drawability, i. e. , formabilityc4'.
A more detailed comparison of the density dis-
tributions of the samples along orfibre and y-fibre is
depicted in Fig. 7. After SCR annealing and DCR annea-
ling, the intensities are both high at { 111}<110> and
quickly lowered down. T h e maximum intensities of
a-fibre are 7.210 and 11.012 for stage 2 of SCR and
stage 4 of DCR, respectively. Sample for stage 4 of
DCR has higher {111}<110> and y-fibre than those
Issue 5 Structure and Texture Formation for N b f Ti Added Interstitial-Free Steels - -
47

I
I I I

20 I 301

40 45 60

@f(")

( a ) Stage 2 of SCR; (b) Stage 4 of DCR.

Fig. 6 Whole ODF sections

12

8
A Stage 2 of SCR
0 Stage 4 of DCR
"lo7
I
12
0
Stage 2 of SCR
Stage 4 of DCR
@ =66"
9 2 =46"

9
4

0 10 30 60 70 90 60 70 80 90
@I("> cpll(")

( a ) a-fibre; (b) y-fibre.

Fig. 7 Textures for stage 2 of SCR and stage 4 of DCR

suffered from stage 2 of SCR.
3 Discussion
The fish-bone structure was observed in both SCR
and DCR samples. For SCR annealing, the fish-bone
structure was replaced by small and equiaxial recrys-
tallization grains while the equiaxial recrystallization
grains of samples with DCR annealing are smaller.
T h e reason for this is not hard to understand as N b ,
which is a very good grain refiner, inhibits grain
growth during recrystallization annealing of DCR
annealing. Although both the samples are in an an-
nealing condition and show recrystallized grains on-
ly, DCR annealed sample is made up of equiaxed grains
of almost uniform size, whereas SCR annealed sam-
ple shows a duplex grain structure, consisting of
both large and small-sized grains.
(Ti, Nb) C and F e ( T i , Nb) P type precipitates
were very rarely observed in SCR annealed and DCR
annealed steels. Nb generally does not give rise to
the formation of free-standing Nb-containing precipi-
tates and thus mostly remains in solid solution. Nb
promotes Ti, C, S, formation and increases the num-
ber of TiN precipitates by increasing the effective
 48 Journal of Iron and Steel Research, International
~
solute concentration of Ti in the matrix. T h e fre-
quency of Fe ( Ti, Nb P precipitates is perceptibly
higher in double annealing. Such precipitates are as-
sumed to be responsible for the deterioration of
properties, mainly formabilityc5]. FeTiP is said to
adversely affect the { 111} recrystallization texture
formation by leaving behind less Ti and Nb in the
matrix to react with C. However, with the same to-
tal cold reduction, r-values of DCR samples in-
creased remarkably in above work. More systematic
and in-depth work is necessary to clarify this aspect.
T h e mechanical properties of extra deep-draw-
ing grade I F steel sheet are remarkably affected by
its cold rolling and recrystallization microstructure
and recrystallization textures. For the samples with
high reduction, the mix dislocations which primarily
belong to edge-dislocation distribute around the slip-
bands. As a result of the existence of shearing stress
concentrated in some narrow region, massive and very
dense shear bands as shapes of parallel sliver have
formed. Intracrystalline shear bands fragmented ND
fibre grains, which are general fragmentation, lead
to the nucleation of ND fibre grains at sites situated
both within the grain and at the grain boundary. ND fi-
bre grains increased and { 111} // ND recrystallization
texture intensified after annealing and second annealing.
T h e intracrystalline shear bands need to be dis-
cussed further. It is different from classifying fish-
bone structure to { 111}<110> oriented grain, and
these bands are considered as near y-fibre grains
possibly. T h e reason is that the { l l o } <110> in-
tensity as shown in Fig. 7 was the weakest compared
with the other orientations of DCR annealed tex-
ture. T h e intracrystalline shear bands indicated that
there should be some special deforming mechanisms
different from the slip and twin-crystal for DCR
process. This may be due to deformation resistance
from the crystal defects, which the rotation could
not be fully achieved.
T h e analysis of the annealed textures described
above indicates that N D fibre textures develop
mainly in the SCR and DCR processes. Annealing
process is the key factor for the development of
{111}<11O> components. In the mean time, the
role of cold reduction during the second deformation
process could not be neglected. T h e intensities of
{lll}<110>, { l l l } < O l l > , { l l l } < 1 2 3 > and
{ 111}<112> textures formed in the DCR annealed
samples are higher than those in the SCR annealed
ones. This is to say, the { 111} < uvw > texture
components which formed in the annealing process
VOl. 20
of SCR were not only remained but also strength-
ened during the DCR annealing process.
High cold reduction introduces a wide orienta-
tion spread in the deformed crystal by forming sub-
grains. Recrystallization nuclei are thought to have
their orientations inside this spread. T h e sub-grain
growth is also taken into account on { 111} < 1 1 O >
nucleation texture formation by N Yoshinags et
alCg3.It was also observed that the maximum inten-
sity along the y-fibre shifts from { l l l } < 1 1 2 > after
cold rolling to { 111} < 110 > after recrystalliza-
tionCIO-lll . A main point is that near {111}<110>
annealing recrystallized texture consumes the high
intensity of near { 111} < 112 > in the cold-rolled
texture preferably.
The a-fibre and y-fibre textures for the annealed
samples with the same total reduction are shown in
Fig. 7. With the 90% total reduction, the maximum
intensity and accumulating degree of ND fibre both
developed. This is another evidence for the role of
cold rolling in the development of recrystallization
texture. It could ,be concluded that increasing the
second cold reduction and adopting proper annealing
time can improve the intensity of ND fibre.
Values of the plastic strain ratio and work hard-
ening coefficient which could reflect the deepdrawing
properties of the relevant samples were also tested.
With the same total cold reduction, r-values of DCR
annealed samples increased. And the total cold re-
duction has little influence on the value of mean
work hardening coefficient.
4 Conclusions
1) The fish-bone structures were observed in both
SCR and DCR samples. DCR annealed sample is made
up of equiaxed grains of almost uniform size, whereas
SCR annealed sample shows a duplex grain structure,
consisting of both large and small-sized grains.
2) (Ti, Nb)C and Fe(Ti, Nb) P type precipitates
were very rarely observed in the SCR annealed and DCR
annealed steels. Nb generally does not give rise to the
formation of freestanding Nb-containing precipi-
tates and thus mostly remains in solid solution. Nb
promotes Ti, C2S2 formation and increases the num-
ber of TiN precipitates by increasing the effective
solute concentration of Ti in the matrix.
3) Double cold rolling process resulted in better
mechanical properties than those for the single cold
rolling process with the same total reduction done.
With the same total cold reduction, r-values of DCR
annealed samples increased. And the total cold re-
Issue 5 Structure and T e x t u r e Formation for Nb+ Ti Added Interstitial-Free Steels
duction has little influence on the value of mean
work hardening coefficient.
4) During the DCR annealing process an obvious
strengthening of y-fibre texture was observed com-
pared to the SCR process. The SCR annealed texture
(111}<110> could remain during the DCR rolling
and ( 111} <110) improved during DCR annealing.
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