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Article(id=1242756978947244370, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.11.008, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1620144000000, receivedDateStr=2021-05-05, revisedDate=1621958400000, revisedDateStr=2021-05-26, acceptedDate=null, acceptedDateStr=null, onlineDate=1774225953085, onlineDateStr=2026-03-23, pubDate=1637510400000, pubDateStr=2021-11-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1774225953085, onlineIssueDateStr=2026-03-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1774225953085, creator=13701087609, updateTime=1774225953085, 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=62, endPage=68, ext={EN=ArticleExt(id=1242756979312148825, articleId=1242756978947244370, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Preparation and Properties of Optical Transparent Polyimides Containing Aliphatic Ring and Amide Structure, columnId=1198664996516360309, journalTitle=Insulating Materials, columnName=Polyimide Film Special Issue, runingTitle=null, highlight=null, articleAbstract=

A novel dianhydride monomer containing alicyclic ring and amide group was synthesized and further polymerized with several diamine monomers to prepare a series of transparent polyimide films. The properties of the films were tested and characterized. The results show that the synthesized polyimide films have excellent optical properties (T550>89%), low coefficient of thermal expansion (CTE<17×10-6 K-1), and higher glass transition temperature (Tg>320℃) because of introducing trans cyclohexane and amide into the structure of dianhydride at the same time. The introduction of alicyclic structure decreases the formation of charge transfer complex, which increases the transparency of the polyimide films. On the other hand, the introduction of amide structure decreases the coefficient of thermal expansion.

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通过合成一种含有脂环及酰胺结构的二酐单体（TCDA），将其与多种不同的二胺聚合，制备了一系列透明聚酰亚胺薄膜，并对薄膜进行了性能测试与表征。结果表明：在二酐结构中同时引入反式环己烷及酰胺结构，使得合成的聚酰亚胺薄膜具有较优异的光学性能（T550>89%）、较低的热膨胀系数（CTE＜17×10-6 K-1）以及较高的玻璃化转变温度（Tg>320℃），表明脂环结构的引入降低了电荷转移络合物的形成，提高了聚酰亚胺薄膜的透明性，而酰胺结构的引入降低了热膨胀系数。

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朴凤玉（1962-），女（朝鲜族），吉林延吉人，教授，博士，主要从事抗癫痫小分子药物合成的研究。
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张婷婷（1997-），女（汉族），辽宁盘锦人，硕士生，主要从事透明聚酰亚胺薄膜的制备及性能的研究。

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张婷婷（1997-），女（汉族），辽宁盘锦人，硕士生，主要从事透明聚酰亚胺薄膜的制备及性能的研究。

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张婷婷（1997-），女（汉族），辽宁盘锦人，硕士生，主要从事透明聚酰亚胺薄膜的制备及性能的研究。

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a function of temperature, figureFileSmall=QEO6jXdgbPrb4IuRb8UZng==, figureFileBig=jChWBS30bPNnA0xkVxmhTA==, tableContent=null), ArticleFig(id=1245100058803286587, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978947244370, language=CN, label=图9, caption=PI薄膜的质量损失随温度的变化曲线, figureFileSmall=QEO6jXdgbPrb4IuRb8UZng==, figureFileBig=jChWBS30bPNnA0xkVxmhTA==, tableContent=null), ArticleFig(id=1245100058908144191, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978947244370, language=EN, label=Tab.1, caption=Optical properties of the PI films, figureFileSmall=null, figureFileBig=null, tableContent=
PI组成光学性能
λcut off/nmT550/%L*a*b*Haze/%YI
PI-1TCDA/TFMB3898996.012.332.570.756.66
PI-2TCDA/t-CHDA3788896.122.112.100.973.23
PI-3TCDA/6FAPB3698995.001.234.442.477.44
PI-4TCDA/ODA3918693.313.9314.12.7622.6
PI-5TCDA/APS3888494.670.472.671.824.75
), ArticleFig(id=1245100059017196097, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978947244370, language=CN, label=表1, caption=

PI薄膜的光学性能

, figureFileSmall=null, figureFileBig=null, tableContent=
PI组成光学性能
λcut off/nmT550/%L*a*b*Haze/%YI
PI-1TCDA/TFMB3898996.012.332.570.756.66
PI-2TCDA/t-CHDA3788896.122.112.100.973.23
PI-3TCDA/6FAPB3698995.001.234.442.477.44
PI-4TCDA/ODA3918693.313.9314.12.7622.6
PI-5TCDA/APS3888494.670.472.671.824.75
), ArticleFig(id=1245100059113665092, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978947244370, language=EN, label=Tab.2, caption=Thermal properties of the PI films, figureFileSmall=null, figureFileBig=null, tableContent=
PI组成Tg/℃T5%/℃CTE/(×10-6 K-1)CTE测试范围
PI-1TCDA/TFMB32041818.950～250
PI-2TCDA/t-CHDA30842416.250～250
PI-3TCDA/6FAPB25743252.450～250
PI-4TCDA/ODA29143440.750～250
PI-5TCDA/APS28440048.150～250
), ArticleFig(id=1245100059184968264, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978947244370, language=CN, label=表2, caption=

PI薄膜的热性能

, figureFileSmall=null, figureFileBig=null, tableContent=
PI组成Tg/℃T5%/℃CTE/(×10-6 K-1)CTE测试范围
PI-1TCDA/TFMB32041818.950～250
PI-2TCDA/t-CHDA30842416.250～250
PI-3TCDA/6FAPB25743252.450～250
PI-4TCDA/ODA29143440.750～250
PI-5TCDA/APS28440048.150～250
), ArticleFig(id=1245100059239494219, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978947244370, language=EN, label=Tab.3, caption=Mechanical properties of the PI films, figureFileSmall=null, figureFileBig=null, tableContent=
PI组成εb/%Et/GPaσm/MPa
PI-1TCDA/TFMB5.9±0.63.1±0.5114±5.9
PI-2TCDA/t-CHDA21.7±8.51.8±0.4113.5±1
PI-3TCDA/6FAPB8.3±0.32.1±0.3101.7±5.3
PI-4TCDA/ODA15.5±1.83.1±0.3146.1±7.5
PI-5TCDA/APS9.8±2.53.1±0.3122.4±6.8
), ArticleFig(id=1245100059314991695, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978947244370, language=CN, label=表3, caption=

PI薄膜的力学性能

, figureFileSmall=null, figureFileBig=null, tableContent=
PI组成εb/%Et/GPaσm/MPa
PI-1TCDA/TFMB5.9±0.63.1±0.5114±5.9
PI-2TCDA/t-CHDA21.7±8.51.8±0.4113.5±1
PI-3TCDA/6FAPB8.3±0.32.1±0.3101.7±5.3
PI-4TCDA/ODA15.5±1.83.1±0.3146.1±7.5
PI-5TCDA/APS9.8±2.53.1±0.3122.4±6.8
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含脂环和酰胺结构透明聚酰亚胺的制备和性能研究
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张婷婷 1 , 杨正慧 2 , 朴凤玉 1 , 郭海泉 2
绝缘材料 | 聚酰亚胺薄膜专题 2021,54(11): 62-68
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绝缘材料 | 聚酰亚胺薄膜专题 2021, 54(11): 62-68
含脂环和酰胺结构透明聚酰亚胺的制备和性能研究
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张婷婷1, 杨正慧2, 朴凤玉1, 郭海泉2
作者信息
  • 1延边大学 理学院，吉林 延吉 133000
  • 2中国科学院长春应用化学研究所 高分子复合材料工程中心，吉林 长春 130021

    • 张婷婷（1997-），女（汉族），辽宁盘锦人，硕士生，主要从事透明聚酰亚胺薄膜的制备及性能的研究。

通讯作者:

朴凤玉（1962-），女（朝鲜族），吉林延吉人，教授，博士，主要从事抗癫痫小分子药物合成的研究。
Preparation and Properties of Optical Transparent Polyimides Containing Aliphatic Ring and Amide Structure
Tingting ZHANG1, Zhenghui YANG2, Fengyu PIAO1, Haiquan GUO2
Affiliations
  • 1College of Science, Yanbian University, Yanji 133000, China
  • 2Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130021, China
出版时间: 2021-11-22 doi: 10.16790/j.cnki.1009-9239.im.2021.11.008
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摘要
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通过合成一种含有脂环及酰胺结构的二酐单体（TCDA），将其与多种不同的二胺聚合，制备了一系列透明聚酰亚胺薄膜，并对薄膜进行了性能测试与表征。结果表明：在二酐结构中同时引入反式环己烷及酰胺结构，使得合成的聚酰亚胺薄膜具有较优异的光学性能（T550>89%）、较低的热膨胀系数（CTE＜17×10-6 K-1）以及较高的玻璃化转变温度（Tg>320℃），表明脂环结构的引入降低了电荷转移络合物的形成，提高了聚酰亚胺薄膜的透明性，而酰胺结构的引入降低了热膨胀系数。

透明聚酰亚胺  /  脂环二酐  /  酰胺二酐  /  低热膨胀系数

A novel dianhydride monomer containing alicyclic ring and amide group was synthesized and further polymerized with several diamine monomers to prepare a series of transparent polyimide films. The properties of the films were tested and characterized. The results show that the synthesized polyimide films have excellent optical properties (T550>89%), low coefficient of thermal expansion (CTE<17×10-6 K-1), and higher glass transition temperature (Tg>320℃) because of introducing trans cyclohexane and amide into the structure of dianhydride at the same time. The introduction of alicyclic structure decreases the formation of charge transfer complex, which increases the transparency of the polyimide films. On the other hand, the introduction of amide structure decreases the coefficient of thermal expansion.

transparent polyimide  /  alicyclic dianhydrid  /  amide dianhydride  /  low coefficient of thermal expansion
张婷婷, 杨正慧, 朴凤玉, 郭海泉. 含脂环和酰胺结构透明聚酰亚胺的制备和性能研究. 绝缘材料, 2021 , 54 (11) : 62 -68 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.008
Tingting ZHANG, Zhenghui YANG, Fengyu PIAO, Haiquan GUO. Preparation and Properties of Optical Transparent Polyimides Containing Aliphatic Ring and Amide Structure[J]. Insulating Materials, 2021 , 54 (11) : 62 -68 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.008
正文
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0 引言
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聚酰亚胺（PI）薄膜具有优异的耐热性能、力学性能及较低的介电常数，已广泛应用于集成电路、微电子、印制电路、航空航天等领域[1-4]。随着显示和光电技术的快速发展，具有优异光学性能和力学性能的透明聚酰亚胺（CPI）薄膜替代了玻璃等硬质透明材料，赋予电子器件柔性、可折叠特征，在柔性显示、柔性电子器件领域显示出巨大的发展潜力[5]。
目前无色透明聚酰亚胺薄膜的研究已成为高性能聚酰亚胺薄膜研究领域的重要内容。传统PI薄膜呈现黄色，其颜色来自于分子结构中二酐单元和二胺单元形成的电荷转移络合物（CTC）[6-7]。因此，通过合理的结构设计，减弱二胺基团的供电子特征和二酐基团的吸电子特征，或者减弱分子链间的相互作用，进而减少电荷转移络合物的形成，减少对可见光的吸收，成为获得高透明性CPI薄膜的主要途径[8]。例如，在PI分子结构中引入含氟结构、脂环结构以及非共平面结构等可减弱分子链共轭特性的结构，这些结构可赋予CPI薄膜良好的光学性能和力学性能[9-12]。M HASEGAWA等[5]通过在PI分子骨架中引入氢化均苯四甲酸二酐及其一系列异构体，所合成CPI薄膜在400 nm处的透光率达到90%，热膨胀系数（CTE）小于27×10-6/K。WANG C Y等[6]合成多种含三氟甲基的二酐单体，将其与含有联苯、醚键等结构单元的二胺进行聚合，所合成CPI薄膜的透光率T450nm为78%～84%。但是，目前制约CPI薄膜发展的主要瓶颈是薄膜的热膨胀系数较高、耐热性较差等问题。较高的热膨胀系数容易造成CPI薄膜在柔性器件制造中出现翘曲，甚至卷曲、碎裂。在结构设计上，降低PI薄膜热膨胀系数的主要方法是在分子结构中引入线性、刚性较强的结构，有利于分子紧密堆积，降低自由体积[5,13-14]。JIANG G L等[13]将氢化邻苯三甲酸酐（HPMDA）和双脂环二酐（HBPDA）与含有棒状酰胺键的二胺聚合，所得薄膜透光率T400nm达到85.8%，并且CTE为33.4×10-6/K。T MATSUMOTO等[14]设计合成了含脂环的二酐单体，与刚性联苯及棒状酰胺结构的二胺聚合，所得CPI薄膜的最低CTE值达到15×10-6/K。
本研究设计并合成了结构中同时含有脂环和酰胺结构的新型二酐单体（TCDA），将其与2,2′-双（三氟甲基）-4,4′-二氨基联苯（TFMB）、反-1,4-环己二胺（t-CHDA）、1,4-双（4-氨基-2-三氟甲基苯氧基）苯（6FAPB）、二氨基二苯醚（ODA）以及3,3′-二氨基苯砜（APS）聚合，研究了同时含有脂环结构和酰胺结构的二酐对透明聚酰亚胺薄膜热膨胀性能、耐热性、光学性能和力学性能的影响规律。
1 实验
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1.1 原材料
反式1,4-环己烷二羧酸、氯化亚砜，上海阿拉丁生化科技股份有限公司；4-氨基邻苯二甲酸，自制；N,N-二甲基乙酰胺、四氢呋喃，天津市富宇精细化工有限公司；醋酸酐，国药集团化学试剂有限公司；甲苯，西陇科学股份有限公司；2,2′-双（三氟甲基）-4,4′-二氨基联苯（TFMB）、1,4-双（4-氨基-2-三氟甲基苯氧基）苯（6FAPB）、3,3′-二氨基苯砜（APS）、二氨基二苯醚（ODA）、反-1,4-环己烷二胺（t-CHDA），萨恩化学技术（上海）有限公司。
1.2 合成部分
1.2.1 含脂环和酰胺结构的二酐单体（TCDA）的合成
称取反式1,4-环己烷二羧酸（0.015 mol，2.582 7 g）于100 mL圆底烧瓶中，加入氯化亚砜（0.225 mol，26.76 g），磁力搅拌，80℃反应3 h。减压蒸馏后干燥，获得2.5 g反式1,4-环己烷二甲酰氯。加入四氢呋喃（25 g）使其溶解，加入4-氨基邻苯二甲酸（0.024 mol，4.352 4 g）磁力搅拌，40℃反应24 h，获得白色固体。过滤，干燥后获得4.25 g四酸TCDA-COOH。将其加入到醋酸酐（0.155 mol，15.77 g）与甲苯（10 g）混合溶液中，磁力搅拌，120℃反应6 h。过滤，真空干燥，获得3.52 g（收率为89.3%）含脂环和酰胺结构的二酐TCDA。合成路线如图1所示。
1.2.2 聚酰亚胺薄膜的制备
采用传统的两步法制备聚酰亚胺，反应式如图2所示。以PI-1为例，在反应瓶中加入二胺TFMB（0.005 mol，1.601 1 g），加入溶剂DMAc（15.64 g）使其完全溶解，再加入二酐TCDA（0.005 mol，2.310 5 g），冰水浴控温，氮气保护，机械搅拌24 h，获得黏稠状的聚酰胺酸溶液，过滤除泡后将其涂布于玻璃板表面，放置于固化箱70℃保持3 h，然后升温至300℃保持1 h，得到聚酰亚胺薄膜，厚度为20 µm左右。
PI-2～PI-5薄膜是由二酐单体TCDA分别与二胺单体t-CHDA、6FAPB、ODA、APS按照类似方法制备而成。
1.3 结构与性能表征
1.3.1 核磁共振测试
室温下采用AVNEO氢谱核磁共振分析仪对合成新型二酐单体进行检测，溶剂为二甲基亚砜-d6（DMSO-d6）。
1.3.2 红外光谱分析
取0.5 g二酐单体进行傅里叶变换红外分析，采用衰减全反射模式测定。取尺寸为1 cm×1 cm的聚酰亚胺薄膜进行傅里叶变换红外分析，采用衰减全反射模式测定。测试范围为500～4 000 cm-1，以确定目标产物中的官能团。测试仪器为Bruker公司Vertex型衰减全反射红外光谱。
1.3.3 光学性能分析
采用岛津公司UV-2600i型紫外分光光度计和柯尼卡美能达CM-3600A型的分光测色计进行测试。
1.3.4 热学性能分析
（1）动态热力学分析
取尺寸为1.0 cm×2.5 cm的透明聚酰亚胺薄膜，采用Rheometric Scientific公司动态热机械分析仪（DMA）进行测试，升温速率为5℃/min，频率为 1 Hz，测试温度为50～450℃。
（2）热膨胀系数测试
取尺寸为0.4 cm×3.0 cm的透明聚酰亚胺薄膜，采用TA公司Q400型热机械分析仪（TMA）在氮气氛围下测试，升温速率为5℃/min，温度区间为50～250℃。
（3）热失重测试
取3～4 mg透明聚酰亚胺薄膜，采用PerkinElmer公司TGA-2型热重分析仪以10℃/min的速率升至100℃，降至室温后加热至800℃，氮气氛围下测试。
1.3.5 力学性能分析
取尺寸为50 mm×10 mm × 20 μm的透明聚酰亚胺薄膜，采用英斯特朗有限公司Instron-1121型力学性能试验机进行测试，拉伸速率为5 mm/min，测试结果取10个样品的有效平均值。
2 结果与讨论
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2.1 聚酰亚胺薄膜的化学结构
二酐TCDA的1HNMR谱图如图3所示，谱图中的各信号峰已进行归属。化学位移a（10.73）对应酰胺中氨基氢；化学位移b、c、d（8.39、8.02、7.95）分别对应苯环上三组氢；化学位移e（2.45）的信号峰对应环己烷中-CH上的两个氢；f、q（2.02、1.52）的信号峰对应环己烷中-CH2的氢。利用ATR-FTIR表征进一步确定TCDA结构，结果如图4所示。1 528 cm-1处为芳香环的特征吸收，1 683 cm-1和1 342 cm-1处为酰胺C=O和C-N的振动特征吸收峰，2 912 cm-1和2 853 cm-1处为-CH2的伸缩振动峰。结果表明成功合成了正确的二酐单体。
图5为PI薄膜的ATR-FTIR光谱。从图5可以看出，1 778 cm-1处为羰基C=O的不对称伸缩振动特征吸收峰，1 703 cm-1为羰基C=O的对称伸缩振动吸收峰，1 495 cm-1为与苯环相连的C-N伸缩振动吸收峰，1 373 cm-1处为C-N的伸缩振动吸收峰。同时，1 615 cm-1处未见明显的N-H弯曲振动吸收峰，表明聚酰亚胺已完全亚胺化。另外，含有-CF3的PI-1（TCDA/TFMB）、PI-3（TCDA/6FAPB）在1 322、1 249、1 159 cm-1附近存在C-F的特征吸收峰，含有醚键的PI-3（TCDA/6FAPB）、PI-4（TCDA/ODA）在1 226 cm-1附近有C-O的伸缩振动吸收峰。以上结果表明，成功合成了预期的PI薄膜。
2.2 聚酰亚胺薄膜的光学性能
利用分光光度计以及分光测色计研究了含脂环及酰胺结构的新型二酐对聚酰亚胺薄膜光学性能的影响，结果如表1及图6所示。由图6可以看出，合成的PI薄膜在可见光区（380～780 nm）均有较高的透过率（T>89%），截止波长（λcut off）在369 nm以上。其中以6FAPB、t-CHDA、TFMB为二胺制得的PI薄膜（PI-1、PI-2、PI-3），在波长550 nm处的透过率（T550）高达88%。而且，即使二胺是ODA，仍然可以得到透过率达到86%的PI薄膜。这表明采用含脂环和酰胺结构的二酐有利于提高PI薄膜的光学透明性[5]。这主要是因为PI的颜色来源于分子内和分子间的电荷转移络合物（CTC），脂肪环结构不存在π电子，能够有效地抑制聚酰亚胺链中电子流动，降低CTC效应，因此合成的PI薄膜均具有优异的光学透明性[4]。对于同一种二酐单体TCDA，将其与不同二胺聚合时，透明度以PI-3（TCDA/6FAPB）、PI-1（TCDA/TFMB）、PI-2（TCDA/t-CHDA）、PI-4（TCDA/ODA）、PI-5（TCDA/APS）的顺序降低，这是因为将具有强吸电子效应的-CF3引入到分子主链上，增加了空间位阻，限制了聚合物主链之间的相互作用和链堆积，抑制分子主链中电子的流动，极大程度地削弱了电荷转移络合物的形成。另外，由于C-F键的极化率较低，分子间作用力减弱，也是透光率提高的原因之一。此外，PI-3较PI-4具有更优异的透光性，这是因为随着醚键密度的增加，会大幅破坏共轭效应和分子链之间的相互作用，从而提高薄膜的透光性[15-16]。采用分光测色计测定了PI薄膜的色度参数(L*、a*、b*)，结果列于表1。PI薄膜的L*介于93～97，表明薄膜具有较高亮度，PI薄膜的b*均为正值，且介于2.10～14.1，表明薄膜呈现偏黄的趋势。PI-1、PI-2、PI-5的黄度指数（YI）较小，表明脂环和-CF3的存在削弱了聚合物分子链中的相互作用。此外，PI薄膜的雾度值（Haze）在0.75～2.76，表明薄膜具有较好的光学性能。综上表明，通过在二酐单体结构中引入环己烷结构，将其与不同二胺聚合，合成的PI薄膜均具有优异的光学透明性。
2.3 聚酰亚胺薄膜的热性能
热稳定性包括高热分解温度、高玻璃化转变温度（Tg）以及高温下的尺寸稳定性，对于PI薄膜在柔性显示和柔性电子中的应用尤为重要[1]，特别是对于含有脂环类结构的PI薄膜。由于脂环基团的热不稳定性，含脂环结构的PI薄膜热性能通常低于全芳香族薄膜，但其热性能劣势可以通过在结构中引入刚性结构来弥补[17-18]。本研究在含脂环结构的二酐单体中引入刚性酰胺键，提高PI薄膜的热性能，分别用TGA、DMA、TMA分析PI薄膜的热稳定性，结果如表2所示。
图7为利用静态热机械分析仪TMA表征的PI薄膜水平尺寸随温度变化的曲线，可直观反映其热膨胀系数（CTE）。从图7可以看出，在50～250℃的宽范围内，由二酐TCDA合成的PI薄膜的热膨胀系数均在（16～53）×10-6 K-1内，最低的热膨胀系数为16.2×10-6 K-1，表明含有酰胺结构单元的透明聚酰亚胺薄膜具有较低的热膨胀系数[5,13-14]。这主要是因为在主链中引入棒状酰胺结构，提高了聚合物分子链线性，而且酰胺结构也容易形成聚合物分子间氢键，提高分子链间相互作用，有利于分子紧密堆积，自由体积减小，热膨胀系数降低[17-18]。PI-1（TCDA/TFMB）和PI-2（TCDA/t-CHDA）具有更低的热膨胀系数，从结构上看，PI的CTE不仅受二酐单体中棒状酰胺结构的影响，而且与二胺结构中刚性的联苯、反式环己烷结构相关。而PI-3（TCDA/6FAPB）、PI-4（TCDA/ODA）、PI-5（TCDA/APS）的分子骨架中含有扭曲的柔性醚键、砜基团，分子链弯曲且易于旋转，构象自由度较大，导致薄膜表现出较明显的热膨胀行为，CTE明显增大。
通过动态热机械分析仪DMA测定PI薄膜的玻璃化转变温度（Tg），结果如图8所示。
从图8可以看出，除了PI-3（TCDA/6FAPB）的玻璃化转变温度较低外（257℃），其他PI薄膜均具有较高的玻璃化转变温度，但是由于脂环结构的引入，其Tg值低于全芳香结构的PI。另外，由于酰胺键的引入可增强聚合物分子链间氢键作用，成为抑制分子链段运动的因素，从而可提高Tg[1,19]。其中具有刚性联苯结构的PI-1（TCDA/TFMB）的Tg达到320℃。相比之下，由于PI-3、PI-4、PI-5聚合物分子骨架中含有大量的扭曲柔性基团醚键，构象的自由度较大使聚合物的热稳定性相对较差。这表明在聚合物分子骨架中引入脂环及酰胺结构单元，不仅可以使得制备的PI薄膜具有优异的光学透明性，对其玻璃化转变温度的提高也具有一定的贡献。
PI薄膜的耐热性通过TGA进行分析，结果如图9所示。从图9可以看出，制备的PI薄膜5%热分解温度均在400℃以上，保持了良好的耐热性。
2.4 聚酰亚胺薄膜的力学性能
PI薄膜的力学性能如表3所示。由表3可以看出，PI薄膜的断裂伸长率（εb）、拉伸模量（Et）和拉伸强度（σm）分别为6%～22%、1.8～3.1 GPa和102～146 MPa，均具有良好的力学性能。PI薄膜的力学与其分子化学结构、分子量以及成型过程有关。对于热膨胀系数最小的PI-2（16.2×10-6 K-1），其平均断裂伸长率达到21.7%，这表明含反式环己烷结构的聚酰亚胺不仅具有较低的热膨胀系数，同时还保持较好的柔韧性。含有柔性二苯醚结构的PI-4（TCDA-ODA），整体呈现出较高的拉伸强度，也具有较好的柔韧性。
3 结论
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通过在二酐单体的分子结构中引入脂环及棒状酰胺键，制得的PI薄膜不仅具有优异的光学性能，而且具有低热膨胀系数、高耐热性的特点，因此可以实现光学透明度较高的同时仍具有较低的热膨胀系数及综合性能，改善了含脂环结构PI薄膜热尺寸稳定性较差的问题。这种在结构中同时引入脂环和酰胺键的方法，可作为制备无色透明聚酰亚胺薄膜较为经济的合成路线。
基金
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  • 吉林省与中国科学院科技合作高新技术产业化专项(2020SYHZ0019)
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2021年第54卷第11期
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doi: 10.16790/j.cnki.1009-9239.im.2021.11.008
  • 接收时间：2021-05-05
  • 首发时间：2026-03-23
  • 出版时间：2021-11-22
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  • 收稿日期：2021-05-05
  • 修回日期：2021-05-26
基金
吉林省与中国科学院科技合作高新技术产业化专项(2020SYHZ0019)
作者信息
    1延边大学 理学院，吉林 延吉 133000
    2中国科学院长春应用化学研究所 高分子复合材料工程中心，吉林 长春 130021

通讯作者:

朴凤玉（1962-），女（朝鲜族），吉林延吉人，教授，博士，主要从事抗癫痫小分子药物合成的研究。
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2种不同金属材料的力学参数
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
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