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It has been rarely reported the morphological control of derivatives of metal‐organic frameworks (MOFs) in hydrothermal conditions for photocatalytic applications. We report here a family of highly efficient composite photocatalysts composed of terephthalic acid/terephthalate (TPA) ligand and TiO2 with various morphologies (e. g., nanoparticles, nanosheets, and nanorods). The composites are synthesized by a simple one‐step hydrothermal method in various solvents (i. e., H2O, HF, H2SO4, HCl, and HNO3) using Ti‐based MOF (MIL‐125(Ti)) as precursor. The formation mechanism of composite materials with different morphological features is discussed. Impressively, the composite of TiO2 nanoparticles/TPA synthesized using H2O as solvent under hydrothermal condition exhibits the highest photocatalytic H2 activity among the studied materials, with a photocatalytic H2 production rate of 6.38 mmol g−1 h−1, which is approximately 7.5‐fold higher than pure TiO2 (Degussa, P25) and prominent apparent quantum efficiency (AQE) of 65 % at 365 nm. Furthermore, the mechanism of boosted photocatalytic H2 production is discussed.

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In this study, Pt-M/WO3 (M = Cu, Co, and Ni) thin films are effectively synthesized by preparing homogeneous precursor sols, spin-coating, toluene-etching, and calcination. Furthermore, the microstructural, chemical, and electrochemical properties of the WO3, Pt-Cu/WO3, Pt-Co/WO3, and Pt-Ni/WO3 thin films are also systematically compared. The results demonstrate that when compared to the WO3 thin film, the photocatalytic capability for methylene blue (MB) solution degradation is greatly increased in the Pt-M/WO3 thin films. Transfer routes for photogenerated charges and an improved photocatalytic process are suggested based on the experimental results. Due to the large difference in the work function (Φ) between the bimetallic alloy Pt-M and WO3, a bending of the energy bands at the Pt-M/WO3 interface is presented. Furthermore, the introduction of transition metals such as Cu, Co, or Ni modifies the electronic structure of Pt-M/WO3 thin films, facilitating the separation and migration of electrons and holes. Specifically, the photogenerated electrons migrate from the CB of WO3 to Pt-Co or Pt-Ni nanoparticles in the samples of Pt-Co/WO3 or Pt-Ni/WO3 thin films, while the hot electrons from the localized surface plasmon resonance (LSPR) effect of Cu could transfer to the conduction band (CB) of WO3 and other electrons generated from the photoexcitation of the WO3 semiconductor itself in the sample of the Pt-Cu/WO3 thin film. In summary, this work proposes a unique strategy for creating electron regulation in Pt-M decorated WO3 thin films for photocatalytic application.