Grain size effects in aluminum processed by severe plastic deformation

Takayuki Koizumi1,*, Mitsutoshi Kuroda2

1
Engineering department, Yamagata University, Jonan 4-3-16, Yonezawa, Yamagata 992-8510, Japan
2
Graduate School of Science and Engineering, Mechanical Engineering, Yamagata University, Jonan
4-3-16, Yonezawa, Yamagata 992-8510, Japan
*Corresponding author. koizumi@yz.yamagata-u.ac.jp.

This online supplementary material includes the following:

Table S1. Magnification and number of measurement points for each sample in

the EBSD observation and analysis.

Table S2. Parameters of the Hall-Petch relation reported in the literature for

pure aluminum at room temperature.

Table S3. The data for the calculation of dislocation density according to XRD

line profiles in present study.

1
Table S1. Magnification and number of measurement points for each sample in the EBSD

observation and analysis.

Refining approach Coarsening approach

Magnification Number of Magnification Number of

Sample measurement Sample measurement
Step size [µm] points Step size [µm] points

250 2000
0 passes 3 8 passes-O1 5
2.0 0.2

250 2000
1 pass 6 8 passes-O2 5
2.0 0.2

250 2000
2 passes 5 8 passes-O3 5
2.0 0.2

2000 2000
3 passes 6 8 passes-O4 5
0.2 0.2

2000 250
4 passes 6 8 passes-O5 5
0.2 2.0

2000 250
5 passes 6 8 passes-O6 5
0.2 2.0

2000 250
6 passes 6 8 passes-O7 5
0.2 2.0

2000 250
7 passes 6 8 passes-O8 5
0.2 2.0

2000 250
8 passes 6 8 passes-O9 5
0.2 2.0

2
Table S2. Parameters of the Hall-Petch relation reported in the literature for pure aluminum at

room temperature.

No. Al Range of grain &' ( Reference

purity size [µm] [MPa] [MPa µm1/2]
1 99.99 18-400 9.7 41.0 [21]

2 99.999 35-1300 5.6 41.1 [41]

3 99.99 71-760 8.5 47.4 [41]

4 99.99 30-490 9.0 63.0 [41]

5 99.99 33-155 12.2 10.0 [41]

6 99.99 35-180 17.0 13.0 [41]

7 99.98 25-1000 3.0 32.0 [41]

8 99.9 15-320 3.0 60.0 [41]

9 99.7 16-40 15.5 36.0 [41]

10 99.5 15-240 18.0 25.3 [41]

11 99.5 12-1200 16.0 40.0 [41]

12 99.2 25-1000 11.0 43.0 [41]

13 99.0 20-200 14.3 65.0 [41]

14 98.65 25-150 12.7 30.0 [41]

15 99.50 35-400 17.2 42.4 [42]

16 68.0 [42]

17 99.70 15-220 9.2 83.1 Present work

Average 11.4 43.5 No.1 No.17

Standard deviation 4.7 18.9 No.1 No.17

3
 Table S3. The data for the calculation of dislocation density according to XRD line profiles in present study (continue).
Reflection peaks Lattice Dislocation
Measurement Measurement Crystallite
strain density
conditions items [deg.] size [nm]
(111) (200) (220) (311) (222) (400) (331) (420) (422) [´10-3] [´1014m-2]
FWHM 0.0993 0.1094 0.1170 0.1558 0.1663 0.1962 0.2360 0.2425 0.4171
-1 0.724 122 0.721
2q 38.4444 44.6864 65.0724 78.1987 82.4031 99.0583 111.9917 116.5103 137.4552
FWHM 0.1035 0.1087 0.1125 0.1436 0.1536 0.2099 0.2185 0.2455 0.4188
1 pass -2 0.709 123 0.697
2q 38.4569 44.6969 65.0672 78.1863 82.3895 98.9932 111.9729 116.5315 137.3402
FWHM 0.0969 0.1019 0.1113 0.1333 0.1513 0.2227 0.2462 0.2518 0.3881
-3 0.836 147 0.689
2q 38.4643 44.7111 65.0860 78.2194 82.4127 99.0268 111.9766 116.5340 137.4386
FWHM 0.0873 0.1031 0.1131 0.1451 0.1224 0.1790 0.2302 0.2553 0.3921
-1 0.797 156 0.621
2q 38.4535 44.7079 65.0728 78.2032 82.4334 99.0467 112.0045 116.5311 137.4343
2 FWHM 0.1036 0.0928 0.1229 0.1434 0.1397 0.1473 0.2290 0.2667 0.4150
-2 0.744 139 0.648
passes 2q 38.4528 44.6960 65.0801 78.2059 82.4084 99.0269 111.9877 116.5395 137.4507
FWHM 0.0960 0.0928 0.1144 0.1379 0.1250 0.1901 0.1842 0.2485 0.4591
-3 0.855 171 0.607
2q 38.4545 44.6882 65.0629 78.1900 82.4030 99.0525 111.9486 116.5310 137.4103
FWHM 0.0926 0.1057 0.1182 0.1499 0.1534 0.1565 0.2208 0.2737 0.3953
-1 0.721 132 0.660
2q 38.4636 44.7161 65.0819 78.2084 82.4060 99.0576 112.0038 116.6001 137.4172
3 FWHM 0.0979 0.0969 0.1095 0.1465 0.1310 0.1666 0.2429 0.2444 0.3650
-2 0.679 134 0.612
passes 2q 38.4625 44.7023 65.0880 78.2041 82.4147 99.0665 112.0160 116.5720 137.4306
FWHM 0.0921 0.1005 0.1272 0.1462 0.1357 0.1986 0.1927 0.2477 0.4037
-3 0.695 131 0.642
2q 38.4678 44.7214 65.0927 78.2209 82.4191 99.1037 112.0076 116.5528 137.4374
FWHM 0.0900 0.1043 0.1152 0.1386 0.1281 0.1883 0.2241 0.2354 0.3725
-1 0.670 134 0.608
2q 38.4561 44.7142 65.0868 78.2175 82.4278 99.0591 112.0077 116.5472 137.4253
4 FWHM 0.0846 0.0937 0.1091 0.1315 0.1355 0.1676 0.2166 0.2203 0.3359
-2 0.615 139 0.535
passes 2q 38.4492 44.7126 65.0859 78.2185 82.4273 99.0814 112.0024 116.5669 137.4332
FWHM 0.0976 0.0973 0.1174 0.1333 0.1386 0.1562 0.2525 0.2635 0.3794
-3 0.755 144 0.635
2q 38.4718 44.7136 65.0951 78.2204 82.4277 99.0518 111.9807 116.5613 137.4492

4
 Table S3. The data for the calculation of dislocation density according to XRD line profiles in present study (continue).
Reflection peaks Lattice Dislocation
Measurement Measurement Crystallite
strain density
conditions items [deg.] size [nm]
(111) (200) (220) (311) (222) (400) (331) (420) (422) [´10-3] [´1014m-2]
FWHM 0.0893 0.0889 0.0985 0.1238 0.1252 0.1646 0.1728 0.2269 0.2656
-1 0.373 118 0.383
2q 38.4548 44.7001 65.0737 78.2012 82.4038 99.0641 112.0131 116.5472 137.3960
FWHM 0.0957 0.0911 0.0956 0.1202 0.1317 0.1517 0.2008 0.2149 0.3114
5 passes -2 0.447 123 0.441
2q 38.4406 44.6907 65.0584 78.1974 82.4033 99.0614 112.0017 116.5449 137.4280
FWHM 0.0885 0.0869 0.0962 0.1157 0.1051 0.1768 0.1846 0.1869 0.3179
-3 0.477 137 0.422
2q 38.4715 44.7141 65.0871 78.2249 82.4260 99.0574 112.0200 116.5342 137.4731
FWHM 0.0856 0.1010 0.1095 0.1187 0.1119 0.1504 0.1792 0.1852 0.2773
-1 0.214 103 0.251
2q 38.4363 44.6891 65.0635 78.1954 82.4110 99.0319 111.9921 116.5609 137.4580
FWHM 0.0886 0.0896 0.0926 0.1156 0.1189 0.1517 0.1663 0.1968 0.2561
6 passes -2 0.255 112 0.276
2q 38.4626 44.7032 65.0799 78.2100 82.4169 99.0831 111.9994 116.5471 137.4211
FWHM 0.0823 0.0853 0.0890 0.1136 0.0987 0.1451 0.1730 0.2039 0.2694
-3 0.396 137 0.350
2q 38.4548 44.7035 65.0803 78.2138 82.4062 99.0364 111.9897 116.5570 137.4197
FWHM 0.0816 0.0877 0.0990 0.1170 0.1207 0.1303 0.1929 0.1992 0.3133
-1 0.479 140 0.414
2q 38.4434 44.6997 65.0787 78.2061 82.4143 99.0658 111.9973 116.5442 137.4420
FWHM 0.0927 0.0879 0.0995 0.1206 0.1218 0.1366 0.1840 0.1870 0.3046
7 passes -2 0.327 116 0.342
2q 38.4698 44.7086 65.0901 78.2185 82.4296 99.0585 112.0129 116.5581 137.4526
FWHM 0.0868 0.0914 0.0995 0.1125 0.1193 0.1448 0.1890 0.2187 0.2818
-3 0.403 125 0.39
2q 38.4672 44.7238 65.0886 78.2201 82.4267 99.0701 111.9925 116.5464 137.4614
FWHM 0.0833 0.0853 0.0995 0.1154 0.1177 0.1212 0.1618 0.1962 0.3034
-1 0.360 128 0.340
2q 38.4443 44.7021 65.0707 78.2095 82.4134 99.0553 111.9921 116.5533 137.4262
FWHM 0.0815 0.0884 0.0984 0.1192 0.1210 0.1710 0.1462 0.2042 0.2892
8 passes -2 0.386 126 0.372
2q 38.4416 44.6945 65.0650 78.1981 82.4039 99.0669 111.9899 116.5343 137.4321
FWHM 0.0845 0.0860 0.0916 0.1131 0.1146 0.1478 0.1657 0.1892 0.2881
-3 0.365 129 0.344
2q 38.4383 44.6901 65.0645 78.2074 82.4115 99.0474 111.9877 116.5171 137.4451

5
 Table S3. The data for the calculation of dislocation density according to XRD line profiles in present study.
Reflection peaks Lattice Dislocation
Measurement Measurement Crystallite
strain density
conditions items [deg.] size [nm]
(111) (200) (220) (311) (222) (400) (331) (420) (422) [´10-3] [´1014m-2]
FWHM 0.0833 0.0797 0.0843 0.1051 0.0998 0.1207 0.1524 0.1712 0.2561
-1 0.234 126 0.225
2q 38.4443 44.6914 65.0707 78.1986 82.4176 99.0574 111.9829 116.5524 137.4341
8 passes FWHM 0.0909 0.0797 0.0859 0.1089 0.1035 0.1493 0.1508 0.1636 0.2822
-2 0.259 121 0.258
-O1 2q 38.4627 44.6974 65.0803 78.2055 82.4199 99.0615 111.9998 116.5797 137.4429
FWHM 0.0808 0.0780 0.0840 0.1044 0.1105 0.1188 0.1717 0.1682 0.2759
-3 0.349 141 0.301
2q 38.4581 44.7054 65.0841 78.2116 82.4159 99.0555 111.9871 116.5904 137.4552
FWHM 0.0910 0.0975 0.0955 0.1085 0.1071 0.1354 0.1614 0.1839 0.2825
-1 0.176 105 0.203
2q 38.4481 44.6950 65.0631 78.1933 82.4090 99.0385 111.9972 116.5480 137.4366
8 passes FWHM 0.0792 0.0838 0.0928 0.1111 0.1073 0.1512 0.1744 0.1839 0.2873
-2 0.428 142 0.366
-O2 2q 38.4323 44.6831 65.0562 78.1879 82.4048 99.0345 111.9783 116.5265 137.4324
FWHM 0.0717 0.0768 0.0915 0.1036 0.1119 0.1493 0.1621 0.1599 0.3054
-3 0.489 166 0.358
2q 38.4292 44.6801 65.0650 78.1849 82.3927 99.0527 111.9957 116.5259 137.3974
8 passes FWHM 0.0795 0.0691 0.0744 0.0834 0.0965 0.1028 0.1233 0.1220 0.2154
-1 0.041 121 0.040
-O3 2q 38.4529 44.6949 65.0646 78.1982 82.4057 99.0450 111.9815 116.5317 137.4314
8 passes FWHM 0.0633 0.0684 0.0620 0.0786 0.0806 0.1013 0.1179 0.1117 0.1703
-1 0.048 138 0.042
-O4 2q 38.4600 44.7183 65.0882 78.2262 82.4317 99.0762 112.0077 116.5489 137.4449