Bin Ahmad Mansor, Gharayebi Yadollah, Salit Mohd Sapuan, Hussein Mohd Zobir, Ebrahimiasl Saeideh, Dehzangi Arash
Department of Chemistry, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia.
Advanced Materials and Nanotechnology Laboratory, Institute of Advanced Technology (ITMA), Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia.
Int J Mol Sci. 2012;13(4):4860-4872. doi: 10.3390/ijms13044860. Epub 2012 Apr 17.
Polyimide/SiO(2) composite films were prepared from tetraethoxysilane (TEOS) and poly(amic acid) (PAA) based on aromatic diamine (4-aminophenyl sulfone) (4-APS) and aromatic dianhydride (3,3,4,4-benzophenonetetracarboxylic dianhydride) (BTDA) via a sol-gel process in N-methyl-2-pyrrolidinone (NMP). The prepared polyimide/SiO(2) composite films were characterized using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscope (SEM) and thermogravimetric analysis (TGA). The FTIR results confirmed the synthesis of polyimide (4-APS/BTDA) and the formation of SiO(2) particles in the polyimide matrix. Meanwhile, the SEM images showed that the SiO(2) particles were well dispersed in the polyimide matrix. Thermal stability and kinetic parameters of the degradation processes for the prepared polyimide/SiO(2) composite films were investigated using TGA in N(2) atmosphere. The activation energy of the solid-state process was calculated using Flynn-Wall-Ozawa's method without the knowledge of the reaction mechanism. The results indicated that thermal stability and the values of the calculated activation energies increased with the increase of the TEOS loading and the activation energy also varied with the percentage of weight loss for all compositions.
聚酰亚胺/SiO₂复合薄膜由四乙氧基硅烷（TEOS）和基于芳香二胺（4-氨基苯砜）（4-APS）与芳香二酐（3,3,4,4-二苯甲酮四羧酸二酐）（BTDA）的聚（酰胺酸）（PAA）在N-甲基-2-吡咯烷酮（NMP）中通过溶胶-凝胶法制备而成。使用X射线衍射（XRD）、傅里叶变换红外光谱（FTIR）、扫描电子显微镜（SEM）和热重分析（TGA）对制备的聚酰亚胺/SiO₂复合薄膜进行了表征。FTIR结果证实了聚酰亚胺（4-APS/BTDA）的合成以及SiO₂颗粒在聚酰亚胺基体中的形成。同时，SEM图像显示SiO₂颗粒在聚酰亚胺基体中分散良好。在N₂气氛中使用TGA研究了制备的聚酰亚胺/SiO₂复合薄膜降解过程的热稳定性和动力学参数。在不了解反应机理的情况下，使用Flynn-Wall-Ozawa方法计算了固态过程的活化能。结果表明，热稳定性以及计算得到的活化能值随TEOS负载量的增加而增加，并且活化能也随所有组合物的失重百分比而变化。
