In order to prepare mesoporous nickel aluminate spinel with high surface area two factors:calcinations temperature and thermal treatment were investigated in this study. The preparedspinels were characterized by a variety of techniques such as XRD. TPR-H2, TEM and nitrogen adsorption. The obtained results showed that. not depending on the synthesis conditions the mainphase as NiAl204 spinel was formed over all of the samples, however. their BET surface areas were considerably effected by changing (he synthesis conditions.