Abstract: in(Ⅳ) oxide aerogels were synthesized by non-alkoxide sol-gel process and CO2 supercritical drying. The morphology of as-synthesized SnO2 aerogels was evaluated by field-emission scanning electron microscope (FESEM), which suggests that the skeleton is composed of spherical particles. The high-resolution transmission electron microscopy (HRTEM) reveals that the primary nano-particles are highly crystalline, and the average size of nano-crystal is between 2-3 nm. The N2 adsorption/desorption shows the aerogel has high BET surface area of 355.65 m2/g. The average skeleton particle size derived from N2 sorption method is about 2.4 nm, which agrees with results from HRTEM resolution.