室温和深冷轧制对纯<strong>Al</strong>再结晶<strong>{111}/{111}</strong>近奇异晶界的影响

doi:10.11900/0412.1961.2024.00035

金属学报

2025, Vol. 61

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

研究论文

本期目录 | 过刊浏览

室温和深冷轧制对纯Al再结晶{111}/{111}近奇异晶界的影响

李振想¹, 王卫国¹^,²(

), Rohrer Gregory S³, 洪丽华¹^,², 陈松¹^,², 林燕¹^,², 周邦新⁴

1 福建理工大学晶界工程研究所福州 350118
2 福建理工大学材料科学与工程学院福州 350118
3 Department of Materials Science and Engineering, Carnegie Mellon University, Pittsburgh, PA15213 -3890, USA
4 上海大学材料研究所上海 200072

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

引用本文:

李振想, 王卫国, Rohrer Gregory S, 洪丽华, 陈松, 林燕, 周邦新. 室温和深冷轧制对纯Al再结晶{111}/{111}近奇异晶界的影响[J]. 金属学报, 2025, 61(11): 1673-1688.
Zhenxiang LI, Weiguo WANG, Gregory S Rohrer, Lihua HONG, Song CHEN, Yan LIN, Bangxin ZHOU. Effects of Ambient and Cryogenic Rolling on {111}/{111} Near Singular Boundary Formation During Subsequent Recrystallization Annealing in Pure Aluminum[J]. Acta Metall Sin, 2025, 61(11): 1673-1688.

全文: PDF(5141 KB) HTML

摘要:

{111}/{111}近奇异晶界比一般晶界更耐蚀，研究此类晶界的形成条件、影响因素和生成机制，设法调控此类晶界并提高其比例是改善相关铝合金晶界间耐腐蚀性能的根本途径。为了解铝合金生成{111}/{111}近奇异晶界的本征行为，本工作选择高纯Al (99.99%)为实验材料，首先经室温反复多向锻造和370 ℃再结晶退火获得晶粒尺寸均匀(平均晶粒尺寸约为20 μm)且晶粒取向随机分布的组织均匀化初始样品；再将初始样品分别在室温(25 ℃)和-196 ℃深冷条件下进行厚度减缩量为80%的轧制变形，及370 ℃、30 min再结晶退火处理。采用EBSD和基于五参数分析的晶界界面匹配定量表征方法对2种样品进行测试和分析。结果表明，经-196 ℃深冷轧制并再结晶的样品，其{111}/{111}近奇异晶界比例达到6.0%，相比室温轧制并再结晶的样品提升了122%。XRD、EBSD及硬度测试结果表明，经室温和-196 ℃深冷轧制的样品中均形成了较强的{011}< $11 1 ¯$ >形变织构；相比于室温轧制，经-196 ℃深冷轧制的样品内残余压应力更大，晶粒碎化更严重、储能更高。在后续370 ℃退火过程中，经室温和-196 ℃深冷轧制的样品，其再结晶机制均以{011}< $01 1 ¯$ >取向生长为主；相比于室温轧制，经-196 ℃深冷轧制的样品可提供更大的晶界迁移驱动力，其样品再结晶组织的平均晶粒尺寸更大且{011}< $01 1 ¯$ >再结晶织构更强。统计结果表明，{011}< $01 1 ¯$ >取向晶粒与其他取向的晶粒毗连所形成的晶界中存在较高比例的{111}/{111}近奇异晶界；同时，{011}< $01 1 ¯$ >取向晶粒与其相邻的且具有{011}< $01 1 ¯$ >漫散取向的晶粒间也形成较多的{111}/{111}近奇异晶界，这是导致经-196 ℃深冷轧制及再结晶的样品中{111}/{111}近奇异晶界比例较高的主要原因。

关键词 ：高纯Al, 深冷轧制, 近奇异晶界, 晶界界面匹配

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

收稿日期: 2024-01-30

ZTFLH:

TG146.2

基金资助:国家自然科学基金项目(51971063);福建省自然科学基金项目(2021J011076)

通讯作者: 王卫国，wang_weiguo@vip.163.com，主要从事金属和无机非金属材料晶界工程研究

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

作者简介: 李振想，男，1998年生，硕士生

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https://www.ams.org.cn/CN/10.11900/0412.1961.2024.00035 或 https://www.ams.org.cn/CN/Y2025/V61/I11/1673

表1 高纯Al样品编号及其加工状态

图1 F和F1样品的显微组织取向成像显微(OIM)图、晶界网络和取向差分布图

表2 F和F1样品中取向差转轴为<111>、<112>和<122>的晶界数量及比例统计

图2 F和F1样品的固定转轴晶界取向差分布图

图3 F样品中存在{111}/{111}-近奇异晶界(NSB)的各组晶界的晶界面分布(GBPD)图(投影在(001)内)

图4 F1样品中存在{111}/{111}-NSB的各组晶界的GBPD图(投影在(001)内)

表3 F和F1样品的{111}/{111}-NSB相关数据统计

图5 A和A1样品的轧面(A-ND和A1-ND)、横切面(A-RD和A1-RD)及纯Al粉末样品(Powder)的XRD谱

图6 轧制样品及轧制后370 ℃退火样品的{022}XRD谱

图7 轧制样品及轧制后370 ℃退火样品沿轧板厚度方向的压应力

图8 轧制样品及轧制后370 ℃退火样品的Vickers硬度

图9 经室温和深冷轧制后再经370 ℃退火不同时间各样品的平均晶粒尺寸

图10 经室温和深冷轧制后再经370 ℃退火不同时间各样品的ODF截面图

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

表4 随机选取3种不同取向的各10个晶粒所关联晶界的特征统计

图11 {011}<011¯>取向晶粒与其他取向晶粒间形成{111}/{111}-NSB的显微组织OIM图和{111}重叠极图晶界迹线分析

图12 {011}<011¯>取向晶粒与其漫散取向晶粒间形成{111}/{111}-NSB的显微组织OIM图和{111}重叠极图晶界迹线分析

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°

表5 {011}<011¯>取向晶粒与其他取向晶粒间形成{111}/{111}-NSB的相关信息(对应图11)

图13 {011}<011¯>取向晶粒(P1和P2)与{011}<011¯>漫散取向晶粒M及其他取向晶粒N之间形成{111}/{111}-NSB的晶胞示意图

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°

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°

表6 {011}<011¯>取向晶粒与{011}<011¯>漫散取向晶粒形成{111}/{111}-NSB的相关信息(对应图12)

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