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The present communication reports on a facile one-step solvothermal synthesis of highly crystallized MoS 2/TiO 2 nanocomposites for the first time. The TEM image shows the generation of a large amount of TiO 2 nanoparticles with diameters in the range of 5–8 nm. The photocurrent measurement suggests that loading a certain amount of MoS 2 can effectively improve separation of photogenerated carries. Cyclic voltammograms measurements reveal that TiO 2 modified with 1.0 wt% MoS 2 can reduce hydrogen reduction overpotential, thereby leading to enhanced photocatalytic activity. Photocatalytic H 2 evolution test suggests that 1.0 wt% MoS 2/TiO 2 nanocomposites show superior photocatalytic activity, and the H 2 production rate achieves 119.5 μmol h −1 g −1 and is about 19 times higher than that of TiO 2 alone, which could be attributed to the short diffusion distance in TiO 2 nanoparticles, efficient interfacial electron transfer from TiO 2 nanoparticles to MoS 2 surface, and reduced hydrogen reduction overpotential. Furthermore, the MoS 2/TiO 2 photocatalysts are stabile during the photocatalytic H 2 evolution test. Graphical abstract: [Figure not available: see fulltext.]. [ABSTRACT FROM AUTHOR]