$Al_2O_3$/NiO powder was obtained through hydrolysis-condensation reactions and thermal treatments. An organic additive, triblock copolymer surfactant P123, was added to the starting materials to control the surface area and morphology. The synthesized powder was characterized by X-ray diffractometry (XRD), field-emission scanning electron microscopy (FE-SEM) and a Brunner-Emmett-Teller surface analysis (BET). The heterogeneous catalytic activity of this powder was applied to an epoxidation reaction of styrene and was monitored using a gas chromatograph with mass spectrophotometry (GC/MS).