Amorphous monodisperse sub-micron spherical zirconia and alumina/zirconia solid solution particles were prepared by hydrolysis of zirconium and aluminum salts in ethanol. The heat-treatment process of the amorphous materials in air atmosphere at 500 degrees C for 2 h leaded to the production of non-porous zirconia and alumina/zirconia solid solution in tetragonal phase. The alkaline etching process of the as-prepared alumina/zirconia solid solution resulted in the formation of mono-modal microporous material with specific surface area of 125.0 m(2) g(-1) in comparison with 2.9 m2 g(-1) for the parent material. Thermal analysis of the solid solution revealed that the incorporation of aluminum ions in the zirconia structure has decreased the phase transformation temperature from amorphous to crystalline structure. Moreover, optical study confirmed the presence of oxygen vacancy defect by substitution of tetravalent cations, Zr4+ by trivalent cations, Al3+ in zirconia lattice. (C) 2012 Elsevier Inc. All rights reserved.