无色透明聚酰亚胺-二氧化硅纳米复合薄膜的制备与性能  

Preparation and properties of colorless and transparent polyimide-silica nanocomposite films

作　　者：任茜 王学伟 李霄 贾延江 职欣心 杨昶旭 王晓蕾 刘金刚[1] REN Xi;WANG Xuewei;LI Xiao;JIA Yanjiang;ZHI Xinxin;YANG Changxu;WANG Xiaolei;LIU Jingang(Engineering Research Center of Ministry of Education for Geological Carbon Storage and Low Carbon Utilization of Resources,School of Materials Science and Technology,China University of Geosciences,Beijing 100083,China;Weihai Newera Kesense New Materials Co.,Ltd.,Weihai 264200,China)

机构地区：[1]中国地质大学(北京)材料科学与工程学院地质碳储与资源低碳利用教育部工程研究中心,北京100083 [2]威海新元科盛新材料有限公司,山东威海264200

出　　处：《绝缘材料》2023年第2期54-62,共9页Insulating Materials

基　　金：深圳市科技计划项目(JSGG20210629144539012);山东省重点研发计划重大科技创新工程项目(2019JZZY020235)。

摘　　要：采用1S,2R,4S,5R-氢化均苯四甲酸二酐(H-PMDA)与含氟芳香族二胺2,2′-双(三氟甲基)联苯二胺(TFMB)通过一步高温溶液缩聚法制备了TFCPI半脂环族聚酰亚胺树脂及相应的无色透明聚酰亚胺薄膜TFCPI-0。采用TFCPI树脂基体,通过机械共混法与胶体纳米二氧化硅(SiO_(2))/N,N-二甲基乙酰胺(DMAC)分散液进行复合,制备了一系列不同SiO_(2)含量的无色透明聚酰亚胺复合薄膜。结果表明:当纳米SiO_(2)在复合薄膜中的质量分数为25%时,制备的TFCPI-25复合薄膜在450 nm波长处的透光率(T_(450))与黄度指数(b^(*))分别为87.8%与1.56,较TFCPI-0薄膜仅略有下降(T_(450)=88.5%,b^(*)=0.91)。TFCPI-25复合薄膜在氮气中的5%失重温度(T_(5%))和玻璃化转变温度(Tg)与TFCPI-0薄膜处于同一水平。但TFCPI-25复合薄膜在50℃时的储能模量(E′)以及50~250℃范围内的线性热膨胀系数(CTE)分别为4.86GPa与30.9×10^(-6)K^(-1),显著优于TFCPI-0薄膜(E′=3.02 GPa,CTE=39.6×10^(-6)K^(-1))。A semi-alicyclic polyimide resin (TFCPI) and the derived colorless and transparent polyimide film (TFCPI-0) were prepared by one-step high-temperature polycondensation using 1S,2R,4S,5R-hydrogenated pyromellitic dianhydride(H-PMDA) and a fluoro-containing aromatic diamine 2,2’-bis(trifluoromethyl)benzidine (TFMB).Then,a series of colorless and transparent polyimide/SiO_(2)composite films with different loading amounts of nano-sized silica fillers were prepared via mechanical blending method by mixing TFCPI matrix with dispersion liquid of colloidal nano-silica/N,N-dimethylacetamide(DMAC).The results show that the loading amounts of nano-silica in the composite films can reach to 25%.The derived composite film TFCPI-25 shows the optical transmittance at the wavelength of 450 nm (T_(450)) and yellow index (b^(*)) values of 87.5% and 1.56,respectively,which are slightly inferior to those of TFCPI-0 (T_(450)=88.5%,b^(*)=0.91).The 5% weight loss temperatures (T_(5%)) and glass transition temperature (Tg) of TFCPI-25 is at the same level with that of TFCPI-0.However,the storage modulus of TFCPI-25 at 50℃(E’50) and its linear coefficient of thermal expansion (CTE) in the range of 50-250℃ is 4.86 GPa and 30.9×10^(-6)K^(-1),respectively,which are obviously superior to those of TFCPI-0 (E’_(50)3.02 GPa,CTE=39.6×10^(-6)K^(-1)).

关 键 词：聚酰亚胺 胶体二氧化硅 纳米复合薄膜 光学性能 热性能 

分 类 号：TM215[一般工业技术—材料科学与工程] TQ323.7[电气工程—电工理论与新技术]