Physical mixing method was employing to prepare composite ZnO – Sb2O3. In this method 1 gm. of ZnO mixed with different weight of Sb2O3 (0.25, 0.50, 0.75, 1gm) and calcing in furnace (700?C) for three hours. The physical properties have been studied using liquid Impregnation Method, such as the effect of apparent porosity, the effect of Pore Volume, the effect of Bulk Density. The effect of Temperature on the physical properties such as Apparent Porosity, Pore Volume and Bulk Density was studied. The coupled characterized were investigated by using FTIR, XRD, and UV-Visible techniques.