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Article(id=1242756978095800654, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.11.013, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1619712000000, receivedDateStr=2021-04-30, revisedDate=1621526400000, revisedDateStr=2021-05-21, acceptedDate=null, acceptedDateStr=null, onlineDate=1774225952885, onlineDateStr=2026-03-23, pubDate=1637510400000, pubDateStr=2021-11-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1774225952885, onlineIssueDateStr=2026-03-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1774225952885, creator=13701087609, updateTime=1774225952885, updator=13701087609, issue=Issue{id=1242756974576775191, tenantId=1146029695717560320, journalId=1149653034449285133, year='2021', volume='54', issue='11', pageStart='1', pageEnd='139', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1774225952044, creator=13701087609, updateTime=1774226047274, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1242757374059066044, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1242757374059066045, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=94, endPage=99, ext={EN=ArticleExt(id=1242756979354091867, articleId=1242756978095800654, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and Properties of BPDA/ODA Polyimide Films with Micro-branched Crosslinked Structure, columnId=1198664996516360309, journalTitle=Insulating Materials, columnName=Polyimide Film Special Issue, runingTitle=null, highlight=null, articleAbstract=

Taking 1,3,5-tri(4-aminophenoxy) benzene (TAPOB) as crosslink agent, a micro-branched crosslinked structure was constructed in 3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA) and 4,4′-diaminodiohenyl ether (ODA) polyimide (PI) film, and a series of PI films with different TAPOB content were prepared. The effects of TAPOB content on the mechanical properties, thermomechanical properties, dielectric properties, and water absorption were studied. The results show that the addition of TAPOB can improve the comprehensive properties of BPDA/ODA PI films significantly. The existence of crosslinked structure is conductive to improve the mechanical properties, decrease the coefficient of thermal expansion (CTE) and water absorption of the film, and the micro-branched structure has a certain effect on reducing the dielectric constant.

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以三官能度的1,3,5-三（4-氨基苯氧基）苯（TAPOB）为交联剂，在3,3′,4,4′-联苯四甲酸二酐（BPDA）和4,4′-二氨基二苯醚（ODA）体系聚酰亚胺（PI）薄膜中构建微支化交联结构，制备出一系列具有不同TAPOB含量的PI薄膜，研究了TAPOB含量对薄膜力学性能、热力学性能、介电性能和吸水率的影响。结果表明：TAPOB的引入可明显提高BPDA/ODA体系PI薄膜的综合性能，交联结构的存在有利于提高薄膜的力学性能、降低热膨胀系数（CTE）和吸水率，微支化结构则对降低介电常数有一定的作用。

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田国峰（1984-），男（汉族），黑龙江伊春人，教授，主要从事高性能及功能型聚酰亚胺及其复合材料的研究。
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韩书豪（1995-），男（汉族），河南周口人，硕士生，主要从事聚酰亚胺薄膜的制备与性能的研究。

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韩书豪（1995-），男（汉族），河南周口人，硕士生，主要从事聚酰亚胺薄膜的制备与性能的研究。

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韩书豪（1995-），男（汉族），河南周口人，硕士生，主要从事聚酰亚胺薄膜的制备与性能的研究。

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Keyword(id=1245100052696383779, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, orderNo=2, keyword=薄膜), Keyword(id=1245100052792852780, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, orderNo=3, keyword=微支化), Keyword(id=1245100052901904691, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, orderNo=4, keyword=交联)], refs=[Reference(id=1245100055699505605, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, doi=null, pmid=null, pmcid=null, year=2006, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=丁孟贤, journalName=聚酰亚胺-化学-结构与性能的关系及材料, refType=null, unstructuredReference=丁孟贤.聚酰亚胺-化学-结构与性能的关系及材料[M].北京:科学出版社,2006., articleTitle=null, refAbstract=null), Reference(id=1245100055812751817, tenantId=1146029695717560320, 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European Polymer Journal, 2020,143:110206., articleTitle=Ultra-low dielectric constant polyimides: Combined efforts of fluorination and micro-branched crosslink structure, refAbstract=null)], funds=[Fund(id=1245100055405904311, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, awardId=51773007, language=CN, fundingSource=国家自然科学基金资助项目(51773007), fundOrder=null, country=null), Fund(id=1245100055506567613, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, awardId=XK1802-2, language=CN, fundingSource=中央高校基本科研业务费专项资金项目(XK1802-2), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1245100049869422683, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, xref=null, ext=[AuthorCompanyExt(id=1245100049873616987, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, companyId=1245100049869422683, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Key Laboratory of Carbon Fiber and Functional Polymers, Beijing University of Chemical Technology, Beijing 100029, China), AuthorCompanyExt(id=1245100049882005597, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, companyId=1245100049869422683, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=北京化工大学 碳纤维及功能高分子教育部重点实验室，北京 100029)])], figs=[ArticleFig(id=1245100053153562951, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Fig.1, caption=Preparation route of BPDA/ODA/TAPOB PI films, figureFileSmall=wSk38uhbXpIf6B7mpZfl9Q==, figureFileBig=O9tMukdkjcF/t1RNyhhRJg==, tableContent=null), ArticleFig(id=1245100053254226256, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=图1, caption=BPDA/ODA/TAPOB体系PI薄膜制备路线图, figureFileSmall=wSk38uhbXpIf6B7mpZfl9Q==, figureFileBig=O9tMukdkjcF/t1RNyhhRJg==, tableContent=null), ArticleFig(id=1245100053367472474, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Fig.2, caption=TMA image of BPDA/ODA/TAPOB PI films, figureFileSmall=YD4CL/akXKO4hm8R4fEMwA==, figureFileBig=9GRQzxFdsDm5UjvOosmiLg==, tableContent=null), ArticleFig(id=1245100053480718689, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=图2, caption=BPDA/ODA/TAPOB体系PI薄膜的TMA图, figureFileSmall=YD4CL/akXKO4hm8R4fEMwA==, figureFileBig=9GRQzxFdsDm5UjvOosmiLg==, tableContent=null), ArticleFig(id=1245100053577187686, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Fig.3, caption=Dielectric properties of BPDA/ODA/TAPOB PI films, figureFileSmall=1WX7vsSwd8QjJl4U7ezdHg==, figureFileBig=MCUJEhmgibLE4SvmEo2VxQ==, tableContent=null), ArticleFig(id=1245100053682045290, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=图3, caption=BPDA/ODA/TAPOB体系PI薄膜的介电性能, figureFileSmall=1WX7vsSwd8QjJl4U7ezdHg==, figureFileBig=MCUJEhmgibLE4SvmEo2VxQ==, tableContent=null), ArticleFig(id=1245100053782708591, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Fig.4, caption=Thermomechanical properties of BPDA/ODA/TAPOB PI films, figureFileSmall=bQ7lmTmLwOpCnjeQ2AcuaQ==, figureFileBig=U4CKoW9EsDeFAprCBpSJjw==, tableContent=null), ArticleFig(id=1245100053862400368, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=图4, caption=BPDA/ODA/TAPOB体系PI薄膜的热力学性能, figureFileSmall=bQ7lmTmLwOpCnjeQ2AcuaQ==, figureFileBig=U4CKoW9EsDeFAprCBpSJjw==, tableContent=null), ArticleFig(id=1245100053933703543, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Fig.5, caption=Performance evaluation of micro-branched crosslinked PI film and pure PI film, figureFileSmall=1oj2NVqhx27LKJHmS7Ie8w==, figureFileBig=UxOsajP1WNHBuw31J2XMIw==, tableContent=null), ArticleFig(id=1245100054025978238, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=图5, caption=微支化交联PI薄膜与纯PI膜的性能评估, figureFileSmall=1oj2NVqhx27LKJHmS7Ie8w==, figureFileBig=UxOsajP1WNHBuw31J2XMIw==, tableContent=null), ArticleFig(id=1245100054105670017, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Tab.1, caption=Monomer composition of BPDA/ODA/TAPOB PI films, figureFileSmall=null, figureFileBig=null, tableContent=
体系BPDA/mmolODA/mmolTAPOB/mmol
BPDA/ODA/TAPOB-05.055.0000
BPDA/ODA/TAPOB-0.055.054.9250.05
BPDA/ODA/TAPOB-0.105.054.8500.10
BPDA/ODA/TAPOB-0.155.054.7750.15
BPDA/ODA/TAPOB-0.205.054.7000.20
), ArticleFig(id=1245100054193750405, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=表1, caption=

BPDA/ODA/TAPOB体系PI薄膜的体系组成

, figureFileSmall=null, figureFileBig=null, tableContent=
体系BPDA/mmolODA/mmolTAPOB/mmol
BPDA/ODA/TAPOB-05.055.0000
BPDA/ODA/TAPOB-0.055.054.9250.05
BPDA/ODA/TAPOB-0.105.054.8500.10
BPDA/ODA/TAPOB-0.155.054.7750.15
BPDA/ODA/TAPOB-0.205.054.7000.20
), ArticleFig(id=1245100054286025094, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Tab.2, caption=Tensile properties and CTE of BPDA/ODA/TAPOB PI films, figureFileSmall=null, figureFileBig=null, tableContent=
体系

拉伸强度

/MPa

断裂伸长率

/%

初始模量

/GPa

CTE

/(×10-6 K-1)

BPDA/ODA/TAPOB-0173.559.32.9640.44
BPDA/ODA/TAPOB-0.05178.657.83.0439.43
BPDA/ODA/TAPOB-0.10180.352.13.0937.93
BPDA/ODA/TAPOB-0.15191.946.83.1234.73
BPDA/ODA/TAPOB-0.20181.336.63.3032.13
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BPDA/ODA/TAPOB体系PI薄膜的拉伸性能与CTE

, figureFileSmall=null, figureFileBig=null, tableContent=
体系

拉伸强度

/MPa

断裂伸长率

/%

初始模量

/GPa

CTE

/(×10-6 K-1)

BPDA/ODA/TAPOB-0173.559.32.9640.44
BPDA/ODA/TAPOB-0.05178.657.83.0439.43
BPDA/ODA/TAPOB-0.10180.352.13.0937.93
BPDA/ODA/TAPOB-0.15191.946.83.1234.73
BPDA/ODA/TAPOB-0.20181.336.63.3032.13
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体系介电常数介质损耗因数
BPDA/ODA/TAPOB-03.300.005 3
BPDA/ODA/TAPOB-0.053.430.004 7
BPDA/ODA/TAPOB-0.103.460.005 2
BPDA/ODA/TAPOB-0.153.270.006 0
BPDA/ODA/TAPOB-0.203.450.005 6
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1 MHz下BPDA/ODA/TAPOB体系PI薄膜的介电常数与介质损耗因数

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体系介电常数介质损耗因数
BPDA/ODA/TAPOB-03.300.005 3
BPDA/ODA/TAPOB-0.053.430.004 7
BPDA/ODA/TAPOB-0.103.460.005 2
BPDA/ODA/TAPOB-0.153.270.006 0
BPDA/ODA/TAPOB-0.203.450.005 6
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体系Tg/℃初始储能模量/MPa
BPDA/ODA/TAPOB-0295.91 619
BPDA/ODA/TAPOB-0.05283.62 056
BPDA/ODA/TAPOB-0.1296.22 094
BPDA/ODA/TAPOB-0.15284.52 576
BPDA/ODA/TAPOB-0.2284.03 055
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BPDA/ODA/TAPOB体系PI薄膜的玻璃化转变温度和初始储能模量

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体系Tg/℃初始储能模量/MPa
BPDA/ODA/TAPOB-0295.91 619
BPDA/ODA/TAPOB-0.05283.62 056
BPDA/ODA/TAPOB-0.1296.22 094
BPDA/ODA/TAPOB-0.15284.52 576
BPDA/ODA/TAPOB-0.2284.03 055
), ArticleFig(id=1245100054919365026, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Tab.5, caption=Water absorption rate of BPDA/ODA/TAPOB PI films, figureFileSmall=null, figureFileBig=null, tableContent=
体系吸水率/%
BPDA/ODA/TAPOB-02.13
BPDA/ODA/TAPOB-0.052.08
BPDA/ODA/TAPOB-0.102.01
BPDA/ODA/TAPOB-0.151.92
BPDA/ODA/TAPOB-0.201.85
), ArticleFig(id=1245100055011639717, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=表5, caption=

BPDA/ODA/TAPOB体系PI薄膜的吸水率

, figureFileSmall=null, figureFileBig=null, tableContent=
体系吸水率/%
BPDA/ODA/TAPOB-02.13
BPDA/ODA/TAPOB-0.052.08
BPDA/ODA/TAPOB-0.102.01
BPDA/ODA/TAPOB-0.151.92
BPDA/ODA/TAPOB-0.201.85
), ArticleFig(id=1245100055120691625, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=EN, label=Tab.6, caption=Four grades of PI film performance, figureFileSmall=null, figureFileBig=null, tableContent=
性能参数相对等级
1234
低热膨胀（LT）CTE/(×10-6 K-1)40～5030～4020～3010～20
低介电常数（LD）介电常数3.4～3.53.3～3.43.2～3.33.1～3.2
低吸水率（LA）吸水率/%2.5～302.0～2.51.5～2.01.0～1.5
高强度（HT）拉伸强度/MPa140～180180～220220～260260～300
高模量（HM）初始模量/GPa2～2.53～3.53.5～44～4.5
), ArticleFig(id=1245100055204577712, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978095800654, language=CN, label=表6, caption=

PI薄膜性能对应的4个等级

, figureFileSmall=null, figureFileBig=null, tableContent=
性能参数相对等级
1234
低热膨胀（LT）CTE/(×10-6 K-1)40～5030～4020～3010～20
低介电常数（LD）介电常数3.4～3.53.3～3.43.2～3.33.1～3.2
低吸水率（LA）吸水率/%2.5～302.0～2.51.5～2.01.0～1.5
高强度（HT）拉伸强度/MPa140～180180～220220～260260～300
高模量（HM）初始模量/GPa2～2.53～3.53.5～44～4.5
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BPDA/ODA体系微支化交联聚酰亚胺薄膜制备与性能研究
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韩书豪 , 周涵 , 王健华 , 齐胜利 , 田国峰 , 武德珍
绝缘材料 | 聚酰亚胺薄膜专题 2021,54(11): 94-99
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绝缘材料 | 聚酰亚胺薄膜专题 2021, 54(11): 94-99
BPDA/ODA体系微支化交联聚酰亚胺薄膜制备与性能研究
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韩书豪, 周涵, 王健华, 齐胜利, 田国峰, 武德珍
作者信息
  • 北京化工大学 碳纤维及功能高分子教育部重点实验室，北京 100029

    • 韩书豪（1995-），男（汉族），河南周口人，硕士生，主要从事聚酰亚胺薄膜的制备与性能的研究。

通讯作者:

田国峰（1984-），男（汉族），黑龙江伊春人，教授，主要从事高性能及功能型聚酰亚胺及其复合材料的研究。
Preparation and Properties of BPDA/ODA Polyimide Films with Micro-branched Crosslinked Structure
Shuhao HAN, Han ZHOU, Jianhua WANG, Shengli QI, Guofeng TIAN, Dezhen WU
Affiliations
  • Key Laboratory of Carbon Fiber and Functional Polymers, Beijing University of Chemical Technology, Beijing 100029, China
出版时间: 2021-11-22 doi: 10.16790/j.cnki.1009-9239.im.2021.11.013
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以三官能度的1,3,5-三（4-氨基苯氧基）苯（TAPOB）为交联剂，在3,3′,4,4′-联苯四甲酸二酐（BPDA）和4,4′-二氨基二苯醚（ODA）体系聚酰亚胺（PI）薄膜中构建微支化交联结构，制备出一系列具有不同TAPOB含量的PI薄膜，研究了TAPOB含量对薄膜力学性能、热力学性能、介电性能和吸水率的影响。结果表明：TAPOB的引入可明显提高BPDA/ODA体系PI薄膜的综合性能，交联结构的存在有利于提高薄膜的力学性能、降低热膨胀系数（CTE）和吸水率，微支化结构则对降低介电常数有一定的作用。

聚酰亚胺  /  薄膜  /  微支化  /  交联

Taking 1,3,5-tri(4-aminophenoxy) benzene (TAPOB) as crosslink agent, a micro-branched crosslinked structure was constructed in 3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA) and 4,4′-diaminodiohenyl ether (ODA) polyimide (PI) film, and a series of PI films with different TAPOB content were prepared. The effects of TAPOB content on the mechanical properties, thermomechanical properties, dielectric properties, and water absorption were studied. The results show that the addition of TAPOB can improve the comprehensive properties of BPDA/ODA PI films significantly. The existence of crosslinked structure is conductive to improve the mechanical properties, decrease the coefficient of thermal expansion (CTE) and water absorption of the film, and the micro-branched structure has a certain effect on reducing the dielectric constant.

polyimide  /  film  /  micro-branched  /  crosslink
韩书豪, 周涵, 王健华, 齐胜利, 田国峰, 武德珍. BPDA/ODA体系微支化交联聚酰亚胺薄膜制备与性能研究. 绝缘材料, 2021 , 54 (11) : 94 -99 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.013
Shuhao HAN, Han ZHOU, Jianhua WANG, Shengli QI, Guofeng TIAN, Dezhen WU. Preparation and Properties of BPDA/ODA Polyimide Films with Micro-branched Crosslinked Structure[J]. Insulating Materials, 2021 , 54 (11) : 94 -99 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.013
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0 引言
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聚酰亚胺（polyimide, PI）薄膜具有优异的力学、耐高低温、耐候、介电和高阻绝缘性能[1-2]，在绝缘和电子材料领域具有广泛应用，如挠性覆铜板、电机和变压器绝缘、柔性显示等[3-4]。在PI薄膜的应用中存在热膨胀系数（coefficient of thermal expansion, CTE）不匹配和介电常数相对偏高的问题，如制备挠性覆铜板，铜的CTE在18×10-6/K附近，而常见的PI薄膜CTE为（30～50）×10-6/K，不匹配的CTE会导致覆铜板电路的失效；大部分PI材料的介电常数在3.3～3.5（1 MHz下）[5]，偏大的介电常数会导致电阻-电容延迟和信号串扰，限制了其应用的进一步推广[6-7]。因此，如何有效降低PI薄膜的CTE和介电常数一直是PI薄膜材料的研究方向之一。目前已有若干种改进途径和方法，比如通过引入氟原子[8-10]、大体积侧基[11]和微孔[12-15]等结构降低PI薄膜的介电常数；通过引入刚性单体或者纳米填料等方式降低PI薄膜的CTE[16-18]。
然而，通常的情况是PI薄膜的CTE和介电常数二者只能平衡而难以兼顾，更难以实现二者的同步降低，这主要是由于介电常数的降低需要增大薄膜内部的自由体积分数或者微孔隙，而CTE的降低则要求薄膜具有低的自由体积分数，两者的设计思路从出发点上就是矛盾的。虽然通过引入具有强吸电子效应的氟元素也可以起到降低介电常数的作用，但是常用的含氟单体通常会因为三氟甲基带来自由体积分数和CTE的提高[19]，这为PI薄膜的高性能发展或者MPI的设计带来了一定的挑战。
针对这一问题，本课题组前期提出了一种微支化交联结构的设计思路[20-21]，利用微支化结构增加分子链之间的距离，提高自由体积分数，降低介电常数；利用交联结构限制分子链的运动，减缓自由体积受热膨胀的速率，降低CTE，从而打破介电常数和CTE的平衡关系，实现二者的同步调控。为了进一步验证这一思路的适用性，本研究采用3,3′,4,4′-联苯四甲酸二酐（BPDA）作为二酐单体，采用4,4′-二氨基二苯醚（ODA）作为二胺单体，采用1,3,5-三（4-氨基苯氧基）苯（TAPOB）作为交联剂，设计制备一系列BPDA/ODA/TAPOB体系的PI薄膜，并对其基本力学性能、介电性能、热力学性能、吸湿率等进行研究，结合之前的研究工作讨论分子链刚柔性对微支化交联结构的影响。
1 实验
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1.1 主要原材料及仪器设备
BPDA、ODA、TAPOB、N,N′-二甲基乙酰胺（DMAc）等均为市售产品；万能材料试验机，美特斯工业（中国）有限公司；Q800型动态热机械分析仪，美国TA公司；Q400型静态机械热分析仪（TMA），美国TA公司；4294A型精密阻抗分析仪，安捷伦科技（美国）有限公司；电子精密天平，梅特勒-托利多集团（METTLER TOLEDO）。
1.2 试样制备
将ODA溶解在20 mLDMAc中，在冰水浴条件下分批次加入BPDA，反应2 h后得到具有一定黏度的聚酰胺酸（PAA）溶液；将不同含量的TAPOB溶解在5 mL DMAc中，逐滴加入到PAA溶液中，继续反应10～15 min，PAA溶液黏度逐渐升高并稳定。静置消泡，在玻璃板上刮涂成膜，挥发大部分溶剂后，在程控烘箱中升温到320℃保温2 h进行热环化，得到不同TAPOB含量的PI薄膜，反应过程如图1所示，单体用量如表1所示。
1.3 测试与表征
力学性能：参考GB/T 1040.3—2006对试样的拉伸强度和断裂伸长率进行测试，初始模量由3%应变处的应力计算得到，拉伸速率为10 mm/min。
热尺寸稳定性：采用TMA仪器测试，氮气气氛，升温速率为5℃/min，取50～200℃之间的数据。
介电性能：使用4294A型精密阻抗分析仪Cp-D模式，测试得到电容和介质损耗因数随频率变化的数据，介电常数由电容值计算得到，测试频率为103～107 Hz。
热力学性能：采用DMA仪器测试得到储能模量和损耗因子（tanδ）随温度的变化，氮气气氛，温度范围为室温至450℃，频率为1 Hz。
吸水率：参考GB/T 1034—2008，计算PI薄膜在去离子水中浸泡前后质量的变化，浸泡时间为24 h。
2 结果与讨论
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2.1 力学性能
表2为不同TAPOB含量的PI薄膜力学性能测试结果。
从表2可以看出，BPDA/ODA型PI薄膜的拉伸强度为173.5 MPa，初始模量为2.96 GPa，表现出优异的力学性能。随着TAPOB含量的增加，PI薄膜的拉伸强度先增大后略微有所减小，断裂伸长率逐渐减小，初始模量逐渐增大，分析其原因是TAPOB的加入使分子链间发生了交联反应，交联结构的存在使得分子链相互作用增强，抵抗形变的能力增加。当TAPOB含量增加到单体总摩尔量的1.5%时，继续增加可能会导致局部过度交联，使得PI薄膜在受力过程中发生应力集中，不能均匀承载，导致拉伸强度减小。
2.2 热尺寸稳定性
图2为BPDA/ODA/TAPOB体系PI薄膜的TMA测试数据，由斜率计算的CTE值列于表2中。
从图2可以看出，随着TAPOB含量的增加，曲线的斜率逐渐降低，表明薄膜的CTE呈现出降低的趋势。从表2中可以更清晰地看出，BPDA/ODA体系的CTE约为40.44×10-6 K-1，当TAPOB的添加量为0.20 mmol时，薄膜的CTE降低到32.13×10-6 K-1，下降幅度约21%。结合PI薄膜初始模量和断裂伸长率的变化规律，能够佐证交联结构对分子链的限制作用。
2.3 介电性能
图3是不同TAPOB含量PI薄膜的介电谱图，在1 MHz下的介电常数与介质损耗因数列于表3中。从图3可以看出，随着测试频率的增加，所有PI薄膜的介电常数均呈现出下降的趋势，介质损耗则呈现出先平缓波动而后快速升高的现象。这与大部分PI薄膜在这一频率范围内的介电测试结果相符。值得注意的是，随着体系内TAPOB含量的增加，薄膜的介电常数并未呈现出规律性降低的趋势，只有BPDA/ODA/TAPOB-0.15体系PI薄膜的介电常数有所降低，其他体系则明显高于BPDA/ODA体系。这个结果可能与分子链的刚柔性有关。与前期研究的BPDA/PDA体系PI薄膜[17]相比，BPDA/ODA的分子链柔性有所增加，分子链的构象旋转更加容易，聚合物线团尺寸比较小，利用多官能度单体的支化作用将分子链“撑开”的效果不明显，反而更容易将分子链“拉近”，所以介电常数略有提升。
2.4 热力学性能
图4为BPDA/ODA/TAPOB体系PI薄膜的DMA谱图，储能模量和玻璃化转变温度（Tg）参数列于表4中。从图4可以看出，随着TAPOB含量的增加，PI薄膜的初始储能模量逐渐增加，与力学测试结果一致，表明材料内部交联程度提升，进一步验证了TAPOB作为交联剂构筑交联结构的作用。在玻璃化转变温度方面，该系列PI薄膜也未呈现出规律性变化的结果，这也可能是由于微支化结构的存在可以增大分子链自由体积分数，降低Tg，而交联网络则会限制分子链运动，提高Tg。受到两种因素的共同作用，Tg未表现出明显的变化规律。
2.5 吸水率
表5为BPDA/ODA/TAPOB体系PI薄膜的吸水率测试值。从表5可以看出，加入TAPOB后，PI薄膜的吸水率随TAPOB含量的增加呈现减小的趋势，这可能是由于交联程度的提高，使得水分子的渗透和扩散难度增加所致。
2.6 PI薄膜综合性能的比较
为较为直观地比较构建微支化交联结构对PI薄膜性能的影响，将以上各性能指标按照表6划分等级，PI薄膜某项性能越好，对应的等级越高。将BPDA/ODA/TAPOB-0与BPDA/ODA/TAPOB-0.15两种PI薄膜的性能作成雷达图（图5），其中实线表示BPDA/ODA体系薄膜，虚线表示BPDA/ODA/TAPOB-0.15体系PI薄膜，可以看出加入TAPOB构建微支化交联结构能够有效提升PI薄膜的综合性能，实现CTE与介电常数的同步调控。
3 结论
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（1）加入TAPOB构建微支化交联结构对PI薄膜的性能有两方面的影响：微支化结构的形成有利于提高自由体积分数，降低介电常数，但会提高CTE值；交联结构的存在可限制分子链运动，提高初始模量，降低CTE。两种结构的平衡调控可实现PI薄膜介电常数和CTE的同步降低。
（2）柔性的主链结构对支化作用的响应要弱于刚性的主链结构，相比于降低介电常数的设计目标，在柔性体系中构建微支化交联结构对降低PI薄膜的CTE值更有作用。
（3）微支化交联结构可提升PI薄膜的综合性能，BPDA/ODA/TAPOB-0.15体系的PI薄膜显示出优于纯BPDA/ODA体系PI薄膜的性质（CTE为（40.44～34.73）×10-6 K-1，介电常数为3.30～3.27），实现了PI薄膜CTE与介电常数的同步调控。
基金
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  • 国家自然科学基金资助项目(51773007)
  • 中央高校基本科研业务费专项资金项目(XK1802-2)
文献
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2021年第54卷第11期
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文章信息
doi: 10.16790/j.cnki.1009-9239.im.2021.11.013
  • 接收时间：2021-04-30
  • 首发时间：2026-03-23
  • 出版时间：2021-11-22
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  • 收稿日期：2021-04-30
  • 修回日期：2021-05-21
基金
国家自然科学基金资助项目(51773007)
中央高校基本科研业务费专项资金项目(XK1802-2)
作者信息
    北京化工大学 碳纤维及功能高分子教育部重点实验室，北京 100029

通讯作者:

田国峰（1984-），男（汉族），黑龙江伊春人，教授，主要从事高性能及功能型聚酰亚胺及其复合材料的研究。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2021.11.013
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2种不同金属材料的力学参数
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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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