β-gallia (β-Ga2O3) has been investigated for adoption in power semiconductor wafers; however, it is a promising scintillating material for X-ray detection screens. Thus, the research on methods for growing β-gallia crystals has attracted considerable attention. Herein, 15-μm thick Ga2O3–Al2O3 solid solution films with β-gallia structure were synthesized using metal–organic chemical vapor deposition (CVD) at deposition rate of 15 μm h−1. A high scintillation light yield of 5400 photons per 5.5 MeV and a fast decay response of 5.1 ns of the produced films were observed, which were comparable or superior to those of the β-Ga2O3 single crystals. CVD method proved advantageous for the rapid synthesis of micrometer-thick Ga2O3-based scintillation screens.