Silica/epoxy resin hybrid materials are prepared with tetraethylorthosilicate (Si(OC2H5)4, TEOS) and γ-aminoproplytriethyoxysiliane (H2N(CH2)3Si(OC2H5)3, APTES) as the silica sources, epoxy resin as the polymer matrix, by the means of in-suit sol-gel method. The dosages of TEOS and APTES in preparation of hybrid materials, and the sol-gel temperature for silica resources are discussed to make sure of the influence of the structure and properties on hybrid materials. The dispersion of Silica in the epoxy resin are examined by transmission electron microscopy (TEM).The image of fracture surfaces of hybrid materials are examined by scanning electron microscopy (SEM). The glass transmission temperatures (Tg) are tested by differential scanning calorimeter (DSC) to characterize the heat resistance of hybrid materials. The optimum mechanical performance and heat resistance for silica/epoxy resin hybrid materials are achieved with 3wt% TEOS and APTES 2wt% employed in this materials when sol-gel temperature is 60°C. In general, the mechanical and thermal properties of the hybrid materials were improved greatly as compared with the pure epoxy resin.