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Acta Metall Sin  2024, Vol. 60 Issue (9): 1165-1178    DOI: 10.11900/0412.1961.2023.00170
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{111}/{111} Near Singular Boundaries in a Dynamically Recrystallized Al-Zn-Mg-Cu Alloy Compressed at Elevated Temperature
LIU Guanghui1, WANG Weiguo1,2(), Rohrer Gregory S3, CHEN Song1,2, LIN Yan1,2, TONG Fang1, FENG Xiaozheng1, 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, PA15213 -3890, USA
4.Institute of Materials, Shanghai University, Shanghai 200072, China
Cite this article: 

LIU Guanghui, WANG Weiguo, Rohrer Gregory S, CHEN Song, LIN Yan, TONG Fang, FENG Xiaozheng, ZHOU Bangxin. {111}/{111} Near Singular Boundaries in a Dynamically Recrystallized Al-Zn-Mg-Cu Alloy Compressed at Elevated Temperature. Acta Metall Sin, 2024, 60(9): 1165-1178.

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Abstract  

Increasing the fraction of {111}/{111} near-singular boundaries ({111}/{111}-NSBs) has been reported as a primary solution to intergranular corrosion failure in Al-Zn-Mg-Cu alloys. The authors' previous work demonstrates that continuous static recrystallization resulting from a specific prestrain and annealing is conducive to the formation of {111}/{111}-NSBs in Al-Zn-Mg-Cu alloys. Therefore, the development of such boundaries in the alloys during dynamic recrystallization (DRX), particularly during discontinuous DRX (DDRX) and continuous DRX (CDRX) at elevated temperatures, should be elucidated. In the present work, an Al-Zn-Mg-Cu alloy containing 7.79%Zn, 1.53%Mg, and 1.68%Cu (mass fraction) was selected as the experimental material. A hot-rolled plate of the alloy was subjected to a two-stage solution treatment at 470oC for 12 h and 520oC for 6 h followed by cold rolling and recrystallization annealing. Three parallel samples cut from the recrystallized plate were compressed at 450, 480, and 520oC at a strain rate of 0.001 s-1 to a true strain of 1.20. The samples were water quenched immediately after the compression. Electron backscatter diffraction and grain boundary inter-connection measurement based on five-parameter analysis were performed to examine the microstructures and grain boundary character distributions of the compressed samples. The results indicate that the microstructures of the samples were uneven, exhibiting fine- and coarse-grained regions. Low-angle grain boundaries are dominant in the fine-grained regions, whereas high-angle grain boundaries are dominant in the coarse-grained regions. The fraction of {111}/{111}-NSBs increases with the compression temperature in fine- and coarse-grained regions. In the sample compressed at 520oC, the {111}/{111}-NSBs from the low-angle grain boundaries constitute 8.77% of all grain boundaries, while those from the high-angle grain boundaries constitute 4.53%. The stress-strain curves and the microstructures of the sample compressed at 450oC to a true strain of 0.36 show that primary DRX occurs at strains from 0.05 to 0.70. Furthermore, the coarse-grained microstructures and high-angle grain boundaries develop during the stage involving steady-state flow. When the strain increases from 0.70 to 1.20, secondary DRX (including DDRX and CDRX) occurs in some regions, leading to dramatic grain refinement and a sharp increase in flow stress. In this stage, CDRX intensifies with increasing compression temperature, and {111}/{111}-NSBs in the low-angle grain boundaries increase rapidly.

Key words:  Al-Zn-Mg-Cu alloy      near singular boundary      grain boundary inter-connection      continuous dynamic recrystallization     
Received:  17 April 2023     
ZTFLH:  TG113  
Fund: National Natural Science Foundation of China(51971063,52271027)
Corresponding Authors:  WANG Weiguo, professor, Tel: (0591)22863515, E-mail: wang_weiguo@vip.163.com

URL: 

https://www.ams.org.cn/EN/10.11900/0412.1961.2023.00170     OR     https://www.ams.org.cn/EN/Y2024/V60/I9/1165

Fig.1  Orientation imaging microscopy (OIM) images (a, d, g), grain boundary network (GBN) maps (b, e, h), and the magnifications of the fine-grained regions as marked by the squares in Figs.1b, e, and h (c, f, i) for the samples A (a-c), B (d-f), and C (g-i) compressed at 450, 480, and 520oC, respectively (In Figs.1b, e, and h, red arrows point at the fine grains aggregated at the initial grain boundaries; the areas framed by the red dotted lines are the coarse-grained regions, the areas framed by the green dotted lines are the fine-grained regions)
Fig.2  Misorientation distribution (MD) maps of the reconstructed grain boundaries in the samples A (a), B (b), and C (c)
SampleRotation axisNBLF / %NF / %
A<001>13402.502.52
<011>34505.726.49
<012>559310.2010.52
<013>53329.9610.03
<111>25944.924.88
<112>644312.0712.12
<113>554510.5910.43
<122>743214.1013.98
B<001>13492.402.44
<011>33856.076.12
<012>562010.0810.16
<013>563610.2410.19
<111>28045.035.07
<112>668212.2812.08
<113>584610.5810.57
<122>771014.0413.94
C<001>13712.732.60
<011>33166.306.29
<012>548410.2110.40
<013>52999.9910.05
<111>25734.794.88
<112>630612.0611.96
<113>550510.5910.44
<122>731813.8313.88
Table 1  Grain boundary (GB) statistics after-filtration according to the 8 low Miller index rotation axes in the samples A-C
Fig.3  MD maps of grain boundaries with specific rotation axis for the samples A-C
(a) rotation around <001> (b) rotation around <011> (c) rotation around <012>
(d) rotation around <013> (e) rotation around <111> (f) rotation around <112>
(g) rotation around <113> (h) rotation around <122>
Fig.4  Five parameter grain boundary plane distributions of the low-angle grain boundary (LAGB) groups containing {111}/{111} near singular boundaries ({111}/{111}-NSB) in the sample C (A projection onto (001); MRD—multiple of random distribution)
(a) <00>/10° (b) <011>/5° (c) <011>/10° (d) <012>/5° (e) <012>/10° (f) <013>/5°
(g) <013>/10° (h) <111>/10° (i) <112>/5° (j) <112>/10° (k) <122>/5° (l) <122>/10°
Fig.5  Five parameter grain boundary plane distributions of the high-angle grain boundary (HAGB) groups containing {111}/{111}-NSB in the sample C (A projection onto (001))
(a) <111>/20° (b) <111>/25° (c) <111>/45° (d) <111>/50° (e) <111>/60° (f) <112>/15°
(g) <112>/20° (h) <112>/25° (i) <122>/15° (j) <122>/25° (k) <122>/30° (l) <122>/35°
Fig.6  Weighted Gaussian misorientation distribution curves of two grain boundary groups containing {111}/{111}-NSBs in the sample C (FWHM—full width half maximum)
(a) <111>/10° (b) <111>/45°
Sample

Misorientation

<uvw>/θ

Pi

%

Mi

Wi

(°)

Fi

%

F

%

A<012>/5°1.161.901.700.624.18
<013>/5°1.111.642.010.58
<111>/5°0.421.862.130.22
<111>/10°0.711.852.090.37
<113>/10°2.131.321.831.11
<122>/10°2.491.372.111.28
B<011>/5°0.661.691.940.354.87
<011>/10°1.111.432.000.58
<112>/5°1.331.552.170.69
<013>/5°1.311.301.780.68
<111>/5°0.441.851.820.23
<111>/10°0.731.612.290.38
<122>/5°1.401.441.980.72
<122>/10°2.391.572.121.24
C<001>/10°0.591.521.850.318.77
<011>/5°0.541.591.690.29
<011>/10°1.092.331.800.59
<012>/5°1.181.512.010.61
<012>/10°2.141.531.901.11
<013>/5°1.251.312.260.64
<013>/10°2.181.342.081.12
<111>/10°0.711.741.800.37
<112>/5°1.411.341.840.73
<112>/10°2.231.492.101.15
<122>/5°1.202.011.400.65
<122>/10°2.321.482.021.20
Table 2  Statistics of the {111}/{111}-NSBs within the LAGB in the samples A-C
Fig.7  Relative frequency of {111}/{111}-NSB from the LAGB and HAGB in samples A-C
Sample

Misorientation

<uvw>/θ

Pi

%

Mi

Wi

(°)

Fi

%

F

%

A<111>/15°0.472.272.250.252.54
<111>/20°0.341.981.790.18
<111>/35°0.342.061.650.19
<111>/40°0.301.322.050.16
<111>/45°0.411.401.770.21
<112>/20°1.041.421.880.54
<122>/20°0.961.572.050.50
<122>/40°0.991.242.150.51
B<111>/25°0.322.402.330.173.69
<111>/30°0.271.551.440.14
<111>/35°0.331.741.870.17
<111>/40°0.361.531.570.19
<111>/50°0.871.451.890.23
<111>/55°0.522.352.070.28
<112>/15°1.601.302.010.84
<1 2>/25°0.841.222.060.43
<112>/30°0.721.622.070.37
<122>/35°0.771.252.060.39
<122>/40°0.931.462.020.48
C<111>/20°0.302.301.960.164.53
<111>/25°0.282.091.720.15
<111>/45°0.421.721.950.22
<111>/50°0.492.221.730.26
<111>/60°0.361.882.170.19
<112>/15°1.441.252.070.74
<112>/20°0.971.292.090.50
<112>/25°0.791.362.070.41
<122>/15°1.201.352.040.62
<122>/25°0.711.361.870.37
<122>/30°0.921.361.740.48
<122>/35°0.821.511.910.43
Table 3  Statistics of the {111}/{111}-NSBs within the HAGB in the samples A-C
Fig.8  Load-displacement (a) and stress-strain (b) curves of samples A-C
Fig.9  OIM images (a, c) and GBN maps (b, d) of the Al-Zn-Mg-Cu alloy compressed at 450oC with a strain rate 0.001 s-1 and true strain 0.36 (The area framed by the red dotted line in Fig.9b is the region where grains begin to refine)
(a, b) compression plane (c, d) cross section
Fig.10  Kernel average misorientations (KAM) maps of fine-grained regions in samples A (a), B (b), and C (c)
Fig.11  GBN maps of HAGB and LAGB with different rotation angles in samples A (a), B (b), and C (c)
Fig.12  Overlapped {111} pole figure trace analyses for the {111}/{111}-NSBs from the LAGB and HAGB in samples A (a-d), B (e-h), and C (i-l)
(a, b) <11¯1¯>/5.7° (c, d) <11¯1¯>/48.4° (e, f) <1¯1¯1>/6.2°
(g, h) <111>/46.1° (i, j) <11¯1>/8.2° (k, l) <1¯11>/17.6°
Fig.13  Area fractions of continuous dynamic recrystallization (CDRX) (ƒCDRX) and discontinuous dynamic recrystallization (DDRX) (ƒDDRX) versus compressing temperatures for Al alloys (Compressed with a strain rate 0.001 s-1 and true strain 1.2)
Fig.14  Area fractions of CDRX and DDRX versus compressing strain rate for Al alloys (Compressed at 520oC with true strain 1.2)
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