Abstract: Nanometer γ-Al2O3 powder was prepared by combustion synthesis method using aluminum nitrate and glycine as raw materials. The prepared γ-Al2O3 powder was characterized by means of X-ray diffraction (XRD), scanning electron microscope (SEM) and thermogravimetric-differential thermal analysis (TG-DTA). The influence of solution pH value, raw materials molar ratio, calcination temperature on the particle size, purity and morphology of γ-Al2O3 powder were investigated. Under the optimal preparation conditions of aluminum nitrate/glycine molar ratio of 3:5, a solution pH value of 2 and a calcination temperature of 750℃, fluffy γ-Al2O3 powder with high purity could be obtained.