In this work, the magnesium aluminum spinel (MgAl <sub>2</sub> O <sub>4</sub> ) was prepared by Mg and Al as precursors through a method of sol-gel subsequent with high temperature calcination. The wide range of synthetic conditions, including organic alcohols, ammonia content, dispersant, alkoxide concentration, hydrolysis time, hydrolysis temperature and calcination temperature were screened over as-prepared samples. This work provides a necessary experimental basis for the synthesis of MgAl <sub>2</sub> O <sub>4</sub> with uniform particle size of spherical structure, which has a potential to be used in many industrial and military applications.
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