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Article(id=1203281641398579422, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2025.06.002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1727193600000, receivedDateStr=2024-09-25, revisedDate=1734451200000, revisedDateStr=2024-12-18, acceptedDate=null, acceptedDateStr=null, onlineDate=1764814299200, onlineDateStr=2025-12-04, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1764814299200, onlineIssueDateStr=2025-12-04, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1764814299200, creator=13701087609, updateTime=1764814299200, updator=13701087609, issue=Issue{id=1203281635908231645, tenantId=1146029695717560320, journalId=1149653034449285133, year='2025', volume='58', issue='6', pageStart='1', pageEnd='148', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=0, articleOrder=1, issueType=-1, specialIssue=null, createTime=1764814297892, creator=13701087609, updateTime=1764815002353, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1203284590690545746, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1203284590694740051, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=9, endPage=15, ext={EN=ArticleExt(id=1203281641629266143, articleId=1203281641398579422, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Research on properties of polyamic acid resin and its film with high solid content and low viscosity, columnId=1203281640207393262, journalTitle=Insulating Materials, columnName=Special Issue on High Performance Polyimide Materials, runingTitle=null, highlight=

A series of resins with ≥30% of solid content and about 4 000 mPa·s of viscosity and their polyimide films were prepared by introducing flexible 4,4′-oxobisphthalic anhydride (ODPA) or twisted non-coplanar structure 3,3′,4,4′-biphenyltetracarboxylic acid dianhydride (BPDA) into the molecular structure of homophthalic tetracarboxylic acid dianhydride-4,4′-diaminodiphenyl ether (PMDA-ODA), and capped with a capping agent. The properties of the films were characterized by tensile testing machine, breakdown voltage tester, TMA, DMA, TGA, and cross-cut tester. The results show that when the solid content of the semi-rigid structure PMDA-ODA resin increases to 30% and the viscosity reduces to about 4 000 mPa·s, the film could not be formed due to the low molecular weight, and the PI film with good electromechanical properties can be prepared through introducing flexible monomer to improve the the polymer flexibility and using norbornene diacetic anhydride (NA) for capping. When continuing to increase the resin solid content and increase the proportion of flexible monomers, the electromechanical properties, heat resistance, ahd the adhesion on the copper sheet of the film decrease. The films with 30% of solid content, about 4 000 mPa·s of viscosity, 30% mole fraction of ODPA, and end-capped with NA show better electromechanical properties, heat resistance, and adhesion, which can be used as a impregnating varnish for insulation protection on the surface of substrate.

, articleAbstract=

A series of resins with ≥30% of solid content and about 4 000 mPa·s of viscosity and their polyimide films were prepared by introducing flexible 4,4′-oxobisphthalic anhydride (ODPA) or twisted non-coplanar structure 3,3′,4,4′-biphenyltetracarboxylic acid dianhydride (BPDA) into the molecular structure of homophthalic tetracarboxylic acid dianhydride-4,4′-diaminodiphenyl ether (PMDA-ODA), and capped with a capping agent. The properties of the films were characterized by tensile testing machine, breakdown voltage tester, TMA, DMA, TGA, and cross-cut tester. The results show that when the solid content of the semi-rigid structure PMDA-ODA resin increases to 30% and the viscosity reduces to about 4 000 mPa·s, the film could not be formed due to the low molecular weight, and the PI film with good electromechanical properties can be prepared through introducing flexible monomer to improve the the polymer flexibility and using norbornene diacetic anhydride (NA) for capping. When continuing to increase the resin solid content and increase the proportion of flexible monomers, the electromechanical properties, heat resistance, ahd the adhesion on the copper sheet of the film decrease. The films with 30% of solid content, about 4 000 mPa·s of viscosity, 30% mole fraction of ODPA, and end-capped with NA show better electromechanical properties, heat resistance, and adhesion, which can be used as a impregnating varnish for insulation protection on the surface of substrate.

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在均苯四甲酸二酐-4,4′-二氨基二苯醚（PMDA-ODA）分子结构中引入柔性4,4′-氧双邻苯二甲酸酐（ODPA）或扭曲非共面结构3,3′,4,4′-联苯四甲酸二酐（BPDA），并采用封端剂进行封端，制备了一系列固含量≥30%、黏度约为4 000 mPa·s的高固含量低黏度树脂及其聚酰亚胺薄膜。采用拉伸试验机、击穿强度测试仪、热机械分析仪、动态热机械分析仪、热重分析仪和百格测试仪对薄膜的性能进行表征。结果表明：当半刚性结构PMDA-ODA树脂的固含量提高至30%、黏度降低至约4 000 mPa·s时，因分子量过低无法成膜，而引入柔性单体，提高聚合物柔韧性，再采用降冰片烯二酸酐（NA）进行封端，使短链段分子通过交联成高聚物后，可以制备出机电性能良好的PI薄膜。继续增大树脂固含量、提高柔性单体比例，薄膜的机电性能和耐热性出现不同程度下降，在铜片上的附着力下降。其中固含量为30%、黏度约为4 000 mPa·s、ODPA摩尔分数为30%、采用NA封端的PI薄膜，其机电性能、耐热性和附着力均较佳，可作为浸渍漆用于基材表面的绝缘防护。

, articleAbstract=

在均苯四甲酸二酐-4,4′-二氨基二苯醚（PMDA-ODA）分子结构中引入柔性4,4′-氧双邻苯二甲酸酐（ODPA）或扭曲非共面结构3,3′,4,4′-联苯四甲酸二酐（BPDA），并采用封端剂进行封端，制备了一系列固含量≥30%、黏度约为4 000 mPa·s的高固含量低黏度树脂及其聚酰亚胺薄膜。采用拉伸试验机、击穿强度测试仪、热机械分析仪、动态热机械分析仪、热重分析仪和百格测试仪对薄膜的性能进行表征。结果表明：当半刚性结构PMDA-ODA树脂的固含量提高至30%、黏度降低至约4 000 mPa·s时，因分子量过低无法成膜，而引入柔性单体，提高聚合物柔韧性，再采用降冰片烯二酸酐（NA）进行封端，使短链段分子通过交联成高聚物后，可以制备出机电性能良好的PI薄膜。继续增大树脂固含量、提高柔性单体比例，薄膜的机电性能和耐热性出现不同程度下降，在铜片上的附着力下降。其中固含量为30%、黏度约为4 000 mPa·s、ODPA摩尔分数为30%、采用NA封端的PI薄膜，其机电性能、耐热性和附着力均较佳，可作为浸渍漆用于基材表面的绝缘防护。

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青双桂（1983-），女（壮族），广西柳州人，高级工程师，主要从事绝缘材料的研究工作。

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青双桂（1983-），女（壮族），广西柳州人，高级工程师，主要从事绝缘材料的研究工作。

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青双桂（1983-），女（壮族），广西柳州人，高级工程师，主要从事绝缘材料的研究工作。

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Preparation and properties of low-viscosity polyimide enameled varnish and its coatings[D]. 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Synthesis of novel polyimides and studies on the adhesion mechanism with copper foil[D]. Guangzhou:Sun Yat-sen University,2009., articleTitle=Synthesis of novel polyimides and studies on the adhesion mechanism with copper foil, refAbstract=null)], funds=[Fund(id=1203362950540140679, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, awardId=任务书编号：桂科AB22035007, language=CN, fundingSource=广西重点研发计划资助(任务书编号：桂科AB22035007), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1203362942763901796, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, xref=null, ext=[AuthorCompanyExt(id=1203362942772290405, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, companyId=1203362942763901796, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Guilin Electrical Equipment Scientific Research Institute Co., Ltd., Guilin 541004, China), AuthorCompanyExt(id=1203362942776484710, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, companyId=1203362942763901796, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=桂林电器科学研究院有限公司，广西 桂林 541004)])], figs=[ArticleFig(id=1203362947654459442, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Fig.1, caption=CTE curves of PO-18, PO3O-N-30, PO4O-N-30, PO4O-N-35, and BO3O-N PI films, figureFileSmall=K2V2PwJvWGHrQtftupWjaw==, figureFileBig=Cp4gkB3aH3rKRzV+SP9viw==, tableContent=null), ArticleFig(id=1203362947759317048, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=图1, caption=PO-18、PO3O-N-30、PO4O-N-30、PO4O-N-35和BO3O-N PI薄膜的热膨胀系数曲线, figureFileSmall=K2V2PwJvWGHrQtftupWjaw==, figureFileBig=Cp4gkB3aH3rKRzV+SP9viw==, tableContent=null), ArticleFig(id=1203362947880951873, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Fig.2, caption=DMA curves of PO3O-N-30, PO4O-N-30, PO4O-N-35, PO5O-N-40, and BO3O-N-30 films, figureFileSmall=ueAlv3MO4/NBOAyxRwryUg==, figureFileBig=7NYhDZCsZiCHPzwUKBsj0w==, tableContent=null), ArticleFig(id=1203362948023558216, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=图2, caption=PO3O-N-30、PO4O-N-30、PO4O-N-35、PO5O-N-40和BO3O-N-30薄膜DMA曲线, figureFileSmall=ueAlv3MO4/NBOAyxRwryUg==, figureFileBig=7NYhDZCsZiCHPzwUKBsj0w==, tableContent=null), ArticleFig(id=1203362948111638605, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Fig.3, caption=TGA curves of PO3O-N-30, PO4O-N-30, PO4O-N-35, and PO5O-N-40 PI films, figureFileSmall=YgmwLNZEqjwnSWJfyQ+JGw==, figureFileBig=kEdFEg4+L6cFxzuFSOfK5Q==, tableContent=null), ArticleFig(id=1203362948174553167, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=图3, caption=PO3O-N-30、PO4O-N-30、PO4O-N-35和PO5O-N-40 PI薄膜的热失重曲线, figureFileSmall=YgmwLNZEqjwnSWJfyQ+JGw==, figureFileBig=kEdFEg4+L6cFxzuFSOfK5Q==, tableContent=null), ArticleFig(id=1203362948245856338, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Table 1, caption=Material proportion of resin in each sample, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成DMAc/gODA/gPMDA/gODPA/gMA or NA/g固含量/%
PO-18-0PMDA0.995-ODA11902021.700018
PO-18PMDA0.97-ODA11882021.200018
PO-30PMDA0.88-ODA1932019.200030
PO-M-30PMDA0.88-ODA1-MA0.24942019.2001.2730
PO-N-30PMDA0.88-ODA1-NA0.241002019.2003.9430
PO3O-30PMDA0.6-ODPA0.3-ODA1992013.159.3030
PO3O-M-30PMDA0.6-ODPA0.3-ODA1-MA0.21002013.159.31.0530
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.21062013.159.33.2830
PO3O-M-35PMDA0.54-ODPA0.3-ODA1-MA0.32792011.769.31.6935
PO3O-N-35PMDA0.54-ODPA0.3-ODA1-NA0.32852011.769.35.2535
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.261102010.3012.44.2630
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.387209.9012.44.9235
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.574205.5015.58.2040
BO3O-N-30BPDA0.61-ODPA0.3-ODA1-NA0.181252021.079.32.9530
), ArticleFig(id=1203362948329742419, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=表1, caption=

各配方树脂物料比例

, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成DMAc/gODA/gPMDA/gODPA/gMA or NA/g固含量/%
PO-18-0PMDA0.995-ODA11902021.700018
PO-18PMDA0.97-ODA11882021.200018
PO-30PMDA0.88-ODA1932019.200030
PO-M-30PMDA0.88-ODA1-MA0.24942019.2001.2730
PO-N-30PMDA0.88-ODA1-NA0.241002019.2003.9430
PO3O-30PMDA0.6-ODPA0.3-ODA1992013.159.3030
PO3O-M-30PMDA0.6-ODPA0.3-ODA1-MA0.21002013.159.31.0530
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.21062013.159.33.2830
PO3O-M-35PMDA0.54-ODPA0.3-ODA1-MA0.32792011.769.31.6935
PO3O-N-35PMDA0.54-ODPA0.3-ODA1-NA0.32852011.769.35.2535
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.261102010.3012.44.2630
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.387209.9012.44.9235
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.574205.5015.58.2040
BO3O-N-30BPDA0.61-ODPA0.3-ODA1-NA0.181252021.079.32.9530
), ArticleFig(id=1203362948422017112, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Table 2, caption=The film-forming property of polyamic acid resins, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成固含量/%树脂黏度/(mPa·s)成膜性
PO-18-0PMDA0.995-ODA118100 000√流平性差
PO-18PMDA0.97-ODA1184 040√
PO-30PMDA0.88-ODA1304 000漆膜开裂
PO-M-30PMDA0.88-ODA1-MA0.24303 900漆膜开裂
PO-N-30PMDA0.88-ODA1-NA0.24304 210漆膜开裂
PO3O-30PMDA0.6-ODPA0.3-ODA1304 030漆膜开裂
PO3O-M-30PMDA0.6-ODPA0.3-ODA1-MA0.2304 010漆膜开裂
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.2304 090√
PO3O-M-35PMDA0.54-ODPA0.3-ODA1-MA0.32354 020漆膜开裂
PO3O-N-35PMDA0.54-ODPA0.3-ODA1-NA0.32353 980漆膜开裂
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.26303 960√
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.3354 070√
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.5404 040√
BO3O-N-30BPDA0.61-ODPA0.3-ODA1-NA0.18304 050√
), ArticleFig(id=1203362948510097498, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=表2, caption=

聚酰胺酸树脂成膜性

, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成固含量/%树脂黏度/(mPa·s)成膜性
PO-18-0PMDA0.995-ODA118100 000√流平性差
PO-18PMDA0.97-ODA1184 040√
PO-30PMDA0.88-ODA1304 000漆膜开裂
PO-M-30PMDA0.88-ODA1-MA0.24303 900漆膜开裂
PO-N-30PMDA0.88-ODA1-NA0.24304 210漆膜开裂
PO3O-30PMDA0.6-ODPA0.3-ODA1304 030漆膜开裂
PO3O-M-30PMDA0.6-ODPA0.3-ODA1-MA0.2304 010漆膜开裂
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.2304 090√
PO3O-M-35PMDA0.54-ODPA0.3-ODA1-MA0.32354 020漆膜开裂
PO3O-N-35PMDA0.54-ODPA0.3-ODA1-NA0.32353 980漆膜开裂
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.26303 960√
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.3354 070√
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.5404 040√
BO3O-N-30BPDA0.61-ODPA0.3-ODA1-NA0.18304 050√
), ArticleFig(id=1203362948614955108, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Table 3, caption=The electromechanical properties of PI films, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成固含量/%拉伸强度/MPa断裂伸长率/%弹性模量/GPa电气强度/(kV/mm)
PO-18-0PMDA-ODA18130372.5310
PO-18PMDA0.97-ODA118127342.6302
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.230127153.4295
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.2630125113.2280
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.335124103.1267
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.54010882.8214
BO3O-N-30BPDA0.61-ODPA0.3-ODA1-NA0.1830127152.6298
), ArticleFig(id=1203362948728201321, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=表3, caption=

PI薄膜机电性能

, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成固含量/%拉伸强度/MPa断裂伸长率/%弹性模量/GPa电气强度/(kV/mm)
PO-18-0PMDA-ODA18130372.5310
PO-18PMDA0.97-ODA118127342.6302
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.230127153.4295
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.2630125113.2280
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.335124103.1267
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.54010882.8214
BO3O-N-30BPDA0.61-ODPA0.3-ODA1-NA0.1830127152.6298
), ArticleFig(id=1203362948828864624, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Table 4, caption=The heat resistance of PI films, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成固含量/%失重5%温度/℃失重10%温度/℃
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.230513551
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.2630504544
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.335489536
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.540462498
), ArticleFig(id=1203362948975665270, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=表4, caption=

PI薄膜耐热性

, figureFileSmall=null, figureFileBig=null, tableContent=
名称化学组成固含量/%失重5%温度/℃失重10%温度/℃
PO3O-N-30PMDA0.6-ODPA0.3-ODA1-NA0.230513551
PO4O-N-30PMDA0.47-ODPA0.4-ODA1-NA0.2630504544
PO4O-N-35PMDA0.45-ODPA0.4-ODA1-NA0.335489536
PO5O-N-40PMDA0.25-ODPA0.5-ODA1-NA0.540462498
), ArticleFig(id=1203362949067939963, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=EN, label=Table 5, caption=The adhesion between the copper sheet and the PI film, figureFileSmall=null, figureFileBig=null, tableContent=
名称亚胺化工艺
程序升温至350℃保温1 h直线升温至350℃保温1 h直线升温至400℃保温10 min
PO-18442
PO3O-N-30110
PO4O-N-30221
PO4O-N-35332
PO5O-N-40443
BO3O-N221
), ArticleFig(id=1203362950351396995, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281641398579422, language=CN, label=表5, caption=

PI漆膜在铜片上的附着力

, figureFileSmall=null, figureFileBig=null, tableContent=
名称亚胺化工艺
程序升温至350℃保温1 h直线升温至350℃保温1 h直线升温至400℃保温10 min
PO-18442
PO3O-N-30110
PO4O-N-30221
PO4O-N-35332
PO5O-N-40443
BO3O-N221
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高固含量低黏度聚酰胺酸树脂及其薄膜性能研究
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青双桂 , 姬亚宁 , 唐小青 , 唐盛东 , 王汝柯 , 刘姣 , 潘钦鹏
绝缘材料 | 高性能聚酰亚胺材料专题 2025,58(6): 9-15
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绝缘材料 | 高性能聚酰亚胺材料专题 2025, 58(6): 9-15
高固含量低黏度聚酰胺酸树脂及其薄膜性能研究
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青双桂, 姬亚宁, 唐小青, 唐盛东, 王汝柯, 刘姣, 潘钦鹏
作者信息
  • 桂林电器科学研究院有限公司，广西 桂林 541004

    • 青双桂（1983-），女（壮族），广西柳州人，高级工程师，主要从事绝缘材料的研究工作。

Research on properties of polyamic acid resin and its film with high solid content and low viscosity
Shuanggui QING, Yaning JI, Xiaoqing TANG, Shengdong TANG, Ruke WANG, Jiao LIU, Qinpeng PAN
Affiliations
  • Guilin Electrical Equipment Scientific Research Institute Co., Ltd., Guilin 541004, China
出版时间: 2025-06-20 doi: 10.16790/j.cnki.1009-9239.im.2025.06.002
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摘要
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在均苯四甲酸二酐-4,4′-二氨基二苯醚（PMDA-ODA）分子结构中引入柔性4,4′-氧双邻苯二甲酸酐（ODPA）或扭曲非共面结构3,3′,4,4′-联苯四甲酸二酐（BPDA），并采用封端剂进行封端，制备了一系列固含量≥30%、黏度约为4 000 mPa·s的高固含量低黏度树脂及其聚酰亚胺薄膜。采用拉伸试验机、击穿强度测试仪、热机械分析仪、动态热机械分析仪、热重分析仪和百格测试仪对薄膜的性能进行表征。结果表明：当半刚性结构PMDA-ODA树脂的固含量提高至30%、黏度降低至约4 000 mPa·s时，因分子量过低无法成膜，而引入柔性单体，提高聚合物柔韧性，再采用降冰片烯二酸酐（NA）进行封端，使短链段分子通过交联成高聚物后，可以制备出机电性能良好的PI薄膜。继续增大树脂固含量、提高柔性单体比例，薄膜的机电性能和耐热性出现不同程度下降，在铜片上的附着力下降。其中固含量为30%、黏度约为4 000 mPa·s、ODPA摩尔分数为30%、采用NA封端的PI薄膜，其机电性能、耐热性和附着力均较佳，可作为浸渍漆用于基材表面的绝缘防护。

高固含量  /  低黏度  /  聚酰胺酸树脂  /  聚酰亚胺

A series of resins with ≥30% of solid content and about 4 000 mPa·s of viscosity and their polyimide films were prepared by introducing flexible 4,4′-oxobisphthalic anhydride (ODPA) or twisted non-coplanar structure 3,3′,4,4′-biphenyltetracarboxylic acid dianhydride (BPDA) into the molecular structure of homophthalic tetracarboxylic acid dianhydride-4,4′-diaminodiphenyl ether (PMDA-ODA), and capped with a capping agent. The properties of the films were characterized by tensile testing machine, breakdown voltage tester, TMA, DMA, TGA, and cross-cut tester. The results show that when the solid content of the semi-rigid structure PMDA-ODA resin increases to 30% and the viscosity reduces to about 4 000 mPa·s, the film could not be formed due to the low molecular weight, and the PI film with good electromechanical properties can be prepared through introducing flexible monomer to improve the the polymer flexibility and using norbornene diacetic anhydride (NA) for capping. When continuing to increase the resin solid content and increase the proportion of flexible monomers, the electromechanical properties, heat resistance, ahd the adhesion on the copper sheet of the film decrease. The films with 30% of solid content, about 4 000 mPa·s of viscosity, 30% mole fraction of ODPA, and end-capped with NA show better electromechanical properties, heat resistance, and adhesion, which can be used as a impregnating varnish for insulation protection on the surface of substrate.

high solid content  /  low viscosity  /  polyamic acid resin  /  polyimide
青双桂, 姬亚宁, 唐小青, 唐盛东, 王汝柯, 刘姣, 潘钦鹏. 高固含量低黏度聚酰胺酸树脂及其薄膜性能研究. 绝缘材料, 2025 , 58 (6) : 9 -15 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.002
Shuanggui QING, Yaning JI, Xiaoqing TANG, Shengdong TANG, Ruke WANG, Jiao LIU, Qinpeng PAN. Research on properties of polyamic acid resin and its film with high solid content and low viscosity[J]. Insulating Materials, 2025 , 58 (6) : 9 -15 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.002
正文
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0 引言
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聚酰亚胺（PI）位居高分子材料金字塔的顶端，是一类分子主链上带有酰亚胺环结构的耐高温高性能材料，具有优异的绝缘性能、良好的尺寸稳定性、出色的耐热性能和较高的机械强度等特点，在电子电工领域得到广泛应用，是关系国家产业安全和可持续发展的战略新兴产业材料，其耐高温、耐辐照等特性使得它在航空航天、风电、新能源汽车等特殊应用领域具有不可替代性[1-4]。PI材料通常采用二胺和二酐在有机溶剂中聚合得到聚酰胺酸树脂，然后将聚酰胺酸树脂（固含量一般≤20%）进行干燥处理以除去80%以上有机溶剂，再经亚胺化反应（温度高达400℃甚至500℃）制备得到。在现有不同的应用场合，合成的聚酰胺酸树脂固含量和黏度也不同，例如，电工电子用PI薄膜所需的聚酰胺酸树脂固含量主要为18%～20%，树脂黏度一般高于50 000 mPa·s；表面涂层、浸渍玻璃布、电机浸渍漆等用途的聚酰胺酸树脂固含量一般＜15%，黏度为几千厘泊，甚至低于1 000 mPa·s，以保证涂覆时的流平性；电机电磁圆线用聚酰胺酸树脂的固含量主要为16%～18%，黏度也只有几千厘泊[5]。随着涂布工艺技术水平的提高以及扁线电机的迅速发展，对高固含量低黏度聚酰胺酸树脂的需求日益增长，高固含量树脂可以减少涂覆或上漆次数，从而提高生产效率，降低生产成本[6]。但高固含量的树脂黏度往往很高，目前用于绝缘漆且已商业化的30%固含量聚酰胺酸树脂，最低黏度也有约2万厘泊，应用于基材浸渍或涂覆，流平性较差，对生产车速和基材的规格要求严格。
目前降低聚酰胺酸树脂黏度的主要方法有两种：一种是高温降解法，将制备好的聚酰胺酸树脂进行高温降黏，使黏度降低至几百或者几千厘泊，但此方法的树脂固含量一般＜15%，因此该方法不适用于高固含量树脂，高固含量树脂在高温后容易发生凝胶；另一种是封端技术，通过减少二胺或者二酐的摩尔量，使二胺和二酐的摩尔比偏离1∶1，形成端基为二胺或二酐的短链段分子，再采用单官能团的封端剂与短链段分子的端氨基或端酐进行反应，阻止分子链段增长，达到降低黏度的作用。但对高固含量聚酰胺酸树脂，需大量减少二胺或二酐的加入量，才能获得低黏度树脂，此时其成膜性会变差甚至无法成膜。因此研究人员采用不饱和封端剂对聚酰胺酸封端以控制分子量，再用高温交联提高加工性，此方法在纤维、工程塑料和复合材料制备中应用广泛[7-10]。
本文采用不饱和封端剂高温交联的方法，在主流配方PMDA-ODA基础上，引入柔性ODPA或扭曲非共面结构BPDA，以提高聚合物固化后的柔韧性，将固含量≥30%的聚酰胺酸树脂黏度降低至4 000 mPa·s 左右，研究高固含量、低黏度的不同配方对PI薄膜力学性能、电气性能、玻璃化转变温度、热稳定性、在铜箔表面附着性的影响。
1 实验
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1.1 主要原材料
4,4′-二氨基二苯醚（ODA），分析纯；均苯四甲酸二酐（PMDA），分析纯；4,4′-氧双邻苯二甲酸酐（ODPA），纯度≥99.9%；3,3′,4,4′-联苯四甲酸二酐（BPDA），纯度≥99.9%；顺丁烯二酸酐（MA），分析纯；降冰片烯二酸酐（NA），分析纯，以上试剂使用前均需干燥处理。乙酰胺（DMAc），分析纯，使用前需蒸馏。试剂厂家均为国药集团化学试剂有限公司。
1.2 实验步骤
1.2.1 无封端剂PMDA-ODA型树脂的合成
在三口烧瓶中，将20 g ODA溶解在DMAc中，待溶解完全后，分多次缓慢加入PMDA，每次加料后均反应1 h，通过控制PMDA的加入量，合成理论固含量接近18%、黏度为100 000 mPa·s和约为4 000 mPa·s的PMDA-ODA型PAA树脂，分别命名为PO-18-0和PO-18。按此工艺，减少DMAc和 PMDA的添加量，合成固含量为30%、黏度约为4 000 mPa·s的PMDA-ODA型PAA树脂，命名为PO-30。各配方树脂合成所需的DMAc和PMDA的量如表1所示。
1.2.2 X（X=NA、MA）封端PMDA-ODA型树脂的合成
在三口烧瓶中，将20 g ODA溶解在DMAc中，待溶解完全后，分多次缓慢加入 PMDA，每次加料后均反应1 h，通过控制PMDA加入量，合成黏度约为4 000 mPa·s的PMDA-ODA树脂，然后加入封端剂，封端剂的加入量为(nODA-nPMDA)×2 mol，得到X（X=MA、NA）封端PMDA-ODA型树脂，分别命名为PO-M-30和PO-N-30，各配方树脂合成所需的DMAc、PMDA和封端剂的量如表1所示。
1.2.3 封端型PMDA（或BPDA）-ODPA-ODA型树脂的合成
在三口烧瓶中，将20 g ODA溶解在DMAc中，待溶解完全后，加入一定量ODPA，继续搅拌反应 1 h，再分多次缓慢加入不超过设定量的PMDA（或BPDA），每次加料后均反应1 h，通过控制PMDA（或BPDA）加入量，合成黏度约为4 000 mPa·s的PMDA（或BPDA）-ODPA-ODA型树脂，然后加入封端剂MA或NA，封端剂的加入量为（nODA-nPMDA（或nBPDA））×2 mol，得到不同封端剂封端、不同固含量和不同ODPA摩尔量的PMDA（或BPDA）-ODPA-ODA型树脂，对应的树脂名称及各配方树脂合成所需的DMAc、PMDA（或BPDA）、ODPA和封端剂的量如表1所示。
1.2.4 PI薄膜的制备
采用自动数控涂布机将上述树脂在玻璃板上刮膜，然后置于烘箱中进行亚胺化得到相应的PI薄膜，处理条件为100℃/1 h+150℃/1 h+200℃/1 h+250℃/1 h+350℃/1 h。为了便于测试对比，涂布的PI薄膜厚度控制在20～30 μm。
1.2.5 PI漆铜片的制备
将100 μm厚无氧铜片用稀酸擦拭，先后经水和乙醇清洗干净后，自然晾干备用。将铜片浸入树脂中，垂直提拉离开树脂水平面后，静置1 min，然后再将铜片置于烘箱中进行亚胺化，处理条件分别为：程序升温至350℃保温1 h、直线升温至350℃保温1 h、直线升温至400℃保温10 min，最后得到PI漆铜片。为了便于测试对比，浸涂的PI漆膜厚度控制在20～30 μm。
1.3 测试方法
采用静态热机械分析仪（型号为TMA/SDTA840e）测试热膨胀系数，升温速率为10℃/min；采用动态热机械分析仪（型号为DMA8000）测试玻璃化转变温度，升温速率为5℃/min；采用热失重分析仪（型号为TGA7）测试氮气气氛下的热失重曲线，升温速率为10℃/min；采用万能试验机（型号为WDW-5）按照GB/T 13542.6—2006测试力学性能；依据ISO 2409-2020划格试验，采用间距为1 mm的多刃切割刀在PI漆铜片上测试漆膜附着力；采用击穿强度测试仪检测电气强度，升压速率为0.2 kV/s，电极直径为6 mm；采用旋转黏度计（型号为NDJ-8s）测试树脂黏度，树脂温度为30℃。
2 结果与讨论
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2.1 成膜性分析
表2为聚酰胺酸树脂在铜片上的成膜性。从表2可以看出，常规固含量为18%、黏度大至100 000 mPa·s的主流配方PMDA-ODA型树脂，分子量较大，制得的薄膜成膜性好，但在铜片上的流平性差，不适合用于基材挂漆；当黏度调降至4 040 mPa·s时，树脂也能在铜片上形成均匀的漆膜；然而增加固含量至30%制成PO-30树脂后，漆膜在铜片上出现开裂起皮现象，即使继续添加含不饱和双键的MA或NA封端剂，使树脂在高温亚胺化时发生一定程度的交联反应，也无法在铜片上获得完整的漆膜。这是由于树脂固含量增加至30%后，PMDA的摩尔量只有ODA摩尔量的88%，远低于固含量为18%时的摩尔量占比97%，分子量远低于PO-18，导致漆膜脆性增加，即使MA或NA在高温下发生交联，使分子量小的短链段分子发生交联，也无法获得完整的漆膜[11]。
本文在PO-30的PMDA-ODA半刚性分子骨架结构上引入具有醚键的ODPA取代30%的PMDA，增加柔性链段，增大分子结构柔韧性，降低分子间的相互作用力[12]，制备得到PO3O-30树脂，其也无法在铜片上获得完整漆膜。但用含不饱和双键的MA和NA封端剂进行封端处理，发现MA封端的PO3O-M-30漆膜开裂，NA封端的PO3O-N-30漆膜完整，说明增大分子结构柔韧性，以及将短链段分子在高温亚胺化时发生交联，都可以在一定程度上提高漆膜的加工性，两者结合后成膜性可明显改善。NA封端比MA封端成膜性更好，可能是由于平面结构的MA在高温发生交联后，分子刚性较大，而NA是通过环戊二烯和MA经Diels-Alder反应得到，具有双环结构，发生交联的双键和聚合物扭曲角度较大，可在一定程度上降低分子结构的规则度，提高树脂的可成膜性。
将树脂固含量从30%增加到35%时，分子链段变短，MA和NA封端的PO3O-M-35树脂和PO3O-N-35树脂都不能获得完整漆膜，其原因与上述分子量过小有关。继续增加柔性醚键ODPA的摩尔分数至40%和50%，得到PO4O-N-30、PO4O-N-35和PO5O-N-40树脂，或采用扭曲非共面BPDA取代PMDA得到BO3O-N-30树脂，都可在铜片上获得完整的漆膜，说明降低聚酰胺酸漆分子结构刚性，增加柔性链段，降低分子结构规整度，是制备高固含量低黏度树脂的有效途径之一。
2.2 薄膜机电性能分析
将能在铜片上制备完整漆膜的树脂在玻璃板上制备PI薄膜并测试其机电性能，结果如表3所示。从表3可以看出，PMDA-ODA配方树脂黏度为100 000 mPa·s时，薄膜的拉伸强度和断裂伸长率良好；黏度降低至4 040 mPa·s时，薄膜的力学性能和电气强度稍有下降；引入柔性醚键和NA封端、固含量在30%的树脂制得的薄膜弹性模量提高，断裂伸长率和电气强度降低；当将ODPA的摩尔分数提高至50%时，PO5O-N-40的机电性能大幅下降。其主要原因是薄膜配方中二酐和二胺的摩尔比与1∶1偏离更大，重复单元数变小，分子链段变短，酰亚胺化结构摩尔数降低，分子排列不紧密，导致薄膜的力学性能和电气强度下降[13]，同时因短链段分子高温交联后，刚性程度增加，使断裂伸长率降低，弹性模量比固含量为18%时明显增大，但随着固含量继续增大，因柔性链段增多，弹性模量逐渐降低。
2.3 热膨胀系数分析
低黏度聚酰胺酸树脂可涂覆在铜材、铁材、石英等表面，起到耐高温或绝缘防护的作用，为了解其热变形情况，采用静态热分析仪测试薄膜的热膨胀系数，结果如图1所示。从图1可以看出，PMDA-ODA薄膜的热膨胀系数为25×10-6 K-1，而引入柔性分子结构的ODPA后，分子链段容易发生缠绕，取向度变低，导致PO3O-N-30的热膨胀系数增大到 50×10-6 K-1，继续增加ODPA的含量，薄膜的热膨胀系数继续增大，达到56×10-6 K-1，而仅仅增加固含量到35%，PO4O-N-35薄膜的热膨胀系数变化不大，说明热膨胀系数主要与分子结构相关，与树脂固含量关系不大。另外，BPDA取代PMDA制备的BO3O-N-30薄膜，由于BPDA的刚性比PMDA小，因此其热膨胀系数比PO3O-N-30大。总体上看，在PMDA-ODA配方体系中引入柔性结构的ODPA或BPDA制得的薄膜，分子结构有序性降低，热膨胀系数增大[14]，热膨胀系数都大于50×10-6 K-1。
2.4 玻璃化转变温度分析
文献报道的PMDA-ODA型和PMDA-PDA型PI薄膜的玻璃化转变温度（Tg）接近或超过400℃[4,15]。本文制备的系列高固含量树脂低黏度配方薄膜玻璃化转变温度见图2。从图2可以看出，PO3O-N-30薄膜的Tg为355℃，当增加ODPA摩尔分数至40%时，PO4O-N-30薄膜的Tg降低至348℃。而当ODPA摩尔分数为40%，固含量为35%时，PO4O-N-35薄膜的Tg为356℃，比固含量30%的PO4O-N-30薄膜的Tg提高了8℃，可能是PO4O-N-35配方中PMDA的摩尔分数占比减少，NA封端剂的摩尔分数占比增多，NA在高温亚胺化时发生交联后，体型结构的聚合物体现出更高的玻璃化转变温度。同理，即使PO5O-N-40中柔性ODPA摩尔分数增大，会使Tg降低，但其高温交联后，分子体积结构增大，运动所需能量增加，仍具有较高的Tg。采用扭曲的非共面结构BPDA取代PMDA制得的BO3O-N-30薄膜，其玻璃化转变温度降低至309℃，耐热性降低明显。
2.5 热稳定性分析
图3为PO3O-N-30、PO4O-N-30、PO4O-N-35和PO5O-N-40 PI薄膜在氮气气氛下的热失重曲线，具体数据如表4所示。
从图3和表4可以看出，随着ODPA的摩尔分数从30%增加到50%时，薄膜失重5%和10%所对应的温度也不断下降，尤其是当ODPA摩尔分数为50%时，薄膜的热分解温度明显下降。一方面，固含量逐渐增大，分子链段越短，分子量越小，耐热性也更差；另一方面，增大分子链中柔性结构的比例，虽然可以提高薄膜的可塑性，但会降低材料的热稳定性[16-17]。
当ODPA的摩尔分数为40%时，将固含量从30%提高到35%，薄膜的耐热性下降，有两个方面的原因：其一是PO4O-N-35的PMDA摩尔分数降低，形成的刚性酰亚胺结构减少，降低了其耐热性；其二是与封端剂NA摩尔分数增大有关，NA在高温下会发生Diels-Alder反应，形成带双键的环状加成物，高温下继续发生交联，交联后虽然因体型结构增大在一定程度上可以提高其玻璃化转变温度，但是交联形成的脂肪环耐热性较差，更容易发生裂解反应，从而影响其耐热性[10,18]。
2.6 PI漆铜片附着力分析
PI漆膜在铜片上的接合机理主要是聚酰亚胺上的羰基与铜箔表面在高温下产生的氧化层发生了化学键合，因此PI漆膜与铜片的附着力不仅与配方相关，还与亚胺化工艺有直接关系。依据ISO 2409-2020测试漆膜的附着力，采用间距为1 mm的多刃切割刀在漆铜片上划透漆膜，依次用软毛刷、3M胶带测试划格阵型图内漆膜脱落情况，以判断薄膜附着力等级。本文对比了漆膜的3个升温亚胺化工艺对漆膜附着力的影响：程序升温至350℃保温1 h、直线升温至350℃保温1 h、直线升温至400℃保温10 min，结果如表5所示。
从表5可以看出，采用最高亚胺化温度为350℃的亚胺化工艺，不管是设置程序升温还是直线升温，得到的漆膜附着力均无法达到0级，且部分漆膜出现明显脱落现象。为尽量模拟工业化生产的快速亚胺化工艺，将亚胺化温度采用直线快速升温的方法，设置最高亚胺化温度为400℃，400℃下保温10 min，各配方漆膜与铜片的附着力均有所提高，但只有PO3O-N-30配方漆膜的附着力能达到0级。研究表明，亚胺化速率慢、温度低，溶剂挥发慢，界面生产的铜氧化物会更容易溶解在溶剂中，并挥发排出体系外，使PI漆膜与铜片的粘接力降低；如果亚胺化速率快、温度高，铜氧化物还未形成时，溶剂已快速挥发排出体系外，在更高的亚胺化温度处理时，界面铜产生铜氧化物得以保留下来，能更好地与PI漆膜接合，从而获得更好的附着力[19]。
3 结论
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通过在PMDA-ODA型PI薄膜中引入摩尔分数为30%的柔性结构ODPA，并采用NA封端，可制备固含量≥30%、黏度约为4 000 mPa·s的树脂，制得的薄膜机电性能良好，Tg为355℃，氮气气氛下失重5%时的温度可达到494℃，且能保持较高的耐热性，在铜片上经400℃快速亚胺化后，与铜箔紧密粘接，附着力达到0级，可作为浸渍漆用于材料表面绝缘防护。
基金
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  • 广西重点研发计划资助(任务书编号：桂科AB22035007)
文献
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2025年第58卷第6期
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doi: 10.16790/j.cnki.1009-9239.im.2025.06.002
  • 接收时间：2024-09-25
  • 首发时间：2025-12-04
  • 出版时间：2025-06-20
补充材料
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  • 收稿日期：2024-09-25
  • 修回日期：2024-12-18
基金
广西重点研发计划资助(任务书编号：桂科AB22035007)
作者信息
    桂林电器科学研究院有限公司，广西 桂林 541004
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2025.06.002
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
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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