Article(id=1228347016510636975, tenantId=1146029695717560320, journalId=1146031591421210625, issueId=1228347007518048984, articleNumber=null, orderNo=null, doi=10.3981/j.issn.1000-7857.2025.11.00024, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1762704000000, receivedDateStr=2025-11-10, revisedDate=1767110400000, revisedDateStr=2025-12-31, acceptedDate=null, acceptedDateStr=null, onlineDate=1770790350319, onlineDateStr=2026-02-11, pubDate=1769529600000, pubDateStr=2026-01-28, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1770393600000, onlineIssueDateStr=2026-02-07, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1770790350319, creator=13701087609, updateTime=1774080633120, updator=sys-migrate, issue=Issue{id=1228347007518048984, tenantId=1146029695717560320, journalId=1146031591421210625, year='2026', volume='44', issue='2', pageStart='1', pageEnd='120', issueExtLink='null', onlineDate='null', pubDate='1769529600000', pubDateStr='2026-01-28', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1770790348176, creator='13701087609', updateTime=1774331262404, updator='13041195026', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1243198678287102659, tenantId=1146029695717560320, journalId=1146031591421210625, issueId=1228347007518048984, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1243198678287102660, tenantId=1146029695717560320, journalId=1146031591421210625, issueId=1228347007518048984, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=98, endPage=107, ext={EN=ArticleExt(id=1228347016938456004, articleId=1228347016510636975, tenantId=1146029695717560320, journalId=1146031591421210625, language=EN, title=Stabilization process of (B4C+Al2O3)/Al neutron absorbing materials, columnId=1150494644690366681, journalTitle=Science & Technology Review, columnName=Papers, runingTitle=null, highlight=null, articleAbstract=

The (B4C+Al2O3)/Al composite is a critical neutron absorbing material for dry storage systems of spent fuel, and its long−term high temperature service reliability is directly associated with the safety of nuclear waste management. As a structural−functional integrated material, it is susceptible to phase transformation of amorphous Al2O3 (am−Al2O3) into γ−Al2O3 at elevated temperatures, which may adversely affect its mechanical properties. However, the microstructural evolution and long−term properties stability of this composite under prolonged thermal exposure remain insufficiently understood. In this work, (B4C+Al2O3)/Al composites were subjected to stabilization treatments at 400°C for 100 h and 550°C for 8 h, followed by long−term annealing at 400°C for up to 4000 h to evaluate their thermal stability. The results demonstrate that, after stabilization, the composites retained tensile strengths exceeding 220.0 MPa at room temperature and 100.0 MPa at 350°C, satisfying the requirements for engineering applications. Microstructural characterization revealed a partial transformation of am−Al2O3 to γ−Al2O3; however, both the microstructure and mechanical properties exhibited stable behavior during prolonged annealing. These findings indicate that both stabilization treatments effectively enhance the thermal stability of the (B4C+Al2O3)/Al composite, thereby providing a materials science basis for the long−term safe service of dry storage containers for spent fuel.

, authors=null, authorsList=Baoming SHI, Yuning ZAN, Quanzhao WANG, Bolü XIAO, Zongyi MA, authorCompany=null, correspAuthors=Yuning ZAN, authorNote=null, correspAuthorsNote=null, copyrightStatement=All rights reserved. Unauthorized reproduction is prohibited., 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=1228347020579110980, articleId=1228347016510636975, tenantId=1146029695717560320, journalId=1146031591421210625, language=CN, title=(B4C+Al2O3)/Al中子吸收材料的稳定化工艺, columnId=1146540929516700224, journalTitle=科技导报, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

(B4C+Al2O3)/Al复合材料作为乏燃料干式贮存系统中的关键中子吸收材料,其在高温下长期服役的可靠性直接关系到核废料安全管理的有效性。该结构功能一体化材料在高温下存在非晶Al2O3(am−Al2O3)向γ−Al2O3相变的风险,可能导致力学性能降低,但目前对其组织演化规律及性能稳定性的认识仍不足。为此,对(B4C+Al2O3)/Al复合材料进行了400°C/100 h和550°C/8 h 2种稳定化工艺处理,并通过400°C下最长4000 h的退火实验验证其长期稳定性。结果表明,经稳定化处理后,复合材料在室温及350°C下的抗拉强度分别保持在220.0和100.0 MPa以上,满足工程应用需求。微观组织分析表明,am−Al2O3部分转化为γ−Al2O3,但材料在退火过程中组织与性能均趋于稳定。2种工艺均能有效提升材料的热稳定性,为(B4C+Al2O3)/Al复合材料制备的乏燃料干式贮存容器实现长期安全服役提供了材料学依据。

, authors=

石宝铭,博士研究生,研究方向为金属基复合材料,电子信箱:

, authorsList=石宝铭, 昝宇宁, 王全兆, 肖伯律, 马宗义, authorCompany=null, correspAuthors=昝宇宁, authorNote=null, correspAuthorsNote=
昝宇宁(通信作者),副研究员,研究方向为金属基复合材料,电子信箱:
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石宝铭,博士研究生,研究方向为金属基复合材料,电子信箱:

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石宝铭,博士研究生,研究方向为金属基复合材料,电子信箱:

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样品 硬度(HV0.2
原始板材 76.0±1.1
400℃/100 h 71.4±1.3
400℃/100 h+400℃/4000 h 71.4±1.2
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(B4C+Al2O3)/Al复合材料及其经过400℃/100 h稳定化处理和400℃/4000 h退火后样品的显微硬度

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样品 硬度(HV0.2
原始板材 76.0±1.1
400℃/100 h 71.4±1.3
400℃/100 h+400℃/4000 h 71.4±1.2
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样品硬度(HV0.2
550℃/8 h70.2±1.0
550℃/8 h+400℃/1000 h70.1±0.8
550℃/8 h+400℃/4000 h69.6±0.7
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550℃/8 h稳定化后的(B4C+Al2O3)/Al复合材料板材继续在400℃下高温退火不同时间的显微硬度变化

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样品硬度(HV0.2
550℃/8 h70.2±1.0
550℃/8 h+400℃/1000 h70.1±0.8
550℃/8 h+400℃/4000 h69.6±0.7
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(B4C+Al2O3)/Al中子吸收材料的稳定化工艺
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石宝铭 , 昝宇宁 * , 王全兆 , 肖伯律 , 马宗义
科技导报 | 研究论文 2026,44(2): 98-107
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科技导报 |研究论文 2026 , 44 (2) : 98 -107
(B4C+Al2O3)/Al中子吸收材料的稳定化工艺
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石宝铭,博士研究生,研究方向为金属基复合材料,电子信箱:

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石宝铭 , 昝宇宁* , 王全兆, 肖伯律, 马宗义
作者信息
  • 中国科学院金属研究所沈阳材料科学国家研究中心,沈阳 110016
通讯作者:
昝宇宁(通信作者),副研究员,研究方向为金属基复合材料,电子信箱:
Stabilization process of (B4C+Al2O3)/Al neutron absorbing materials
Baoming SHI , Yuning ZAN* , Quanzhao WANG, Bolü XIAO, Zongyi MA
Affiliations
  • Shenyang National Laboratory for Materials Science,Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
出版时间: 2026-01-28 doi: 10.3981/j.issn.1000-7857.2025.11.00024
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(B4C+Al2O3)/Al复合材料作为乏燃料干式贮存系统中的关键中子吸收材料,其在高温下长期服役的可靠性直接关系到核废料安全管理的有效性。该结构功能一体化材料在高温下存在非晶Al2O3(am−Al2O3)向γ−Al2O3相变的风险,可能导致力学性能降低,但目前对其组织演化规律及性能稳定性的认识仍不足。为此,对(B4C+Al2O3)/Al复合材料进行了400°C/100 h和550°C/8 h 2种稳定化工艺处理,并通过400°C下最长4000 h的退火实验验证其长期稳定性。结果表明,经稳定化处理后,复合材料在室温及350°C下的抗拉强度分别保持在220.0和100.0 MPa以上,满足工程应用需求。微观组织分析表明,am−Al2O3部分转化为γ−Al2O3,但材料在退火过程中组织与性能均趋于稳定。2种工艺均能有效提升材料的热稳定性,为(B4C+Al2O3)/Al复合材料制备的乏燃料干式贮存容器实现长期安全服役提供了材料学依据。

中子吸收材料  /  (B4C+Al2O3)/Al复合材料  /  稳定化工艺  /  力学性能  /  微观组织

The (B4C+Al2O3)/Al composite is a critical neutron absorbing material for dry storage systems of spent fuel, and its long−term high temperature service reliability is directly associated with the safety of nuclear waste management. As a structural−functional integrated material, it is susceptible to phase transformation of amorphous Al2O3 (am−Al2O3) into γ−Al2O3 at elevated temperatures, which may adversely affect its mechanical properties. However, the microstructural evolution and long−term properties stability of this composite under prolonged thermal exposure remain insufficiently understood. In this work, (B4C+Al2O3)/Al composites were subjected to stabilization treatments at 400°C for 100 h and 550°C for 8 h, followed by long−term annealing at 400°C for up to 4000 h to evaluate their thermal stability. The results demonstrate that, after stabilization, the composites retained tensile strengths exceeding 220.0 MPa at room temperature and 100.0 MPa at 350°C, satisfying the requirements for engineering applications. Microstructural characterization revealed a partial transformation of am−Al2O3 to γ−Al2O3; however, both the microstructure and mechanical properties exhibited stable behavior during prolonged annealing. These findings indicate that both stabilization treatments effectively enhance the thermal stability of the (B4C+Al2O3)/Al composite, thereby providing a materials science basis for the long−term safe service of dry storage containers for spent fuel.

neutron absorbing materials  /  (B4C+Al2O3)/Al composite  /  stabilization process  /  mechanical properties  /  microstructure
石宝铭, 昝宇宁, 王全兆, 肖伯律, 马宗义. (B4C+Al2O3)/Al中子吸收材料的稳定化工艺. 科技导报, 2026 , 44 (2) : 98 -107 . DOI: 10.3981/j.issn.1000-7857.2025.11.00024
Baoming SHI, Yuning ZAN, Quanzhao WANG, Bolü XIAO, Zongyi MA. Stabilization process of (B4C+Al2O3)/Al neutron absorbing materials[J]. Science & Technology Review, 2026 , 44 (2) : 98 -107 . DOI: 10.3981/j.issn.1000-7857.2025.11.00024
随着核电的发展与普及,反应堆运行过程中产生的乏燃料管理问题逐渐成为核能可持续发展的重大科学与工程挑战[1]。乏燃料中所含放射性核素将对环境与人类健康构成威胁[2],因而,实现安全、经济且可持续的乏燃料贮存是核燃料循环体系中至关重要的环节。在此背景下,中子吸收材料的应用具有关键意义。其中,B4C/Al复合材料因材料均匀性良好、力学性能优异、耐高温性、抗辐射性、制备工艺简便及原材料成本低廉等优势,已经成为广泛研究的焦点[34]
乏燃料的中期贮存主要采用湿式贮存和干式贮存2种方式[56]。由于干式贮存在安全性和经济性方面的固有优势,其正逐渐取代传统的湿式贮存方式。核工业中干式贮存系统的广泛使用,对传统的中子吸收材料也提出了新的要求。有研究表明,乏燃料干式贮存工况下服役温度最高超过300℃[78]。并且,根据美国核管理委员会的国际通用多用途存储系统安全评估报告可知[9],多数干式贮存系统在设计与监管审查中以60年作为目标服役期。由此可见,在干式贮存系统中服役的中子吸收材料需在高温环境下长期服役[10]。基于上述服役条件,Zan等[11]在传统B4C/Al复合材料制备工艺的基础上,通过室温下铝粉的原位氧化引入了非晶Al2O3(am−Al2O3),研制出有优异高温性能的(B4C+Al2O3)/Al中子吸收材料。该材料中的am−Al2O3在制备过程中可钉扎晶界、抑制晶界滑动,配合挤压过程可显著细化晶粒,形成超细晶组织,从而有效提升材料的初始高温强度与综合性能。然而有研究表明,am−Al2O3在高温下吉布斯自由能高于γ−Al2O3,因而在服役温度下am−Al2O3有转变为结晶态γ−Al2O3的隐患[12]。值得注意的是,作为材料中的关键高温强化相,am−Al2O3一旦发生晶化,可能削弱复合材料的力学性能[1213]。因此,尽管am−Al2O3在制备过程中细化晶粒对提升高温强度具有不可替代的作用,但其作为亚稳相,在长期高温服役中强化效果的稳定性仍有待进一步验证,并需据此提出有效策略。
关于(B4C+Al2O3)/Al复合材料在长期高温热暴露下微观组织与力学性能的演化行为,特别是其中am−Al2O3的热稳定性,尚缺乏系统认识。因此,系统研究(B4C+Al2O3)/Al复合材料的稳定性,对于阐明其组织性能演化规律、保障其在长期服役过程中的可靠性至关重要,有助于推动材料在干式贮存领域的工程化应用。本研究对(B4C+Al2O3)/Al复合材料板材分别进行400℃/100 h和550℃/8 h稳定化工艺处理,并对处理后的样品在400℃下进行最长4000 h的退火试验,以验证稳定化处理的效果。通过系统分析不同热暴露时间下的拉伸性能和微观组织特征,探索复合材料在高温服役条件下的稳定状态,为材料的工程化应用提供数据支撑。
本研究采用粉末冶金工艺制备(B4C+Al2O3)/Al复合材料。选择平均粒径分别为1.2与8 μm的铝粉与B4C颗粒作为原材料,复合材料中的Al2O3由铝粉表面的自然氧化引入。将铝粉与B4C颗粒(质量分数为10%)置于混料机中机械混合8 h,以确保颗粒分布均匀。随后,混合粉末经冷压、脱气处理后在530℃下进行真空热压,制成致密的复合材料坯锭。将坯锭在450℃下以9∶1的挤压比热挤压成板材。对挤压态板材分别进行2种稳定化处理:400℃/100 h与550℃/8 h。之后,将经稳定化处理的样品置于400℃环境下进行最长4000 h的退火实验,以模拟长期热暴露并评估其组织与性能稳定性。
为系统评价不同热处理状态下材料的性能与组织演变,本研究对挤压态、稳定化处理及400℃退火后的样品分别进行了微观组织观察与力学性能测试。微观组织分析沿板材挤压方向进行。采用金相显微镜(optical microscope,OM,DMi8,Leica)和透射电子显微镜(transmission electron microscopy,TEM, Talos F200x,Thermo Fisher)分别进行宏观与微观尺度的观察。将OM样品经砂纸逐级研磨后,采用SiO2颗粒悬浮液进行最终抛光以获得光滑表面。对于TEM观察,样品先经砂纸研磨并利用Gatan Model 656进行凹坑处理,最终通过离子减薄仪(PIPS Model 695,Gatan)进行离子减薄。使用扫描电子显微镜(scanning electron microscope, SEM,Sigma 55,Zeiss)进行电子背散射衍射(electron backscattered diffraction,EBSD,Symmetry S2,Oxford)分析。使用三离子束切割机(EM TIC 3X,Leica)对待观察样品表面进行抛光处理制备EBSD样品。
沿板材挤压方向加工棒状拉伸试样,其平行段直径为5 mm,平行段长度为35 mm。每组实验条件下至少制备并测试3个有效试样,以确保数据的统计可靠性。拉伸实验在应变速率为10−3 s−1的条件下进行。其中,室温拉伸测试使用Instron 5982型电子万能试验机,而高温(350℃)拉伸测试使用Sans MTS E45.105型电子万能试验机。试样断裂后,采用SEM对其断口形貌进行观察,以分析断裂机理。
经400℃/100 h稳定化处理及不同时长退火后,(B4C+Al2O3)/Al复合材料在室温与350℃下的力学性能演变如图1所示。400℃/100 h稳定化处理后,(B4C+Al2O3)/Al复合材料板材在室温下的抗拉强度Rm为233.0 MPa,较原始板材下降了6.9%。350℃下的Rm为118.7 MPa,较原始板材下降了16.2%。在后续400℃退火500、1000、2000、4000 h的过程中,样品的力学性能已不再发生明显变化。由此可确认服役前对材料进行稳定化处理的必要性,400℃/100 h的稳定化处理工艺可使复合材料的力学性能达到稳定状态。虽然强度有所下降,但其Rm仍高于Qin等[14]报道的B4C体积分数为15%的B4C/1100Al复合材料(在基体中加入质量分数为0.4% Sc和质量分数为0.24% Zr)经300℃退火后的Rm(室温及300℃下的Rm分别为210.0和65.0 MPa),也高于Zan等[15]报道的400℃退火8000 h后的B4C/6061Al复合材料(在350℃下Rm为77.0 MPa)。此外,经稳定化处理后,板材的Rm还高于其他的一些中子吸收材料,例如Wang等[16]报道的经400℃退火5000 h的Al−10Gd合金,其室温下的Rm仅为189.0 MPa。
(B4C+Al2O3)/Al复合材料板材及其经过400℃/100 h稳定化处理和400℃/4000 h高温退火后的显微硬度如表1所示。结果表明,经400℃/100 h稳定化处理后,复合材料的显微硬度较初始状态出现明显下降。复合材料显微硬度的下降可能与微观组织的改变(am−Al2O3→γ−Al2O3转变)有关,且在相关文献中也有相似的报道。Samelor等[17]使用金属有机化学气相沉积方法制备了am−Al2O3的薄膜,结果表明随着加工温度的提高,am−Al2O3的薄膜转变为纳米结构的γ−Al2O3薄膜,并且显微硬度发生下降。Yan等[18]使用微弧氧化的方法制备了主要由am−Al2O3和γ−Al2O3组成的薄膜,结果表明,随着am−Al2O3转变为γ−Al2O3,其显微硬度同样存在下降的趋势。
图2所示为(B4C+Al2O3)/Al复合材料板材在初始状态、经400℃/100 h稳定化处理及经400℃/4000 h高温退火后的OM图像。可以观察到经过400℃/100 h稳定化及400℃/4000 h退火后,B4C颗粒的分布未发生明显变化,颗粒依然在Al基体中均匀分布,且未见界面反应产物。
(B4C+Al2O3)/Al复合材料板材沿挤压方向获得的反极图(inverse pole figure,IPF)揭示了复合材料在400℃/100 h稳定化处理和400℃/4000 h退火后的晶粒形貌。可以观察到,原始板材中晶粒呈现出在挤压方向上被拉长的晶粒结构(图3(a)),其平均晶粒尺寸为1.5 μm。经稳定化处理后,微观组织仍为拉长的晶粒结构(图3(b)),晶粒尺寸约为1.7 μm。板材经400℃/4000 h退火后,微观组织(图3(c))对比稳定化后的微观组织(图3(b))未发生明显变化,其平均晶粒尺寸为1.6 μm。值得注意的是,板材在长时间退火过程中,Al基体中低角度晶界(low angle grain boundary,LAGB)有所减少,晶粒尺寸未有明显变化,高角度晶界(high angle grain boundary,HAGB)仍然占主导地位,反映了复合材料具有良好的热稳定性。
(B4C+Al2O3)/Al复合材料板材在初始状态、经400℃/100 h稳定化处理及经400℃/4000 h高温退火后的TEM图像如图4所示。从原始板材的TEM图像(图4(a)和(d))可见,沿挤压方向上,Al2O3在Al晶粒晶界处呈网状分布。在400℃/100 h稳定化处理后(图4(b)和(e)),大部分am−Al2O3仍然存在且保持片层状,但在其周围出现了颗粒状的γ−Al2O3,表明部分am−Al2O3的晶型发生了转变。与其他研究相似,Nanda Kumar等[19]在对am−Al2O3薄膜在350℃下退火1 h后,同样发现了γ−Al2O3的存在,并进一步提出am−Al2O3通过局部原子重新排列诱导转化成核的转变机制[19],其生长沿着相邻晶核的有利晶面进行聚集。尽管400℃低于文献中报道的am−Al2O3向γ−Al2O3转变所需的结晶温度[12],但是长时间的热暴露同样可能促进am−Al2O3向γ−Al2O3的晶化过程。am−Al2O3骨架向γ−Al2O3颗粒的结晶转变会降低材料的力学性能[20],因此在400℃/100 h稳定化后复合材料的力学性能会有所下降。400℃/100 h稳定化复合板材在400℃/4000 h退火后(图4(c)和(f)),板材的微观组织与稳定化后的微观组织相似。由此可见,复合材料在稳定化处理后微观组织进入了稳定状态,从而使复合材料在室温及高温下的力学性能均趋于稳定。此外,γ−Al2O3能够有效阻碍铝晶粒的生长,在稳定化的过程中没有出现晶粒长大的现象[20]
(B4C+Al2O3)/Al复合材料板材在初始状态、经400℃/100 h稳定化处理及经400℃/4000 h高温退火后的样品室温拉伸断口的SEM图像如图5所示。原始板材的断口整体表现出韧性断裂的特征(图5(a)),在断裂的颗粒及颗粒拔出留下的孔洞周围,断裂面较为平整,基体表面存在细小的韧窝。400℃/100 h稳定化处理和400℃/4000 h退火后的复合材料断口形貌具有相似的特征(图5(b)和(c)),但韧窝和撕裂棱更为明显,且在撕裂棱周围分布着和原始板材拉伸断口相似的细小韧窝。韧窝尺寸和断口形貌的变化与颗粒–基体之间的界面脱粘形成的孔洞及微观组织的变化有关。
原始板材在350℃下的断口形貌如图6(a)所示,其表面分布有大量尺寸较大、形状接近等轴的韧窝,显示出典型的高温韧性断裂特征。高倍观察(图6(d))可见韧窝底部较为干净,未见明显第二相颗粒残留。经400℃/100 h稳定化处理和400℃/4000 h退火后,复合材料整体仍保持韧性断裂特征,但断口形貌出现明显变化,在韧窝内部可见沿晶断裂特征(图6(b)和(c)),表现为表面光滑、棱角清晰的小平面。进一步高倍观察(图6(e)和(f))可见,在部分韧窝底部出现颗粒状断裂形貌,其间隙表明相邻晶粒间发生了相对滑移。结合文献报道,在使用细铝粉制备的Al2O3/Al复合材料中,断裂起源位置常与γ−Al2O3的分布密切相关[21]。在本研究中,断口形貌的转变可归因于热暴露过程中am−Al2O3向γ−Al2O3的相变。γ−Al2O3的形成弱化了晶界结合强度,促使裂纹沿晶界扩展,从而在宏观上表现为高温断裂形貌的改变。
图7所示为经过550℃/8 h稳定化处理后的复合材料及其继续在400℃下高温退火后的力学性能,抗拉强度的数值在图中进行了标注。结果表明,在高温退火过程中,复合材料室温下的Rm均在220.0 MPa以上,350℃下的高温Rm均在100.0 MPa以上。其力学性能与经400℃/100 h稳定化处理板材的力学性能相近。
结合图7可知,材料经550℃/8 h稳定化后,在400℃下高温退火过程中的室温及高温力学性能均保持稳定。550℃/8 h稳定化后的(B4C+Al2O3)/Al复合材料板材继续在400℃下高温退火不同时间的显微硬度变化如表2所示。能够看到经过550℃/8 h处理的样品,在400℃退火后其维氏硬度依然保持稳定,约为70.0HV0.2
550℃/8 h稳定化后的(B4C+Al2O3)/Al复合材料板材以及其在400℃下高温退火1000和4000 h的OM图像如图8所示。与400℃下稳定化的复合材料OM图像相似,B4C颗粒依然在基体中分布得较为均匀,并未随退火时间的延长而发生改变。
550℃/8 h稳定化处理后的(B4C+Al2O3)/Al复合材料板材以及其继续在400℃下退火1000和4000 h后的IPF图像如图9所示。与400℃/100 h下稳定化的板材不同,550℃/8 h稳定化的板材中虽然整体仍然呈现出挤压方向上被拉长的晶粒结构,但与母材相比出现了较明显的变化,晶粒的长径比减小,且出现少量等轴晶。3个时间点的样品平均晶粒尺寸分别为1.6、1.7、1.7 μm,表明后续400℃退火并不导致晶粒尺寸的变化。
经550℃/8 h稳定化处理的(B4C+Al2O3)/Al复合材料板材及其继续在400℃退火的样品沿挤压方向的TEM图像如图10所示。与前文提及的400℃/100 h的稳定化工艺有所区别,可以观察到经过550℃/8 h稳定化处理后,复合材料板材的晶界附近出现了大量的颗粒状γ−Al2O3。并且,虽然am−Al2O3仍然存在,但由原始板材中片层状转变为块状。Trunov等[22]报道过对铝粉的热处理实验中铝粉表面am−Al2O3厚度增加的现象。在后续的400℃高温退火过程中,复合材料的微观组织未发生明显变化,Al2O3集中在晶界附近分布,am−Al2O3仍保持块状,其周围存在着大量颗粒状的γ−Al2O3。由此可见,复合材料板材在经过550℃/8 h稳定化处理后,复合材料的微观组织进入了稳定状态,并未在后续的长时间400℃退火过程中发生改变。
550℃/8 h稳定化处理后的(B4C+Al2O3)/Al复合材料板材以及其在400℃下高温退火1000和4000 h后的样品室温拉伸断口的SEM图像如图11所示。能够观察到3个断口的形貌较为相似,均存在颗粒与基体的脱粘和颗粒断裂的现象,且在大韧窝的撕裂棱周围分布着较为细小的韧窝。由此可见,后续的400℃退火对经稳定化的材料在室温下的断裂行为无明显影响。
550℃/8 h稳定化处理后的(B4C+Al2O3)/Al复合材料板材以及其在400℃下继续高温退火1000和4000 h后的样品在350℃下拉伸断口的SEM图像如图12所示。3个断口在350℃下的断裂形貌同样较为相似,与前文400℃稳定化处理后样品的高温拉伸断口略有不同,经550℃稳定化后,高温拉伸断口中的部分区域未观察到韧窝的存在(图12(a)、(b)和(c)),其表面颗粒状断裂形貌的间隙表明晶间断裂的发生。部分区域的断裂形貌与400℃稳定化工艺的高温断口相同(图12(d)、(e)和(f)),在韧窝中能够观察到晶间断裂的特征。
综合上述分析,400℃/100 h与550℃/8 h 2种稳定化工艺均能使(B4C+Al2O3)/Al复合材料在长期热暴露下保持组织与力学性能的稳定,且均高于国外主流的结构功能一体化中子吸收材料Metamic−HT(B4C质量分数为10%)的力学性能,因此满足工程应用需求[2324]。尽管550℃/8 h工艺引发更显著的am−Al2O3向γ−Al2O3转变(图10),但其力学性能与400℃/100 h工艺相当(图7),且显微硬度在4000 h退火后未发生波动(表2)。这表明,较高温度的短时稳定化处理可通过加速相变过程快速达到稳定状态,而较低温度的长时间处理同样有效。2种工艺均能避免晶粒长大和界面反应(图8图9),确保了材料在350℃高温下的可靠性。上述发现为优化(B4C+Al2O3)/Al中子吸收材料的稳定化工艺提供了理论支撑,并为其在乏燃料干式贮存系统中的工程应用奠定了基础。
1) 复合材料板材经400℃/100 h稳定化处理后,其力学性能略有下降,室温Rm为233.0 MPa,350℃下Rm为118.7 MPa,显微硬度由76.0 HV0.2降至约71.4 HV0.2。在随后进行的高温退火验证中,材料的力学性能未发生明显变化。
2) 经550℃/8 h稳定化处理后,复合材料板材的力学性能同样仅出现轻微下降,室温Rm为227.8 MPa,350℃下Rm为110.1 MPa,显微硬度约为70.2 HV0.2。在随后进行的高温退火验证中,材料的力学性能同样未发生明显变化。
3) 微观组织分析表明,2种稳定化处理工艺均促进了am−Al2O3向γ−Al2O3的转变,其中550℃工艺转变更剧烈,但未引发晶粒粗化或界面失效。550℃/8 h稳定化工艺可在更短时间内实现力学性能和微观组织稳定,因而展现出更优的综合效果,具有更高的工程应用潜力。
  • 国家自然科学基金项目(52203385)
  • 国家自然科学基金项目(52322106)
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2026年第44卷第2期
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doi: 10.3981/j.issn.1000-7857.2025.11.00024
  • 接收时间:2025-11-10
  • 首发时间:2026-02-11
  • 出版时间:2026-01-28
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  • 收稿日期:2025-11-10
  • 修回日期:2025-12-31
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国家自然科学基金项目(52203385)
国家自然科学基金项目(52322106)
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    中国科学院金属研究所沈阳材料科学国家研究中心,沈阳 110016

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昝宇宁(通信作者),副研究员,研究方向为金属基复合材料,电子信箱:
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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
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
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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