Despite numerous advances in the preparation and use of GaN, and many leading-edge applications in lighting technologies, the preparation of high-quality GaN powder remains a challenge. Ammonolytic preparations of polycrystalline GaN have been studied using various precursors, but all were time-consuming and required high temperatures. In this study, an efficient and low-temperature method to synthesize high-purity hexagonal GaN powder is developed using sub-micron Ga2O3 powder as a starting material. The sub-micron Ga2O3 powder was prepared by an ultrasonic spray pyrolysis process. The GaN powder is synthesized from the sub-micron Ga2O3 powder through a nitridation treatment in an NH3 flow at 800℃. The characteristics of the synthesized powder are systematically examined by X-ray diffraction, scanning and transmission electron microscopy, and UV-vis spectrophotometer.