Effects of Grain Growth on the {111}/{111} Near Singular Boundaries in High Purity Aluminum
FENG Xiaozheng1, WANG Weiguo1,2(), Gregory S. Rohrer3, CHEN Song1,2, HONG Lihua1,2, LIN Yan1,2, WANG Zongpu1, ZHOU Bangxin4
1 Institute of Grain Boundary Engineering, Fujian University of Technology, Fuzhou 350118, China 2 School of Materials Science and Technology, Fujian University of Technology, Fuzhou 350118, China 3 Department of Materials Science and Engineering, Carnegie Mellon University, Pittsburgh, PA 15213-3890, USA 4 Materials Institute, Shanghai University, Shanghai 200072, China
Cite this article:
FENG Xiaozheng, WANG Weiguo, Gregory S. Rohrer, CHEN Song, HONG Lihua, LIN Yan, WANG Zongpu, ZHOU Bangxin. Effects of Grain Growth on the {111}/{111} Near Singular Boundaries in High Purity Aluminum. Acta Metall Sin, 2024, 60(1): 80-94.
The {111}/{111} near singular boundary is more resistant to intergranular corrosion than random boundary. At present, enhancing the fraction of such boundary to improve the performance against intergranular corrosion has been the latest issue in microstructure design and control for aluminum and its alloys. In the current work, high-purity aluminum was selected as an experimental material, and the effects of grain growth on {111}/{111} near singular boundary were investigated. First, the sample was given multi-directional forging at room temperature followed by recrystallization annealing at 370oC. The recrystallized samples were heated at 500oC for varied time to promote grain growth and to obtain microstructures with various grain sizes. Then, the {111}/{111} near singular boundary in the samples was measured by grain boundary inter-connection characterization, which was established on the basis of EBSD and five-parameter analysis. Results show that the length fraction of {111}/{111} near singular boundary increases with the increase of grain size. For example, the fraction of {111}/{111} near singular boundaries is 3.91% when the averaged grain size is 38 μm, whereas it increases to 6.56% as the averaged grain size reaches 77 μm. Off-line in situ EBSD coupled with grain boundary trace analysis indicates that the {111}/{111} near singular boundary is primarily formed via the encounter of two growing grains with <111>/θ misorientation relationships (θ is the rotation angle). Meanwhile, the {111}/{111} near singular boundary is also formed via the re-orientation of grain boundaries with <111>/θ misorientation. HRTEM observation reveals that the {111}/{111} near singular boundary has disclination, and the degree of atomic ordering of such a boundary is higher than that of random boundaries. Therefore, such a boundary is more resistant to intergranular corrosion compared with random boundary.
Fund: National Natural Science Foundation of China(51971063);Special Program for Guiding Local Science and Technology Development by the Central Government(2019L3010)
Corresponding Authors:
WANG Weiguo, professor, Tel: (0591)22863515, E-mail: wang_weiguo@vip.163.com
Fig.1 Microstructure analyses of high purity aluminum after multi-directional forging followed by recrystallization at 370oC (a) orientation imaging microscopy (OIM) (b) grain boundary networks (GBN) (c) misorientation distribution
Fig.2 OIM (a-c) and misorientation distributions (d-f) of high purity aluminum heated at 500oC for 1 min (a, d), 5 min (b, e), and 30 min (c, f) after recrystallization (Solid areas show the uneven grain size zones, and dashed areas show the microtexture zones)
Fig.3 Misorientation distributions of grain boundaries with specific rotation axis in high purity aluminum heated at 500oC for varied time after recrystallization (a) <111> (b) <112> (c) <122>
Fig.4 Grain boundary plane distributions (GBPDs) of {111}/{111} near singular boundary with varied misorientations in the high purity aluminum heated at 500oC for 1 min (projection on (001)) (MRD—multiple of random distribution) (a) [111]/35° (b) [111]/40° (c) [111]/50° (d) [111]/55° (e) [112]/20° (f) [112]/30° (g) [122]/15° (h) [122]/40°
Fig.5 GBPDs of {111}/{111} near singular boundary with varied misorientations in the high purity aluminum heated at 500oC for 5 min (projection on (001)) (a) [111]/15° (b) [111]/30° (c) [111]/35° (d) [111]/40° (e) [111]/45° (f) [111]/55° (g) [112]/25° (h) [112]/30° (i) [122]/20° (j) [122]/25° (k) [122]/35° (l) [122]/40°
Annealing time at 500oC / min
GB rotation axis
GB number
GB
Length fraction / %
number fraction / %
1
<111>
4313
7.48
7.70
<112>
6963
12.08
12.04
<122>
9560
16.58
16.95
5
<111>
5228
7.91
8.24
<112>
7918
11.98
12.03
<122>
11314
17.12
17.42
30
<111>
4659
8.17
8.801
<112>
6947
12.18
12.02
<122>
10084
17.68
18.24
Table 1 After-filtration statistics of the grain boundaries (GBs) with the rotation axes of <111>, <112>, and <122> in the high purity aluminum heated at 500oC for varied time after recrystallization
Fig.6 GBPDs of {111}/{111} near singular boundary with varied misorientations in the high purity aluminum heated at 500oC for 30 min (projection on (001)) (a) [111]/20° (b) [111]/35° (c) [111]/40° (d) [111]/45°(e) [111]/50° (f) [111]/55° (g) [112]/15° (h) [112]/20°(i) [112]/30° (j) [122]/25° (k) [122]/30° (l) [122]/35° (m) [122]/40°
Annealing time min
[uvw]/θ
Pi / %
Mi
Wi / (°)
Fi / %
Ftotal =Fi / %
1
[111]/35°
0.51
1.37
2.50
0.26
3.91
[111]/40°
0.64
2.08
2.15
0.34
[111]/50°
0.12
1.48
2.17
0.59
[111]/55°
1.25
1.47
2.21
0.64
[112]/20°
0.68
1.56
2.15
0.35
[112]/30°
0.98
1.48
1.89
0.51
[122]/15°
0.66
1.20
2.05
0.34
[122]/40°
1.70
1.56
2.09
0.88
5
[111]/15°
0.26
1.43
1.77
0.14
5.48
[111]/30°
0.40
2.15
2.01
0.21
[111]/35°
0.55
1.87
1.87
0.29
[111]/40°
0.73
2.44
2.40
0.39
[111]/45°
1.01
1.41
2.07
0.52
[111]/55°
1.57
1.20
2.12
0.80
[112]/25°
0.77
1.25
2.28
0.39
[112]/30°
1.00
1.12
2.04
0.51
[122]/20°
0.64
1.27
2.49
0.33
[122]/25°
0.83
1.34
1.97
0.43
[122]/35°
1.36
1.12
2.11
0.69
[122]/40°
1.52
1.34
2.16
0.78
30
[111]/20°
0.31
2.91
1.69
0.17
6.56
[111]/35°
0.49
1.76
2.35
0.25
[111]/40°
0.70
1.34
1.82
0.36
[111]/45°
1.02
1.72
2.09
0.53
[111]/50°
1.31
1.61
2.09
0.68
[111]/55°
1.90
1.80
2.24
0.99
[112]/15°
0.69
1.60
2.23
0.36
[112]/20°
0.69
1.54
2.82
0.35
[112]/30°
0.89
1.40
2.47
0.45
[122]/25°
0.77
1.70
2.01
0.40
[122]/30°
1.04
1.30
2.04
0.53
[122]/35°
1.22
1.53
2.53
0.62
[122]/40°
1.70
1.41
2.20
0.87
Table 2 Statistics of the parameters relevant to {111}/{111} near singular boundaries in the high purity aluminum heated at 500oC for varied time after recrystallization
Fig.7 Off-line in situ orientation imaging microscopies and grain boundary trace analyses showing the formation of the {111}/{111} near singular boundaries by the encountering of two nonadjacent growing grains having <111>/θ misorientation in the high purity aluminum heated at 500oC (a-c) encountering of grain 1 and grain 8 at 2 min (a), 3 min (b), and 5 min (c), respectively (e-g) encountering of grain 15 and grain 22 at 1 min (e), 2 min (f), and 4 min (g), respectively (i-k) encountering of grain 26 and grain 37 at 5 min (i), 6 min (j), and 7 min (k), respectively (d, h, l) overlapped {111} pole figures of grain 1 and grain 8 in Fig.7c (d), grain 15 and grain 22 in Fig.7g (h), and grain 26 and grain 37 in Fig.7k (l), respectively, showing the GB trace normals are passing through the overlapped {111} poles, indicating they have {111}/{111} GBICs
Fig.8 Off-line in situ orientation imaging microscopies and grain boundary trace analyses showing the formation of the {111}/{111} near singular boundaries by the re-orientation of the grain boundaries having <111>/θ misorientation in the high purity aluminum heated at 500oC (a-c) re-orientation of the boundary between grain 1 and grain 6 at 1 min (a), 2 min (b), and 5 min (c), respectively (e-g) re-orientation of the boundary between grain 15 and grain 20 at 1 min (e), 4 min (f), and 6 min (g), respectively (i-k) re-orientation of the boundary between grain 23 and grain 29 at 0 min (i), 1 min (j), and 4 min (k), respectively (d, h, l) overlapped {111} pole figures of grain 1 and grain 6 in Fig.8c (d), grain 15 and grain 20 in Fig.8g (h), and grain 23 and grain 29 in Fig.8k (l), respectively (Blue and red GB traces are the GB positions before and after re-orientation, respectively, showing all the GB trace normals are passing through the overlapped {111} poles after GB re-orientation, indicating they have {111}/{111} GBICs)
Grain No.
Euler angle of growing grain
Euler angle of the grain adjacent to growing grain
Misorientation between growing grain and the adjacent grain
1
(289.1° 20.1° 49°)
-
-
2
(0.8° 36.4° 84.6°)
[]/36.6°
3
(170.8° 42.3° 10.5°)
[]/47.5°
4
(257.9° 43.3° 16°)
[123]/40.5°
5
(79.1° 33° 64.7°)
[]/52.5°
6
(343.6° 39.8° 7.1°)
[]/32.6°
7
(358.2° 43.7° 60.3°)
[432]/43.5°
8
(145.8° 38.1° 48.8°)
-
-
1
(289.1° 20.1° 49°)
[]/52.3°
2
(0.8° 36.4° 84.6°)
[]/35.3°
7
(358.2° 43.7° 60.3°)
[]/31.6°
10
(153.5° 47.8° 30.7°)
[]/16.6°
11
(32° 47.2° 64.6°)
[]/23.6°
12
(300.7° 26.6° 54.2°)
[]/58.1°
9
(139.4° 53° 47.2°)
[]/16.7°
13
(286.4° 25.9° 4.7°)
[]/40.1°
14
(342° 32.3° 71.3°)
[]/46.4°
15
(149.1° 33.3° 38.8°)
-
-
16
(334.8° 19.4° 26.3°)
[]/53.0°
17
(286.4° 32.6° 16.5°)
[]/38.6°
18
(36.3° 32° 31.9°)
[]/41.3°
19
(77.3° 32.1° 64.3°)
[]/52.0°
20
(89.2° 30.2° 64.3°)
[]/40.4°
21
(262° 44.9° 50.6°)
[]/31.7°
22
(281.3° 29.4° 49.1°)
-
-
15
(149.1° 33.3° 38.8°)
[]/49.1°
21
(262° 44.9° 50.6°)
[]/23.8°
23
(20.2° 18.4° 57.4°)
[]/38.6°
24
(92.7° 41.7° 67.3°)
[233]/44.3°
25
(236° 39.7° 25.4°)
[]/38.9°
26
(256.8° 26.1° 29.7°)
-
-
27
(268.1° 32.1° 31.3°)
[]/14.1°
28
(247.6° 31.6° 37.2°)
[310]/7.1°
29
(117.8° 35.8° 22.2°)
[]/52.1°
30
(203.9° 3° 82.7°)
[]/24.4°
31
(248.3° 10.3° 57.6°)
[]/25.4°
32
(207.7° 36.6° 58.9°)
[]/30.0°
33
(168.2° 38.5° 4.5°)
[]/47.0°
34
(66.4° 10.3° 65.7°)
[111]/43.9°
35
(322.3° 36.4° 41.9°)
[]/39.1°
36
(271.3° 29.1° 34.3°)
[]/18.9°
37
(81.1° 30° 65.4°)
-
-
26
(256.8° 26.1° 29.7°)
[]/52.0°
32
(207.7° 36.6° 58.9°)
[]/42.8°
38
(19.1° 11.3° 65.1°)
[]/40.1°
39
(29.5° 18.9° 25.5°)
[149]/23.2°
40
(38.1° 24.4° 15.7°)
[]/20.1°
33
(168.2° 38.5° 4.5°)
[]/48.5°
Table 3 Orientation statistics of the grains around the nonadjacent growing grains having <111>/θ misorientation in the high purity aluminum heated at 500oC (See in Fig.7)
Grain No.
Euler angle of adjacent grains
Euler angles of grains around two adjacent grains
Misorientation between grains and two adjacent grains
1
(82.3° 35.5° 10.9°)
-
-
2
(97.1° 39.8° 1°)
[]/10.2°
3
(12° 28.3° 40.7°)
[]/47.8°
4
(5.7° 44° 16.6°)
[111]/57.1°
5
(45.3° 43.2° 58.4°)
[]/30.5°
6
(231° 43.7° 50.2°)
[]/44.7°
7
(347.2° 11.8° 71.1°)
[]/48.9°
6
(231° 43.7° 50.2°)
-
-
5
(45.3° 43.2° 58.4°)
[]/49.5°
8
(55.8° 36.3° 36.9°)
[]/59.4°
10
(157.8° 24.9° 50.5°)
[]/49.6°
11
(172.8° 25.8° 34.9°)
[]/43.6°
12
(221.9° 32.3° 43.2°)
[]/19.0°
13
(234.5° 24.6° 33.2°)
[]/23.8°
14
(240.2° 27.6° 11.1°)
[]/35.7°
7
(347.2° 11.8° 71.1°)
[]/53.2°
15
(337.4° 36.7° 9.2°)
-
-
16
(335° 18° 68.7°)
[]/37.5°
17
(176.5° 39.3° 88.9°)
[]/19.0°
18
(163.5° 7.7° 85.8°)
[071]/44.9°
19
(2.3° 47.5° 57.7°)
[313]/30.1°
20
(142.2° 37.9° 29.3°)
[]/29.9°
21
(196.9° 27.1° 40°)
[]/38.0°
20
(142.2° 37.9° 29.3°)
-
-
19
(2.3° 47.5° 57.7°)
[]/13.8°
22
(41.6° 45.2° 60.7°)
[]/41.1°
21
(196.9° 27.1° 40°)
[]/43.7°
23
(195.4° 38.7° 73.3°)
-
-
24
(160.7° 43.3° 1°)
[]/24.6°
25
(318.3° 32.6° 88.2°)
[]/52.0°
26
(259.4° 29° 46.6°)
[]/45°
27
(279.6° 29.5° 78.1°)
[]/46.1°
28
(305.7° 7.1° 8.9°)
[]/59.5°
29
(329.1° 48.9° 43.7°)
-
-
23
(195.4° 38.7° 73.3°)
[]/24.8°
28
(305.7° 7.1° 8.9°)
[233]/53.3°
31
(292.6° 44.3° 18.2°)
[203]/46.9°
32
(264.2° 41.1° 13.6°)
[]/46.5°
33
(217.9° 34.7° 53°)
[]/26.5°
30
(184.2° 38.8° 83.4°)
[]/29.4°
Table 4 Orientation statistics of the grains around two adjacent grains having <111>/θ misorientation in the high purity aluminum heated at 500oC (See in Fig.8)
Fig.9 HRTEM images and SAED patterns (Insets) of {111}/{111} near singular boundaries in the high purity aluminum (d{111}—interplanar spacing) (a) with a misorientation of []/33.3° (b) with a misorientation of []/24.2°
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