In this study, (GaN)_1-x(ZnO)_x solid solution nanoparticles with a high zinc content are prepared by ultrasonic spray pyrolysis and subsequent nitridation. The structure and morphology of the samples are investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The characterization results show a phase transition from the Zn and Ga-based oxides (ZnO or ZnGa₂O₄) to a (GaN)_1-x (ZnO)_x solid solution under an NH3 atmosphere. The effect of the precursor solution concentration and nitridation temperature on the final products are systematically investigated to obtain (GaN)_1-x(ZnO)_x nanoparticles with a high Zn concentration. It is confirmed that the powder synthesized from the solution in which the ratio of Zn and Ga was set to 0.8:0.2, as the initial precursor composition was composed of about 0.8-mole fraction of Zn, similar to the initially set one, through nitriding treatment at 700°C. Besides, the synthesized nanoparticles exhibited the typical XRD pattern of (GaN)_1-x(ZnO)_x, and a strong absorption of visible light with a bandgap energy of approximately 2.78 eV, confirming their potential use as a hydrogen production photocatalyst.