In this work, the photocatalytic water splitting under visible light irradiation for hydrogen production was investigated by using Eosin Y-sensitized Pt-loaded mesoporous-assembled TiO 2 –ZrO 2 mixed oxide nanocrystal photocatalysts. The mesoporous-assembled TiO 2 –ZrO 2 mixed oxide with the TiO 2 -to-ZrO 2 molar ratio of 95:5 (i.e. 0.95TiO 2 –0.05ZrO 2 ) was synthesized by using a sol–gel process with the aid of a structure-directing surfactant. The Pt loading was comparatively performed via two different effective methods: single-step sol–gel (SSSG) and photochemical deposition (PCD). The synthesized photocatalysts were methodically characterized by N 2 adsorption–desorption, XRD, UV–visible spectroscopy, SEM–EDX, TEM–EDX, TPR, and H 2 chemisorption analyses. The results revealed that the Pt loading by the PCD method greatly enhanced the photocatalytic hydrogen production activity of the synthesized mesoporous-assembled 0.95TiO 2 –0.05ZrO 2 mixed oxide photocatalyst more than that by the SSSG method. The optimum Pt loading by the PCD method was experimentally observed at 0.5wt.%, which was well associated with the maximum Pt dispersion. In addition, the PCD conditions, i.e. UV light irradiation time and UV light intensity, were investigated and optimized to be 2h and 44W, respectively.