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Article(id=1304923091197522089, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1304923090710982825, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2026.04.001, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1747584000000, receivedDateStr=2025-05-19, revisedDate=1749916800000, revisedDateStr=2025-06-15, acceptedDate=null, acceptedDateStr=null, onlineDate=1789047509240, onlineDateStr=2026-09-10, pubDate=1776614400000, pubDateStr=2026-04-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1789047509240, onlineIssueDateStr=2026-09-10, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1789047509240, creator=13701087609, updateTime=1789047509240, updator=13701087609, issue=Issue{id=1304923090710982825, tenantId=1146029695717560320, journalId=1149653034449285133, year='2026', volume='59', issue='4', pageStart='1', pageEnd='144', 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=1789047509124, creator='13701087609', updateTime=1789118076681, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1305219072573071941, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1304923090710982825, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1305219072573071942, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1304923090710982825, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=1, endPage=8, ext={EN=ArticleExt(id=1304923091377877162, articleId=1304923091197522089, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Study on structural design and drawing process of high heat-resistant and low thermal expansion polyimide films, columnId=1190369066675179686, journalTitle=Insulating Materials, columnName=Material Research, runingTitle=null, highlight=null, articleAbstract=

Drawing technology is one of the important methods for preparing electronic-grade polyimide (PI) films used in flexible printed circuits (FPC). Compared to single chemical structure regulation methods, drawing technology offers higher flexibility and can effectively regulate the coefficient of thermal expansion (CTE) of different systems of PI films over a wide range. However, in the pursuit of high glass transition temperature (Tg), monomers with rigid property and hydrogen bond are often partially or fully employed, leading to reduced molecular chain mobility and impairing the drawing processability. This paper addressed the challenging contradiction between the high glass transition temperature (Tg) of polyimide (PI) films and their drawing processability. Taking pyromellitic dianhydride (PMDA) and 4,4′-diaminodiphenyl ether (ODA) as basic system, a series of homopolymer and copolymer PI films were designed and prepared by introducing p-phenylenediamine (p-PDA), 2,5-dimethy-phenylenediamine (DPD), and m-phenylenediamine (m-PDA). Through molecular simulation and experimental analysis, the effects of the main chain structure on its segment mobility and drawing process were studied systematically. The results show that the introduction of m-PDA can simultaneously improve the rigidity of PI molecular chains in the PMDA/ODA system below Tg and the mobility above Tg, thereby enabling it to have a high Tg and excellent drawing processability. By employing DMA for high-temperature drawing and orientation of this system film, PI film samples with high Tg (about 428℃) and CTE-adjustable (1.7×10-6-34.1×10-6℃-1) were successfully prepared.

, authors=Jianhua WANG, Gaojie WU, Hongjie XU, Guofeng TIAN, Shengli QI, Dezhen WU*, authorsList=Jianhua WANG, Gaojie WU, Hongjie XU, Guofeng TIAN, Shengli QI, Dezhen WU, authorCompany=null, correspAuthors=Dezhen WU, 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=1304923092858466487, articleId=1304923091197522089, tenantId=1146029695717560320, journalId=1149653034449285133, language=CN, title=高耐热低膨胀聚酰亚胺薄膜结构设计与牵伸工艺研究, columnId=1190369066813591720, journalTitle=绝缘材料, columnName=材料研究, runingTitle=null, highlight=null, articleAbstract=

牵伸技术是制备柔性印刷电路板（FPC）用电子级聚酰亚胺（PI）薄膜的重要方法之一。相较于单一的化学结构调控法，牵伸技术具有更高的灵活性，可在大范围内有效调控不同体系PI薄膜的热膨胀系数（CTE）。然而，在追求高玻璃化转变温度（Tg）时通常部分或全部采用具有刚直、含氢键等特征的单体，导致分子链运动能力降低，损害牵伸工艺性。本文针对PI薄膜高玻璃化转变温度（Tg）与牵伸工艺性之间的矛盾难题，以均苯四甲酸二酐（PMDA）和二氨基二苯醚（ODA）为基础体系，通过引入对苯二胺（p-PDA）、2,5-二甲基对苯二胺（DPD）和间苯二胺（m-PDA），设计制备一系列均聚和共聚体系PI薄膜。通过分子模拟和实验分析，系统研究了主链结构对其链段运动能力和牵伸工艺的影响。结果表明：m-PDA的引入可以同步提高PMDA/ODA体系PI分子链在Tg以下的刚性和Tg以上的运动能力，从而使其具有高Tg和良好的牵伸工艺性能；采用DMA对该体系薄膜进行高温牵伸取向，成功制备出高Tg（约为428℃）和CTE可调（1.7×10-6～34.1×10-6℃-1）的PI薄膜样品。

, authors=王健华, 吴高洁, 徐鸿杰, 田国峰, 齐胜利, 武德珍*, authorsList=王健华, 吴高洁, 徐鸿杰, 田国峰, 齐胜利, 武德珍, authorCompany=null, correspAuthors=武德珍, authorNote=

王健华（1991-），男（汉族），河北沧州人，博士生，主要从事高尺寸稳定性聚酰亚胺薄膜牵伸加工工艺的研究

田国峰（1984-），男（汉族），黑龙江伊春人，教授，主要从事聚酰亚胺材料结构设计与合成制备的研究；

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武德珍（1963-），女（汉族），北京人，教授，主要从事聚酰亚胺材料合成与制备、塑料改性等研究。
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王健华（1991-），男（汉族），河北沧州人，博士生，主要从事高尺寸稳定性聚酰亚胺薄膜牵伸加工工艺的研究

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王健华（1991-），男（汉族），河北沧州人，博士生，主要从事高尺寸稳定性聚酰亚胺薄膜牵伸加工工艺的研究

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田国峰（1984-），男（汉族），黑龙江伊春人，教授，主要从事聚酰亚胺材料结构设计与合成制备的研究；

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田国峰（1984-），男（汉族），黑龙江伊春人，教授，主要从事聚酰亚胺材料结构设计与合成制备的研究；

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Journal of Thermal Analysis and Calorimetry,2000,60(2):377-390., articleTitle=Determination of activation energy for glass transition of an epoxy adhesive using dynamic mecha-nical analysis, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1304923093105930424, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, xref=null, ext=[AuthorCompanyExt(id=1304923093118513337, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, companyId=1304923093105930424, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Key Laboratory of Carbon Fiber and Functional Polymers, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029, China), AuthorCompanyExt(id=1304923093126901946, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, companyId=1304923093105930424, 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=1304923095307940065, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Fig.1, caption=Geometric structures and electrostatic potential distributions of different PI structural units, figureFileSmall=ezEOh9B4zAjNlF5ZuasyMA==, figureFileBig=zl1XwtCOLmw4X/wj1ukbCg==, tableContent=null), ArticleFig(id=1304923095442157794, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=图1, caption=不同体系PI结构单元的几何结构及静电势分布, figureFileSmall=ezEOh9B4zAjNlF5ZuasyMA==, figureFileBig=zl1XwtCOLmw4X/wj1ukbCg==, tableContent=null), ArticleFig(id=1304923095622512867, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Fig.2, caption=The relationship between rotational energy and rotational angle, figureFileSmall=F+RuHQ8EzuHCv/B8LdBeLg==, figureFileBig=RLer4YK/O9c51Nnd0qH/LQ==, tableContent=null), ArticleFig(id=1304923095710593252, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=图2, caption=旋转能量与旋转角的关系, figureFileSmall=F+RuHQ8EzuHCv/B8LdBeLg==, figureFileBig=RLer4YK/O9c51Nnd0qH/LQ==, tableContent=null), ArticleFig(id=1304923095765119205, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Fig.3, caption=DMA curves of different PI films, figureFileSmall=9SlYwPZNxkaay9yb4am0CQ==, figureFileBig=Tfu/gd430a8T2uwsgh1XXQ==, tableContent=null), ArticleFig(id=1304923095823839462, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=图3, caption=不同PI薄膜的DMA曲线, figureFileSmall=9SlYwPZNxkaay9yb4am0CQ==, figureFileBig=Tfu/gd430a8T2uwsgh1XXQ==, tableContent=null), ArticleFig(id=1304923095890948327, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Fig.4, caption=Activation energy of glass transition of different PI films, figureFileSmall=EDV0Vd3p5wce5nVFMi1gtQ==, figureFileBig=+YfPW2ru9r8jke8cfCOmqw==, tableContent=null), ArticleFig(id=1304923095958057192, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=图4, caption=不同PI薄膜的玻璃化转变活化能, figureFileSmall=EDV0Vd3p5wce5nVFMi1gtQ==, figureFileBig=+YfPW2ru9r8jke8cfCOmqw==, tableContent=null), ArticleFig(id=1304923096016777449, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Fig.5, caption=TGA curves of different PI films under inert atmosphere, figureFileSmall=gH37mgQ/DjZXZHfOBaa9Lg==, figureFileBig=QwAi4z79nt/Tpyo2KrY/Ng==, tableContent=null), ArticleFig(id=1304923096083886314, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=图5, caption=不同PI薄膜在惰性气氛中的热失重曲线

(a) PMDA/ODA/p-PDA体系 (b) PMDA/ODA/DPD体系 (c) PMDA/ODA/m-PDA体系

, figureFileSmall=gH37mgQ/DjZXZHfOBaa9Lg==, figureFileBig=QwAi4z79nt/Tpyo2KrY/Ng==, tableContent=null), ArticleFig(id=1304923096150995179, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Fig.6, caption=Stress-strain curves of different PI films at 420℃, figureFileSmall=6oQS4JtfDvJ1LV7hSBGB8Q==, figureFileBig=FscFREhhOmQ94vge/2kvDw==, tableContent=null), ArticleFig(id=1304923096230686956, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=图6, caption=不同PI薄膜在420℃条件下的应力-应变曲线，

(a) PMDA/ODA/p-PDA体系 (b) PMDA/ODA/DPD体系 (c) PMDA/ODA/m-PDA体系

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The names, systems, and monomer molar amounts used for preparation of different PI film samples

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试样名称体系名称单体用量/mol
PMDAODAPDADPDm-PDA
p-PDA-10PMDA/ODA/p-PDA0.100 50.090.01——
p-PDA-300.100 50.070.03——
p-PDA-500.100 50.050.05——
DPD-10PMDA/ODA/DPD0.100 50.09—0.01—
DPD-300.100 50.07—0.03—
DPD-500.100 50.05—0.05—
m-PDA-10PMDA/ODA/m-PDA0.100 50.09——0.01
m-PDA-300.100 50.07——0.03
m-PDA-500.100 50.05——0.05
), ArticleFig(id=1304923096364904686, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=表1, caption=

不同PI薄膜试样的名称、所属体系及制备所用单体摩尔量

, figureFileSmall=null, figureFileBig=null, tableContent=
试样名称体系名称单体用量/mol
PMDAODAPDADPDm-PDA
p-PDA-10PMDA/ODA/p-PDA0.100 50.090.01——
p-PDA-300.100 50.070.03——
p-PDA-500.100 50.050.05——
DPD-10PMDA/ODA/DPD0.100 50.09—0.01—
DPD-300.100 50.07—0.03—
DPD-500.100 50.05—0.05—
m-PDA-10PMDA/ODA/m-PDA0.100 50.09——0.01
m-PDA-300.100 50.07——0.03
m-PDA-500.100 50.05——0.05
), ArticleFig(id=1304923096457179375, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Table 2, caption=

Thermal performance parameters of different PI films

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试样名称Tonset/℃Tpeak/℃VpeakTd0.1/℃Td1/℃Td5/℃CTE/(×10-6℃-1)
p-PDA-10365.7397.20.323439527.8565.234.2
p-PDA-30370.1421.20.251441534.1571.327.7
p-PDA-50372.2448.90.148438533.3577.213.8
DPD-10379.1414.00.318435500.7547.331.4
DPD-30382.0446.70.231416475.7532.224.2
DPD-50391.9458.80.119420474.1529.721.2
m-PDA-10384.6414.40.358443524.4564.035.1
m-PDA-30397.0421.60.522438514.9559.734.5
m-PDA-50406.5428.40.746437523.9566.234.1
), ArticleFig(id=1304923096566231280, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=表2, caption=

不同PI薄膜的热性能参数

, figureFileSmall=null, figureFileBig=null, tableContent=
试样名称Tonset/℃Tpeak/℃VpeakTd0.1/℃Td1/℃Td5/℃CTE/(×10-6℃-1)
p-PDA-10365.7397.20.323439527.8565.234.2
p-PDA-30370.1421.20.251441534.1571.327.7
p-PDA-50372.2448.90.148438533.3577.213.8
DPD-10379.1414.00.318435500.7547.331.4
DPD-30382.0446.70.231416475.7532.224.2
DPD-50391.9458.80.119420474.1529.721.2
m-PDA-10384.6414.40.358443524.4564.035.1
m-PDA-30397.0421.60.522438514.9559.734.5
m-PDA-50406.5428.40.746437523.9566.234.1
), ArticleFig(id=1304923096645923057, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=EN, label=Table 3, caption=

Mechanical properties, orientation degree, and CTE of m-PDA-50 PI films with different draw ratios

, figureFileSmall=null, figureFileBig=null, tableContent=
牵伸比/%模量/GPa断裂强度/MPa断裂伸长率/%CTE/(×10-6℃-1)取向度
01.65119.240.334.10.017 8
252.20168.739.828.10.094 9
502.69182.435.719.40.176 3
753.22201.733.210.80.251 5
1003.70210.930.11.70.336 5
), ArticleFig(id=1304923096721420530, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1304923091197522089, language=CN, label=表3, caption=

m-PDA-50 PI薄膜的力学性能、取向度和CTE随牵伸比的变化

, figureFileSmall=null, figureFileBig=null, tableContent=
牵伸比/%模量/GPa断裂强度/MPa断裂伸长率/%CTE/(×10-6℃-1)取向度
01.65119.240.334.10.017 8
252.20168.739.828.10.094 9
502.69182.435.719.40.176 3
753.22201.733.210.80.251 5
1003.70210.930.11.70.336 5
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高耐热低膨胀聚酰亚胺薄膜结构设计与牵伸工艺研究
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王健华 , 吴高洁 , 徐鸿杰 , 田国峰 , 齐胜利 , 武德珍 *
绝缘材料 | 材料研究 2026,59(4): 1-8
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绝缘材料 |材料研究 2026 , 59 (4) : 1 -8
高耐热低膨胀聚酰亚胺薄膜结构设计与牵伸工艺研究
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王健华, 吴高洁, 徐鸿杰, 田国峰, 齐胜利, 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
通讯作者:
武德珍（1963-），女（汉族），北京人，教授，主要从事聚酰亚胺材料合成与制备、塑料改性等研究。
作者简介:

王健华（1991-），男（汉族），河北沧州人，博士生，主要从事高尺寸稳定性聚酰亚胺薄膜牵伸加工工艺的研究

田国峰（1984-），男（汉族），黑龙江伊春人，教授，主要从事聚酰亚胺材料结构设计与合成制备的研究；

Study on structural design and drawing process of high heat-resistant and low thermal expansion polyimide films
Jianhua WANG, Gaojie WU, Hongjie XU, Guofeng TIAN, Shengli QI, Dezhen WU*
Affiliations
  • Key Laboratory of Carbon Fiber and Functional Polymers, Ministry of Education, Beijing University of Chemical Technology, Beijing 100029, China
出版时间: 2026-04-20 doi: 10.16790/j.cnki.1009-9239.im.2026.04.001
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牵伸技术是制备柔性印刷电路板（FPC）用电子级聚酰亚胺（PI）薄膜的重要方法之一。相较于单一的化学结构调控法，牵伸技术具有更高的灵活性，可在大范围内有效调控不同体系PI薄膜的热膨胀系数（CTE）。然而，在追求高玻璃化转变温度（Tg）时通常部分或全部采用具有刚直、含氢键等特征的单体，导致分子链运动能力降低，损害牵伸工艺性。本文针对PI薄膜高玻璃化转变温度（Tg）与牵伸工艺性之间的矛盾难题，以均苯四甲酸二酐（PMDA）和二氨基二苯醚（ODA）为基础体系，通过引入对苯二胺（p-PDA）、2,5-二甲基对苯二胺（DPD）和间苯二胺（m-PDA），设计制备一系列均聚和共聚体系PI薄膜。通过分子模拟和实验分析，系统研究了主链结构对其链段运动能力和牵伸工艺的影响。结果表明：m-PDA的引入可以同步提高PMDA/ODA体系PI分子链在Tg以下的刚性和Tg以上的运动能力，从而使其具有高Tg和良好的牵伸工艺性能；采用DMA对该体系薄膜进行高温牵伸取向，成功制备出高Tg（约为428℃）和CTE可调（1.7×10-6～34.1×10-6℃-1）的PI薄膜样品。

电子级PI薄膜  /  牵伸工艺  /  玻璃化转变温度  /  热膨胀系数

Drawing technology is one of the important methods for preparing electronic-grade polyimide (PI) films used in flexible printed circuits (FPC). Compared to single chemical structure regulation methods, drawing technology offers higher flexibility and can effectively regulate the coefficient of thermal expansion (CTE) of different systems of PI films over a wide range. However, in the pursuit of high glass transition temperature (Tg), monomers with rigid property and hydrogen bond are often partially or fully employed, leading to reduced molecular chain mobility and impairing the drawing processability. This paper addressed the challenging contradiction between the high glass transition temperature (Tg) of polyimide (PI) films and their drawing processability. Taking pyromellitic dianhydride (PMDA) and 4,4′-diaminodiphenyl ether (ODA) as basic system, a series of homopolymer and copolymer PI films were designed and prepared by introducing p-phenylenediamine (p-PDA), 2,5-dimethy-phenylenediamine (DPD), and m-phenylenediamine (m-PDA). Through molecular simulation and experimental analysis, the effects of the main chain structure on its segment mobility and drawing process were studied systematically. The results show that the introduction of m-PDA can simultaneously improve the rigidity of PI molecular chains in the PMDA/ODA system below Tg and the mobility above Tg, thereby enabling it to have a high Tg and excellent drawing processability. By employing DMA for high-temperature drawing and orientation of this system film, PI film samples with high Tg (about 428℃) and CTE-adjustable (1.7×10-6-34.1×10-6℃-1) were successfully prepared.

electronic-grade PI film  /  drawing process  /  glass transition temperature  /  coefficient of thermal expansion
王健华, 吴高洁, 徐鸿杰, 田国峰, 齐胜利, 武德珍. 高耐热低膨胀聚酰亚胺薄膜结构设计与牵伸工艺研究. 绝缘材料, 2026 , 59 (4) : 1 -8 . DOI: 10.16790/j.cnki.1009-9239.im.2026.04.001
Jianhua WANG, Gaojie WU, Hongjie XU, Guofeng TIAN, Shengli QI, Dezhen WU. Study on structural design and drawing process of high heat-resistant and low thermal expansion polyimide films[J]. Insulating Materials, 2026 , 59 (4) : 1 -8 . DOI: 10.16790/j.cnki.1009-9239.im.2026.04.001
正文
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0　引言
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聚酰亚胺（PI）材料因其刚性的芳杂环结构而具有优异的耐高低温、耐辐照、耐腐蚀和低介电、高绝缘等性能特点，在电工电子、航空航天等领域具有重要应用[1-3]。尤其是电子级PI薄膜，其既保留了PI材料突出的耐高温性能[4]，还因牵伸工艺实现了低热膨胀系数（CTE）和低收缩率等特点。电子级PI薄膜既可以抵御锡焊加工时的瞬时高温，还可以避免因环境温度变化导致的应力开裂等问题，满足长期使用的可靠性要求[5]，因而成为柔性印刷电路板（FPC）的核心基体材料。
低CTE的本质是链段的面内取向对体膨胀系数（CVE）的重新分配[6-7]，这一过程常发生于聚酰胺酸（PAA）薄膜的干燥阶段和酰亚胺化的反应阶段[8-9]，由于薄膜体积大幅收缩而面积并未减小，产生等效面内牵伸[10]，从而导致面内取向度增加、CTE降低[11]。通过化学结构设计提高分子链的刚性和线性度有利于提高其在上述过程中的自发面内取向和规整性[12]，如引入高刚性单体和含有曲柄轴结构的单体等[13-14]。但该方法需要合成新的结构单体，存在制备难度高、工程周期长等问题[15]。牵伸加工是提高PI分子链取向度，实现其低CTE的重要途径。为了尽量提高PI薄膜的取向度、消除内应力，必须在高于其玻璃化转变温度（Tg）的温度下进行牵伸[16]。但PI薄膜的Tg较高（高于350℃），分子链间相互作用力较强，分子链运动能力较低，导致其牵伸应力增大，工艺难度提高[17]。本课题组前期研究显示，可以利用非线性刚性单体的刚性结构保证PI薄膜优异的耐高温性能，同时利用其非线性结构提高加工工艺性能[18]，为高Tg PI薄膜的牵伸加工提供了新的结构设计思路。
本研究以均苯四甲酸二酐（PMDA）和4,4′-二氨基二苯醚（ODA）为基础体系，通过引入对苯二胺（p-PDA）、2,5-二甲基对苯二胺（DPD）和间苯二胺（m-PDA），设计制备一系列均聚和共聚体系PI薄膜，系统研究主链结构特征对其链段运动能力和牵伸工艺性能的影响，并以PMDA/50ODA/50m-PDA体系为研究对象，分析牵伸工艺对薄膜力学性能和热膨胀系数的影响，以期为电子级PI薄膜的结构调控和双拉工艺优化提供新的设计思路和解决方案。
1　实验
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1.1　主要原料和试剂
均苯四甲酸二酐（PMDA，纯度为99%）、4,4′-二氨基二苯醚（ODA，纯度为99.8%）、对苯二胺（p-PDA，纯度为99.9%）、2,5-二甲基对苯二胺（DPD，纯度为98%）、间苯二胺（m-PDA，纯度为99%），福斯曼（北京）科技有限公司；N,N′-二甲基乙酰胺（DMAC），分析纯，福晨（天津）化学试剂有限公司。
1.2　PI薄膜制备
不同PI薄膜试样的名称、所属体系及制备所用单体摩尔量如表1所示。以m-PDA-50 PI薄膜为例，具体制备方法如下：将ODA（0.05 mol）与m-PDA（0.05 mol）加入三口烧瓶中，然后加入溶剂DMAC并充分搅拌，待物质完全溶解后分批加入PMDA（0.100 5 mol），在冰水浴条件搅拌约5 h，得到固含量为10%的PAA溶液。将PAA溶液涂覆于玻璃板上并置于水平超净台中自然干燥得到PAA薄膜。将干燥后的PAA薄膜用方形金属框架固定，在程控烘箱中以2℃/min的速率升温至380℃并保温0.5 h，得到PI薄膜试样（m-PDA-50），其厚度约为40 μm。
1.3　 m-PDA-50 PI薄膜高温牵伸处理
将PI薄膜裁成哑铃型样条，中间矩形段宽度为3 mm、长度为10 mm（标距），将其置于动态热机械分析仪（DMA，型号为D850，美国TA公司）中进行高温牵伸处理。在氮气气氛下，以20℃/min的速率升温至420℃，待温度波动小于0.1℃时，以20%/min的应变速率拉伸至不同的预设牵伸比（0%、25%、50%、75%、100%）。牵伸比定义为样条的长度增量与原始标距的比值。
1.4　测试与表征
采用DMA对试样进行高温力学性能测试，试样为哑铃状样条（中间受力区域长×宽=10 mm×3 mm）。在氮气气氛下，以20℃/min的速率升温至420℃，待温度波动小于0.1℃时，以20%/min应变速率拉伸至试样断裂或达到设备的行程极限，并绘制应力-应变曲线。
采用偏振全反射红外光谱仪（FTIR，型号为is-5，美国赛默飞公司）测试薄膜的取向度（P），计算公式如式（1）所示[19]。以牵伸方向为平行方向，采用羰基的对称振动峰作为二色比（R）的计算依据，以苯环的红外峰面积作为内参。二色比R的计算如式（2）所示。
P=C×R-1R+2
式（1）中：常数项C的值与被观察基团有关，根据文献[19]，羰基对称振动峰对应C值为-2.769；R为二色比。
R=A///A//,benzA⊥/A⊥,benz
式（2）中：A//和A⊥分别为羰基对称振动峰在平行方向和垂直方向上的吸光度；A//,benz和A⊥,benz分别为苯环振动峰在平行方向和垂直方向上的吸光度。
采用万能材料试验机（型号为3365，美国 Instrong公司）测试经高温牵伸处理之后薄膜的力学性能，根据1.3中拉伸试样的牵伸比对各试样的标距和横截面积进行修正，以20%/min的应变速率拉伸。
采用静态热机械分析仪（TMA，型号为Q400EM，美国TA公司）测试薄膜的CTE，以50 mL/min的流速通入氮气，载荷为0.05 N，升温速率为5℃/min，在第2次升温过程中计算温度为0～200℃的平均CTE。
采用DMA测试薄膜的Tg，在氮气气氛下，以3℃/min的升温速率由室温升温至500℃，同时施加0.1%/1 Hz的正弦应变。
采用热失重分析仪（TGA，型号为Q50，美国TA公司）测试薄膜的热稳定性，以50 mL/min的速率通入氮气，首先在150℃保温30 min以去除水分，自然冷却至35℃后，以10℃/min的升温速率升温至900℃。
采用Material Studio软件绘制包含2个二酐和1个二胺的结构单元，通过Dmol3模块进行几何优化、计算静电势并绘制静电势分布图。绘制包含1个PMDA和1个m-PDA的结构单元，采用Conformers工具计算酰亚胺环在围绕C-N键发生相对于 m-PDA旋转时的能量曲线。绘制包含1个ODA的结构单元，将一侧苯环设置为与C-O-C共平面，采用Conformers工具计算另一侧苯环围绕C-O键旋转时的能量曲线。
2　结果与讨论
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2.1　主链几何结构特征与构象转变能力
不同体系PI链段的几何结构及静电势分布如图1所示。从图1可以看出，PMDA/ODA和PMDA/ODA/m-PDA体系的分子链表现出较大的弯曲程度，当薄膜受到外力牵伸作用时，PMDA/ODA的分子链可以通过ODA中醚键的旋转改变构象；PMDA/ODA/m-PDA则可以通过酰亚胺环相对于m-PDA中苯环的旋转改变构象。相比而言，PMDA/ODA/p-PDA体系和PMDA/ODA/DPD体系则具有较高的线性度，不利于牵伸时的构象转变。
静电势分布反映了静电力的作用范围与正负电性。对于ODA结构单元，当一侧苯环与醚键共平面时，其静电力的作用范围会向另一侧苯环靠近。在此情况下，另一侧苯环在围绕C-O键旋转时，极易出现两侧苯环静电力（同为正电性）作用范围高度重叠的现象，这在一定程度提高了苯环构象转变的难度。对于p-PDA和m-PDA结构单元，C-N键邻位的氢原子与羰基氧距离适中，且电性相反，使得PMDA与p-PDA或m-PDA之间在围绕C-N键发生相对旋转时的阻力较小。对于DPD结构单元，其在p-PDA的C-N键邻位增加了侧甲基，由于甲基与羰基氧距离过近，PMDA与DPD之间的相对旋转受到限制，也不利于构象转变。
在忽略链段之间空间位阻效应的前提下，通过分子模拟计算了m-PDA和ODA两种结构单元在分子链旋转过程中的能量变化，结果如图2所示。从图2可以看出，在m-PDA结构单元中，酰亚胺环在围绕C-N键发生相对于m-PDA的旋转时，最高能垒仅为3.27 kcal/mol，展现出卓越的构象转变能力。在ODA结构单元中，当一侧苯环与醚键共平面时，另一侧苯环围绕C-O键的旋转引起了极大的能量变化，能垒超过了21 000 kcal/mol，严重限制了ODA的旋转自由度，进而削弱了链段协同运动的能力[20]。
因此，以上4个体系的结构和运动特点可总结为：PMDA/ODA/DPD体系表现为高线性度且相对旋转严重受限，PMDA/ODA/p-PDA体系表现为高线性度但相对旋转容易，PMDA/ODA体系表现为较高的弯曲程度和相对旋转受限，PMDA/ODA/m-PDA体系表现为较高的弯曲程度且相对旋转容易。
2.2　玻璃化转变温度与链段运动能力
Tg是表征材料耐热性能的重要指标，同时也是牵伸加工温度的重要参考。不同PI薄膜试样的DMA曲线如图3所示，相关特征温度列于表2。其中，储能模量的起始转变温度（Tonset）表示材料开始从较为刚硬的玻璃态向较为柔软的橡胶态转变；损耗因子曲线的峰值温度（Tpeak）和峰值（Vpeak）很大程度上反映了材料的阻尼性能，表征链段在Tg以上温度的运动能力。从图3和表2可以看出，随着p-PDA或DPD比例的提高，PI薄膜的储能模量曲线逐渐向上移动，表明分子链的刚性增加；Vpeak大幅降低，表明链段在Tg以上温度的运动能力降低；Tonset和Tpeak向高温方向移动，表明材料的耐热性能提高。这些性能变化与p-PDA和OPD刚直性的主链结构特征相符。引入m-PDA后，由于m-PDA中的苯环具有较大的尺寸，并向链段外侧大幅度延伸，导致其构象的改变极易受到邻侧链段的空间位阻效应影响，使其分子链在紧密堆积的情况下表现出刚性，而非2.1节中描述的柔性特征。因此，随着m-PDA比例的提高，PI薄膜在Tonset及其以下的储能模量提高。然而，当分子链堆积松散时，空间位阻效应的减弱使m-PDA构象在转变时更接近2.1节中的单分子链的情形，具有显著的柔性特征。因此，在Tg以上的温度区间，随着m-PDA比例的提高，PI薄膜的储能模量大幅降低，最低仅为32 MPa；Vpeak大幅提高，最高达到0.746，表明m-PDA的引入改善了分子链在Tg以上的运动能力。
根据式（3）可计算不同体系PI薄膜的玻璃化转变活化能[21]，结果如图4所示。
∆E=-Rd(lnf)d(1/Tg)
式（3）中：ΔE为活化能；R为气体常数；f为频率。
从图4可以看出，p-PDA和DPD的加入导致薄膜的玻璃化转变活化能升高。采用线性拟合的方法可以计算每加入10份p-PDA或DPD，玻璃化转变活化能分别增加约263.3 kJ/mol和544.3 kJ/mol。玻璃化转变活化能的升高表明分子链协同运动需要更多的能量，将显著提高薄膜的牵伸难度。与p-PDA和DPD相反，m-PDA的加入可以有效降低薄膜的玻璃化转变活化能，每加入10份m-PDA，薄膜的玻璃化转变活化能降低约49.1 kJ/mol，表明PMDA/ODA/m-PDA体系在Tg以上可表现出优于PMDA/ODA体系的运动能力。因此，m-PDA的引入同时实现了在Tg以下分子链的高刚性和Tg以上分子链的高运动能力，这种特性有利于在实现PI薄膜高Tg的同时提高其牵伸工艺性能。
热分解温度是决定加工温度上限的重要依据，不同体系PI薄膜试样的热失重曲线及相关数据如图5和表2所示。由表2可知，PMDA/ODA/p-PDA和PMDA/ODA/m-PDA体系PI薄膜表现出较高的热分解温度，0.1%分解温度（Td0.1）均超过430℃。对于PMDA/ODA/DPD体系PI薄膜，随着DPD含量的提高，Td0.1整体呈降低趋势，最低为416℃，这可能与DPD侧甲基的低热稳定性有关。
2.3　牵伸工艺对PI薄膜力学性能和CTE的影响
断裂伸长率是材料力学性能的重要指标，它反映了材料在受力条件下的变形能力。综合考虑Tg与Td0.1，确定以420℃为薄膜的牵伸温度，通过DMA测试得到该温度下不同PI薄膜试样的应力-应变曲线，结果如图6所示。从图6可以看出，PMDA/ODA/DPD体系由于高刚性结构和侧甲基的空间位阻效应表现出最低的断裂伸长率；PMDA/ODA/p-PDA体系和PMDA/ODA/m-PDA体系均表现出较高的断裂伸长率，但PMDA/ODA/m-PDA体系具有更低的牵伸应力，且随着m-PDA含量的增加，应力-应变曲线的高度逐渐降低，呈现出“软而韧”的力学特性。以上结果表明，PMDA/ODA/m-PDA体系可以更好地满足薄膜牵伸工艺要求，为此选择m-PDA-50PI薄膜进行后续牵伸取向与性能关系研究。
以m-PDA-50 PI薄膜为研究对象，在420℃条件下进行牵伸处理，研究了牵伸比对薄膜取向度、CTE以及力学性能的影响，结果如表3所示。从表3可以看出，随着牵伸比的提高，薄膜的取向度呈升高趋势，CTE呈降低趋势。其中，CTE由未牵伸时的34.1×10-6℃-1降低至牵伸比为100%时的1.7×10-6℃-1。在力学性能方面，随着牵伸比的提高，薄膜的模量和断裂强度提高，断裂伸长率降低。模量和断裂强度分别由未牵伸时的1.65 GPa和119.2 MPa提高至牵伸比为100%时的3.7 GPa和210.9 MPa，断裂伸长率由未牵伸时的40.3%降低至牵伸比为100%时的30.1%。
3　结论
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（1）本文利用非线性刚性单体（m-PDA），以传统的PMDA/ODA体系为基础，通过热酰亚胺化法成功制备了兼具高Tg和良好牵伸工艺性的高耐热低膨胀PI薄膜，该薄膜在420℃条件下表现出极高的断裂伸长率和较低的应力，有希望满足高温条件下的牵伸加工要求。
（2）m-PDA-50 PI薄膜Tg达到428℃，经高温牵伸处理后，其CTE可在1.7×10-6～34.1×10-6℃-1之间调控，同时表现出优异的力学性能。

文献
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2026年第59卷第4期
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doi: 10.16790/j.cnki.1009-9239.im.2026.04.001
  • 接收时间：2025-05-19
  • 首发时间：2026-09-10
  • 出版时间：2026-04-20
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  • 收稿日期：2025-05-19
  • 修回日期：2025-06-15
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    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

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武德珍（1963-），女（汉族），北京人，教授，主要从事聚酰亚胺材料合成与制备、塑料改性等研究。
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2种不同金属材料的力学参数
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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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