Effects of Ambient and Cryogenic Rolling on {111}/{111} Near Singular Boundary Formation During Subsequent Recrystallization Annealing in Pure Aluminum

doi:10.11900/0412.1961.2024.00035

Acta Metall Sin

2025, Vol. 61

Issue (11): 1673-1688 DOI: 10.11900/0412.1961.2024.00035

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Effects of Ambient and Cryogenic Rolling on {111}/{111} Near Singular Boundary Formation During Subsequent Recrystallization Annealing in Pure Aluminum

LI Zhenxiang¹, WANG Weiguo¹^,²(

), Rohrer Gregory S³, HONG Lihua¹^,², CHEN Song¹^,², LIN Yan¹^,², 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

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LI Zhenxiang, WANG Weiguo, Rohrer Gregory S, HONG Lihua, CHEN Song, LIN Yan, ZHOU Bangxin. Effects of Ambient and Cryogenic Rolling on {111}/{111} Near Singular Boundary Formation During Subsequent Recrystallization Annealing in Pure Aluminum. Acta Metall Sin, 2025, 61(11): 1673-1688.

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Abstract

Recent advancements in grain boundary engineering have revealed that the {111}/{111} near singular boundary (NSB) exhibits superior resistance to corrosion attacks than the random boundary in aluminum and its alloys. Thus, understanding the influential factors and formation mechanisms of the {111}/{111} NSB, as well as regulating such boundaries, is crucial for enhancing the resistance performance of aluminum and its alloys against intergranular corrosion attacks. To intrinsically comprehend the formation mechanism of the {111}/{111} NSB in aluminum alloys, this study used high purity aluminum (99.99%) as the experimental material. Initially, the starting samples were synthesized through multidirectional forging at room temperature (25 ^oC), followed by recrystallization annealing at 370 ^oC. The as-synthesized starting samples exhibited uniform microstructures with an average grain size of 20 μm and random grain orientations. Subsequently, two parallel starting samples were rolled at 25 ^oC and at the cryogenic temperature (-196 ^oC), respectively, with an 80% thickness reduction, followed by immediate recrystallization annealing at 370 ^oC for 30 min. Later, a quantitative grain boundary inter-connection characterization method based on EBSD and five parameter analysis was employed to statistically analyze the grain boundary character distributions within the samples. The results revealed that the cryo-rolled and recrystallized sample featured a higher proportion of the {111}/{111} NSB compared to the 25 ^oC-rolled and recrystallized sample. Specifically, the {111}/{111} NSB fraction in the former reached 6.0%, 2.22 times that in the latter. XRD analysis, hardness testing, and EBSD measurements revealed the development of a strong {011}< $11 1 ¯$ > deformation texture in the samples rolled at 25 ^oC or the cryogenic temperature. In particular, cryo-rolling was found to impede dynamic recovery; hence, the sample rolled at this temperature featured higher levels of residual compression stress, increased grain fragmentation, and higher stored energy compared to the sample rolled at 25 ^oC. Owing to the higher driving force and more active {011}< $01 1 ¯$ >-oriented growth, the cryo-rolled sample formed larger grains and stronger {011}< $01 1 ¯$ > recrystallization textures during the subsequent recrystallization annealing. Statistical analysis based on grain boundary tracing demonstrated that the grain boundaries between {011}< $01 1 ¯$ >-oriented grains and other oriented grains contained higher proportions of the {111}/{111} NSB compared to the grain boundaries between two randomly oriented grains. Moreover, boundaries between the {011}< $01 1 ¯$ >- oriented grains and their diffusive orientations featured notably high proportions of the {111}/{111} NSB. This explains the higher content of the {111}/{111} NSB observed in the cryo-rolled and recrystallized sample than that in the 25 ^oC-rolled and recrystallized sample.

Key words: high purity aluminum cryo-rolling near singular boundary grain boundary inter-connection

Received: 30 January 2024

ZTFLH:

TG146.2

Fund: National Natural Science Foundation of China(51971063);Natural Science Foundation of Fujian Province(2021J011076)

Corresponding Authors: WANG Weiguo, professor, Tel: (0591)22863515, E-mail: wang_weiguo@vip.163.com

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	LI Zhenxiang
	WANG Weiguo
	Rohrer Gregory S
	HONG Lihua
	CHEN Song
	LIN Yan
	ZHOU Bangxin

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https://www.ams.org.cn/EN/10.11900/0412.1961.2024.00035 OR https://www.ams.org.cn/EN/Y2025/V61/I11/1673

Table 1 High purity aluminum samples and treatments

Fig.1 Orientation imaging microscopy (OIM) images (a, d), grain boundary networks (b, e), and misorientation distributions (c, f) of sample F (a-c) and sample F1 (d-f) (LAGB—low-angle grain boundary)

Table 2 After-filtration statistics of the grain boundaries (GBs) with the rotation axes of <111>, <112>, and <122> in samples F and F1

Fig.2 Misorientation distributions of grain boundaries with specific rotation axis for samples F and F1
(a) rotation around <111>
(b) rotation around <112>
(c) rotation around <122>

Fig.3 Grain boundary plane distribution (GBPD) maps of the grain boundaries with varied misorientations containing {111}/{111} near singular boundary (NSB) in sample F (MRD—multiple of random distribution)
(a) [111]/20° (b) [111]/25° (c) [111]/30°
(d) [111]/55° (e) [112]/30°
(f) [122]/20° (g) [122]/30°

Fig.4 GBPD maps of the grain boundaries with varied misorientations containing {111}/{111}-NSB in sample F1
(a) [111]/15° (b) [111]/25° (c) [111]/30° (d) [111]/35° (e) [111]/40° (f) [111]/45°
(g) [111]/50° (h) [111]/55° (i) [112]/25° (j) [122]/20° (k) [122]/25° (l) [122]/30°
(m) [122]/35° (n) [122]/40°

Table 3 Statistics of the {111}/{111}-NSB in samples F and F1

Fig.5 XRD spectra of sample A (a) and sample A1 (b) obtained from the rolling planes (A-ND and A1-ND), the planes perpendicular to rolling direction (A-RD and A1-RD), and from the sample of powdered pure aluminum (Powder) (ND—normal direction, RD—rolling direction)

Fig.6 XRD spectra of the rolled samples and the samples annealed at 370 ^oC for varied time after rolling
(a) {022}diffraction peaks of the samples A, A1, B, B1, and powder (θ_i —diffraction angle of sample i)
(b) {022} diffraction peaks of samples A-F and A1-F1

Fig.7 Compressive stresses in normal direction of the rolled samples and the samples annealed at 370 ^oC for varied time after rolling

Fig.8 Vickers hardnesses of the rolled samples and the samples annealed at 370 ^oC for varied time after rolling

Fig.9 Average grain sizes of the samples annealed at 370 ^oC for varied time after rolling at room temperature (RT) and cryo-temperature (CT)

Fig.10 Orientation distribution function (ODF) sections (φ₂ = 45º) of the samples annealed at 370 ^oC for varied time after rolling at room temperature and cryo-temperature (Φ, φ₁, φ₂—Euler angles)
(a) sample B (b) sample D (c) sample F
(d) sample B1 (e) sample D1 (f) sample F1

Rolling	Grain	Number of	Number of	Number of NSB	Percentage of
temperature	orientation	grain	boundary		NSB / %
RT	{100}<001>	10	73	3	4.1
	{011}< $01 1 ¯$ >	10	64	4	6.3
	{111}< $01 1 ¯$ >	10	74	3	4.0
CT	{100}<001>	10	76	4	5.3
	{011}< $01 1 ¯$ >	10	63	6	9.5
	{111}< $01 1 ¯$ >	10	70	2	2.9

Table 4 Characteristic statistics of the grain boundaries associated with every ten grains of three different orientations

Fig.11 {111}/{111}-NSB (GB_GJ, GB_HK, and GB_IL) formed between {011}< $01 1 ¯$ > oriented grains (grains G, H, and I) and other oriented grains (grains J, K, and L)
(a-c) OIM images (d-f) {111} overlapped pole figure grain boundary trace analyses

Fig.12 {111}/{111}-NSB (GB_AD, GB_BE, and GB_CF) formed between {011}< $01 1 ¯$ > oriented grains (grains A, B, and C) and grains of {011}< $01 1 ¯$ > diffusive orientation (grains D, E, and F)
(a-c) OIM images (d-f) {111} overlapped pole figure grain boundary trace analyses

Grain boundary	Orientation of grains G, H, and I		Orientation of grains J, K, and L		Misorientation [uvw]/θ'
Grain boundary	Euler angle (φ₁, Ф, φ₂)	Miller indexed	Euler angle (φ₁, Ф, φ₂)	Miller indexed	Misorientation [uvw]/θ'
GB_GJ	G: 1°, 90°, 39°	{011}< $01 1 ¯$ >	J: 212°, 21°, 27°	{126}< $2 ¯ 4 1 ¯$ >	[ $1 1 ¯ 1$ ]/41.4°
GB_HK	H: 359°, 91°, 42°	{011}< $01 1 ¯$ >	K: 226°, 33°, 57°	{326}< $215 6 ¯$ >	[ $1 1 ¯ 1$ ]/35.8°
GB_IL	I: 356°, 86°, 45°	{011}< $01 1 ¯$ >	L: 59°, 32°, 69°	{314}< $0 4 ¯ 1$ >	[ $1 1 ¯ 1$ ]/45.8°

Table 5 Information related to the formation of {111}/{111}-NSB as shown in Fig.11

Fig.13 Schematics of unit cell showing the formation of {111}/{111}-NSB abutted by {011}< $01 1 ¯$ > oriented grain (P1 and P2) with grain M of {011}< $01 1 ¯$ > diffusive orientation (a) and grain N of other orientation (b)表7 {011}< $01 1 ¯$ >取向晶粒(P1和P2)与{011}< $01 1 ¯$ >漫散取向晶粒M及其他取向晶粒N的取向信息及其关联晶界的取向差信息(对应图13)

Orientation of grains P1 and P2

Orientation of grains M and N

Misorientation

[uvw]/θ'

Euler angle

(φ₁, Ф, φ₂)

Miller indexed

Euler angle

(φ₁, Ф, φ₂)

Miller indexed

P1: -4.6°, 89°, 43°

{011}<

01 1 ¯

M: 11°, 88°,5 5°

{320}<

3 4 ¯ 1

[111]/19.9°

P2: 0°, 90°, 46°

{011}<

01 1 ¯

N: 55°, 32°, 45°

{112}<

0 2 ¯ 1

[

1 1 ¯ 1

/29.5°

Table 7 Information related to the formation of {111}/{111}-NSB as shown in Fig.13

Grain boundary	Orientation of grains A, B, and C		Orientation of grains D, E, and F		Misorientation [uvw]/θ'
Grain boundary	Euler angle (φ₁, Ф, φ₂)	Miller indexed	Euler angle (φ₁, Ф, φ₂)	Miller indexed	Misorientation [uvw]/θ'
GB_AD	A: 357°, 89°, 39°	{011}< $01 1 ¯$ >	D: 10°, 89°, 46°	{110}< $4 4 ¯ 1$ >	[111]/15.2°
GB_BE	B: 356°, 92°, 39°	{011}< $01 1 ¯$ >	E: 19°, 90°, 57°	{320}< $6 9 ¯ 4$ >	[ $1 1 ¯ 1$ ]/28.8°
GB_CF	C: 356°, 87°, 45°	{011}< $01 1 ¯$ >	F: 12°, 86°, 56°	{320}< $6 9 ¯ 2$ >	[111]/20.3°

Table 6 Information related to the formation of {111}/{111}-NSB as shown in Fig.12

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