A novel organic and inorganic hybrid aerogel of RF/SiO2 is synthesized by one-step method of sol-gel polycondensation reaction using resorcinol-formaldehyde and tetramethoxysilane (TMOS) in ethanol solution, followed by supercritical drying with petroleum ether. The influence of the ratio of raw material on the structure and properties of samples was studied by high resolution electron microscope (HREM), nitrogen adsorption-desorption and infrared ray technology (IR). The results showed that the network structures of RF/SiO2 hybrid aerogels were constituted by an intercross framework of RF and SiO2. The hybrid aerogels can be tuned in bulk density from 0.098 g/cm3 to 0.062 g/cm3 according to the ratio of raw materials. The data of nitrogen adsorption-desorption showed that BET specific surface area was changed from 254 cm2/g to 545 cm2/g, and the pore size of aerogels was in the wide range of 2-10 nm. The investigation of IR spectrum analysis exhibited that there were no chemical bonds formed between SiO2 and RF aerogel.