Article(id=1321935431877378134, tenantId=1146029695717560320, journalId=1220038251117760515, issueId=1321927083589227197, articleNumber=null, orderNo=null, doi=10.11868/j.issn.1001-4381.2025.000121, pmid=null, cstr=32421.14.j.issn.1001-4381.2025.000121, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1741017600000, receivedDateStr=2025-03-04, revisedDate=null, revisedDateStr=null, acceptedDate=1746720000000, acceptedDateStr=2025-05-09, onlineDate=1793103567332, onlineDateStr=2026-10-27, pubDate=1776614400000, pubDateStr=2026-04-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793103567332, onlineIssueDateStr=2026-10-27, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793103567332, creator=13701087609, updateTime=1793103567332, updator=13701087609, issue=Issue{id=1321927083589227197, tenantId=1146029695717560320, journalId=1220038251117760515, year='2026', volume='54', issue='4', pageStart='1', pageEnd='345', issueExtLink='null', onlineDate='null', pubDate='1776614400000', pubDateStr='2026-04-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1793101576945, creator='13701087609', updateTime=1793101576945, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext=null, issueFiles=null, downloadFileDto=null}, startPage=229, endPage=236, ext={EN=ArticleExt(id=1321935432082899031, articleId=1321935431877378134, tenantId=1146029695717560320, journalId=1220038251117760515, language=EN, title=Effect of solution treatment on grain boundary structure of Inconel 617 alloy bar, columnId=1220689384450478826, journalTitle=Journal of Materials Engineering, columnName=RESEARCH ARTICLE, runingTitle=null, highlight=null, articleAbstract=

The grain-boundary microstructure of Inconel 617 alloy hot-rolled rods during cold drawing and subsequent solution treatment is investigated using the electron backscattering diffraction (EBSD) technique. The results reveal that the microstructure of the hot-rolled rods contains a substantial number of coincidence site lattice (CSL) grain boundaries, predominantly Σ3 grain boundaries. Following cold drawing, the proportion of CSL grain boundaries decreases significantly, while the proportion of low-angle grain boundaries experiences a sharp increase. After solution treatment at 1120 ℃, low-angle grain boundaries are almost entirely replaced by high-angle and CSL grain boundaries. As the solution temperature rises, the proportion of Σ3 grain boundaries increases, whereas the proportions of Σ9 and Σ27 grain boundaries decline. Within a specific grain-size range, the proportion of Σ3 grain boundaries rises with an increase in grain size. During the solution treatment process, annealing twin boundaries with “cluster” and “island” morphologies emerge, and there exists a Σ3 n orientation relationship between adjacent grains.

, authors=Jun LU1, Chunlei YANG1, Haijun SHEN1, 2, Zixing WANG1, 2, authorsList=Jun LU, Chunlei YANG, Haijun SHEN, Zixing WANG, authorCompany=null, correspAuthors=Chunlei YANG, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1321935435211849832, articleId=1321935431877378134, tenantId=1146029695717560320, journalId=1220038251117760515, language=CN, title=固溶处理对Inconel 617合金棒材晶界组织的影响, columnId=1220689384622445292, journalTitle=材料工程, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

利用电子背散射衍射技术研究了Inconel 617合金热轧棒在冷拉和固溶处理过程中的晶界组织变化。结果表明:热轧棒组织中含有大量的CSL晶界,主要以Σ3晶界为主。经过冷拉变形后CSL晶界含量降低,小角度晶界含量急剧增加。1120 ℃固溶处理后,小角度晶界基本被大角度晶界和CSL晶界取代。随着固溶温度的升高,Σ3晶界含量增加,Σ9和Σ27晶界含量降低。在一定晶粒尺寸范围内,Σ3晶界含量随晶粒尺寸的增大而增加。固溶处理过程中出现了“团簇”状和“孤岛”状退火孪晶界,且相邻晶粒之间具有Σ3 n 的位向关系。

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杨春雷(1991—),男,工程师,硕士,研究方向为变形高温合金及特殊钢,联系地址:江苏省苏州市常熟金门路2号集萃金属研发厂房(215558),E-mail:
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UK:Cambridge University Press,1996., articleTitle=null, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1321935435450925161, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, xref=1., ext=[AuthorCompanyExt(id=1321935435459313770, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, companyId=1321935435450925161, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.Suzhou Jicui Gaohe Material Technology Co. ,Ltd. ,Suzhou 215558,Jiangsu,China), AuthorCompanyExt(id=1321935435467702379, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, companyId=1321935435450925161, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1.苏州集萃高合材料科技有限公司,江苏 苏州 215558)]), AuthorCompany(id=1321935435589337196, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, xref=2., ext=[AuthorCompanyExt(id=1321935435593531501, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, companyId=1321935435589337196, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.Institute of Novel Metals and Applied Technologies,Jiangsu Industrial Technology Research Institute,Suzhou 215506,Jiangsu,China), AuthorCompanyExt(id=1321935435601920110, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, companyId=1321935435589337196, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2.江苏省产业技术研究院 先进金属材料及应用技术研究所,江苏 苏州 215506)])], figs=[ArticleFig(id=1321935439989162127, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=EN, label=Fig. 1, caption=CSL diagram of hot-rolled(1) and cold-drawn(2) bars at different positions

(a)edge;(b)0.5R;(c)center

, figureFileSmall=hdV4q/CoaaEikkQndWAPLQ==, figureFileBig=XFfp0j/vAIm+l+EanthDpw==, tableContent=null), ArticleFig(id=1321935440052076688, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=CN, label=图1, caption=热轧态(1)和冷拉态(2)棒材不同位置的CSL图

(a)边缘;(b)0.5R;(c)中心

, figureFileSmall=hdV4q/CoaaEikkQndWAPLQ==, figureFileBig=XFfp0j/vAIm+l+EanthDpw==, tableContent=null), ArticleFig(id=1321935440295346321, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=EN, label=Fig.2, caption=Grain boundary content(1) and misorientation angle grain boundary content(2) at different locations

(a)hot-rolled bars;(b)cold-drawn bars

, figureFileSmall=sCfhRn7RqTWeFTp8XKTLOw==, figureFileBig=YpPzcFPABouUEdls/jxsJA==, tableContent=null), ArticleFig(id=1321935440396009618, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=CN, label=图2, caption=不同位置CSL晶界含量(1)及大小角度晶界含量(2)

(a)热轧棒;(b)冷拉棒

, figureFileSmall=sCfhRn7RqTWeFTp8XKTLOw==, figureFileBig=YpPzcFPABouUEdls/jxsJA==, tableContent=null), ArticleFig(id=1321935440463118483, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=EN, label=Fig.3, caption=CSL diagram of cold-drawn bar at different positions after different solution treatment processes

(a)1120 ℃;(b)1150 ℃;(c)1160 ℃;(1)edge;(2)0.5R;(3)center

, figureFileSmall=TmZiNMuRZh8/QbJFT1VP3g==, figureFileBig=CnlLqdKwR+FvfhprzyD1VA==, tableContent=null), ArticleFig(id=1321935440538615956, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=CN, label=图3, caption=冷拉态棒材经不同温度固溶处理后不同位置的CSL图

(a)1120 ℃;(b)1150 ℃;(c)1160 ℃;(1)边缘;(2)0.5R;(3)中心

, figureFileSmall=TmZiNMuRZh8/QbJFT1VP3g==, figureFileBig=CnlLqdKwR+FvfhprzyD1VA==, tableContent=null), ArticleFig(id=1321935440601530517, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=EN, label=Fig. 4, caption=Content of CSL grain boundaries of cold-drawn bar at different positions after different solution treatment processes, figureFileSmall=9ekvc3KETrZbpBiLYL7l3Q==, figureFileBig=SQonZGqooeuiemteJyzysg==, tableContent=null), ArticleFig(id=1321935440685416598, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=CN, label=图4, caption=冷拉态棒材经不同温度固溶处理后不同位置的CSL晶界含量

(a)1120 ℃;(b)1150 ℃;(c)1160 ℃

(a)1120 ℃;(b)1150 ℃;(c)1160 ℃

, figureFileSmall=9ekvc3KETrZbpBiLYL7l3Q==, figureFileBig=SQonZGqooeuiemteJyzysg==, tableContent=null), ArticleFig(id=1321935440752525463, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=EN, label=Fig.5, caption=Schematic diagram of grain growth and twinning changes

(a)before growth;(b)after growth (the red line and the black line respectively represent the twinning boundary and the common grain boundary,and the green arrow indicates the direction of grain boundary migration)

, figureFileSmall=aZv8+9dt0aFq9CbA7QFNzw==, figureFileBig=cQz4bZPHyf+/6zteyj6gVA==, tableContent=null), ArticleFig(id=1321935440828022936, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=CN, label=图5, caption=晶粒长大和孪晶变化示意图

(a)长大前;(b)长大后(红线和黑线分别代表孪晶界和普通晶界,绿色箭头代表晶界迁移方向)

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(a)IPF图及选区;(b)晶粒1和2在极图中的取向分布图;(c) 晶粒1和2在反极图中的取向分布图

, figureFileSmall=3CKWxMWc6zVQXhdPSOtx3Q==, figureFileBig=hI5thSZGTShZZCu7lrdeXQ==, tableContent=null), ArticleFig(id=1321935441444585632, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1321935431877378134, language=EN, label=Table 1, caption=

Main chemical composition of the Inconel 617 alloy (mass fraction/%)

, figureFileSmall=null, figureFileBig=null, tableContent=
CCrMoCoAlTiSiFeMnNi
0.1022.048.9412.531.080.420.0560.220.014Bal.
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Inconel 617合金的主要化学成分(质量分数/%)

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CCrMoCoAlTiSiFeMnNi
0.1022.048.9412.531.080.420.0560.220.014Bal.
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Orientation relationship of adjacent grains in grain clusters

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Grain numberAxis-angle pairCSL typeAngle deviationGrain numberAxis-angle pairCSL typeAngle deviation
1/259.82°/[1¯11¯]Σ30.41°3/759.80°/[1¯1¯1]Σ30.28°
1/459.88°/[11¯1]Σ30.39°3/838.59°/[110]Σ90.88°
1/659.97°/[1¯1¯1]Σ30.42°4/638.97°/[101]Σ90.24°
2/359.95°/[111]Σ30.30°6/959.96°/[11¯1]Σ30.21°
3/435.11°/[210]Σ27b0.68°7/832.13°/[1¯1¯0]Σ27a0.85°
3/539.02°/[11¯0]Σ90.11°9/1059.37°/[11¯1]Σ30.56°
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晶粒团簇内相邻晶粒的位向关系

, figureFileSmall=null, figureFileBig=null, tableContent=
Grain numberAxis-angle pairCSL typeAngle deviationGrain numberAxis-angle pairCSL typeAngle deviation
1/259.82°/[1¯11¯]Σ30.41°3/759.80°/[1¯1¯1]Σ30.28°
1/459.88°/[11¯1]Σ30.39°3/838.59°/[110]Σ90.88°
1/659.97°/[1¯1¯1]Σ30.42°4/638.97°/[101]Σ90.24°
2/359.95°/[111]Σ30.30°6/959.96°/[11¯1]Σ30.21°
3/435.11°/[210]Σ27b0.68°7/832.13°/[1¯1¯0]Σ27a0.85°
3/539.02°/[11¯0]Σ90.11°9/1059.37°/[11¯1]Σ30.56°
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固溶处理对Inconel 617合金棒材晶界组织的影响
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卢俊 1 , 杨春雷 1 , 沈海军 1, 2 , 王资兴 1, 2
材料工程 | 研究论文 2026,54(4): 229-236
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材料工程 |研究论文 2026 , 54 (4) : 229 -236
固溶处理对Inconel 617合金棒材晶界组织的影响
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卢俊1, 杨春雷1 , 沈海军1, 2, 王资兴1, 2
作者信息
  • 1.苏州集萃高合材料科技有限公司,江苏 苏州 215558
  • 2.江苏省产业技术研究院 先进金属材料及应用技术研究所,江苏 苏州 215506
通讯作者:
杨春雷(1991—),男,工程师,硕士,研究方向为变形高温合金及特殊钢,联系地址:江苏省苏州市常熟金门路2号集萃金属研发厂房(215558),E-mail:
Effect of solution treatment on grain boundary structure of Inconel 617 alloy bar
Jun LU1, Chunlei YANG1 , Haijun SHEN1, 2, Zixing WANG1, 2
Affiliations
  • 1.Suzhou Jicui Gaohe Material Technology Co. ,Ltd. ,Suzhou 215558,Jiangsu,China
  • 2.Institute of Novel Metals and Applied Technologies,Jiangsu Industrial Technology Research Institute,Suzhou 215506,Jiangsu,China
出版时间: 2026-04-20 doi: 10.11868/j.issn.1001-4381.2025.000121
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利用电子背散射衍射技术研究了Inconel 617合金热轧棒在冷拉和固溶处理过程中的晶界组织变化。结果表明:热轧棒组织中含有大量的CSL晶界,主要以Σ3晶界为主。经过冷拉变形后CSL晶界含量降低,小角度晶界含量急剧增加。1120 ℃固溶处理后,小角度晶界基本被大角度晶界和CSL晶界取代。随着固溶温度的升高,Σ3晶界含量增加,Σ9和Σ27晶界含量降低。在一定晶粒尺寸范围内,Σ3晶界含量随晶粒尺寸的增大而增加。固溶处理过程中出现了“团簇”状和“孤岛”状退火孪晶界,且相邻晶粒之间具有Σ3 n 的位向关系。

Inconel 617合金  /  冷拉  /  固溶处理  /  CSL晶界  /  退火孪晶界

The grain-boundary microstructure of Inconel 617 alloy hot-rolled rods during cold drawing and subsequent solution treatment is investigated using the electron backscattering diffraction (EBSD) technique. The results reveal that the microstructure of the hot-rolled rods contains a substantial number of coincidence site lattice (CSL) grain boundaries, predominantly Σ3 grain boundaries. Following cold drawing, the proportion of CSL grain boundaries decreases significantly, while the proportion of low-angle grain boundaries experiences a sharp increase. After solution treatment at 1120 ℃, low-angle grain boundaries are almost entirely replaced by high-angle and CSL grain boundaries. As the solution temperature rises, the proportion of Σ3 grain boundaries increases, whereas the proportions of Σ9 and Σ27 grain boundaries decline. Within a specific grain-size range, the proportion of Σ3 grain boundaries rises with an increase in grain size. During the solution treatment process, annealing twin boundaries with “cluster” and “island” morphologies emerge, and there exists a Σ3 n orientation relationship between adjacent grains.

Inconel 617 alloy  /  cold drawing  /  solution treatment  /  CSL grain boundary  /  annealing twin boundary
卢俊, 杨春雷, 沈海军, 王资兴. 固溶处理对Inconel 617合金棒材晶界组织的影响. 材料工程, 2026 , 54 (4) : 229 -236 . DOI: 10.11868/j.issn.1001-4381.2025.000121
Jun LU, Chunlei YANG, Haijun SHEN, Zixing WANG. Effect of solution treatment on grain boundary structure of Inconel 617 alloy bar[J]. Journal of Materials Engineering, 2026 , 54 (4) : 229 -236 . DOI: 10.11868/j.issn.1001-4381.2025.000121
Inconel 617合金作为第四代核能系统关键热端构件的优选材料,是一种采用固溶强化及碳化物强化机理设计的镍基高温合金。该合金组织中的碳化物主要是M6C和M23C6,M23C6在1190 ℃时全部回溶到基体,M6C型碳化物在固溶温度高于1190 ℃时,才开始逐渐回溶到基体。该合金在700~750 ℃条件下具有卓越的高温力学稳定性、优异的抗氧化特性以及持久耐热腐蚀能力。目前不仅在航空航天推进系统、石油化工高温反应装置等工业场景实现规模化应用,而且被国际核能界列为第四代核反应堆蒸汽发生器、中间换热器等核心部件的重点候选材料[1-3]。
晶界作为晶体结构相同,但晶格取向各异的晶粒间界面,其微观特征对材料的物理化学性能具有显著调控作用。通过系统调控晶界的微观结构、化学特性与空间分布特征,可定向优化材料的宏观力学性能(如强度、韧度及抗疲劳特性),从而为高性能材料设计提供关键调控路径。Watanabe[4]在1984年基于形变热处理工艺提出的“晶界设计”理念以实现合金耐蚀性优化,后面逐步发展为现代晶界工程(grain boundary engineering, GBE)。其核心机制在于利用退火孪晶界(Σ3)的界面反应动力学,通过Σ3 n 与Σ3 n+1的迭代重组(反应式:Σ3+Σ3 n →Σ3 n+1,Σ3 n +Σ3 n+1→Σ3),定向构筑高比例低Σ值晶界(Σ<29),为开发耐蚀合金提供材料基因组层面的解决方案[5-6]。GBE技术能够打断普通晶界的连续性,优化晶界分布,从而改善材料与晶界有关的多种性能,如抗腐蚀、抗晶界退化以及力学性能等。Pande等[7]揭示了退火孪晶界在室温条件下诱导的晶粒细化效应,通过孪晶界面分割母晶粒形成亚结构,有效晶粒尺寸的减小显著提升了合金的室温屈服强度,为晶界工程调控金属材料强度提供了关键实验支撑。研究者们发现,纳米金属铜中的退火孪晶界作为强化相界,通过晶界钉扎效应可以提高铜的室温强度,而孪晶界面的共格特性维持了位错滑移通道,使其伸长率也保持在较高的水平[8-10]。Boehlert 等[11] 在In 718合金中基于形变热处理调控工艺获得不同含量的退火孪晶界,研究表明,In 718合金中退火孪晶界密度与力学性能呈正相关,能同时提高该合金的室温性能和高温性能。
Inconel 617合金冷拉棒是加工核反应堆用螺栓等紧固件的重要材料,与常用的热轧棒材和锻制棒材相比,冷拉棒的表面粗糙小,尺寸精度高等。目前大量的研究集中在Inconel 617 镍基高温合金热变形过程中的力学行为和再结晶机制等方面[12-13],对于冷变形及后续热处理过程中晶界演变的研究较少。刘昱君等[14]研究发现Inconel 617合金管随着固溶温度的升高,晶粒的平均尺寸增大,并且晶粒内部出现较多的孪晶。Bhuyan等[15]研究发现低ΣCSL晶界在抗晶间腐蚀、抑制沿晶裂纹萌生与扩展等方面均表现出优于随机晶界的特性。夏爽等[16]通过研究Inconel 690合金晶界特征分布及其对晶界腐蚀的影响,发现低ΣCSL晶界比例高的样品比低ΣCSL晶界比例低的样品明显耐晶间腐蚀。材料的组织决定性能,而组织的演变又与晶界密切相关,因此研究Inconel 617合金在固溶及冷变形过程中的晶界组织演变具有重要的理论意义。
实验用Inconel 617合金棒材的主要化学成分见表1。首先,将Φ14 mm热轧棒材通过双链式拉拔机冷拉至Φ12.5 mm,冷拉变形量约为20%,然后将冷拉后的棒材进行固溶处理,固溶工艺分别为1120 ℃/20 min、1150 ℃/20 min和1160 ℃/20 min,空冷。将冷拉前、冷拉后以及固溶处理后的棒材沿径向剖开,随后对样品纵截面进行机械研磨抛光,最后高氯酸酒精溶液进行电解抛光,高氯酸和酒精的体积比为1∶9,抛光电压20 V,抛光时间10~15 s。抛光完成后用装配有电子背散射衍射(electron backscatter diffraction,EBSD)系统的Gemini500型场发射扫描电镜(SEM),分析该合金在冷拉和固溶过程中的晶界组织演变规律。在EBSD测试中,样品需以70°倾角放置在专用样品台上,加速电压设置为20 kV,工作距离约为15 mm。扫描步长根据晶粒尺寸动态调整,通常设置为平均晶粒尺寸的1/10~1/5。
图1为热轧态和冷拉态棒材不同位置的低Σ重位点阵(coincidence site lattice,低 ΣCSL,<Σ29)晶界分布图,图中红色线条代表Σ3晶界、绿色线条代表Σ9晶界、蓝色线条代表Σ27晶界、 图中灰色线条代表小角度晶界(通常指2°~15°)。由图1可知热轧态棒材不同位置的组织都是均匀细小的等轴晶,经统计得到边部、0.5R和中心的平均晶粒尺寸分别为8.6、9.7 μm和10.4 μm,对于该晶粒尺寸的差异因为在热轧过程中轧棒表面与轧辊接触,温降从表面至中心逐渐减小,所以平均晶粒尺寸从表面至中心逐渐增大。由图1(a-1)~(c-1)可知,热轧态棒材中含有大量的Σ3晶界,Σ9晶界含量相对较少,而Σ27晶界的含量非常低。
图2为热轧态和冷拉态棒材不同位置,CSL晶界的含量及大小角度晶界含量。经过图2(a-1)统计得到热轧态Σ3晶界含量从边部到中心逐渐增加,分别为34.83%、36.67%和39.83%,而Σ9晶界含量与之相反,分别为1.89%、1.71%和1.54%,Σ27晶界的含量基本保持在0.34%左右。在热轧变形过程中的低Σ重位点阵具有Σ3晶界的特征,说明Σ3、Σ9和Σ27晶界之间相互作用的发生具有偶然性,与其他牌号的镍基合金相似[17]。
经过冷拉变形后,CSL晶界的含量急剧减少,由图2(b-1)可知,冷拉态Σ3晶界含量从边缘部到中心逐渐增加,分别为5.04%、5.54%和5.99%,而不同位置的Σ9晶界含量基本一致,保持在0.18%左右,Σ27晶界的含量保持在0.06%左右,与轧态相比均大量减少。由图2(a-2),(b-2)可知,热轧态棒材不同位置主要以大角度晶界为主,达到了95%以上,经过冷拉变形后小角度晶界急剧增加,大角度晶界减少。
小角度晶界基本上都是由位错构成,如刃型位错和螺型位错。在冷拉变形过程中,位向最有利的晶粒最先开始发生塑性变形,此时该晶粒滑移面上的位错源开动,不断沿着滑移面进行运动,但由于周围的晶粒位向不同,滑移系也不同,因此运动的位错并不能越过晶界发展到另一个晶粒中,位错在运动过程中遭遇晶界阻碍,从而在晶界前沿聚集,形成平面塞积群,所以经过冷拉变形后组织中会形成大量的小角度晶界。从图中还可以看出,边部的变形最大,因此,小角度晶界最多,从边部到中心变形量逐渐减小,小角度晶界也逐渐减少。
图3为冷拉态棒材经不同温度固溶处理后不同位置的CSL晶界分布图(红色线条代表Σ3晶界、绿色线条代表Σ9晶界、蓝色线条代表Σ27晶界),固溶温度分别为1120、1150 ℃和1160 ℃,保温时间均为20 min。由图3(a-1)~(a-3)可知,经过1120 ℃固溶处理后冷拉组织中的小角度晶界基本被大角度晶界和CSL晶界取代,说明在该温度固溶处理时完成了再结晶,再结晶后的晶粒大小与热轧态基本一致。随着固溶温度升高,晶粒逐渐发生粗化现象,当固溶温度为1150 ℃时,组织中出现了晶粒的异常长大,即二次再结晶。固溶温度升高到1160 ℃,边部的晶粒均匀长大,0.5R和中心出现了双重晶粒,且中心的晶粒级差最大。
再结晶可理解为冷变形金属在热作用下经历的一种组织重构过程,其核心机制是小角度晶界逐渐演化为大角度晶界,并通过晶界迁移消除变形过程中形成的缺陷结构。檀校等[18]研究表明,再结晶过程是通过新的大角度晶界的形成和迁移进行的,储存能的降低提供了再结晶的驱动力。
图4为冷拉态棒材经不同温度固溶处理后不同位置的CSL晶界含量。与冷拉态相比,经过1120 ℃处理后,组织中的CSL晶界含量大量增加,且从边部到中心逐渐增加。随着固溶温度的升高,Σ3晶界含量增加,而Σ9和Σ27晶界含量降低,说明在固溶过程中发生了Σ3 n +Σ3 n+1=Σ3的界面反应。由图4(b)发现,当固溶温度为1150 ℃时,Σ3晶界含量从边部到中心出现了先减少再增加的现象,结合图3(b-1)~(b-3)可知,Σ3晶界含量与晶粒大小密切相关,经过统计得到边缘、0.5R和中心的平均晶粒尺寸分别为12.3、12.4 μm和14.3 μm。由于中心的平均晶粒尺寸最大,因此Σ3晶界含量最高,边部和0.5R的平均晶粒尺寸虽然相差不大,但由于边部出现了较多的异常长大的晶粒,所以Σ3晶界含量比0.5R位置的高。固溶温度为1160 ℃时,Σ3晶界含量继续增加,而Σ9和Σ27晶界含量则继续降低,说明Σ3 n +Σ3 n+1=Σ3的界面反应在继续进行。由图4(c)发现,1160 ℃固溶时,Σ3晶界含量从边部到中心逐渐降低,结合图3(c-1)~(c-3)进一步证明了Σ3晶界含量与晶粒大小有关。
根据Frank标准极图分析,退火孪晶与母体晶粒间呈现典型的〈111〉/60°取向差,这种关系符合Σ3重位点阵的晶体学特征,这种特殊取向关系源于面心立方结构中{111}密排面的镜面对称操作。Grube等[19]研究指出,退火孪晶界的形核机制与晶粒粗化过程密切相关,其典型特征表现为在三叉晶界交汇区域,通过能量驱动的晶界迁移作用形成孪晶界面结构。Randle 等[20]针对金属镍的晶体学研究表明,其退火孪晶界表现出独特的迁移动力学特性。作为典型的Σ3晶界结构,这类孪晶界的迁移具有自主性,其动力学过程独立于常规晶界迁移机制。晶粒长大的本质是通过减小体系内界面总面积以降低系统自由能、提升热力学稳定性的自组织过程,其热力学驱动力来源于总界面能的降低。图5为固溶过程中晶粒长大的示意图。在固溶过程中,由于孪晶界的界面能显著低于常规高角度晶界,在热力学驱动力主导下,高角度晶界A、B倾向于沿曲率驱动力方向(即向曲率中心迁移,对应绿色箭头方向)发生择优迁移。而低能孪晶界因迁移势垒较高,表现出相对稳定性,最终导致高能晶界主导的晶粒粗化。在晶界A、B的曲率驱动迁移过程中,其邻近的孪晶界T1和T2因几何约束效应逐渐收缩,而位于晶粒合并前缘的孪晶界T3和T4则通过界面重组机制延伸扩展,此消彼长的动态演化最终有可能导致孪晶界T1和T2的湮灭。在晶界A、B的迁移过程中,受剪切应力场作用,晶界前沿发生局部原子堆垛次序的剪切失配,形成面缺陷型层错。随着晶界持续迁移,层错区域通过位错分解机制沿{111}滑移系扩展,最终形成具有镜面对称性的共格孪晶界T5和T6。
退火孪晶作为面心立方金属中具有Σ3重位点阵特征的典型界面结构,其形成密度与材料层错能呈负相关。在低层错能体系中,基于不全位错滑移的孪生机制与再结晶过程中晶界迁移的协同作用,促使退火孪晶得以大量形成并稳定存在,其本质上属于亚结构的一种,会影响材料的组织和性能。由于镍基高温合金的层错能较低,再结晶过程中会产生大量层错,导致合金的固溶组织中形成退火孪晶[21]。有研究[22]发现GH4080A合金经过不同温度固溶处理后也会产生大量的退火孪晶。
退火孪晶界的形成机制之一是再结晶过程中发生的“生长事故”[23]。在这个过程中,由于某些意外的原因, 造成在迁移的晶界某些位置上堆垛次序错误累积, 使该晶界被分解成孪晶界。按照该理论可知,面心立方金属中的退火孪晶通常呈现Σ3{111}共格界面主导的平直或平行对生特征,然而该合金在1150 ℃固溶过程中形成了具有多重拓扑形貌特征的“团簇”状孪晶网络。图6是图3(b-1)的局部放大图,由图可知,经过固溶处理后,大部分的退火孪晶界是直线或直线对状,如图6中黑色箭头所示,但还有一小部分“团簇”状和“孤岛”状孪晶界,如图6中黑色圆圈所示。
对于该“团簇”状和“孤岛”状退火孪晶界的形成,有学者认为[5]低层错能面心立方结构的金属再结晶完成后,在共享Σ3取向关系的相邻晶粒体系中,当两个晶粒均含有高迁移率的Σ3共格孪晶界时,其晶粒粗化过程中的交互作用将触发晶界反应机制。依据重位点阵理论,两个Σ3晶界的拓扑重构形成具有Σ3-Σ3-Σ9特征的三叉晶界构型,该过程受界面能各向异性与几何必要位错密度梯度的双重调控。基于晶界反应动力学理论,高迁移率的Σ9晶界在扩展过程中与相邻Σ3共格孪晶界相遇时,会触发符合Brandon准则的界面拓扑重构机制,形成另一个Σ3-Σ3-Σ9三岔界面。该三岔界面中有一个Σ3界面为非共格界面,在迁移过程中与 Σ9界面相遇时生成新的 Σ3界面,即Σ3+Σ3 n =Σ3 n+1,Σ3 n +Σ3 n+1=Σ3晶界反应。
图7为1150 ℃固溶处理后,边部位置的晶粒取向分布图、晶界特征分布图以及图7(b)中黑色方框区域内不同类型晶界图。由图可知,晶粒团簇内有许多Σ3 n 晶界,构成Σ3-Σ3-Σ9或Σ3-Σ9-Σ27晶界。表2为经过统计图7(c)得到的相邻晶粒之间的位向关系。由表2可知,在同一个晶粒团簇内,相邻晶粒之间均具有Σ3 n 的位向关系,并且主要以Σ3晶界为主。Inconel 617合金是中低层错能面心立方镍基高温合金,在固溶处理时会产生大角度晶界的新晶粒,在这个过程中易形成退火孪晶界(Σ3晶界),并且不同类型的晶界在迁移过程中也会发生交互作用,形成新的Σ3晶界。
图8为经过1150 ℃固溶处理后边部的IPF图以及红色方框内选区的极图和反极图,在低层错能镍基高温合金体系中,退火孪晶界严格遵循Σ3重位点阵(CSL)的晶体学规律,其几何构型可通过Brandon判据精确定义为〈111〉/60°轴角对体系。此外,共格孪晶界与理论的Σ3晶界(〈111〉/60°)取向差角的畸变通常小于1.7°[24],而非共格Σ3晶界会有更大的取向差角的畸变。图中选区内的两个晶粒的取向分别为1[12¯1]∥DD和2[6¯52¯]∥DD,DD代表冷拉拔方向,两个晶粒以[1¯1¯1]晶向为轴,通过旋转59.96°后两者可以重合,与轴角对〈111〉/60°的取向差角的畸变为0.04°,满足Brandon标准[25],说明该孪晶界是共格孪晶界。共格孪晶界作为一种无结构畸变的孪晶界类型,其界面能显著低于常规晶界,仅为普通晶界能的1/10。这种低能态特性使其具备优异的稳定性,因而成为材料中普遍存在的孪晶界形式。
(1)热轧态棒材中含有大量的CSL晶界,其中Σ3晶界含量最多,且从边部到中心含量逐渐增加,Σ9含量次之,Σ27含量最低。经过冷拉变形后,CSL晶界含量急剧减少,而小角度晶界大量增加。
(2)冷拉棒经过1120 ℃固溶处理后,小角度晶界含量减少,大角度和CSL晶界含量增加。随着固溶温度的升高 ,Σ3晶界含量增加,而Σ9和Σ27晶界含量降低,说明发生了Σ3 n +Σ3 n+1=Σ3的界面反应。Σ3晶界含量与晶粒大小有关,在一定范围内,Σ3晶界含量随晶粒尺寸的增大而增加。
(3)固溶处理过程中出现了“团簇”状和“孤岛”状退火孪晶界,在同一个晶粒团簇内,相邻晶粒之间均具有Σ3 n 的位向关系,主要以Σ3晶界为主。

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doi: 10.11868/j.issn.1001-4381.2025.000121
  • 接收时间:2025-03-04
  • 首发时间:2026-10-27
  • 出版时间:2026-04-20
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  • 收稿日期:2025-03-04
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    1.苏州集萃高合材料科技有限公司,江苏 苏州 215558
    2.江苏省产业技术研究院 先进金属材料及应用技术研究所,江苏 苏州 215506

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杨春雷(1991—),男,工程师,硕士,研究方向为变形高温合金及特殊钢,联系地址:江苏省苏州市常熟金门路2号集萃金属研发厂房(215558),E-mail:
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2种不同金属材料的力学参数
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
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