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In this work, an Au modified Bi2O3-TiO2 (Au/Bi2O3-TiO2) hybrid is developed as a simple and effective photocatalyst for the production of H2O2. The modification of Bi2O3 improves the charge separation of photocatalyst and significantly enhances the photocatalytic activity of Au/TiO2 for H2O2 production. In-situ electron spin resonance studies shows stepwise single-electron oxygen reduction reaction (ORR) on the Au/Bi2O3-TiO2 photocatalyst for the production of H2O2. This work demonstrates the importance of heterojunction structure photocatalyst for improved performance of TiO2 in order to produce concentrated H2O2.