Abstract: High purity Al2O3 powders were deposited successfully by the spray pyrolysis method using AlCl3·6H2O as raw material. The phase composition and the micro-morphology of pyrolysis products were studied by X-ray diffraction (XRD) and SEM. Specific surface area was also analyzed by specific surface area analyzer. The thermodynamics results showed that the main pyrolysis reaction happens in the range of 800~2200 K and increasing the reaction temperature is advantageous to the reaction. The pyrolysis temperature is 800°C for AlCl3 by DSC-TGA analysis. The experimental results indicated that the optimum conditions are as follows: the mass fraction of AlCl3 solution is 15%; the pyrolysis time is 20 min in the range of 750~850°C. Meanwhile, the pyrolysis products meet the demands of electronic aluminum.