Effect of calcination temperature has been studied on tap density, surface area, porosity, O/U ratio, morphology and crystal phases of uranium oxides. The oxides were produced by calcination of ammonium diuranate (ADU). It has been observed that O/U ratio reduces with an increase in temperature. Surface area and porosity increases with temperature, passes through maxima and then reduces. These observations have been explained using high resolution SEM. The crystal phase analysis has shown that the heating of ADU results in to α-U₃O₈ via β-UO₃.