《聚酰亚胺SiO2-TiO2杂化薄膜的制备与表征》-毕业论文.DOCVIP

哈尔滨理工大学工学硕士学位论文 哈尔滨理工大学理学硕士学位论文 - PAGE II - - PAGE III - 聚酰亚胺/SiO2-TiO2杂化薄膜的制备与表征 摘要 目前，人们已将聚酰亚胺与SiO2、TiO2和蒙脱土等单组分无机物制成杂化材料，并且表现出优异的物理化学性能，但是将两种组分同时掺入PI基体中，由于工艺、制备等因素的复杂性，该方面的报道较少。 本文以正硅酸乙酯和钛酸四丁酯为前驱体，采用原位溶胶-凝胶法和两相原位同步法制备了一系列不同含量的聚酰亚胺/SiO2-TiO2杂化薄膜，利用红外光谱、扫描电镜和XRD观察了薄膜的化学结构和微观结构，并测试了薄膜的热稳定性、电击穿场强和耐电晕性。 红外光谱分析表明两种方法制备的杂化薄膜亚胺化都很完全且杂化薄膜中存在Si-O-Ti键；扫描电镜分析表明采用两相原位同步法，以盐酸为催化剂制备的杂化薄膜中，无机粒子均匀地分散在PI基体中，粒子尺寸小于100nm，而以醋酸为催化剂制备的杂化薄膜中，无机粒子出现团聚现象。由X-射线衍射实验可知，纯PI薄膜具有一定有序度，在原位溶胶-凝胶法制备和两相原位同步法中以盐酸为催化剂制备的杂化薄膜中，这种有序程度没有被破坏，而以醋酸为催化剂制备的杂化薄膜则完全呈现无序结构。 性能测试结果表明采用两相原位同步法，以盐酸为催化剂制备的杂化薄膜的热稳定性、电击穿场强和耐电晕性较其它薄膜都有明显优势。热稳定性测试结果表明杂化薄膜热稳定性随无机含量的增加而增加，最高值为595.7℃。电性能测试中，含量为4%，二氧化硅与二氧化钛质量比为2:1的F1薄膜综合性能最好，其电击穿场强为233.7 kV/mm，耐电晕时间达到了135.5h，是纯膜耐电晕时间的61倍。 关键词　聚酰亚胺；二氧化硅；二氧化钛；原位溶胶-凝胶法；两相原位同步法 PREPARATION AND CHARACTERIZATION OF POLYIMIDE/SiO2-TiO2 HYBRID FILM Abstract At present, polyimide matrix has been hybridized with fillers such as TiO2, SiO2 and montmorillonite. Moreover some of the favorable results have been obtained. But previous studies about polyimide/inorganic hybrids were concentrated on the binary systems, in which exists a sort of inorganic portion. Due to the key challenge for complicated techniques and preparation, there were few reports about ternary systems. A series of polyimide/SiO2-TiO2 hybrid films with different contents of inorganic particle were fabricated using tetraethoxyl silicane and tetrabutyl titanate as precursor in situ with sol-gel method and both phases in situ. Chemical structure, micro-morphology and thermal stability of hybrid films was studied by means of SEM , IR and XRD，TGA ，breakdown strength and corona resistance of polyimide hybrid films was also tested. Fourier transform infrared spectra analysis show imidization of hybrid films is complete and Si-O-Ti bonds exsisted in the hybrid films. The results of SEM indicated that inorganic particles distributed uniformly in the polyimide matrix using hydrochloric catalyst and the average diameter of the particles is le