Si_(3)N_(4)/PI纳米纤维自增强低膨胀系数膜的制备及表征  

Preparation and characterization of Si_(3)N_(4)/PI nanofiber self-reinforced film with low thermal expansion coefficient

作　　者：石红[1] 孙志腾 刘学清[1] Shi Hong;Sun Zhiteng;Liu Xueqing(Key Laboratory of Optoelectronic Chemical Materials and Devices of Ministry of Education,School of Chemistry and Environmental Engineering,Jianghan University,Wuhan 430056)

机构地区：[1]江汉大学光电化学材料与器件教育部重点实验室,化学环境工程学院,武汉430056

出　　处：《化工新型材料》2022年第3期100-103,共4页New Chemical Materials

基　　金：湖北省教育厅团队创新项目(T201935);海军工程大学国防科技重点实验室基金项目(6142204200608)。

摘　　要：先制备聚酰胺酸(PAA)溶液,再与纳米氮化硅(Si_(3)N_(4))混合。利用静电纺丝技术,制备氮化硅/聚酰胺酸(Si_(3)N_(4)/PAA)复合纳米纤维膜。该膜经高温亚胺化后得到氮化硅/聚酰亚胺(Si_(3)N_(4)/PI)复合纳米纤维膜,通过在Si_(3)N_(4)/PI复合纤维膜上涂敷厚度均匀的PAA溶液,再次高温亚胺化,得到一种低热膨胀系数的自增强聚酰亚胺(PI)薄膜。利用扫描电镜(SEM)、红外吸收光谱分析仪(FT-IR)、热机械分析(TMA)和动态热机械分析(DMA)等测试仪器,研究了Si_(3)N_(4)/PI纳米纤维的形貌、PAA最佳亚胺化温度以及Si_(3)N_(4)/PI纳米纤维的薄膜热膨胀系数等。结果表明:制得的纳米纤维复合膜直径均匀,PAA在300℃下亚胺化较完全,Si_(3)N_(4)/PI纳米纤维膜自增强薄膜的热膨胀系数较纯PI薄膜的热膨胀系数下降了45.4%~56.5%,Si_(3)N_(4)/PI纳米纤维膜自增强薄膜的储能模量较纯PI增加了1.36~1.78倍。An electrocalic solution was prepared by mixing an amic acid(PAA)solution with nano-silicon nitride(Si_(3)N_(4)).A silicon nitride/polyamic acid(Si_(3)N_(4)/PAA)composite nanofiber membrane was prepared by electrospinning technique.The Si_(3)N_(4)/PAA was subjected to high temperature imidization to obtain a silicon nitride/polyimide(Si_(3)N_(4)/PI)composite nanofiber membrane by applying PAA solution with the uniform thickness on the Si_(3)N_(4)/PI.At high temperature imidization,the polyimide(PI)film with low coefficient of thermal expansion was repared.The appearance,PAA optimal imidization temperature and the thermal expansion coefficient of Si_(3)N_(4)/PI nanofibers were studied by scanning electron microscopy(SEM),infrared absorption spectroscopy(FT-IR),thermomechanical analysis(TMA),and dynamic thermomechanical analysis(DMA).The results of scanning electron microscopy showed that the Si_(3)N_(4)/PAA prepared had uniform fiber diameter.The infrared absorption peak of the imidized PI film at different temperatures indicated that the PAA was more imidized at 300℃.The TMA analysis shown that the thermal expansion coefficient of Si_(3)N_(4)/PI self-reinforced film was 45.4%~56.5%times lower than that of pure PI film.Dynamic thermomechanical analysis shown that the storage modulus of Si_(3)N_(4)/PI was 1.36~1.78 times high than that of pure PI film.

关 键 词：聚酰亚胺 氮化硅 静电纺丝 自增强薄膜 热膨胀系数 

分 类 号：TQ325.9[化学工程—合成树脂塑料工业]