Al 2 O 3 SiO 2 aerogel was prepared through mixed solgel process and ethanol supercritical drying technology using aluminum chloride hexahydrate (AlCl 3 ·6H 2 O) and tetraethoxysilane (TEOS) as precursors. Under the condition of the propylene oxide used as gelation initiators, during the process, a kind of Al 2 O 3 SiO 2 aerogel with porous and large specific surface area were achieved in our experiments. Structures and properties of Al 2 O 3 SiO 2 aerogel are investigated by means of X-ray Diffraction, Nitrogen adsorption/desorption analysis, Scanning Electron Microscopy, Fourier Transform Infrared Spectroscope, and Thermogravimetry-Differential Thermal analysis. The results showed that the Al 2 O 3 SiO 2 aerogel with the mole ratio of Al/Si = 3/1 possessed better heat-insulation performance and high-temperature stability. And it possessed a porous network structure made up of leaf shape particles. At the same time, Al 2 O 3 SiO 2 aerogel showed a low density of 0.071 g/cm 3 at room temperature, specific surface areas of 708 m 2 /g at 600°C, as well as 255 m 2 /g at 1200°C. The Al 2 O 3 SiO 2 aerogel is the polycrystalline boehmite (£-AlOOH) phase at room temperature. As the temperature growing, it transferred to £-Al 2 O 3 at 600°C, and mullite phase at 1200°C.