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Received 22 November 2004; received in revised form 10 March 2005; accepted 16 March 2005
Abstract
The evolution of microstructure and texture during cold rolling of commercial-purity titanium (CP-Ti) was studied with particular reference
to deformation twinning and dislocation slip. For low to intermediate deformation up to 40% in thickness reduction, the external strain was
accommodated by slip and deformation twinning. In this stage, both compressive ({1 1 2̄ 2}1 1 2̄ 3̄) and tensile ({1 0 1̄ 2}1 0 1̄ 1̄) twins,
as well as, secondary twins and tertiary twins were activated in the grains of favorable orientation, and this resulted in a heterogeneous
microstructure in which grains were refined in local areas. For heavy deformation, between 60 and 90%, slip overrode twinning and shear
bands developed. The crystal texture of deformed specimens was weakened by twinning but was strengthened by slip, resulting in a split-basal
texture in heavily deformed specimens.
© 2005 Elsevier B.V. All rights reserved.
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doi:10.1016/j.msea.2005.03.019
210 Y.B. Chun et al. / Materials Science and Engineering A 398 (2005) 209–219
purity titanium (CP-Ti) under cold rolling conditions and to thinned to 60 m and then twin-jet electro-polished at 30 V
establish how twinning affects the formation of basal and and −40 ◦ C using the solution previously described.
other types of textures. The textures developed during rolling were quantified us-
ing a Rigaku RINT2500 X-ray diffractometer. For this pur-
pose, five pole figures ((1 0 1̄ 0), (0 0 0 2), (1 0 1̄ 1), (1 1 2̄ 0)
2. Experimental procedures and (1 0 1̄ 2)) were obtained from the plate/sheet surface
using the Schulz reflection method. Using the five incom-
The material used in this work was commercial-purity tita- plete pole figures so obtained, the orientation distribution
nium received as 12-mm-thick hot-rolled and annealed plate function (ODF) was calculated with the commercial pro-
whose measured composition is given in Table 1. Samples gram LaboTexTM based on the arbitrarily defined cell (ADC)
measuring 150 mm × 200 mm were cold rolled by reversing method [17]. From the ODFs, complete pole figures were
the rolling direction between each pass at room temperature reconstructed. Euler angles were represented with reference
to a total thickness reduction of 90% in a two-high mill with to a crystal coordinate system consisting of X = [2 1̄ 1̄ 0],
220 mm diameter rolls using a rolling speed of 13.8 m/min. Y = [0 1 1̄ 0] and Z = [0 0 0 2].
During each pass, the thickness was reduced by 0.2 mm with
the aid of oil lubrication.
Following cold working, optical microscopy, EBSD anal- 3. Results
ysis and TEM were conducted on transverse cross-sections
cut from the rolled samples. For optical microscopy and 3.1. Starting material
EBSD analysis, specimens were mechanically polished and
then electro-polished in a solution consisting of 5 ml per- Optical microscopy showed that the starting material com-
chloric acid and 95 ml methanol at 30 V and −40 ◦ C. Subse- prised single-phase, equiaxed ␣-Ti with an average grain size
quently, the samples were etched with a solution consisting of 30 m (Fig. 1(a)). In addition, XRD analysis revealed
of 1 ml HNO3 , 2 ml HF and 40 ml H2 O. peaks only for the ␣-phase, and back-scatter-electron imaging
Grain-boundary character distributions (GBCD) in the in the SEM confirmed that there was no second phase (such as
rolled specimens were established via EBSD using a Hi- -phase). These analytical results indicated that the program
tachi 3400S field emission gun scanning electron micro- material (as-received CP-Ti) was indeed composed solely of
scope (FEG-SEM) and TSL-OIMTM software. The statisti- ␣-phase despite being commercial grade, most likely due to
cal certainty of the EBSD analysis, especially for the highly the low levels of impurities (Table 1). In particular, the level
strained materials, is significantly affected by the level of of iron, a potent -stabilizer in titanium alloys, was approx-
confidence index (CI) for which the software allowed during imately 200 wppm, or only half the maximum solubility of
post-processing of measured EBSD data. Preliminary EBSD Fe in the ␣-phase (∼400 wppm), thus resulting in a very low
experiment for cold rolled ␣-Ti revealed that the fractions probability for the retention of -phase at room temperature.
of random high angle boundaries decreased with increasing Hence, the possible effect of second phases on the deforma-
CImin (the minimum CI allowed in EBSD post-processing) tion behavior of CP-Ti can be excluded from consideration.
in the range of CImin from 0 to 0.1. This is mainly due to The as-received CP-Ti plate, which had been hot rolled
random orientation relationship between incorrectly indexed and then annealed in the ␣-phase region, had a moderate tex-
points (generally having low CI) and their neighboring points. ture (Fig. 1(b)). The (0 0 0 2) pole figure revealed a bimodal
In the range of CImin higher than 0.1; however, the overall distribution of basal poles, a texture commonly found in cold
aspect of misorientation angle distribution was unaffected by rolled pure Ti; the maximum intensity (4.4 × random) was
CImin . Based on these, any measured points whose CI is less found at locations tilted ±35◦ from the ND toward the TD.
than 0.1 were excluded from the analysis of the EBSD data A second, weaker component comprising (1 1 2̄ 0) poles at
in the present study. locations tilted 15◦ from the RD toward the ND suggested
To determine the substructure developed during rolling, the development of a recrystallization texture also. In the
TEM analysis was performed using a Philips CM200 trans- (1 0 1̄ 0) pole figure, the maximum intensity was found at the
mission electron microscope. Specimens for TEM were RD, indicating that a considerable amount of rolling texture,
which had developed during hot rolling, remained. From the
Table 1 pole figure analysis, therefore, it was confirmed that the as-
Chemical composition of commercial-purity titanium program material received texture comprised both rolling and recrystallization
Element Composition (wt.%) components.
H 0.0015
C 0.005 3.2. Microstructure evolution during low-to-medium
N 0.01 levels of deformation
O 0.06
Fe 0.02
Ti Balance
Low-to-medium levels of deformation resulted in the de-
velopment of heterogeneous microstructures due to the frag-
Y.B. Chun et al. / Materials Science and Engineering A 398 (2005) 209–219 211
Fig. 2. EBSD (inverse-pole-figure) maps for the RD direction of CP-Ti cold rolled to thickness reductions of (a) 10%, (b) 20%, (c) 30% and (d) 40%, showing
activation of deformation twins in some but not all grains. In (c) and (d), NT indicates grains without twins.
servations thus indicate that the activation of {1 1 2̄ 2}1 1 2̄ 3̄ of the activation of {1 1 2̄ 2}1 1 2̄ 3̄ twins on the matrix ori-
compressive twins was most likely dependent on the ori- entation decreased. At the same time, other types of twins,
entation of the matrix and the difficulty of accommodating such as {1 1 2̄ 1}1̄ 1̄ 2 6 and {1 0 1̄ 1}1 0 1̄ 2̄, were observed
compression near the c-axis via slip processes. In addition, occasionally.
{1 0 1̄ 2}1 0 1̄ 1̄ tensile twinning appeared to have been acti- Secondary twins were observed for thickness reduc-
vated without a noticeable dependence on matrix orientation tions above 20%. When the primary twins were of the
(Fig. 4(c)). The formation tendency of particular twins in a {1 1 2̄ 2}1 1 2̄ 3̄ compressive type, the secondary twins
grain was also affected by the orientations of the surround- within the primary twins were of the {1 0 1̄ 2}1 0 1̄ 1̄ ten-
ing grains in addition to that of the matrix grain because, as sile type (Fig. 5), thus also indicating a dependence of twin
shown in Fig. 4(b and c), either compressive twins or tensile activity on parent orientation.
twins were generated in similarly oriented grains. For thick- Pole figures determined from X-ray diffraction (XRD)
ness reductions higher than 20%; however, the dependence measurements revealed that the initial split-basal texture was
Y.B. Chun et al. / Materials Science and Engineering A 398 (2005) 209–219 213
Fig. 3. Grain-boundary misorientation distribution for CP-Ti cold rolled to a reduction of (a) 10%, (b) 20%, (c) 30% or (d) 40%. The peaks at 65◦ and 85◦
correspond to {1 1 2̄ 2}1 1 2̄ 3̄ compressive twins and {1 0 1̄ 2}1 0 1̄ 1̄ tensile twins, respectively. LAB: low angle boundaries of less than 15◦ misorientation.
transformed to a basal texture as the reduction was increased grains reflected the amount of deformation imposed dur-
to 40%. After 20% reduction, the original basal poles of the ing cold rolling. EBSD analysis showed that the elongated
bimodal distribution along the ND–TD began to be dispersed coarse grains (Fig. 7(c)), had orientations in the range ϕ1 = 0◦ ,
toward the ND (Fig. 6(b)). As a result, the maximum basal- Φ = 30–90◦ and ϕ2 = 30◦ . Also, a small amount of macro-
pole intensity after 30–40% reduction was observed parallel scopic shear banding which had not been found during re-
to the ND (Fig. 6(c and d)). Unlike the distribution of the ductions equal to or below 40% was noted at high reductions.
basal poles, the maximum intensities for the prism poles, al- After 90% cold reduction, the microstructure became
though not very strong, were found along the RD and were much more refined and the macroscopic shear banding was
not affected noticeably by the level of cold reduction. more evident (Fig. 7(b)). The thickness of the elongated
coarse grains had been reduced to 3 m. The orientation im-
3.3. Microstructure evolution during higher levels of age for the sample rolled to 90% reduction (Fig. 7(d)) also
deformation showed that the lattice was so severely deformed that it was
impossible to analyze approximately 70% of the data points
At yet higher levels of thickness reduction (≤90%), the via EBSD. The orientation of the elongated coarse grains
microstructure became more refined, but more heterogeneous in the sample rolled to 90% reduction was in the range of
as well. After 60% reduction, elongated, coarse grains (with ϕ1 = 0◦ , Φ = 30–50◦ and ϕ2 = 30◦ , thus indicating that the
a thickness of 10 m) were interspersed with fine grains (de- basal poles near the TD moved toward the ND as the amount
veloped at lower reductions due to twinning), as shown in of deformation increased.
Fig. 7. Because the as-received CP-Ti was equiaxed with an TEM analysis of CP-Ti samples rolled to 60% reduction
average grain size of 30 m, the aspect ratio of the coarse revealed a fine lamellar structure with high dislocation den-
214 Y.B. Chun et al. / Materials Science and Engineering A 398 (2005) 209–219
Fig. 7. Microstructures of CP-Ti cold rolled to reductions of (a) 60% (optical micrograph), (b) 90% (optical micrograph), (c) 60% (EBSD-orientation image)
and (d) 90% (EBSD-orientation image). Insert: stereographic color key for the rolling direction inverse-pole-figure maps shown in (c) and (d).
Fig. 10. ODF maps for the ϕ2 = 30◦ section: (a) initial CP-Ti material and after cold reductions of (b) 10%, (c) 40%, (d) 60% and (e) 90%. In the deformed
specimens, the maximum intensity was observed at ϕ1 = 0◦ , Φ = 35◦ and ϕ2 = 30◦ .
5. Conclusions
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