| Summary: | MoS<sub>2</sub>/C<sub>3</sub>N<sub>4</sub> (MS-CN) composite photocatalysts have been synthesized by three different methods, i.e., in situ-photodeposition, sonochemical, and thermal decomposition. The crystal structure, optical properties, chemical composition, microstructure, and electron transfer properties were investigated by X-ray diffraction, UV-vis diffuse reflectance spectroyscopy, X-ray photoelectron spectroscopy, electron microscopy, photoluminescence, and in situ electron paramagnetic resonance spectroscopy. During photodeposition, the 2H MoS<sub>2</sub> phase was formed upon reduction of [MoS<sub>4</sub>]<sup>2−</sup> by photogenerated conduction band electrons and then deposited on the surface of CN. A thin crystalline layer of 2H MoS<sub>2</sub> formed an intimate interfacial contact with CN that favors charge separation and enhances the photocatalytic activity. The 2H MS-CN phase showed the highest photocatalytic H<sub>2</sub> evolution rate (2342 μmol h<sup>−1</sup> g<sup>−1</sup>, 25 mg catalyst/reaction) under UV-vis light irradiation in the presence of lactic acid as sacrificial reagent and Pt as cocatalyst.
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