Poly(amide-imide)-silica hybrid films were prepared using the sol-gel process of tetraethoxysilane (TEOS). A dianhydride-terminated poly(amide-imide) oligomer was prepared by the reaction of 4,4`-diphenylmethanediisocyanate (MDI) and trimellitic andydride (TMA) (MDI:TMA = 2:3 equivalents) in N-methylpyrrolidone (NMP) at 120 °C. One equivalent of 4,4′-diaminodiphenylmethane (DADPM) was added to the oligomer solution at room temperature to form the poly(amide-imide) precursor having carboxylic acid groups.The hydrolysis-polycondensation of TEOS could be carried out in the solution, and the poly(amide-imide)-silica hybrid film was obtained by casting the homogeneous silica-containing solution onto a glass plate, followed by heating at 300 °C. The silica content was 33 wt%, and silica particles with diameter of about 2 μm were observed in the hybrid films by scanning electron microscopy (SEM).
Keywords:sol-gel process, poly(amide-imide)-silica hybrid, 4,4`-diphenylmethanediisocyanate, trimellitic andydride, 4,4′-diaminodiphenylmethane, tetraethoxysilane
IntroductionThe sol-gel process is a method for preparation of inorganic metal oxides starting from organic metal alkoxides.The reaction consists of hydrolysis of the metal alkoxides, followed by polycondensation of the hydrolyzed intermediates. The sol-gel process has been applied in a polymer matrix to prepare inorganic and organic hybrid materials [1]. Polyimide-silica hybrid films have been successfully prepared by the sol-gel reaction of TEOS in polyamic acid solution, with subsequent heating of the resulting film at 270 °C. The hybrid film exhibited a higher modulus, lower coefficient of thermal expansion, and higher10 wt% loss temperature than non-hybrid films [2].We produced enameled wire having a polyimide-silica hybrid insulation layer prepared by the sol-gel process of TEOS [3,4]. TEOS was hydrolyzed and then polycondensed in a Kapton-type polyamic acid varnish, which is NMP solution, and the conductor was coated with the