Carbon aerogels are prepared by sol-gel process via reaction of resorcinol and formaldehyde with ammonia water as catalyst and afterward ambient drying followed by carbonization. The structure of products is characterized by X-ray diffraction, gas physisorption, scanning electron microscopy and energy spectrum analysis. Results indicte that the carbon aerogels with ammonia as catalyst show a coarser surface, and its specific surface area is about 900 m2/g, presenting continuous granular.