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Article(id=1241795750103941909, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.08.001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1597507200000, receivedDateStr=2020-08-16, revisedDate=1599321600000, revisedDateStr=2020-09-06, acceptedDate=null, acceptedDateStr=null, onlineDate=1773996778274, onlineDateStr=2026-03-20, pubDate=1629388800000, pubDateStr=2021-08-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773996778274, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773996778274, creator=13701087609, updateTime=1773996778274, updator=13701087609, issue=Issue{id=1241795749348967189, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='8', pageStart='1', pageEnd='114', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773996778094, creator=13701087609, updateTime=1773997690758, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241799577397953390, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241799577397953391, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1241795749348967189, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1, endPage=7, ext={EN=ArticleExt(id=1241795750397543192, articleId=1241795750103941909, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Research Progress of Corona Resistant Polyimide Films, columnId=1198667062026531195, journalTitle=Insulating Materials, columnName=Review, runingTitle=null, highlight=null, articleAbstract=

This paper summarized the global patent layout of corona resistant PI films, the influencing factors of corona resistance for inorganic nano hybrid films, and introduced the application status of corona resistant PI films at liquid nitrogen temperature, as well as the future development of corona resistant PI films.

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本文综述了国内外耐电晕聚酰亚胺薄膜的专利布局、无机纳米杂化薄膜耐电晕性能的影响因素，介绍了耐电晕聚酰亚胺薄膜在液氮温度下的应用现状，并对耐电晕聚酰亚胺未来的发展方向进行了展望。

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闵永刚（1963-），男（汉族），湖北黄冈人，教授，主要从事特种聚酰亚胺及其产业化研究。
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李清玲（1997-），女（汉族），广东深圳人，硕士生，主要从事功能化聚酰亚胺薄膜制备的研究。

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李清玲（1997-），女（汉族），广东深圳人，硕士生，主要从事功能化聚酰亚胺薄膜制备的研究。

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李清玲（1997-），女（汉族），广东深圳人，硕士生，主要从事功能化聚酰亚胺薄膜制备的研究。

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申请年份专利权人专利名称创新点
2018株洲时代华昇新材料技术有限公司一种耐电晕聚酰亚胺复合薄膜及其制备方法[13]在热固性聚酰亚胺薄膜正反至少一面涂覆一层热塑性聚酰亚胺薄膜，用热塑性PI替代传统的氟胶层，避免因聚酰亚胺与氟树脂附着力差而出现脱胶现象，在减小薄膜厚度的同时又提升耐电晕寿命。
2016深圳瑞华泰薄膜科技有限公司一种耐电晕聚酰亚胺-聚全氟乙丙烯复合薄膜及其制备方法[14]复合薄膜有A-B两层结构和B-A-B三层结构，A层为填充无机纳米粒子的PI层，B层为填充无机纳米粒子的聚全氟乙丙烯树脂，复合薄膜具备两种材料的优异性能。
2016福建师范大学一种耐电晕聚酰亚胺/二氧化硅纳米复合薄膜及其制备方法[15]该杂化薄膜通过溶胶-凝胶法制备，其中纳米二氧化硅表面与聚酰亚胺通过氢键和化学键作用实现紧密结合，制备方法不仅操作简便，还能实现纳米SiO2粒子在PI基体中均匀稳定分散。
2015北京科技大学一种纳米Al2O3复合的耐电晕聚酰亚胺薄膜[16]通过新型硅烷偶联剂和钛酸酯偶联剂对纳米金属氧化物表面进行改性，使其在高浓度时也能与有机相均匀混合，且机械强度没有降低。用此方法制备聚酰亚胺薄膜掺入的纳米氧化铝质量分数最高达30%。
2014天津市天缘电工材料有限责任公司一种耐电晕聚酰亚胺薄膜及其制造方法[17]采用高压乳化技术，在纳米金属氧化物中加入乳化剂和分散剂，使其在高浓度下仍能在聚酰胺酸（PAA）中均匀分散，制备出的杂化薄膜耐电晕寿命长。
), ArticleFig(id=1245062204811231826, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1241795750103941909, language=CN, label=表1, caption=

国内已授权的耐电晕聚酰亚胺制备方法专利概况

, figureFileSmall=null, figureFileBig=null, tableContent=
申请年份专利权人专利名称创新点
2018株洲时代华昇新材料技术有限公司一种耐电晕聚酰亚胺复合薄膜及其制备方法[13]在热固性聚酰亚胺薄膜正反至少一面涂覆一层热塑性聚酰亚胺薄膜，用热塑性PI替代传统的氟胶层，避免因聚酰亚胺与氟树脂附着力差而出现脱胶现象，在减小薄膜厚度的同时又提升耐电晕寿命。
2016深圳瑞华泰薄膜科技有限公司一种耐电晕聚酰亚胺-聚全氟乙丙烯复合薄膜及其制备方法[14]复合薄膜有A-B两层结构和B-A-B三层结构，A层为填充无机纳米粒子的PI层，B层为填充无机纳米粒子的聚全氟乙丙烯树脂，复合薄膜具备两种材料的优异性能。
2016福建师范大学一种耐电晕聚酰亚胺/二氧化硅纳米复合薄膜及其制备方法[15]该杂化薄膜通过溶胶-凝胶法制备，其中纳米二氧化硅表面与聚酰亚胺通过氢键和化学键作用实现紧密结合，制备方法不仅操作简便，还能实现纳米SiO2粒子在PI基体中均匀稳定分散。
2015北京科技大学一种纳米Al2O3复合的耐电晕聚酰亚胺薄膜[16]通过新型硅烷偶联剂和钛酸酯偶联剂对纳米金属氧化物表面进行改性，使其在高浓度时也能与有机相均匀混合，且机械强度没有降低。用此方法制备聚酰亚胺薄膜掺入的纳米氧化铝质量分数最高达30%。
2014天津市天缘电工材料有限责任公司一种耐电晕聚酰亚胺薄膜及其制造方法[17]采用高压乳化技术，在纳米金属氧化物中加入乳化剂和分散剂，使其在高浓度下仍能在聚酰胺酸（PAA）中均匀分散，制备出的杂化薄膜耐电晕寿命长。
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耐电晕聚酰亚胺薄膜研究进展
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李清玲 1 , 刘存生 1 , 翁梦蔓 1 , 刘屹东 1, 2 , 张继升 3 , 马小华 3 , 闵永刚 1, 2
绝缘材料 | 综述 2021,54(8): 1-7
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绝缘材料 | 综述 2021, 54(8): 1-7
耐电晕聚酰亚胺薄膜研究进展
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李清玲1, 刘存生1, 翁梦蔓1, 刘屹东1, 2, 张继升3, 马小华3, 闵永刚1, 2
作者信息
  • 1广东工业大学 材料与能源学院，广东 广州 510006
  • 2东莞华南设计创新院，广东 东莞 523808
  • 3慧迈材料科技（广东）有限公司，广东 佛山 528200

    • 李清玲（1997-），女（汉族），广东深圳人，硕士生，主要从事功能化聚酰亚胺薄膜制备的研究。

通讯作者:

闵永刚（1963-），男（汉族），湖北黄冈人，教授，主要从事特种聚酰亚胺及其产业化研究。
Research Progress of Corona Resistant Polyimide Films
Qingling LI1, Cunsheng LIU1, Mengman WENG1, Yidong LIU1, 2, Jisheng ZHANG3, Xiaohua MA3, Yonggang MIN1, 2
Affiliations
  • 1School of Materials and Energy, Guangdong University of Technology, Guangzhou 510006, China
  • 2Dongguan South China Design Innovation Institute, Dongguan 523808, China
  • 3Huimai Material Technology (Guangdong) Co., Ltd., Foshan 528200, China
出版时间: 2021-08-20 doi: 10.16790/j.cnki.1009-9239.im.2021.08.001
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摘要
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本文综述了国内外耐电晕聚酰亚胺薄膜的专利布局、无机纳米杂化薄膜耐电晕性能的影响因素，介绍了耐电晕聚酰亚胺薄膜在液氮温度下的应用现状，并对耐电晕聚酰亚胺未来的发展方向进行了展望。

聚酰亚胺  /  专利布局  /  影响因素  /  低温应用

This paper summarized the global patent layout of corona resistant PI films, the influencing factors of corona resistance for inorganic nano hybrid films, and introduced the application status of corona resistant PI films at liquid nitrogen temperature, as well as the future development of corona resistant PI films.

polyimide  /  patent layout  /  influence factor  /  low temperature application
李清玲, 刘存生, 翁梦蔓, 刘屹东, 张继升, 马小华, 闵永刚. 耐电晕聚酰亚胺薄膜研究进展. 绝缘材料, 2021 , 54 (8) : 1 -7 . DOI: 10.16790/j.cnki.1009-9239.im.2021.08.001
Qingling LI, Cunsheng LIU, Mengman WENG, Yidong LIU, Jisheng ZHANG, Xiaohua MA, Yonggang MIN. Research Progress of Corona Resistant Polyimide Films[J]. Insulating Materials, 2021 , 54 (8) : 1 -7 . DOI: 10.16790/j.cnki.1009-9239.im.2021.08.001
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0 引言
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聚酰亚胺（PI）是一类具有酰亚胺环结构的聚合物材料，主链中含有非常稳定的芳杂环结构，使其具有优异的耐热性能、力学性能和电性能[1-3]等特点，也因此被广泛应用在电动机匝间绝缘、电缆绕包绝缘等领域。近年来，中国高铁动车技术的迅猛发展给电气设备带来许多新的问题。变频调速电机是高铁动车组最重要的设备之一，被用作高铁的动力驱动器，它的安全运行是目前国内外的研究热点。变频电机主要采用脉宽调制（PWM）驱动技术[4-5]，其性能是保证高铁动车运行稳定的关键，然而PWM技术脉冲过电压产生的局部放电会使变频电机的匝间绝缘材料快速老化，并在短时间内被电晕击穿导致电机发生故障[6]。因此提升变频电机匝间绝缘材料的耐电晕性能非常关键。聚酰亚胺薄膜作为牵引电机绝缘系统中的绕组绝缘材料已有40多年历史[7]，但随着电机领域变频技术的飞速发展，纯聚酰亚胺薄膜很难满足更高的耐电晕要求[8-9]。近年来研究发现，通过掺杂一定量的无机纳米粒子可以改善聚酰亚胺薄膜的介电性能，同时可以大幅提高绝缘材料的耐电晕性能。1995年，杜邦公司与ABB、西门子合作研制出三层结构的耐电晕聚酰亚胺杂化薄膜（100CR），通过在纯聚酰亚胺中掺杂50～500 nm的气相Al2O3，使其耐电晕性能与粉云母的接近[10]，与纯聚酰亚胺薄膜（100HN）相比，杂化薄膜（100CR）的耐电晕性能提高了10倍以上[11]。这一重要研究成果引起国内外的关注，使其成为研究热点。随后，许多科研团队成功地通过掺杂无机纳米粒子提高了聚酰亚胺薄膜的耐电晕性能[12]。本文主要分析近年来耐电晕聚酰亚胺薄膜的专利布局、耐电晕机理与研究进展以及未来的发展趋势。
1 国内外耐电晕聚酰亚胺专利现状
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1.1 国内耐电晕聚酰亚胺专利概况
近年来国内关于耐电晕聚酰亚胺薄膜制备方法的专利数量较少。专利申请数量较多的专利申请人有：深圳瑞华泰薄膜科技有限公司、株洲时代新材料科技股份有限公司、中国科学院长春应用化学研究所等。表1为国内已授权的耐电晕聚酰亚胺薄膜制备方法专利概况。
1.2 国外耐电晕聚酰亚胺专利概况
日本日立在专利JP4584014B2中公开了一种耐电晕绝缘涂料的制备方法，由于有机硅溶胶与N-甲基吡咯烷酮（NMP）溶剂的相容性差，该发明用γ-丁内酯替代传统的NMP作为合成聚酰胺酸的主要溶剂，可以使二氧化硅颗粒在膜中均匀分散而不集聚[18]。专利JP2009212034A在耐电晕漆胶体中掺杂中空多孔的金属氧化物细颗粒或氧化硅颗粒，可以降低薄膜的介电常数同时抑制其被局部放电腐蚀，从而获得优异耐电晕性能的漆包线[19]。日本住友专利WO2017006999A1向树脂中掺杂具有层状结构的双层氢氧化物，层状结构的氢氧化物是由金属氢氧化物层和阴离子与层间水组成的中间层交替堆叠的结构，当局部放电时层状氢氧化物会释放出水分并且能有效吸收电晕放电产生的热能，从而减少热击穿[20]。通用电气加拿大公司在专利US5989702A公开了一种夹心型绝缘材料，将云母纸通过环氧树脂层压到添加了纳米粒子的耐电晕聚酰亚胺薄膜上，所得的层压带具有优异的物理性能和耐电晕性能[21]。德国西门子公司在专利DE102010032949A1中公开了一种绝缘胶带的制备方法，云母纸具有良好的耐电晕性能，但其力学性能较差，该发明是将至少添加了一种无机纳米粒子的聚酰亚胺树脂作为粘合剂，借助粘合剂将云母纸与具有高机械强度的载体材料粘合起来制备出一种高机械强度的抗局部放电的绝缘胶带，纳米粒子的掺入使材料具有更长的耐电晕老化寿命[22]。美国杜邦在专利US2013209769A1公开了一种耐电晕材料结构，其中耐电晕结构中含有耐电晕聚酰亚胺层，该层是由聚酰亚胺和无机纳米颗粒通过化学亚胺化的方法制得，与热亚胺化法制得的耐电晕聚酰亚胺层相比，化学亚胺化法制得的耐电晕聚酰亚胺层无机纳米颗粒具有更好的分散性，且具有更好的电气强度、拉伸强度、断裂伸长率和耐电晕性[23]。
2 影响杂化薄膜耐电晕性能的因素
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2.1 无机纳米粒子的导热性
聚酰亚胺薄膜热导率较低，当牵引电机过载运行或局部放电时会产生大量的热，使得聚酰亚胺薄膜在短时内会发生热击穿导致绝缘材料失效，最终导致电机故障。张明玉等[24]对PI/Al2O3杂化薄膜进行了10次电晕老化测试，并利用表征技术观察和研究电晕放电下杂化薄膜从老化到击穿的全过程，结果如图1所示。从图1可以看出，击穿点大多数出现在电晕破坏环与中心区之间的边缘区，少数出现在中心区，而电晕破坏环上没有出现击穿点，说明电晕老化击穿主要是由电晕放电产生的热量积累且散热困难引起薄膜发生热击穿，而不是电击穿引起的。
高温是导致绝缘材料的绝缘性能和寿命降低的主要原因之一，将高绝缘的纳米粒子（如氮化硼或氧化铝粒子）引入聚合物基体是改善聚合物导热、耐热性能最有效的方法。纳米粒子相互接触形成局部链状或网状的导热通道，可使电晕放电过程产生的热量快速散出，不仅可以提高绝缘材料的热导率，而且还能削弱空间电荷注入和局部放电对薄膜的损坏[25]。普通聚酰亚胺薄膜的热导率为0.15 W/(m·K)，而100CR薄膜的热导率为0.45 W/(m·K)，100CR薄膜的无机纳米粒子分布在薄膜表层，有利于热量散出，从而降低热击穿的危险[26]。日本钟渊化学工业株式会社发明了一种在纯聚酰亚胺薄膜上、下至少一个表面上涂覆一层热导率高于15 W/(m·K)、表面电阻低于1012 Ω且体积电阻率高于1015 Ω·cm的含无机填料的高导热耐电晕聚酰亚胺薄膜，这种结构的耐电晕聚酰亚胺薄膜不仅成本低且导热性能优异[27]。
氮化硼纳米粒子具有高导热和高温绝缘性能，是一种理想的散热材料和绝缘材料。一些研究学者通过引入改性的氮化硼粒子以提高聚酰亚胺薄膜的热导率从而增强其耐电晕性能。
DU B X等[28]在聚酰亚胺基体中混入六方氮化硼（h-BN）颗粒，制备了不同质量分数的PI/h-BN复合薄膜，并对其进行耐电晕测试，研究热导率对耐电晕性能的影响。结果表明，随着h-BN质量分数增加，耐电晕寿命延长，当h-BN质量分数为80%时，热导率达到2.58 W/(m·K)。h-BN颗粒可以提高热导率，加速高频局部放电产生的热量散发，对抑制薄膜受热击穿起到重要作用。
LIU X X等[29]通过引入氧氮化硼（OBNNS）到聚酰亚胺基体中制备出厚度为40～50 μm的OBNNS/PI复合薄膜，当OBNNS含量为0.25%时，复合薄膜的热导率为0.291 W/(m·K)，比纯聚酰亚胺薄膜高50%。耐电晕寿命也随着OBNNS含量的增加而增加，当OBNNS的含量为3%时，复合薄膜在室温下的耐电晕寿命为18.2 h，大约是纯聚酰亚胺薄膜（3.1 h）的6倍。
ZHAO H等[30]采用原位聚合法将二维（2D）氮化硼掺入到聚酰亚胺/氮化铝（PI/AlN）中制备出一种厚度约为40 μm的三元复合薄膜，并研究其耐电晕性能。结果表明，三元复合薄膜的耐电晕时间为65 h，是纯聚酰亚胺薄膜的21.6倍，BN纳米片可以延长电荷载流子的传输路径从而改善耐电晕寿命和击穿性能，三元复合薄膜的耐电晕机理模型如图2所示。
马莉莉等[31]用硅烷偶联剂对h-BN粒子进行改性，以减少粒子在聚酰亚胺基体中出现团聚现象，再通过原位聚合法制备出改性六方氮化硼（f-BN）/聚酰亚胺复合薄膜。结果表明，当改性后的六方氮化硼（f-BN）含量为15%时，复合薄膜的耐电晕寿命达到最大值，为纯聚酰亚胺薄膜的7倍，当填料含量继续增加，复合薄膜耐电晕寿命呈下降趋势，这是过多的填料在PI基体中分散不均匀造成的。
刘松等[32]通过原位聚合法成功制备出不同含量的BN/PI复合薄膜（厚度为50 μm），耐电晕测试结果表明，当BN颗粒的掺杂量为20%时，复合薄膜的耐电晕时间最长，为纯聚酰亚胺薄膜的116.7倍。
夏旭[33]通过原位聚合法制备了PI/BN+Al2O3复合薄膜，复合薄膜的平均厚度为（30±2）μm。试验数据表明，复合薄膜的导热性与耐电晕寿命有关。随着BN+Al2O3组分增加，复合薄膜的导热性不断提高，当无机填料含量为20%时，复合薄膜的热导率为0.21 W/(m·K)，是纯聚酰亚胺薄膜的1.6倍。耐电晕寿命则呈现先增加后减少的趋势，当BN+Al2O3组分为15%时，耐电晕寿命达到最高81.1 h，此时的交流击穿性能也最佳。
2.2 杂化薄膜的结构
1995年杜邦公司与ABB、西门子合作研制的耐电晕聚酰亚胺薄膜有三层，呈“三明治”结构，无机纳米粒子分布在薄膜表层，聚酰亚胺夹在中间。当纳米粒子的含量达到某一临界值时，聚合物基体中的粒子与粒子之间会相互接触，形成一个相互贯穿的网络结构，从而提高复合薄膜的电导率和热导率。当受到外加电场作用时，聚酰亚胺降解，裸露的无机纳米粒子迅速地塌陷形成一个网状保护层阻挡电晕继续向纵向深入破坏薄膜内层，中间层聚酰亚胺则保证整个复合薄膜的介电性能和机械强度[34]。
目前已研制出的耐电晕聚酰亚胺薄膜有以下3种结构：①在聚酰胺酸（PAA）中均匀填充无机纳米填料后涂覆及热亚胺化得到的单层结构；②两层都填充了无机纳米填料但含量不同或是一层无填料一层含填料的双层结构；③在单层纯聚酰亚胺薄膜正、反面各涂覆一层耐电晕层的“三明治”结构，或者在单层纯聚酰亚胺薄膜一面或两面通过蒸镀法、浸胶法等方式增加一层或两层无机化合物/聚酰亚胺杂化耐电晕层构成的多层结构[35]。
目前大多数团队研究的耐电晕聚酰亚胺薄膜基本上为单层结构。孔宇楠等[36]采用原位聚合法制备出厚度为50 μm的单层聚酰亚胺/纳米二氧化钛复合薄膜，通过表征发现，纳米二氧化钛（TiO2）粒子较好地镶嵌在聚酰亚胺薄膜上，在一定场强下，复合薄膜的耐电晕寿命随二氧化钛含量增加而增加，当TiO2含量为20%时，复合薄膜的耐电晕寿命是纯聚酰亚胺薄膜的8.3倍。江苏冰城电材有限公司[37]发明了一种成品率较高的单层结构耐电晕聚酰亚胺薄膜，采用粒径小于50 nm的纳米金属氧化物颗粒在高速剪切分散器中与N,N-二甲基乙酰胺（DMAc）混合制出均匀的悬浮液，然后制得耐电晕聚酰亚胺薄膜。研究发现，单层结构的耐电晕聚酰亚胺薄膜中无机填料的含量越高，薄膜的耐电晕性能就越好，但是当填料含量超过一定值时，杂化聚酰亚胺薄膜的力学性能尤其是断裂伸长率急剧下降，影响耐电晕聚酰亚胺薄膜的成品率。
近年来研究发现，通过“掺少量填料，涂覆多层膜”的形式可以有效地提升复合薄膜的多种性能。ZHONG X等[38]采用原位聚合法制备了一种总厚度为（50±4）μm的双层结构PI/Al2O3复合薄膜，复合薄膜的结构如图3所示，一层为纯聚酰亚胺膜，另一层为Al2O3-PI杂化膜。通过扫描电镜（SEM）表征其微观结构，并对双层薄膜的正、反面进行耐电晕性能测试。结果表明，当双层膜正面（Al2O3-PI杂化层在上，纯聚酰亚胺层在下）与棒电极接触时耐电晕寿命比纯聚酰亚胺单层高出152.5%，当双层膜的反面（纯聚酰亚胺层在上，Al2O3-PI杂化层在下）与棒电极接触时耐电晕寿命则比纯聚酰亚胺单层高出115.3%，说明纳米粒子可以提升耐电晕寿命。
深圳瑞华泰薄膜科技有限公司[35]发明了一种双层结构的耐电晕聚酰亚胺薄膜。该薄膜分为两层，一层为主体结构，主要成分是含有少量无机填料（5%～30%）的聚酰亚胺，能为薄膜提高良好的力学性能；另一层富含无机填料（5%～60%）及少量聚酰亚胺，为薄膜提高耐电晕性能。该薄膜在一定场强下，耐电晕寿命大于105 h。
桂林电器科学研究院有限公司[39]发明了一种三层结构耐电晕聚酰亚胺薄膜，在纯聚酰亚胺薄膜的上、下两个表面各涂覆一层耐电晕聚酰亚胺（薄膜总厚度为25 μm，纯聚酰亚胺薄膜层厚度为20 μm，上、下两层厚度各为2.5 μm）。当无机填料含量为30%时，与单层厚度同为25 μm的耐电晕聚酰亚胺薄膜相比，三层结构的薄膜耐电晕寿命比单层薄膜的寿命长3 h，抗张强度也比单层薄膜的高34 MPa，说明该技术不仅改善薄膜的耐电晕性，也使得薄膜具有良好的力学性能。
王志强等[40]采用原位聚合法制备了三层结构的SiO2-PI/PI/SiO2-PI复合薄膜，每层薄膜厚度均为10 μm，通过透射电镜（TEM）观察到无机填料在聚酰亚胺基体均匀分散，当无机纳米粒子含量为20%时，三层结构的复合薄膜耐电晕寿命最长达到157 h，这是由于中间层纯聚酰亚胺薄膜阻挡了电晕往纵向传导，电荷只在掺杂层发生横向传导，提高耐电晕寿命的同时也提升整个复合薄膜的电气强度。
杨瑞宵等[41]采用多次浸胶的方法制备了五层结构的SiO2-Al2O3/PI复合薄膜，其分布为Am/An/P/An/A，如图4所示，其中P为纯聚酰亚胺，外层Am和次外层An分别为SiO2-Al2O3含量不同的聚酰亚胺杂化膜（P层厚度为13 μm，Am层厚度为3 μm，An层厚度为3 μm，薄膜总厚度为25 μm）。对复合薄膜进行耐电晕测试，结果表明，当Am层纳米粒子质量分数为32%，An层纳米粒子质量分数为16%时，复合薄膜的耐电晕寿命最长，为23.4 h，说明纳米粒子对薄膜起到保护作用，这也是影响复合薄膜耐电晕性的主要因素，五层结构设计在保证力学性能的同时提高了耐电晕性能。
3 耐电晕聚酰亚胺薄膜在液氮下的应用研究进展
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聚酰亚胺在低温下有较好的介电性能。ZHANG H等[42]研究发现聚酰亚胺薄膜的电气强度会随着温度的降低而增加，单层聚酰亚胺薄膜在78 K时的电气强度比300 K时提高了约23.9%。DU B X等[43]对聚酰亚胺薄膜在液氮和室温下的局部放电特性进行研究，结果表明聚酰亚胺薄膜在液氮下的局部放电起始电压是室温下的两倍，其认为低温可能会抑制聚酰亚胺局部放电的发生。超导系统低温绝缘失效是引起超导失超的主要原因之一[44-45]，因此聚酰亚胺也通常被作为高温超导的绕组绝缘材料。纯聚酰亚胺薄膜达不到超导技术的要求，其在低温局部放电下易被击穿，最后将会大幅降低超导电机的使用寿命。因此需要通过改性聚酰亚胺薄膜来提高其在低温条件下的耐电晕性能。表面氟化是最直接有效和最常见的改性方法，通过氟化可以改善空间电荷迁移率和电导率，抑制聚酰亚胺薄膜中空间电荷的积累。LI J等[46]对聚酰亚胺薄膜的表面进行氟化处理，然后进行击穿试验，并使用原子力显微镜（AFM）对样品表面进行形貌观察。结果发现，氟化改性后的聚酰亚胺薄膜耐电晕性能提升，氟化技术可以显著地抑制薄膜表面电荷的积累从而影响聚酰亚胺薄膜的局部放电特性和击穿特性。通过AFM可以观察到氟化后的聚酰亚胺薄膜表面比未处理的聚酰亚胺薄膜要光滑得多，未处理的聚酰亚胺薄膜击穿电压为8.2 kV，而氟化45 min后的聚酰亚胺薄膜最大击穿电压为11.7 kV，击穿电压明显增大。
然而氟化时间过长会导致聚酰亚胺分子链断裂，其绝缘性能会大幅降低。除了用氟化方法提高聚酰亚胺薄膜在低温下的耐电晕老化寿命以外，一些科研团队发现掺杂无机填料的聚酰亚胺薄膜也能提高其在液氮下的耐电晕性能。
WEI B等[47]针对在77 K温度下纯聚酰亚胺薄膜（100HN）和掺杂无机纳米粒子的聚酰亚胺薄膜（100CR）在直流电压下的电气强度进行对比试验，液氮环境下的直流击穿测试装置如图5所示。根据10次测量数据的平均值及Weibull分布参数可知，100CR和100HN的63.2%电气强度分别是433.96 kV/mm和406.44 kV/mm，100CR的63.2%电气强度约为100HN的1.1倍。说明掺杂纳米材料的聚酰亚胺100CR电气强度优于纯聚酰亚胺100HN，即纳米材料的掺杂使100CR耐受直流电压性能优于100HN。无机填料的引入使纯聚酰亚胺薄膜内部形成大量有机-无机陷阱，在对薄膜放电时，这些陷阱可以捕捉更多的电荷，空间电荷会改变材料内部的局部电场，使电场均匀化，因此耐电晕寿命提高。此外还可能是因为100CR为三层结构，100HN为单层，多层结构对薄膜的耐电晕寿命也有一定的影响。
4 结束语
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近年来，我国对耐电晕聚酰亚胺薄膜产品的需求量大幅提升，国内不少厂家也尝试对耐电晕聚酰亚胺薄膜进行研发并产业化，但由于起步较晚、技术不够成熟，国内的一些大型电机仍需从国外进口价格昂贵的耐电晕聚酰亚胺薄膜材料。
目前，耐电晕聚酰亚胺薄膜需要研究的重点及未来发展方向为：①纳米粒子的分散状态会影响薄膜的耐电晕性，可以通过物理交联或化学交联以增加聚合物与无机填料之间的相容性，形成有机-无机网络结构，既减少纳米粒子在聚合物基体的团聚现象，还提高杂化薄膜的结构稳定性和耐电压冲击性；②由于纳米粒子掺杂量增加会使薄膜的力学性能呈下降趋势，可以对薄膜的结构进行设计，通过“少掺杂，多层膜”的方式提高耐电晕寿命的同时又保证薄膜的其他物理性能优异；③超导电机的输电容量大、损耗低、资源的利用率大幅提高，是今后电力系统技术的发展方向。绝缘材料是超导电机中必不可少的组成部分。目前超导电机的绝缘材料仍多是使用聚丙烯层压纸（PPLP）。关于不同种类的无机填料掺杂聚酰亚胺形成的杂化薄膜在液氮低温环境下的性能研究及测试报道也较少。因此耐电晕聚酰亚胺薄膜的结构及掺杂的填料种类对其在液氮环境下的性能影响也是今后一个很好的研究方向。
基金
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  • 广东省“珠江人才计划”引进创新创业团队资助项目(2016ZT060412)
  • 广东工业大学百人计划(220418095)
  • 佛山市科技创新团队(1920001000108)
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2021年第54卷第8期
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doi: 10.16790/j.cnki.1009-9239.im.2021.08.001
  • 接收时间：2020-08-16
  • 首发时间：2026-03-20
  • 出版时间：2021-08-20
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  • 收稿日期：2020-08-16
  • 修回日期：2020-09-06
基金
广东省“珠江人才计划”引进创新创业团队资助项目(2016ZT060412)
广东工业大学百人计划(220418095)
佛山市科技创新团队(1920001000108)
作者信息
    1广东工业大学 材料与能源学院，广东 广州 510006
    2东莞华南设计创新院，广东 东莞 523808
    3慧迈材料科技（广东）有限公司，广东 佛山 528200

通讯作者:

闵永刚（1963-），男（汉族），湖北黄冈人，教授，主要从事特种聚酰亚胺及其产业化研究。
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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
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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