Sustainability in catalysis is increasingly becoming the primary target in academic and industrial studies. Regarding the material perspective, designing heterojunction nanocatalysts to produce small molecules, such as hydrogen peroxide (H 2 O 2 ), has been an attractive research theme in recent decades. Nonetheless, most reported materials suffer from a complicated synthetic process with various steps and using unbenign solvents, hindering practical applications on an industrial scale. This study proposed a facile one-step way to fabricate heterostructured CdS/g-C 3 N 4 nanocatalysts to produce H 2 O 2 from water and oxygen under light and ultrasound irradiation. The results showed that the formation of H 2 O 2 mainly relies on oxygen radical species. Oxygen is initially converted into superoxide via excited electrons from CdS, followed by the formation of singlet oxygen from the oxidation process in g-C 3 N 4 sites. Interestingly, the formation of H 2 O 2 in an inert atmosphere is associated with the in situ evolution of oxygen from water oxidation due to the suitable electronic band position of g-C 3 N 4 to drive multioxidation reactions. Charge transfer characterizations illustrate the S-scheme mechanism in the catalytic process, giving a better understanding of the charge transportation phenomenon, thus providing a critical pathway in designing and developing heterojunction materials for catalysis with easier catalyst preparation and operation processes. KEYWORDS: g-C 3 N 4 , CdS, solid-state synthesis, S-scheme heterojunctions, H 2 O 2 , piezo-photocatalysis