采用硅烷偶联剂KH550对介孔分子筛MCM-41内、外表面进行改性,并利用氮气吸附-脱附,傅里叶红外光谱以及小角X衍射等进行表征,其结果显示KH550分子被引入MCM-41纳米孔道中,且—NH_2基团成功嫁接到MCM-41纳米颗粒表面.凝胶液相色谱实验结果证实本文中采用的双酚A型环氧树脂为低分子量环氧.随后,采用原位聚合的方法制备不同MCM-41含量环氧树脂纳米复合材料.最后,利用正电子湮没寿命谱测量复合材料自由体积孔洞;利用透射电镜,动态热机械分析和交流击穿对复合材料宏观性能进行研究.复合材料超薄切片TEM观察结果显示,在低MCM-41添加含量时,MCM-41颗粒可在复合材料中良好分散.同时,环氧分子在外施作用力和硅烷偶联剂功能作用下引入纳米孔道,形成"有机-无机"互穿结构复合材料体系,增强MCM-41和环氧树脂间相互作用力,在低MCM-41添加含量下提高复合材料玻璃化温度(15.1%↑)和击穿电压(22.6%↑).
The silane coupling agent( KH550) was applied to modify the surface of MCM-41 and then the nitrogen absorption-desorption,Fourier transform infrared spectroscopy( FTIR) and small angel X-ray diffraction( XRD) were used to investigate the MCM-41 before and after modification. The results show that the KH550 molecules were introduced into the nanopores of MCM-41,and the —NH2group was grafted on the nanopore surface of MCM-41 particles. Besides,the gel permeation chromatography( GPC) was used to measure the epoxy relative molecular mass. The in situ method was used to cure epoxy composite with different KH550 modified MCM-41 contents. After that,the MCM-41/EP composite was measured by different tests,including positron annihilation lifetime spectroscopy( PALS) which was applied to measure the composite free volume,and the TEM,dynamic mechanical analysis( DMA) and alternate current( AC) breakdown test were used to indicate the composite macroscopic propertes. The TEM result shows that MCM-41 could be dispersed well in epoxy at contents lower than 1. 5% while agglomerate at 2. 5% content. The PALS results show that the epoxy molecules were introduced into and partly occupied the mesoporous channels by the applied force and functional effect of KH550. Then,an organic-inorganic interpenetrating network nanocomposite system could be formed. Therefore the glass transition temperature( 15. 1% ↑) and breakdown strength( 22. 6% ↑) of the composites were improved at low MCM-41 contents.