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This study provided a novel method for depositing high-quality GaOxNyfilm by plasma-enhanced atomic layer deposition (ALD). To obtain a uniform nitrogen and oxygen composition, O2and NH3were led into the ALD chamber at the same time. It was found that the growth rate, composition, and optical properties of the GaOxNyfilm could be precisely controlled by adjusting the O2:NH3ratio. The energy band gap was well tuned from 3.46 to 4.78 eV with increased O2ratios. The detailed analysis of the X-ray photoelectron spectra proved the existence of Ga–O, Ga–N, and N–Ga–O bonds in prepared GaOxNyfilm. The surface, interface, and construction of the GaOxNyfilms were different with GaN and Ga2O3films through transmission electron microscope characterization. Then a possible growth mechanism was demonstrated based on these findings. The energy band structure of all GaOxNyfilms deposited in this study was obtained from a detailed analysis of the valence band spectra. Importantly, the GaOxNywas found to exhibit lower leakage current and higher breakdown voltage than both GaN and Ga2O3. These findings offered a foundation and proved this material will present brilliant application prospects in photodetection, photoelectrochemical water splitting, and high-voltage devices.