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Abstract
A split sample of Al0.1%Mn has been deformed by a series of compression tests in a channel-die at 400 C to a nal strain of 1.6. The
orientations of 176 grains in a 4 4 mm2 internal surface were followed by high-resolution electron backscatter diraction at four different strains to compare with crystal plasticity models. Typically 3000 orientations per grain were used to quantify the average lattice
rotations of each grain together with their orientation spreads (termed microtexture tracking). The average orientations tend towards the
standard b-bre plane-strain compression texture components, albeit with some variations. The in-grain orientation spreads develop
strongly at rst, then tend to saturate at high strains. Finally, the inuence of grain environment on lattice rotation is examined by means
of the rotation variability at constant orientation. On average and at the beginning of the deformation, two grains of the same initial
orientation, but dierent neighbours, would rotate by angles that vary by 25% and axes separated by 37; their orientations at e 1:2
would vary by 12.
2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Microstructure; Plastic deformation; Deformation structure; Electron backscattering diraction (EBSD); Aluminium alloys
1. Introduction
Accurate deformation texture simulations require
advanced models of polycrystal deformation for which
there are now several new variations that go beyond the
standard Taylor model to incorporate grain interaction
eects [14]. These models, although based on the behaviour of the individual grains in an aggregate, are usually
evaluated by a comparison of the experimental and simulated macrotextures of a large number of grains. Clearly,
a comparison of the rotations of individual grains in their
environments would be much more instructive. However,
there are relatively few such studies, since they require difcult experimental procedures.
*
Corresponding author. Present address: Sibley School of Mechanical
and Aerospace Engineering, Cornell University, Ithaca, NY 14853, USA.
E-mail addresses: quey@emse.fr (R. Quey), piot@emse.fr (D. Piot),
driver@emse.fr (J.H. Driver).
A rst approach is to use two-dimensional (2-D) microstructures, as done by Skalli et al. [5] and later Fortunier
and Driver [6] using large-grained aluminium. A similar
method is to use a columnar grain structure, within the limitations of a h1 0 0i-bre texture [7]. These studies are of
interest, but may not be representative of what occurs in
a real polycrystal. Two strategies have been proposed to
follow grains in a 3-D polycrystal. In situ 3-D X-ray diffraction characterization of grain average rotations has
been used by Poulsen et al. [8], but up to now the technique
appears limited to a tensile strain less than 0.1. The other
method is to use a split sample, as rst done by Barrett
and Levenson [9] for uniaxial compression, then by Panchanadeeswaran et al. [10] for hot plane-strain compression
(PSC). In the latter case, an AA 1050 sample was split in
half perpendicular to the transverse direction and grain orientations were measured by electron backscatter diraction
(EBSD) on the internal surface before and after a strain
of 0.5. In these studies on 3-D polycrystals, the experimental rotations were compared to those predicted by the
1359-6454/$36.00 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.actamat.2009.11.007
1630
Taylor model. Their conclusions are contradictory: from 3D X-ray diraction microscopy, Winther et al. [11] found
the Taylor model to be successful for 75% of the grains,
whereas Panchanadeeswaran et al. [10] concluded that it
fails almost completely.
Although Panchanadeeswaran et al. [10] have demonstrated the potential of the split-sample technique to follow
grains in a polycrystal during large deformations, their
study is not really satisfactory because few orientation
measurements per grain were made and an accidental
macroscopic shear strain (as large as 1/3 of the imposed
PSC) occurred in the sample during the deformation.
In a recent study by Quey et al. [12], a split sample of
Al0.1 wt.%Mn was deformed in PSC at 400 C to a strain
of 0.4. After each of the two passes, the sample was
quenched to avoid recrystallization, and the deformation
microstructure was analysed by EBSD. In the present
study, this experiment has been repeated with another sample, up to a strain of 1.6. The same 176 grains were followed throughout the deformation with an average of
3000 measurements per grain. This paper rst discusses
the inuence of analysing grain rotations on the internal
surface of a split sample. Then, the rotation properties of
the 176 grains are described in detail, in terms of average
rotations and in-grain orientation spreads. Finally, a
method is proposed to investigate the possible eects of
grain interaction on these rotation properties.
A comparison between the experimental results and the
predictions of various polycrystal deformation model is
provided in a second article [13].
2. Experimental
The high-purity binary Al0.1 wt.%Mn alloy was provided by the Alcan Research Centre at Voreppe. After casting, it was cold-rolled 50% then recrystallized at 530 C for
5 min. The resulting microstructure showed near-equiaxed
grains of size about 300 lm and a weak crystallographic texture. A split sample of 8 7 10 mm (along the rolling
direction (RD), transverse direction (TD) and normal direction (ND), respectively) was used. It was made of two identical parts assembled along the transverse direction, see
Fig. 1. The sample surfaces were machined at, and both
internal surfaces were mechanically then electrolytically
polished. At the centre of one of them, a 4 4 mm2 observation zone was marked with microhardness indentations of
diameter about 30 lm, located 1 mm apart. The sample
was deformed by successive heating, compression and
quenching cycles, as illustrated in Fig. 2. In this way, the
microstructure could be analysed at successive (logarithmic)
strains of 0, 0.19, 0.42, 0.77, 1.2, and 1.6. After closing, the
two parts of the sample were held together through glued
points at the corner of the internal surface, and then wrapped
in Teon lms to reduce friction eects. The hot channel-die
compression was imposed at a strain rate of 1 s1 and a temperature of 400 C in the equipment described by Maurice
et al. [14]. Typical heating times to temperature stabilization
ND
TD
RD
T ( C)
PSC to
0.19
PSC to
0.42
PSC to
0.77
PSC to
1.2
PSC to
1.6
400
Heating ( 60 s)
Deformation at 1 s
Quenching (
2 s)
20
EBSD
time
(EBSD)
EBSD
EBSD
EBSD
(EBSD)
(a)
The fact that grains are observed on the internal surfaceof the sample is the main limitation of the method
and could be open to criticism concerning its relevance to
the behaviour of grains in a real polycrystal. The purpose
of this section is to ensure, as far as possible, that this does
not signicantly aect grain rotations. This is achieved
partly by following the methodology introduced by Panchanadeeswaran et al. [10].
1 mm
30
20
10
0
10
20
30
7 6 5 4 3 2 1 0
altitude [m]
(b)
30
20
10
0
10
20
30
7 6 5 4 3 2 1 0
1 mm
distance [mm]
Fig. 4. Internal surface rumpling analysed by rugosimetry proles along
(a) ND and (b) RD. Measurements carried out on a sample deformed at
e 0:42. Note that there are two orders of magnitude between the
horizontal and vertical axes, and that the local slopes are more
pronounced along ND.
1 mm
(a)
1631
distance [mm]
altitude [m]
1 mm
(b)
(c)
1 mm
(d)
(e)
Fig. 3. Array of microhardness indentations at successive strains: (a) e 0, (b) e 0:19, (c) e 0:42, (d) e 0:77, and (e) e 1:2.
1632
(a)
(b)
Fig. 5. The inuence of the internal surface on the macrotexture. (a) Macrotexture measured on the internal surface of the split sample. (b) Macrotexture
measured on a cut surface of a standard sample. Both measured at e 0:77.
1633
(b)
(a)
1
4
5
2
4
5
Fig. 6. The inuence of the internal surface on the microtexture of a sample deformed at e 0:5. Rodrigues vector maps measured (a) on the internal
surface andp(b) in subsurface
p
(after removal of 3050 lm of material). (R being a Rodrigues vector, the RGB colour levels are
255 Ri 2 1= 2 2 1 with i 2 f1; 2; 3g, respectively; grey is for non-indexed points). The seven grains considered are marked.
Table 1
Inuence of the internal surface on the microtexture: dierence between the orientations of grains measured in surface and subsurface (after removal of
3050 lm of material), as illustrated in Fig. 6. (a) Average orientations and (b) average in-grain disorientations hd .
(a)
n
Surface orientation u1 ; /; u2 ()
Subsurface orientation u1 ; /; u2 ()
disorientation ()
1
2
3
4
5
6
7
0.7
1.3
0.9
1.0
0.8
1.0
1.2
Average = 1.0
(b)
n
Surface hd ()
Subsurface hd ()
1
2
3
4
5
6
7
6.4
5.2
5.8
9.9
11.0
7.7
5.8
6.0
5.7
6.1
10.6
10.6
6.8
6.2
6
10
5
7
4
12
7
Average = 7
vention): (90, 27.5, 45), (57.5, 30, 75) and (35, 35,
80), respectively. The grains are characterized in terms
of their average orientations, and are assigned to a component using the standard 15 criterion. The results at the successive strains are reported in Table 2. It appears that each
b-bre component systematically increases, while the number of grains outside the bre continuously decreases.
These results are consistent with previous hot-deformation
macrotexture studies (e.g. [17]).
4.2. Average rotations
The average rotations are expressed in the sample coordinate system as axis/angle pairs r; h. One can consider
either the rotations at the successive strains e measured
from the initial orientations, noted re0 ; he0 , or the rotations
for the successive strain increments, called incremental
rotations and noted rei ; hei . A study of the rotation axis
r requires particular precautions, especially when there
are uncertainties for the rotation angle h. Bate et al. [18]
have shown that the angular accuracy b of the axis r is
given by tan1 d=h, where h is the rotation angle and d
1634
(a)
035
034
169 026
063
007
099
189
056
085
087
173
016
149
158
073
120
101 068
191
021
010
170
024
090
137
096
076
138
041 168
075 143
118
185 197
188
178
124
047 205 200
032
042
135
179203
136 196 102 095
062
183193 043
036
119 150
164
019
088
125
003
054
013
072
162
097
015
038
172
037
018
057
081
070
094
017
011
050
152
161
121
199
159
006
020
116 069
089
083
051
201
167
130
105
139
100
059
080
030
049
053
065
151140
142
009
045
014
184
175 145
112 115
084
111
001
160
002
171
061
148
126
123
165 129
023
128
156
027
048
110
195
109
202 092
082
103
077
177
044
012
182
146
033
133
131
104 064 079
055 204 052 107 174 098
207
153
141
127 122
060
039
066 198
093 091
190
058
029
154
186
194
008
206 031
192
040
181
132 046 074
157 108
028
005
144
155
113
078
067
106
086
022
147
176
134 180
071
117 163114
004
187 025
166
(b)
035
105
034
116
063
089
159
083
099
189
056
020
026
169
007
085
016
069 199
057
161
017
018
011
173 087
081
038
021
120
101
191
024
090
006
094
015
088
068
070
172
121
042
179 203
193
183
043
119
150
072
010
170
054
162
045
080 059
184
139
137
100
175
115 145
076 138
030
112
168
041
050
084
152
053
065
151 140 049
111
075 143
158
061
171
009
142
118 185
148
073
123
165
197 188
129
023
128
126
156 110
103
082
177
202 092
077
195 027
109
146
182
012
133
174 098
052 107
204
055
033
044
079
207
104 064
131
122
198
127
141
066
190
153
091
093
029
039
060
058
186
192
206 031
154
040
194
181
157
008
108
074
005
144
132 046
155
106
067
028
113
086
078
149
096
062
164
003
051
201
037
167
178
130
047 205 124 200
032
136 196 102
095
036
019
125
013
097
014
160
001
002
048
147
117 163
022
134
114
176
180
071
004
187
025
166
Fig. 7. Microtextures at successive strains: (a) e 0, (b) e 0:42, (c) e 0:77 and (d) e 1:2 (Rodrigues vector maps). The 176 grains are numbered and
the black lines represent (a) the boundaries >5, (bd) the contours of the same grains at the subsequent strains.
(c)
1635
004
025
163 114
187
147
117
002
184
059
112 175
111
053
065
148
061
129
023
165
082
103
182
077
177
146
133
098207
174
052 107
204
122 190
127
066
029
206
031
192
157
108
040
181
106
067 144
080
005
055
091
093
155
086
104
039
194
132 046
078
044
153
028
131
113
008
060
033
154
186
079
074
141
058
128
092
064
027
195
159
083
126
109
152
073
056
016
158 050
118
075
185 197
143
096
087
173
038
149
085
007
012
009
076
151
041
081
021
137
168
011
116
063
026
169
089
034
010
090
100
138
049
140
171
142
123
024
068
101
069
035
057
020
017
120
015
161
139
030
170
018
094
088
072
119
054
070
042
203
179 183 193
150
162
045
115 145
084
043
048
014
003
062
164
006
166
180
001
022
134
071
201
167
130
032
036
125
051
136
013
047
196
176
037
178
205
124
102
019
097
095
(d)
Fig. 7 (continued)
1636
(a)
(b)
{111}
stereo. proj.
{111}
stereo. proj.
TD
TD
RD
(c)
RD
(d)
{111}
stereo. proj.
1/2-width: 2
levels: 1, 5, 10, 20, 50, 100
{111}
stereo. proj.
TD
1/2-width: 2
levels: 1, 5, 10, 20, 50, 100
RD
TD
RD
1/2-width: 2
levels: 1, 5, 10, 20, 50, 100
Fig. 8. Example of the unimodal rotation of a grain (number 062). (a) e 0, (b) e 0:42, (c) e 0:77, and (d) e 1:2. Note the average rotation and the
orientation spread.
Table 2
Macrotexture evolution through strain, in terms of number of grains
within 15 of the b-bre components (total number of grains = 157).
Component
e0
e 0:42
e 0:77
e 1:2
Copper
Brass
Others
3
11
14
15
7
20
35
44
25
40
42
42
122
86
66
56
1637
(a)
(b)
TD
ND
RD
equal-area. proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
TD
ND
RD
equal-area. proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
r00.42
r00.77
TD
ND
RD
equal-area. proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
r01.2
Fig. 9. Rotations with respect to the initial orientations, at the successive strains: (a) rotation angle h0 and (b) rotation axis r0 . Each dot represents a grain;
the contour plots highlight their distributions.
The alternative approach that we propose is to determine the average of the VCO over all orientations. This
is done by a comparison of the rotations of grains of dierent orientations taking all pairs of grains into consideration. This method involves three steps, which lead to
Fig. 13a and c:
1. For every pair of grains, one calculates (i) the disorientation between their initial orientations, allowing for
both the crystal and sample symmetries, and (ii) the differences between their rotations Dr h and a. On the gures, for every pair of grains, Dr h and a are
represented as a function of the disorientation, which
is limited to 20.
2. The average variabilities by disorientation levels are calculated using intervals of 4 . This value has been chosen
to obtain a smooth evolution of the average tendency.
The averages at zero disorientation obviously cannot
be calculated this way because of the absence of data.
3. The values at zero disorientation are calculated by
extrapolating the average tendency from higher disorientations. By denition, the corresponding value of
Dr h or a is the dierence between the rotations of
grains having the same orientation, i.e. the VCO.
The values obtained in the present study are:
Dr h 0:25 (25%) for the rotation angle and a 37
for the rotation axis.
1638
(a)
(b)
TD
ND
RD
equal-area. proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
TD
ND
RD
equal-area. proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
ri0.42
ri0.77
TD
ND
RD
equal-area. proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
ri1.2
Fig. 10. Incremental rotations. (a) Rotation angle ^hi and (b) rotation axis ri . Each dot represents a grain; the contour plots highlight their distributions.
Another quantity of interest is the rotation relative variability at constant orientation (RVCO). It is dened by
the VCO divided by the overall variability, the latter
being obtained by averaging over all pairs of grains. By
denition, the RVCO takes values between 0 and 1, and
the higher the value, the lower the eect of the orientation
and the stronger the eect of grain interaction. For the
rotation angle and axis, the overall variabilities are
Dr h 53% and a 83 , respectively, and so the RVCO
values are 0.50 and 0.45, respectively.
A non-zero (R)VCO is incompatible with the Taylor
model, for which rotations depend only on orientation.
To validate the method, it has been applied to the rotations provided by the Taylor model for the same set of
176 grainssee Fig. 13b and d. The VCO obtained in
this way are 9%/8, i.e. are not strictly zero, which is
attributed to the limited number of data. For conrmation, the same study was repeated with a more representative set of 2000 random orientations, leading to
variabilities very close to zero. The dierences between
the two can be associated with the statistical error arising
from the limited number of data, and which can therefore be considered to represent the possible error of
the experimental values. One can note, however, that
these errors are small when compared to the experimental VCO, which ensures that the latter can be considered
as valid measurements.
The rotation axis/angle VCO acting through deformation leads to a nal-orientation VCO. The nal orientations are compared by the disorientation angle between
them, and the results obtained are illustrated in
Fig. 14. The nal-orientation VCO is 12 (with an error
of 2.4).
4.4.2. In-grain orientation spreads
The same characterization can be applied to the in-grain
orientation spreads at e 1:2. The dierence in spreads of
two grains can be quantied as for the rotation angles,
hd hd
2
2
Dr hd 2 1d
h1 hd2
One can study the relation between the in-grain orientation spreads and the initial orientations (as before) or the
current orientations. The results are illustrated in Fig. 15.
The VCO obtained are Dr hd 31% for the initial orientation and Dr hd 24% for the current orientation. The orientation spread is therefore more dependent on the current
orientation than on the initial orientation (lower VCO).
As for average orientations, these values are to be compared to the overall variability, whose value is
Dr hd 34%. For the current orientation, the RVCO is
equal to 0.71. Such a high value means that the dependence
of the in-grain orientation spreads on the grain orientation
is small.
(a) TD
ND
RD
equal-area proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
TD
ND
RD
equal-area proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
TD
ND
RD
equal-area proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
ri0.77
ri0.42
(b) TD
ND
RD
equal-area proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
ri1.2
TD
ND
RD
equal-area proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
TD
ND
RD
equal-area proj.
1/2-width: 7
levels: 1,2,3,4,5,6,7
ri0.77
ri0.42
1639
ri1.2
Fig. 11. Relation of the incremental rotation axes to the texture development. (a) Case of the grains that converge into the b-bre. (b) Case of the other
grains. Note that grains in (a) show the same distribution as all grains (see Fig. 10).
0.28
= 0.42
= 0.77
= 1.20
0.24
Frequency
0.2
0.16
0.12
0.08
0.04
0
11
13
15
17
19
21
Disorientation [degrees]
Fig. 12. In-grain orientation spreads through strain. hd is the average
disorientation with respect to the mean grain orientation.
5. Discussion
5.1. The experiments
This study provides the rst statistically sound set of
rotations of grains in a polycrystal undergoing a large plastic deformation. The rotations of 176 grains were measured
during hot PSC applied in several passes up to a strain of
1.2. The advantage of high-temperature deformation is
twofold: rst the ease of EBSD measurements up to high
1640
(a)
(c)
180
pair of grains
average
160
140
140
[degrees]
r [%]
100
80
V = 53
40
20
0
120
100
V = 83
80
60
40
20
VCO = 25
0
pair of grains
average
160
120
60
180
12
16
20
VCO = 37
0
pair of grains
average
2000 grains
160
140
r [%]
120
16
20
140
80
60
VCO = 9
40
pair of grains
average
2000 grains
160
100
120
100
80
60
VCO = 8
40
20
20
0
12
(d) 180
180
[degrees]
(b)
Disorientation [degrees]
Disorientation [degrees]
12
16
20
Disorientation [degrees]
12
16
20
Disorientation [degrees]
0:42
Fig. 13. Variability at constant orientation (VCO) of the grain rotations obtained during the rst increment r0:42
0 ; h0 . (a and b) Rotation angle in the
experiments and for the Taylor model, respectively. (c and d) Rotation axis in the experiments and for the Taylor model, respectively. V stands for the
overall variability, which is calculated with no limitation of disorientation (x-axis). For (b) and (d), the VCO does not fall to zero due to the limited
number of grains in use, but does with a more representative set of 2000 grains.
(a) 140
pair of grains
average
pair of grains
average
120
100
80
60
56
52
48
44
40
36
32
28
24
20
16
12
8
4
0
r [%]
(a)
60
V = 34
40
20
VCO = 12
0
12
16
20
VCO = 31
0
Disorientation [degrees]
12
16
20
(b) 140
pair of grains
average
2000 grains
pair of grains
average
120
100
80
60
56
52
48
44
40
36
32
28
24
20
16
12
8
4
0
Disorientation [degrees]
r [%]
(b)
1641
60
40
VCO = 2.4
V = 34
20
0
12
16
20
Disorientation [degrees]
Fig. 14. Variability at constant orientation (VCO) of the nal orientation
e 1:2: (a) experimental results and (b) Taylor model.
VCO = 24
0
12
16
20
Disorientation [degrees]
Fig. 15. Variability at constant orientation (VCO) of the orientation
spread hd at e 1:2. V stands for the overall variability, which is
calculated with no limitation of disorientation (x-axis). (a) Initial
orientation and (b) nal orientation.
1642
6. Conclusions
Acknowledgments
Supplementary data
References
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conference on recrystallization and grain growth, vol. 2. SpringerVerlag; 2001. p. 1053.
[3] Van Houtte P, Delannay L, Kalidindi SR. Int J Plasticity
2002;18:359.
[4] Quey R, Ringeval S, Piot D, Driver J. Mater Sci Forum
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