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Abstract: A typical of network-like polyimide/silica composite microspheres with a high SiO2 content was successfully prepared by a suspension polymerization method. The microstructure, morphology, surface composition and thermal property were characterized by infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and thermogravimetric analyzer (TGA), respectively. The results showed that the size of PI/SiO2 composite microspheres with 20–25μm presented rough surface and an interpenetrating network had formed inside the spheres. The temperature of 5% weight loss was at about 503°C, having higher thermal stability than pure PI. [Copyright &y& Elsevier]