The zinc spinel (gahnite) formation by a treatment of reaction mixtures of Zn and Al oxides, hydroxides, and salts was investigated. The influence of a preliminary mechanical activation by impact (planetary mill) and attrition (ball-ring mill) action as well as a microwave treatment was analyzed. The combined method consisting of a mechanical treatment of nitrates mixture in a planetary mill and the subsequent burning in a thermal kiln was considered as the most effective as it resulted in practically single product.