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Article(id=1203281640601657849, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1203281635908231645, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2025.06.005, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1727452800000, receivedDateStr=2024-09-28, revisedDate=1732464000000, revisedDateStr=2024-11-25, acceptedDate=null, acceptedDateStr=null, onlineDate=1764814299011, onlineDateStr=2025-12-04, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1764814299011, onlineIssueDateStr=2025-12-04, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1764814299011, creator=13701087609, updateTime=1764814299011, 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=35, endPage=42, ext={EN=ArticleExt(id=1203281640903647747, articleId=1203281640601657849, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Synthesis of PTFE/FPI fluoropolyimide composite films and their dielectric properties under high frequency working conditions, columnId=1203281640207393262, journalTitle=Insulating Materials, columnName=Special Issue on High Performance Polyimide Materials, runingTitle=null, highlight=

To develop polyimide (PI)-based composite films with low dielectric constant (Dk), low dielectric loss (Df), and high temperature resistance at high frequency, a water-soluble polyamic salt (PAAS) was prepared by adding organic base into the polyamic acid, which is the precursor of fluoropolyimide (FPI), and composite films were prepared by compounding low dielectric polytetrafluoroethylene (PTFE) concentrated dispersion with the dried PAAS to form a water dispersion system. The effects of PTFE content on the dielectric, thermal, and mechanical properties of the composite films were studied. The experimental results show that with the increase of PTFE content, the dielectric constant of the composite films decreases continuously, but there will be some effects on the thermal stability and mechanical properties. The dielectric constant of 50%PTFE/FPI reaches the minimum value (Dk=1.5@8.5 GHz), and the dielectric loss of 10%PTFE/FPI in the frequency band of 9.25-10.25 GHz is less than 0.005. The glass transition temperature of the composite films is in the range of 289-297℃, and the thermal decomposition temperature at 5% is higher than 508℃. The thermal expansion coefficient of 40%PTFE/FPI is as low as 59.67×10-6 K-1. The tensile strength of 20%PTFE/FPI is 70 MPa, the tensile modulus is 1.59 GPa, and the elongation at break is 7.7%.

, articleAbstract=

To develop polyimide (PI)-based composite films with low dielectric constant (Dk), low dielectric loss (Df), and high temperature resistance at high frequency, a water-soluble polyamic salt (PAAS) was prepared by adding organic base into the polyamic acid, which is the precursor of fluoropolyimide (FPI), and composite films were prepared by compounding low dielectric polytetrafluoroethylene (PTFE) concentrated dispersion with the dried PAAS to form a water dispersion system. The effects of PTFE content on the dielectric, thermal, and mechanical properties of the composite films were studied. The experimental results show that with the increase of PTFE content, the dielectric constant of the composite films decreases continuously, but there will be some effects on the thermal stability and mechanical properties. The dielectric constant of 50%PTFE/FPI reaches the minimum value (Dk=1.5@8.5 GHz), and the dielectric loss of 10%PTFE/FPI in the frequency band of 9.25-10.25 GHz is less than 0.005. The glass transition temperature of the composite films is in the range of 289-297℃, and the thermal decomposition temperature at 5% is higher than 508℃. The thermal expansion coefficient of 40%PTFE/FPI is as low as 59.67×10-6 K-1. The tensile strength of 20%PTFE/FPI is 70 MPa, the tensile modulus is 1.59 GPa, and the elongation at break is 7.7%.

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为开发在高频工况下兼具低介电常数（Dk）、低介电损耗（Df）和耐高温性的聚酰亚胺（PI）基复合薄膜，在制备含氟聚酰亚胺（FPI）的前驱体聚酰胺酸中加入有机碱，制得水溶性聚酰胺酸盐（PAAS），采用低介电聚四氟乙烯（PTFE）浓缩分散液与干燥后的PAAS进行复合形成水分散体系制备PTFE/FPI复合薄膜，通过改变PTFE含量，研究其对复合薄膜介电性能、耐热性能和力学性能的影响。结果表明：随着PTFE含量的增加，复合薄膜的Dk不断降低，但对热稳定性和力学性能会有一定影响。50%PTFE/FPI的Dk达到最小值（Dk=1.5@8.5 GHz），10%PTFE/FPI在9.25～10.25 GHz频段内的Df小于0.005，系列复合薄膜的玻璃化转变温度为289～297℃，5%热分解温度大于508℃，40%PTFE/FPI的热膨胀系数低至59.67×10-6 K-1，20%PTFE/FPI的拉伸强度为70 MPa，拉伸模量为1.59 GPa，断裂伸长率为7.7%。

, articleAbstract=

为开发在高频工况下兼具低介电常数（Dk）、低介电损耗（Df）和耐高温性的聚酰亚胺（PI）基复合薄膜，在制备含氟聚酰亚胺（FPI）的前驱体聚酰胺酸中加入有机碱，制得水溶性聚酰胺酸盐（PAAS），采用低介电聚四氟乙烯（PTFE）浓缩分散液与干燥后的PAAS进行复合形成水分散体系制备PTFE/FPI复合薄膜，通过改变PTFE含量，研究其对复合薄膜介电性能、耐热性能和力学性能的影响。结果表明：随着PTFE含量的增加，复合薄膜的Dk不断降低，但对热稳定性和力学性能会有一定影响。50%PTFE/FPI的Dk达到最小值（Dk=1.5@8.5 GHz），10%PTFE/FPI在9.25～10.25 GHz频段内的Df小于0.005，系列复合薄膜的玻璃化转变温度为289～297℃，5%热分解温度大于508℃，40%PTFE/FPI的热膨胀系数低至59.67×10-6 K-1，20%PTFE/FPI的拉伸强度为70 MPa，拉伸模量为1.59 GPa，断裂伸长率为7.7%。

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董明（1978-），男（汉族），陕西西安人，教授，主要从事电力设备电气绝缘技术、状态监测等方面的研究工作。
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孙维凯（1998-），男（汉族），江苏盐城人，博士生，主要从事高电气性能复合绝缘材料的研究工作；

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孙维凯（1998-），男（汉族），江苏盐城人，博士生，主要从事高电气性能复合绝缘材料的研究工作；

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孙维凯（1998-），男（汉族），江苏盐城人，博士生，主要从事高电气性能复合绝缘材料的研究工作；

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Progress in Materials Science,2012,57(4):660-723., articleTitle=Fundamentals, processes and applications of high-permittivity polymer-matrix composites, refAbstract=null), Reference(id=1203362957976646002, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, doi=null, pmid=null, pmcid=null, year=2018, volume=47, issue=1, pageStart=41, pageEnd=44,48, url=null, language=null, rfNumber=[29], rfOrder=32, authorNames=李国平, 张晨晖, 刘亚中, journalName=当代化工, refType=null, unstructuredReference=李国平,张晨晖,刘亚中,等.Ag/PAMAM树形分子纳米复合材料对PTFE膜性能的影响[J].当代化工,2018,47(1):41-44,48., articleTitle=Ag/PAMAM树形分子纳米复合材料对PTFE膜性能的影响, refAbstract=null), Reference(id=1203362958085697912, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, doi=null, pmid=null, pmcid=null, year=2018, volume=47, issue=1, pageStart=41, pageEnd=44,48, url=null, language=null, rfNumber=[29], rfOrder=33, authorNames=LIGuoping, ZHANGChenhui, LIUYazhong, journalName=Contemporary Chemical Industry, refType=null, unstructuredReference=LIGuoping, ZHANGChenhui, LIUYazhong, et al. Effect of Ag/PAMAM nanocomposite on the properties of PTFE membrane[J]. Contemporary Chemical Industry,2018,47(1):41-44,48., articleTitle=Effect of Ag/PAMAM nanocomposite on the properties of PTFE membrane, refAbstract=null)], funds=[Fund(id=1203362954830917860, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, awardId=2023YFB2406900, language=CN, fundingSource=国家重点研发计划项目(2023YFB2406900), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1203362943753761554, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, xref=null, ext=[AuthorCompanyExt(id=1203362943762150163, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, companyId=1203362943753761554, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1. 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(a) 干燥PTFE粉末的实物照片 (b) PTFE颗粒的SEM照片

, figureFileSmall=axKDNEwOgrobOkzDm2yQJw==, figureFileBig=+Ng+bqv2XeI1hIiyT0oE7g==, tableContent=null), ArticleFig(id=1203362951550972012, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, language=EN, label=Fig.3, caption=FT-IR spectra of PTFE and PTFE/FPI composite films, figureFileSmall=p/OYm+JG9ZxAM7qcsKuSXA==, figureFileBig=SQ/4sBqaEeMRfC1+4/e0Rg==, tableContent=null), ArticleFig(id=1203362951655829621, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, language=CN, label=图3, caption=PTFE及PTFE/FPI复合薄膜的FT-IR谱图, figureFileSmall=p/OYm+JG9ZxAM7qcsKuSXA==, figureFileBig=SQ/4sBqaEeMRfC1+4/e0Rg==, tableContent=null), ArticleFig(id=1203362951752298620, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, language=EN, label=Fig.4, caption=XRD spectra of PTFE and PTFE/FPI composite films, figureFileSmall=jMy7D3M7lx51zx53TS5kvw==, figureFileBig=Svl6U2pJKP0K+9J7DfEzGA==, 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journalId=1149653034449285133, articleId=1203281640601657849, language=EN, label=Fig.6, caption=Dielectric constant and dielectric loss curves of PTFE and PTFE/FPI composite films at high frequencies, figureFileSmall=Nmx0pGhWhUo2QxkwS8VE5w==, figureFileBig=WdDgg+ATmNhaqRkKeEWz6A==, tableContent=null), ArticleFig(id=1203362952402415775, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, language=CN, label=图6, caption=PTFE和PTFE/FPI复合薄膜在高频下的介电常数和介电损耗曲线, figureFileSmall=Nmx0pGhWhUo2QxkwS8VE5w==, figureFileBig=WdDgg+ATmNhaqRkKeEWz6A==, tableContent=null), ArticleFig(id=1203362952507273384, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1203281640601657849, language=EN, label=Fig.7, caption=Thermogravimetric and temperature-deformation curves of PTFE and PTFE/FPI composite films, figureFileSmall=30stlBg6n3zT9edyWior2g==, figureFileBig=hTrensOpPw78gBBXKT50hw==, tableContent=null), ArticleFig(id=1203362952616325295, 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PTFE/FPI含氟聚酰亚胺复合薄膜的制备及高频工况下的介电性能研究
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孙维凯 1 , 傅雅琴 2 , 常昊鑫 1 , 戴景琪 1, 3 , 付文光 4 , 王健一 5 , 董明 1
绝缘材料 | 高性能聚酰亚胺材料专题 2025,58(6): 35-42
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绝缘材料 | 高性能聚酰亚胺材料专题 2025, 58(6): 35-42
PTFE/FPI含氟聚酰亚胺复合薄膜的制备及高频工况下的介电性能研究
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孙维凯1, 傅雅琴2, 常昊鑫1, 戴景琪1, 3, 付文光4, 王健一5, 董明1
作者信息
  • 1.西安交通大学 电气工程学院，陕西 西安 710049
  • 2.浙江理工大学 材料科学与工程学院， 浙江 杭州 310018
  • 3.内蒙古电力（集团）有限责任公司，内蒙古 呼和浩特 010020
  • 4.内蒙古电力（集团）有限责任公司内蒙古电力科学研究院分公司，内蒙古 呼和浩特 010020
  • 5.中国电力科学研究院有限公司，北京 100192

    • 孙维凯（1998-），男（汉族），江苏盐城人，博士生，主要从事高电气性能复合绝缘材料的研究工作；

通讯作者:

董明（1978-），男（汉族），陕西西安人，教授，主要从事电力设备电气绝缘技术、状态监测等方面的研究工作。
Synthesis of PTFE/FPI fluoropolyimide composite films and their dielectric properties under high frequency working conditions
Weikai SUN1, Yaqin FU2, Haoxin CHANG1, Jingqi DAI1, 3, Wenguang FU4, Jianyi WANG5, Ming DONG1
Affiliations
  • 1. School of Electrical Engineering, Xi′an Jiaotong University, Xi′an 710049, China
  • 2. School of Materials Science and Engineering, Zhejiang Sci-Tech University, Hangzhou 310018, China
  • 3. Inner Mongolia Power (Group) Co., Ltd., Hohhot 010020, China
  • 4. Inner Mongolia Power Research Institute Branch, Inner Mongolia Power (Group) Co., Ltd., Hohhot 010020, China
  • 5. China Electric Power Research Institute, Beijing 100192, China
出版时间: 2025-06-20 doi: 10.16790/j.cnki.1009-9239.im.2025.06.005
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摘要
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为开发在高频工况下兼具低介电常数（Dk）、低介电损耗（Df）和耐高温性的聚酰亚胺（PI）基复合薄膜，在制备含氟聚酰亚胺（FPI）的前驱体聚酰胺酸中加入有机碱，制得水溶性聚酰胺酸盐（PAAS），采用低介电聚四氟乙烯（PTFE）浓缩分散液与干燥后的PAAS进行复合形成水分散体系制备PTFE/FPI复合薄膜，通过改变PTFE含量，研究其对复合薄膜介电性能、耐热性能和力学性能的影响。结果表明：随着PTFE含量的增加，复合薄膜的Dk不断降低，但对热稳定性和力学性能会有一定影响。50%PTFE/FPI的Dk达到最小值（Dk=1.5@8.5 GHz），10%PTFE/FPI在9.25～10.25 GHz频段内的Df小于0.005，系列复合薄膜的玻璃化转变温度为289～297℃，5%热分解温度大于508℃，40%PTFE/FPI的热膨胀系数低至59.67×10-6 K-1，20%PTFE/FPI的拉伸强度为70 MPa，拉伸模量为1.59 GPa，断裂伸长率为7.7%。

含氟聚酰亚胺复合薄膜  /  介电常数  /  高频工况  /  耐热性能  /  全有机体系

To develop polyimide (PI)-based composite films with low dielectric constant (Dk), low dielectric loss (Df), and high temperature resistance at high frequency, a water-soluble polyamic salt (PAAS) was prepared by adding organic base into the polyamic acid, which is the precursor of fluoropolyimide (FPI), and composite films were prepared by compounding low dielectric polytetrafluoroethylene (PTFE) concentrated dispersion with the dried PAAS to form a water dispersion system. The effects of PTFE content on the dielectric, thermal, and mechanical properties of the composite films were studied. The experimental results show that with the increase of PTFE content, the dielectric constant of the composite films decreases continuously, but there will be some effects on the thermal stability and mechanical properties. The dielectric constant of 50%PTFE/FPI reaches the minimum value (Dk=1.5@8.5 GHz), and the dielectric loss of 10%PTFE/FPI in the frequency band of 9.25-10.25 GHz is less than 0.005. The glass transition temperature of the composite films is in the range of 289-297℃, and the thermal decomposition temperature at 5% is higher than 508℃. The thermal expansion coefficient of 40%PTFE/FPI is as low as 59.67×10-6 K-1. The tensile strength of 20%PTFE/FPI is 70 MPa, the tensile modulus is 1.59 GPa, and the elongation at break is 7.7%.

fluoropolyimide composite films  /  dielectric constant  /  high frequency working conditions  /  heat resistance  /  all-organic system
孙维凯, 傅雅琴, 常昊鑫, 戴景琪, 付文光, 王健一, 董明. PTFE/FPI含氟聚酰亚胺复合薄膜的制备及高频工况下的介电性能研究. 绝缘材料, 2025 , 58 (6) : 35 -42 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.005
Weikai SUN, Yaqin FU, Haoxin CHANG, Jingqi DAI, Wenguang FU, Jianyi WANG, Ming DONG. Synthesis of PTFE/FPI fluoropolyimide composite films and their dielectric properties under high frequency working conditions[J]. Insulating Materials, 2025 , 58 (6) : 35 -42 . DOI: 10.16790/j.cnki.1009-9239.im.2025.06.005
正文
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0 引言
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随着5G、6G高频通讯技术的迅猛发展，电子元器件也相应地朝着高传输速度和高集成度方向快速发展。然而，超大规模集成电路布线密度的增加会伴随产生电阻电容延迟效应，导致信号传输延迟和功率损耗等不良影响[1]，这对通讯设备中的低介电聚合物材料提出了更高的要求[2-3]。目前市面上的电介质材料的高介电常数和高介电损耗不能满足高频高温应用场景的使用需求，亟需降低电介质材料的介电常数和介电损耗，促使其在高频通讯领域的应用[4-6]，如天线、层间介质、通信电缆等。无机材料作为传统层间介质材料，存在脆性大、加工困难等问题[7-8]。而有机聚合物在介电常数、力学性能和加工性能方面具有一定的优势[9]。
随着高速通讯智能终端轻薄化和柔性化的发展，通讯领域对有机柔性低介电绝缘薄膜提出了更高的要求[10-14]。传统聚酰亚胺（PI）有着优异的低介电性能、电气绝缘性能、耐热性能和力学性能，是当前柔性印刷电路板绝缘薄膜的主要使用材料。但随着5G、6G通讯频率的提高，传统PI相对高的介电常数和介电损耗导致信号传输出现长延迟和高损耗等问题。目前研究者们已对PI的改性进行了大量尝试[15-23]，虽然在降低介电常数和介电损耗上取得一定进展，但仍存在如中间产物易水解、无机填料改性复杂且易团聚、使用大量有机溶剂、对复合材料介电性能改善程度有限等不足之处。
针对上述问题，本研究通过制备中间产物稳定且环境友好型的含氟PI，引入本征低介电聚四氟乙烯（PTFE）有机填料，形成全有机体系，改善复合薄膜的介电性能，使薄膜具有较好的综合性能。以4,4′-（六氟异丙烯）二酞酸酐（6FDA）为二酐单体，以4,4′-二氨基二苯醚（ODA）为二胺单体进行共聚，得到前驱体聚酰胺酸（PAA）。在PAA中加入有机碱三乙胺（TEA）得到水溶性聚酰胺酸盐（PAAS），将PTFE浓缩分散液与PAAS物理共混得到水分散体系，通过阶梯高温亚胺化得到复合薄膜。通过改变PTFE的含量，研究其对复合薄膜介电性能、力学性能和耐热性能的影响，以期获得适应高频工况的全有机PI基复合薄膜，为制备适应5G通讯等领域用柔性薄膜提供试验依据。
1 试验
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1.1 主要原材料
4,4′-（六氟异丙烯）二酞酸酐（6FDA，纯度为99%）、4,4′-二氨基二苯醚（ODA，纯度为98%）、N,N-二甲基乙酰胺（DMAc，纯度为99.0%）、聚四氟乙烯（PTFE）浓缩分散液（质量分数为60%）、丙酮（纯度为99.5%），上海阿拉丁试剂有限公司；有机碱三乙胺（TEA，纯度为99.0%），氢化钙（CaH2，纯度为98.5%），上海麦克林生化科技有限公司。
1.2 PTFE/FPI复合薄膜的制备
1.2.1 PAAS的制备
（1）试剂的纯化
将一定量的6FDA和ODA放置在110℃的烘箱中干燥5 h；在DMAc中加入少量的CaH2，在190℃油浴中回流5 h，减压蒸馏得到无水DMAc。
（2）PAAS的制备
取一定量的ODA溶解在DMAc中超声30 min，转移到三口烧瓶中，将三口烧瓶置于冰水浴中进行机械搅拌，向三口烧瓶中分批次加入6FDA，控制6FDA与ODA的物质的量之比为1.03∶1。溶液出现黏稠后将三口烧瓶转移至室温继续搅拌5 h，量取一定量的TEA，在10 min内滴入三口烧瓶，继续搅拌2 h得到均匀黏稠的PAAS溶液。溶液静置消泡后缓慢倒入丙酮溶液中析出，得到半透明白色线状物，放置一天后倒出上层丙酮溶液，在通风橱中自然风干24 h，将线状物剪成颗粒继续风干24 h，得到无DMAc无丙酮的PAAS颗粒。
1.2.2 PTFE/FPI复合薄膜的制备
将PAAS加入去离子水中，磁力搅拌4 h至PAAS基本溶解，按照TEA与水的体积比为2∶100的比例补充TEA，继续搅拌至PAAS完全溶解，加入计算量的PTFE分散液（使PTFE固体颗粒占成型后PTFE/FPI复合薄膜中的质量分数为10%～50%），再依次超声和磁力搅拌2 h。接着采用流延法利用刮膜机将混合均匀的分散液刮涂在玻璃板上，装在表面有密集小孔的塑料盒中，在30℃烘箱中烘12 h，得到PTFE/PAAS预制膜。
将PTFE/PAAS预制膜在马弗炉中按照100℃/ 1 h+200℃/1 h+300℃/1 h的程序进行阶梯升温，得到厚度约为20 μm的PTFE/FPI复合薄膜。按照PTFE的填充量，将最终复合薄膜分别命名为pure FPI、10%～50%PTFE/FPI。制备流程如图1所示。
1.3 测试与表征
采用场发射扫描电子显微镜（FESEM，Hitachi S-4800）对PTFE颗粒和PTFE/FPI复合薄膜的截面进行观察分析，通过调整倍率大小观察得到PTFE颗粒和PTFE/FPI复合薄膜的形貌和尺寸等信息。
采用傅里叶红外光谱仪（FT-IR，Thermo Electron Corp）对PTFE/FPI复合薄膜官能团结构进行表征分析（ATR法），波数为500～2 000 cm-1。
采用X射线衍射仪（XRD，D8 discover，Bruker）对PTFE、PTFE/FPI复合薄膜的晶态结构进行测试分析。将PTFE/FPI复合薄膜裁剪成大小为3 cm×3 cm的方块，在80℃烘箱中烘干2 h，避免水分对测试结果造成影响，2θ为3°～50°，步进速度为0.2°/s。
采用矢量网络分析仪（E5071C，Agilent Technologies）测试PTFE/FPI复合薄膜的介电参数，测试方法为波导法，测试频率为8.2～10.5 GHz。其中Dk用复介电常数的实部（ε'）表示，Df用复介电常数的虚部（ε″）除以实部，即损耗角正切值来表征，计算公式如式（1）所示。
tanδ=ε″ε'
使用热重分析仪（TGA/DSC 2，Mettler Toledo）对PTFE/FPI复合薄膜进行热重分析，为接近实际使用工况，测试在空气氛围中进行，升温速率为10℃/min，温度为室温～800℃。
使用热机械分析仪（TMA，Q800，TA）测定PTFE/FPI复合薄膜的玻璃化转变温度（Tg），在恒定力0.05 N的负载状态下测试，温度为20～350℃，升温速率为10℃/min。
使用热机械分析仪（TMA，Q400EM，TA）测试PTFE/FPI复合薄膜的热膨胀系数（CTE），负载恒定为0.05 N，温度为20～250℃，升温速率为10℃/min，升温至250℃20 min后降温至20℃，循环3次，分析薄膜尺寸的变化率，拟合线性方程，取线性方程斜率的算术平均值得到CTE。
使用万能材料试验机（Instron-3367，Instron）对PTFE/FPI复合薄膜的力学性能进行测试，试样尺寸为25 mm×5 mm，拉伸速度为2 mm/min，有效样本容量为5。
2 结果与讨论
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2.1 PTFE颗粒和PTFE/FPI复合薄膜的形貌结构分析
取适量的PTFE分散液置于一次性试管中，经过充分干燥后得到白色粉末PTFE，如图2(a)所示。将少许PTFE颗粒分散在大量乙醇中，取少许分散液滴在硅片上，待完全烘干后用扫描电镜观察其微观形貌，如图2(b)所示，可以看出PTFE平面投影类似圆柱体状，高约为200 nm，底面直径为80 nm。
利用红外光谱仪分析PTFE/FPI复合薄膜的化学结构，结果如图3所示。
从图3可以看出，经过阶梯化升温，PAAS的C=O酰胺峰（1 656 cm-1）和C-NH弯曲峰（1 546 cm-1）完全消失，此外观察到1 783、1 718 、1 373、721 cm-1处PI的典型吸收峰，分别对应于酰亚胺环C=O双键的不对称伸缩振动、C=O双键的对称伸缩振动、亚胺环C-N键的拉伸振动和亚胺环的面内弯曲振动，证明亚胺化已经完成，PAAS已经成功闭环转变为FPI[24]。由于PTFE中C-F键与6FDA中的C-F键在1 202 cm-1和1 145 cm-1处的特征吸收峰有所重叠，无法说明填料与基体之间的结合情况，利用X射线衍射仪对纯FPI膜和PTFE/FPI复合薄膜的晶态结构进行分析，结果如图4所示。
从图4可以看出，纯FPI膜在15°左右出现1个宽峰，表明FPI为无定型聚合物。而PTFE因其规整对称结构在18°出现了明显的衍射峰，因此PTFE/FPI复合薄膜在18°附近也出现了较强的衍射峰。随着PTFE填充量的增加，可以观察到复合薄膜的晶面衍射角略有增大，根据布拉格方程（nλ=2dsinθ）可以得知，聚合物的链间距减小，说明PTFE的掺入使得界面相互作用增强，聚集态结构得到优化，链间相互作用得到增强。
SEM可以提供直观的试样形貌和分散情况信息。纯FPI膜和PTFE/FPI复合薄膜的截面SEM图如图5所示。PTFE颗粒表面带有负电荷，而PAAS中的季铵基团带有正电荷[25]，两者之间存在库伦引力，通过静电吸引力达到类似自主装的效果，可以使得有机填料在有机基体中分散性更好。
从图5可以看出，纯FPI膜的截面较为致密，PTFE/FPI复合薄膜中的PTFE颗粒相对均匀地分散在基体之中，没有明显的团聚现象。当PTFE填充量较低时（质量分数为10%～20%），可以清晰地观察到PTFE颗粒镶嵌在FPI基体中；当填充量提高时（质量分数为30%～40%），PTFE颗粒明显变得更为密集，仍呈现出被基体所包裹的状态；当PTFE质量分数达到50%时，PTFE在基体中出现粘结团聚的现象，会对复合薄膜的综合性能产生一定的负面影响。
2.2 PTFE/FPI复合薄膜的介电性能分析
高频下PTFE和PTFE/FPI复合薄膜的介电常数和介电损耗变化情况如图6所示。
从图6(a)可以看出，纯FPI膜在8.2～10.5 GHz内的介电常数（Dk）为2.3～2.9，整体数值低于3，这是因为低极性、具有空间位阻效应的三氟甲基（-CF3）的引入限制了FPI的弛豫和取向。PTFE的介电常数最低，因此随着其填充量的增加，PTFE/FPI复合薄膜的介电常数不断降低。当PTFE质量分数在20%以上时，其对PTFE/FPI复合薄膜介电性能的改善效果较好。当PTFE质量分数达到50%时，PTFE/FPI复合薄膜的Dk降低至1.5～2.4，这是因为本征低极性改性和低介电有机填充物的掺杂协同作用，即在链骨架的侧基上引入了低极性和大空间效应的-CF3，另外还引入了低介电PTFE颗粒，协同降低了复合薄膜的Dk。随着PTFE填充量的增加，一方面单位体积内可极化的PI分子数减少，另一方面PTFE在一定程度上阻碍了PI分子链的运动，降低了电子的迁移能力，最终降低了电子极化率[26]。此外，颗粒和基体之间存在库伦引力作用，使得低填充量PTFE在FPI中有着良好的分散，但两者之间仍存有部分空隙，这些空隙的存在对复合薄膜介电常数的降低也有促进的作用。
介电损耗（Df）也是高频介电材料的重要参考参数，对通讯设备的热管理有较大的影响。从图6(b)可以看出，PTFE/FPI复合薄膜的Df整体有一定的波动性，在8.2～9.6 GHz范围内出现了不同强度的共振峰，且随着PTFE填充量的增加，共振峰强度有所减弱，向着低频移动，在大于9.2 GHz的频段，Df又呈上升趋势。其中10%PTFE/FPI的Df小于0.05，部分频段（9.25～10.25 GHz）的Df小于0.005，可满足高频通讯低介电损耗的要求。PTFE/FPI复合薄膜的整体Df仍偏大，可能是因为填料和基体之间良好的结合作用使得运动单元的转动需要克服很大的阻力，而相对低填充量的复合薄膜中结合作用不强且破坏了PI的链间作用，阻止了PI分子的极化，因此Df呈较低的水平。
2.3 PTFE/FPI复合薄膜的热稳定性分析
通过TGA和TMA综合分析复合薄膜的热稳定性，为接近实际工况，试验在空气中进行，复合薄膜热失重曲线如图7(a)所示。从图7(a)可以看出，PTFE/FPI复合薄膜的5%热分解温度（T5%）随着PTFE含量的增加略有下降，但都在508℃以上，表现出良好的热稳定性，这得益于填料和基体本身较好的耐高温特性。
利用TMA测得复合薄膜的尺寸随温度变化的情况，从而得到玻璃化转变温度（Tg），复合薄膜的温度-形变曲线如图7(b)所示。从图7(b)可以看出，Tg从纯FPI膜的291℃先下降到10%PTFE/FPI的289℃，这是因为PTFE本身拥有相对低的Tg（<130℃）[27]，而PTFE的掺入破坏了基体的规整排列，之后Tg又上升到40%PTFE/FPI的297℃，这是因为随着PTFE含量的增加，填料和基体之间的静电吸引力增强，也有可能是两者之间产生了氢键作用，使得Tg上升[28-29]。
纯FPI膜和PTFE/FPI复合薄膜的长度变化率和温度的关系如图8所示，CTE的平均值如图9所示。从图9可以看出，纯FPI膜的CTE为83.37×10-6 K-1，当PTFE质量分数为20%时，复合薄膜的CTE大幅降低至66.6×10-6 K-1，PTFE质量分数继续增加至40%时，复合薄膜的CTE达到最低值59.67×10-6 K-1，较纯FPI膜下降了28.4%。这是因为填料和基体间的强吸引作用，阻碍了PI分子链段的运动，另外PTFE中的氟原子具有高电负性，可以与PI中的碳原子形成氢键，从而增强了其结合力[28-29]。
2.4 PTFE/FPI复合薄膜的力学性能分析
纯FPI膜和PTFE/FPI复合薄膜的应力-应变曲线、拉伸强度和拉伸模量如图10所示。从图10可以看出，纯FPI膜的拉伸强度为75.5 MPa，拉伸模量为2.3 GPa。随着PTFE含量的增加，复合薄膜的拉伸强度不断降低，断裂伸长率呈先增后减的趋势，当PTFE质量分数高于40%时，复合薄膜的断裂伸长率则低于纯FPI膜。当PTFE质量分数为50%时，复合薄膜的拉伸强度达最小值29.6 MPa，当PTFE质量分数为30%时，复合薄膜的拉伸模量达最小值1.56 GPa。这些现象的原因是PTFE作为分子链中的润滑剂，会出现蠕变现象，使得复合薄膜的刚性降低，断裂伸长率升高，而PTFE填充量增加时则会出现团聚现象，使得复合薄膜的拉伸强度和断裂伸长率降低。当PTFE质量分数为20%时，复合膜的拉伸强度为70 MPa，拉伸模量为1.59 GPa，断裂伸长率为7.7%，综合力学性能良好。
3 结论
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为了得到高频下具有优异介电性能且综合性能良好的PI薄膜，采用含三氟甲基的6FDA、含有醚键的ODA和TEA制得绿色稳定的前驱体PAAS，与本征低介电PTFE颗粒进行简单高效的物理共混制得PTFE/FPI复合薄膜。通过调整PTFE的含量，分析其对复合薄膜介电性能、耐热性能和力学性能的影响，主要得到以下结论：
（1）PTFE的填充可以有效降低PI复合薄膜在高频下的介电常数和介电损耗。随着PTFE含量的增加，复合薄膜的介电常数不断降低，当PTFE质量分数为50%时，复合薄膜的介电常数在8.5 GHz达到最小值（Dk=1.5）；当PTFE质量分数为10%时，复合薄膜在9.25～10.25 GHz频段内的介电损耗小于0.005。
（2）经过PTFE掺杂的复合薄膜保持着优异的热稳定性，其T5%均大于508℃，Tg在290℃以上，CTE最小值为59.67×10-6 K-1，较纯FPI膜下降了28.4%。
（3）经过PTFE掺杂的复合薄膜仍保持着良好的力学性能。当PTFE质量分数为20%时，复合薄膜的拉伸强度为70 MPa，拉伸模量为1.59 GPa，断裂伸长率为7.7%。
基金
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  • 国家重点研发计划项目(2023YFB2406900)
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.2025.06.005
  • 接收时间：2024-09-28
  • 首发时间：2025-12-04
  • 出版时间：2025-06-20
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  • 收稿日期：2024-09-28
  • 修回日期：2024-11-25
基金
国家重点研发计划项目(2023YFB2406900)
作者信息
    1.西安交通大学 电气工程学院，陕西 西安 710049
    2.浙江理工大学 材料科学与工程学院， 浙江 杭州 310018
    3.内蒙古电力（集团）有限责任公司，内蒙古 呼和浩特 010020
    4.内蒙古电力（集团）有限责任公司内蒙古电力科学研究院分公司，内蒙古 呼和浩特 010020
    5.中国电力科学研究院有限公司，北京 100192

通讯作者:

董明（1978-），男（汉族），陕西西安人，教授，主要从事电力设备电气绝缘技术、状态监测等方面的研究工作。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2025.06.005
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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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