γ-LiAlO2 plate-like nanostructures have been synthesized by lyophilization of a gel precursor prepared by coprecipitation process. Aqueous solutions of Al(NO3)3.9H2O and LiNO3 were used as precursors, and NaOH was used as precipitant agent. After freeze-drying, the samples were calcined at several temperatures for characterization. The lyophilization process allowed the preparation of γ-LiAlO2 phase at 750 °C, which remained stable until temperatures about 1150 ºC, without the formation of other undesired phases as LiAl5O8.