A silicon-containing arylacetylene resin, poly[(dimethylsilyl)eneethynylene phenyleneethynylene] with methoxy silyl terminal group (abbreviated MSAR) was synthesized. The resin and tetraethoxysilane (abbreviated TEOS) were used to prepare silicon-containing arylacetylene resin (abbreviated SAR) /SiO2 hybrid materials by a sol-gel method. Both the curing process of the xerogel and thermal properties of the hybrid materials were studied by FT-IR, DSC and TGA. The thermogravimetric analysis of the hybrid materials showed that Td5 (temperature of 5% weight loss) was 696°C and char yield was 92.1% at 800°C in nitrogen. A Si-C-O ceramic residue was obtained in high yield(86.8%) by sintering up to 1450°C in nitrogen.