| Summary: | The drawback of the hydrothermal technique is driven by the fact that it is a time-consuming operation, which greatly impedes its commercial application. To overcome this issue, conventional hydrothermal synthesis can be improved by the implementation of microwaves, which should result in enhanced process kinetics and, at the same time, pure-phase and homogeneous products. In this study, nanometric zinc aluminate (ZnAl<sub>2</sub>O<sub>4</sub>) with a spinel structure was obtained by a hydrothermal method using microwave reactor. The average ZnAl<sub>2</sub>O<sub>4</sub> crystallite grain size was calculated from the broadening of XRD lines. In addition, BET analysis was performed to further characterize the as-synthesized particles. The synthesized materials were also subjected to microscopic SEM and TEM observations. Based on the obtained results, we concluded that the grain sizes were in the range of 6–8 nm. The surface areas measured for the samples from the microwave reactor were 215 and 278 m<sup>2</sup> g<sup>−1</sup>.
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