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Article(id=1242756978670420305, tenantId=1146029695717560320, journalId=1149653034449285133, issueId=1242756974576775191, articleNumber=null, orderNo=null, doi=10.16790/j.cnki.1009-9239.im.2021.11.015, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1617292800000, receivedDateStr=2021-04-02, revisedDate=1620403200000, revisedDateStr=2021-05-08, acceptedDate=null, acceptedDateStr=null, onlineDate=1774225952986, onlineDateStr=2026-03-23, pubDate=1637510400000, pubDateStr=2021-11-22, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1774225952986, onlineIssueDateStr=2026-03-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1774225952986, creator=13701087609, updateTime=1774225952986, 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=108, endPage=113, ext={EN=ArticleExt(id=1242756979773522280, articleId=1242756978670420305, tenantId=1146029695717560320, journalId=1149653034449285133, language=EN, title=Influence of Dianhydride Composition on Aggregated Structure and Thermomechanical Properties of PI Films, columnId=1198664996516360309, journalTitle=Insulating Materials, columnName=Polyimide Film Special Issue, runingTitle=null, highlight=null, articleAbstract=

In order to prepare polyimide (PI) films with high order degree and stable thermomechanical properties, pyromellitic dianhydride (PMDA) monomer was introduced into biphenyltetracarboxylic acid dianhydride-p-phenylenediamine (BPDA-PDA) system, and PI films were prepared by random copolymerization method. The aggregation structure and physical properties of the PI films were analyzed by XRD, TMA, DMA, TGA, prism coupling instrument, and universal testing machine. The results show that different dianhydride composition has a significant effect on the aggregation structure and thermal mechanical properties of PI films. With the increase of PMDA-PDA segment composition, the molecular chain order degree increases, and the molecular chain spacing decreases from 0.469 nm to 0.436 nm. The birefringence value shows an upward trend in the range of 0.18‒0.22. The glass transition temperature (Tg) decreases at first and then increases in the range of 379.86‒439.05℃. The thermal expansion coefficient (CTE) increases at first and then decreases in the range of 0‒7×10-6 K-1. The tensile strength and 5% thermal decomposition temperature (T5%) show a downward trend in the range of 166‒225 MPa and 576.8‒590.4℃, respectively. When the mole fraction of PMDA is 60%, the PI film has excellent comprehensive properties with 0.22 of birefringence, 439.05℃ of Tg, 0.012 5×10-6 K-1 of CTE, 302.5℃ of heat resistance index(THRI) , and 576.8℃ of T5%.

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为了制备兼具有序度高和热力学性能稳定的聚酰亚胺（PI）薄膜，在联苯四甲酸二酐-对苯二胺（BPDA-PDA）体系中引入均苯四甲酸二酐（PMDA）单体，通过无规共聚法制备了PI薄膜，采用XRD、TMA、DMA、TGA、棱镜耦合仪和万能试验机对PI薄膜聚集态结构和物理力学性能进行分析。结果表明：不同二酐组成对PI薄膜的聚集态结构和热力学性能有显著影响，随着PMDA-PDA链段组分的增加，分子链有序度得到提高，分子链间距从0.469 nm降低至0.436 nm；双折射值在0.17～0.23内呈上升趋势，玻璃化转变温度（Tg）在379.00～439.05℃内先下降后上升，热膨胀系数（CTE）在0～7×10-6 K-1内先上升后下降，拉伸强度和5%热分解温度（T5%）分别在165～226 MPa和576.8～590.4℃内呈下降趋势。当PMDA摩尔分数为60%时，薄膜的双折射率达到最高值0.224 71，Tg为439.05℃，CTE为0.012 5×10-6 K-1，耐热指数（THRI）达到302.0℃，T5%达到576.8℃，综合热力学性能优异。

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马传国（1978-），男（汉族），山东临清人，教授，博士，主要从事高分子复合材料及功能材料的研究。
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李诗卉（1996-），女（汉族），江西上饶人，硕士生，主要从事高分子材料合成与改性的研究。

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李诗卉（1996-），女（汉族），江西上饶人，硕士生，主要从事高分子材料合成与改性的研究。

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李诗卉（1996-），女（汉族），江西上饶人，硕士生，主要从事高分子材料合成与改性的研究。

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薄膜类型拉伸强度/MPa断裂伸长率/%弹性模量/GPa
BPDA-PDA225.1±7.811.3±0.315.7±0.2
PMDA2-BPDA8-PDA212.6±5.95.6±0.305.1±0.16
PMDA4-BPDA6-PDA209.7±3.43.7±0.254.9±0.37
PMDA5-BPDA5-PDA177.7±8.83.6±0.214.6±0.14
PMDA6-BPDA4-PDA166.0±4.73.3±0.404.5±0.23
), ArticleFig(id=1245100053350695256, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978670420305, language=CN, label=表1, caption=

PI薄膜的力学性能

, figureFileSmall=null, figureFileBig=null, tableContent=
薄膜类型拉伸强度/MPa断裂伸长率/%弹性模量/GPa
BPDA-PDA225.1±7.811.3±0.315.7±0.2
PMDA2-BPDA8-PDA212.6±5.95.6±0.305.1±0.16
PMDA4-BPDA6-PDA209.7±3.43.7±0.254.9±0.37
PMDA5-BPDA5-PDA177.7±8.83.6±0.214.6±0.14
PMDA6-BPDA4-PDA166.0±4.73.3±0.404.5±0.23
), ArticleFig(id=1245100053476524384, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978670420305, language=EN, label=Tab. 2, caption=TGA results of PI films with different PMDA contents, figureFileSmall=null, figureFileBig=null, tableContent=
薄膜类型T5% /℃T30% /℃THRI /℃
BPDA-PDA590.4662.7310.6
PMDA2-BPDA8-PDA584.9657.5307.9
PMDA4-BPDA6-PDA583.8647.9304.9
PMDA5-BPDA5-PDA580.8645.2303.5
PMDA6-BPDA4-PDA576.8644.5302.6
), ArticleFig(id=1245100053568799077, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978670420305, language=CN, label=表2, caption=

不同PMDA含量的PI薄膜的热失重分析结果

, figureFileSmall=null, figureFileBig=null, tableContent=
薄膜类型T5% /℃T30% /℃THRI /℃
BPDA-PDA590.4662.7310.6
PMDA2-BPDA8-PDA584.9657.5307.9
PMDA4-BPDA6-PDA583.8647.9304.9
PMDA5-BPDA5-PDA580.8645.2303.5
PMDA6-BPDA4-PDA576.8644.5302.6
), ArticleFig(id=1245100053686239595, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978670420305, language=EN, label=Tab.3, caption=Comparison of mechanical and thermal properties of PI films with different chain skeletons, figureFileSmall=null, figureFileBig=null, tableContent=
类型Tg/℃T 5%/℃CTE/(×10-6 K-1)拉伸强度/MPa参考文献
6FDA-BPDA-TFMB317.4525.329.084.3[7]
BTDA-ODA-DAPBI370.0523.015.2157.8[6]
BPDA-ODA-PDA299.0573.017.0231.0[4]
PMDA6-BPDA4-PDA439.1576.80.01166.0本研究
), ArticleFig(id=1245100053782708592, tenantId=1146029695717560320, journalId=1149653034449285133, articleId=1242756978670420305, language=CN, label=表3, caption=

不同链骨架PI薄膜的力学性能与热性能比较

, figureFileSmall=null, figureFileBig=null, tableContent=
类型Tg/℃T 5%/℃CTE/(×10-6 K-1)拉伸强度/MPa参考文献
6FDA-BPDA-TFMB317.4525.329.084.3[7]
BTDA-ODA-DAPBI370.0523.015.2157.8[6]
BPDA-ODA-PDA299.0573.017.0231.0[4]
PMDA6-BPDA4-PDA439.1576.80.01166.0本研究
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二酐组成对PI薄膜聚集态结构和热力学性能的影响
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李诗卉 1 , 马传国 1, 2, 3 , 戴培邦 1, 2, 3 , 青双桂 4
绝缘材料 | 聚酰亚胺薄膜专题 2021,54(11): 108-113
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绝缘材料 | 聚酰亚胺薄膜专题 2021, 54(11): 108-113
二酐组成对PI薄膜聚集态结构和热力学性能的影响
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李诗卉1, 马传国1, 2, 3, 戴培邦1, 2, 3, 青双桂4
作者信息
  • 1桂林电子科技大学 材料科学与工程学院，广西 桂林 541004
  • 2广西电子信息材料构效关系重点实验室，广西 桂林 541004
  • 3电子信息材料与器件教育部工程研究中心，广西 桂林 541004
  • 4桂林电器科学研究院有限公司，广西 桂林 541004

    • 李诗卉（1996-），女（汉族），江西上饶人，硕士生，主要从事高分子材料合成与改性的研究。

通讯作者:

马传国（1978-），男（汉族），山东临清人，教授，博士，主要从事高分子复合材料及功能材料的研究。
Influence of Dianhydride Composition on Aggregated Structure and Thermomechanical Properties of PI Films
Shihui LI1, Chuanguo MA1, 2, 3, Peibang DAI1, 2, 3, Shuanggui QING4
Affiliations
  • 1School of Material Science and Engineering, Guilin University of Electronic Technology, Guilin 541004, China
  • 2Guangxi Key Laboratory of Electronic Information Materials, Guilin 541004, China
  • 3Engineering Research Center of Ministry of Education for Electronic Information Materials and Devices, Guilin 541004, China
  • 4Guilin Electrical Equipment Scientific Research Institute Co., Ltd., Guilin 541004, China
出版时间: 2021-11-22 doi: 10.16790/j.cnki.1009-9239.im.2021.11.015
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摘要
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为了制备兼具有序度高和热力学性能稳定的聚酰亚胺（PI）薄膜，在联苯四甲酸二酐-对苯二胺（BPDA-PDA）体系中引入均苯四甲酸二酐（PMDA）单体，通过无规共聚法制备了PI薄膜，采用XRD、TMA、DMA、TGA、棱镜耦合仪和万能试验机对PI薄膜聚集态结构和物理力学性能进行分析。结果表明：不同二酐组成对PI薄膜的聚集态结构和热力学性能有显著影响，随着PMDA-PDA链段组分的增加，分子链有序度得到提高，分子链间距从0.469 nm降低至0.436 nm；双折射值在0.17～0.23内呈上升趋势，玻璃化转变温度（Tg）在379.00～439.05℃内先下降后上升，热膨胀系数（CTE）在0～7×10-6 K-1内先上升后下降，拉伸强度和5%热分解温度（T5%）分别在165～226 MPa和576.8～590.4℃内呈下降趋势。当PMDA摩尔分数为60%时，薄膜的双折射率达到最高值0.224 71，Tg为439.05℃，CTE为0.012 5×10-6 K-1，耐热指数（THRI）达到302.0℃，T5%达到576.8℃，综合热力学性能优异。

聚酰亚胺薄膜  /  聚集态结构  /  热膨胀系数  /  热力学性能

In order to prepare polyimide (PI) films with high order degree and stable thermomechanical properties, pyromellitic dianhydride (PMDA) monomer was introduced into biphenyltetracarboxylic acid dianhydride-p-phenylenediamine (BPDA-PDA) system, and PI films were prepared by random copolymerization method. The aggregation structure and physical properties of the PI films were analyzed by XRD, TMA, DMA, TGA, prism coupling instrument, and universal testing machine. The results show that different dianhydride composition has a significant effect on the aggregation structure and thermal mechanical properties of PI films. With the increase of PMDA-PDA segment composition, the molecular chain order degree increases, and the molecular chain spacing decreases from 0.469 nm to 0.436 nm. The birefringence value shows an upward trend in the range of 0.18‒0.22. The glass transition temperature (Tg) decreases at first and then increases in the range of 379.86‒439.05℃. The thermal expansion coefficient (CTE) increases at first and then decreases in the range of 0‒7×10-6 K-1. The tensile strength and 5% thermal decomposition temperature (T5%) show a downward trend in the range of 166‒225 MPa and 576.8‒590.4℃, respectively. When the mole fraction of PMDA is 60%, the PI film has excellent comprehensive properties with 0.22 of birefringence, 439.05℃ of Tg, 0.012 5×10-6 K-1 of CTE, 302.5℃ of heat resistance index(THRI) , and 576.8℃ of T5%.

polyimide film  /  aggregate structure  /  coefficient of thermal expansion  /  thermomechanical property
李诗卉, 马传国, 戴培邦, 青双桂. 二酐组成对PI薄膜聚集态结构和热力学性能的影响. 绝缘材料, 2021 , 54 (11) : 108 -113 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.015
Shihui LI, Chuanguo MA, Peibang DAI, Shuanggui QING. Influence of Dianhydride Composition on Aggregated Structure and Thermomechanical Properties of PI Films[J]. Insulating Materials, 2021 , 54 (11) : 108 -113 . DOI: 10.16790/j.cnki.1009-9239.im.2021.11.015
正文
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0 引言
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聚酰亚胺（PI）薄膜由于其耐高温、耐腐蚀、突出的热性能和物理力学特性，作为工程塑料在电子信息、国防科技、航空航天和医疗等领域发挥了重要的作用[1]。其中，PI薄膜材料在电子封装材料中的应用倍受关注[2]，随着现代电子信息技术的快速发展，对电子封装材料提出了更高要求。热力学性能是影响薄膜作为封装材料的重要因素，控制薄膜的聚集态结构以提高其热力学性能是解决问题的关键。目前，对PI薄膜聚集态结构进行调控的常用策略是通过单体的选择进行分子结构设计。一般刚性棒状PI分子链的结构更加规整，易于有序排列，将刚性棒状、平面结构或短链二酐和二胺单体引入PI分子链中，能有效促进分子链的有序排列和分子取向[3]。通常选择两种及以上性质差异较大的二胺单体并通过改变二胺的组成，实现对PI分子链结构及性能的调控。韩松锋等[4-5]采用BPDA与3种不同二胺4,4′-二胺基二苯醚（ODA）、对苯二胺（PDA）和2-（4-氨基苯基）-5-氨基苯并噁唑（DAPBO）聚合反应制备PI薄膜，通过调控刚性和柔性二胺的比例，显著改变了PI薄膜的聚集态结构以及热力学性能。YU X等[6]通过调整ODA和2-（4-氨基苯基）-5-氨基苯并咪唑（DAPBI）两种二胺的比例，合成含有不同比例ODA-BTDA和DAPBI-BTDA链段的PI薄膜，结果显示，当刚性的DAPBI-BTDA链段含量为80%时，薄膜的热膨胀系数（CTE）下降至与铜箔进行良好匹配。相关研究表明，调控两种二酐单体同样适用于制备高性能PI薄膜。张明艳等[7]将刚性二酐BPDA引入4,4′-（六氟异丙烯）二酞酸酐（6FDA）-4,4′-二氨基-2,2′-双三氟甲基联苯（TFMB）链段中，通过优化PI分子链结构制得兼具高透明与优异热力学性能的PI薄膜。吴晓等[8]将刚性均苯甲酸二酐（PMDA）引入3,3′,4,4′-二苯醚四羧酸二酐（ODPA）-4,4′-二氨基联苯（BZD）链段中，随着PMDA含量的增加，PI薄膜的有序度上升。颜善银等[9]制备了共聚二酐4-苯基-2,6-双（4-氨基苯基）吡啶（PBAP）-ODPA-双酚A型二酐（BPADA）型PI薄膜，不仅改进了PI薄膜的溶解性，且实现了对热性能和力学性能的调控。
从前人研究可知，联苯型PI薄膜是迄今有机聚合物中拥有最高耐热性的材料，但联苯结构存在一定空间位阻，使分子链运动困难、有序度下降，导致其综合热力学性能较差，CTE依旧处于较高水平，限制了其在电子封装材料领域的应用。本文通过调控两种二酐的方式，在耐热性优异的BPDA-PDA链段中引入刚性棒状短链二酐PMDA，在保证高热稳定性的情况下，促进分子链形成规整的排列，继而改善PI薄膜的聚集态结构以及提高热力学性能。采用两步热亚胺化法制备了二酐比例不同的三元型PI薄膜，系统研究不同比例二酐对PI薄膜聚集态及热力学性能的影响，通过调节两种二酐的比例调控二酐型PI薄膜的性能，继而满足电子封装材料的技术指标。
1 实验
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1.1 主要原材料
均苯四甲酸二酐（PMDA）、3,3′,4,4′-联苯四甲酸二酐（BPDA）、对苯二胺（PDA）和二甲基乙酰胺（DMAc）均购于上海阿拉丁生化科技股份有限公司。
1.2 实验步骤
（1）聚酰胺酸（PAA）合成：将二酐和二胺等摩尔量进行实验，首先在250 mL烧瓶中加入适量的二胺PDA与一定量的极性溶剂DMAc，在电动搅拌机300 r/min转速下进行搅拌溶解，待PDA溶解完全后开始加入二酐，每半小时依次加入50%、20%、20%、10%的二酐，选取PMDA、BPDA的摩尔比为0∶10、 2∶8、4∶6、5∶5、6∶4，先将BPDA加入完成后再加入PMDA，完成之后搅拌反应2 h生成PAA。
（2）热亚胺法制备PI薄膜：将上一步合成的PAA在框式涂覆器的辅助下在干净的玻璃板上涂覆成膜，然后放入烘箱中按照60℃/1 h+100℃/1 h+150℃/1 h+200℃/1 h+250℃/1 h +300℃/0.5 h+380℃/0.5 h的升温程序进行热亚胺化处理，结束后，待玻璃板冷却后放入热水中进行揭膜，经干燥后即制得最终薄膜，厚度在0.04 mm左右。根据PMDA m-BPDA n-PDA进行命名，其中m为PMDA的摩尔量，n为BPDA的摩尔量（m+n=10）。图1给出了PI薄膜的反应方程式。
1.3 测试方法及仪器设备
采用X射线衍射仪（XRD，D8-ADVANCE型，德国布鲁克公司）测试PI薄膜的聚集态结构，测试范围为10°～80°。采用静态热机械分析仪 （TMA，Q400型，TA公司）测试薄膜的热膨胀系数（TE），试样尺寸为16 mm×4.5 mm，预加载力为0.05 N，从室温升温至300℃，加热速率为10℃/min，取温度为50～200℃的数据用于计算CTE。采用动态热机械分析仪（DMA，Q800型，TA公司）测试薄膜的玻璃化转变温度Tg，试样尺寸为18 mm×6 mm，温度范围为室温至520℃，加热速率为10℃/ min。采用热重分析仪（TGA，SDT-Q600型，TA公司）测试薄膜的热稳定性，测试温度范围为20～900℃，升温速率为10℃/min。采用电子万能试验机（KDL型，扬州市江都区凯德试验机械有限公司） 按照GB/T 1040.1—2006进行拉伸试验，试样尺寸为150 mm×15 mm，加载速度为2 mm/min，每组测试5个试样。采用棱镜耦合仪 （Prism Coupler，2010M型，美国Metricon公司）以横向电（TE）和横向磁（TM）模式进行折射率测量，平面内和平面外折射率之差为样品的双折射率。
2 结果与讨论
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2.1 聚集态结构分析
采用广角 X 射线衍射仪对不同PMDA含量的PI薄膜的聚集态结构进行分析，结果如图2所示。
由图2可知，只有BPDA-PDA型PI薄膜在18.9°、21.3°以及25.5°出现了弱的衍射峰，其他薄膜仅在20°左右出现一个宽峰，且随着PMDA含量的增加，宽峰向右偏移，对应BPDA-PDA在25.5°出现的衍射峰逐渐消失。根据布拉格方程2dsinθ=nλ（λ=0.154 06 nm，n=1）计算得出，随着PMDA含量的增加，该系列薄膜的分子链间距（d）从0.469 nm降低至0.436 nm，表明刚性PMDA-PDA链段的增加使分子链引入更多的高规整有序结构，促进聚合物面内取向的发展，分子链间的相互作用增大[10]。利用ChemDraw软件建立了BPDA-PDA和PMDA-PDA二聚体结构的分子模型，其能量构象最低的模型如图3所示。BPDA-PDA分子链虽呈平面结构但是分子链与X轴方向有一定角度呈现弯曲构像，而PMDA-PDA二聚体分子链呈现刚直性，有利于在面内取向，这与XRD结论相符。
2.2 面内取向度分析
通常，在热亚胺化过程中溶剂挥发、分子链收缩会促使自发取向[11]。双折射率为平面内和平面外折射率之差Δn（∆n=nTE-nTM），用于表征平面内分子取向[12]。图4是不同分子结构PI薄膜的双折射率，双折射率越高表示PI分子链面内取向度越高。从图4可以看出，随着PMDA含量的增加，薄膜的双折射率基本上呈线性上升的趋势，当PMDA的摩尔分数为60%时，PI薄膜达到最高的双折射率0.224 71，较BPDA-PDA二聚体的双折射率0.175 36提高了28%，说明此含量下PI薄膜面内取向度达到最高。
2.3 拉伸强度
表1为不同二酐组成的PI薄膜的力学性能情况。
由表1可知，PI薄膜的拉伸强度在165～225 MPa，断裂伸长率在3.3%～11.3%，弹性模量在4.5～5.7 GPa，随着PMDA含量的增加，取向度和堆砌密度增加，拉伸强度、断裂伸长率及弹性模量呈下降趋势，这是因为刚棒型的PMDA-PDA链段比半刚型BPDA-PDA链段的结晶性好，而结晶性好的聚合物结晶一般是分布不均匀的，会存在缺陷导致应力集中，从而导致拉伸强度下降。同时PMDA-PDA刚性大且含量多时，体系中大分子链的刚性增强，链不易旋转，导致苯环密度高，不易弯曲变形而发生脆性断裂，所以PI薄膜的断裂伸长率和弹性模量下降。值得注意的是，在PMDA摩尔分数大于40%后，拉伸强度陡然下降，暗示着对应薄膜的聚集态结构发生显著变化。
2.4 热性能分析
不同PMDA含量的PI薄膜的热失重曲线如图5所示。
由图5可知，不同PI薄膜呈现一样的热失重趋势，在100℃之前有大约1%的质量损失，这是由于薄膜在空气中吸附的水分挥发所致。从100～500℃，PI薄膜没有明显的热损失，PI分子链结构未发生剧烈变化，此时PI薄膜内部主要在进行结构重排[13-14]；在500～600℃，PI薄膜出现最大失重率，薄膜发生热分解反应，O元素和N元素以气体的形式逸出[15]。在700℃之后，PI薄膜的失重情况减缓至近乎没有变化，此时薄膜中大部分杂原子以气体形式逸出结束，薄膜进入碳化阶段，若继续热解，少部分残留的杂原子将会出现第二阶段逸出[16]。具体热失重分析数值如表2所示，T5%为576～591℃，T30%为644～663℃，THRI都为300℃以上。其中，随着PMDA含量的增加，T5%、T30%及THRI均呈下降趋势，这是由于随着PMDA-PDA刚性链段含量的增加，分子链间的距离减小，薄膜的密度增大，受热后分子链蠕动困难，热量积聚在内部难以扩散，失重现象显著。
图6为不同PMDA含量的PI薄膜尺寸随温度变化以及CTE折线图。热膨胀在一定程度上依赖分子间的相互作用力以及聚合物聚集态结构。
从图6可以观察到，在150℃以下不同分子结构的PI薄膜尺寸都呈现负增长的趋势，这是由于在测试初期对薄膜施加了预加载力，由于预加载力过小没有影响薄膜宏观上尺寸的变化，但此时分子链受到力的作用有序性提高，当预加载力卸载后又伴随着温度的升高，分子链发生解取向重新回归无序的状态，宏观表现为尺寸负增长；随着温度的继续上升，链段运动引起的热膨胀行为使薄膜尺寸正增长，随着PMDA含量的增加，CTE在0～7×10-6 K-1内表现为先上升后下降的趋势，这是因为刚加入PMDA形成少量的PMDA-PDA链段扰乱了原来规整的BPDA-PDA链段，使链段运动的阻力变小，当温度逐渐上升，分子链有较低的立体阻碍，即运动剧烈表现为薄膜的线性膨胀，所以PMDA添加量少时CTE变大；但当PMDA添加到一定量时，分子链趋向于规整平面的共轭刚棒状，CTE开始下降[19]。当PMDA摩尔分数为60%时，PI薄膜的CTE为0.012 5×10-6 K-1，相比于纯BPDA-PDA型PI薄膜的CTE（4.463×10-6 K-1）降低了99.7%。
采用动态热机械分析仪对薄膜的储能模量以及损耗因子进行测试，其中定义损耗因子的峰值温度为玻璃化转变温度，结果如图7所示。
由图7(a)储能模量可知，该系列PI薄膜在100℃的储能模量为5.5～7.0 GPa，并且450 ℃仍然保留有50～900 MPa，说明该系列PI薄膜具有优异的耐热性。在450℃时，随着PMDA的含量增加，储能模量呈现先下降后上升的趋势，当PMDA摩尔分数达到50%时，储能模量有较大程度增加，这归因于刚性PMDA-PDA链段的引入提高了分子链的有序结构，同时提高了分子链间的相互作用。由图7(b)可知，该系列PI薄膜的Tg均在379.00 ℃以上，随着PMDA含量的增加，Tg出现先下降后上升的趋势，这是由于刚加入PMDA形成少量的PMDA-PDA链段扰乱了原来规整的BPDA-PDA链段，分子堆砌密度下降，自由体积增加，使链段运动的阻力变小，即Tg减小；而当PMDA继续添加，刚性PMDA-PDA链段增加，聚合物主链刚性增加且逐渐趋向于规整，同时结合XRD结果可知PMDA含量增加，分子链间相互作用增加，分子链堆砌更加紧密，链段的运动受到限制，自由体积减小，从而使Tg增加[20]。当PMDA摩尔分数达到60%时，Tg达到439.05℃。
表3比较了近年来不同链骨架PI薄膜的力学性能与热性能，不同链骨架的PI薄膜性差异明显。随着刚性单体PMDA的加入，分子链刚性增加，热尺寸变化小，PI薄膜的热性能得到明显提高，从表3中可知本研究制备的PI薄膜具有优异的综合力学性能和热性能，具有用于电子产业封装材料的潜力。
3 结论
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（1）二酐的组成对PI薄膜的聚集态结构影响显著。刚性单体PMDA的加入使分子链更加规整，分子链间距从0.469 nm降至0.436 nm，分子链间相互作用力增大，此外，薄膜的面内取向度随着PMDA含量的增加在0.175～0.225区间内呈上升趋势。
（2）二酐的组成对PI薄膜的热力学性能影响显著。PI薄膜的拉伸强度在165～226 MPa内呈下降趋势，耐热指数在302.6～310.6℃内呈下降趋势，CTE在0～7×10-6 K-1内呈先上升后下降的趋势，Tg在379～440℃内呈先下降后上升的趋势。
（3）当PMDA摩尔分数为60%时，PI薄膜的综合性能达到最优。此时，PI分子链间距为0.436 nm，双折射值达到0.224 71，同时拉伸强度为166 MPa，Tg为439.05℃，T5%达到576.8℃，THRI达到302.0℃，CTE降至0.012 5×10-6 K-1。
基金
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  • 国家自然科学基金资助项目(51763006)
  • 广西科技重大专项课题（桂科AA18242010-2）
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2021年第54卷第11期
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doi: 10.16790/j.cnki.1009-9239.im.2021.11.015
  • 接收时间：2021-04-02
  • 首发时间：2026-03-23
  • 出版时间：2021-11-22
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  • 收稿日期：2021-04-02
  • 修回日期：2021-05-08
基金
国家自然科学基金资助项目(51763006)
广西科技重大专项课题（桂科AA18242010-2）
作者信息
    1桂林电子科技大学 材料科学与工程学院，广西 桂林 541004
    2广西电子信息材料构效关系重点实验室，广西 桂林 541004
    3电子信息材料与器件教育部工程研究中心，广西 桂林 541004
    4桂林电器科学研究院有限公司，广西 桂林 541004

通讯作者:

马传国（1978-），男（汉族），山东临清人，教授，博士，主要从事高分子复合材料及功能材料的研究。
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https://castjournals.cast.org.cn/joweb/jycl/CN/10.16790/j.cnki.1009-9239.im.2021.11.015
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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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