In this study, the effect of Al₂O₃ addition as a diluent during mechanically activated self-propagating high temperature synthesis (MASHS) of Al₂O₃-ZrB₂ composite was investigated. For this purpose, the thermite mixture of Al, ZrO₂, H₃BO₃ and different amounts of Al₂O₃ (0, 3, 6, 9 wt.%) were used as the raw materials and mechanically activated for 5 h, then furnace sintering was performed at 650 °C. The results showed that by increasing the Al₂O₃ content up to 6 wt.%, the intensity of exothermic peak in the DSC curves increases, but for higher additive contents it decreases. In this case, more homogenous distribution of ZrB₂ particles with finer grain size was observed.