Abstract: In this papar, the macrostructure of ZnO/γ-Al₂O₃ samples prepared by impregnation method has been investigated systematically. The pattern of change in crystallite size and in specific surface area of the formed zinc-deficient zinc aluminate (Zn_x Al₂O_3+x 02O₃ was found to be roughly retained in Zn_xAl₂O_3+x prepared by impregnation at the temperature used in preparation and operation of catalysts, so by using the impregnation method one can prepare Zn_xAl₂O_3+x of different pore structure to satisfy various demands, Which is hardly realized in coprecipitation method.