Nanocrystalline nickel phosphide (Ni _(12) P _(5) ) was successfully synthesized by a simple hydrothermal method via using NiCl _(2) and red phosphorus as raw materials. The crystal structure, morphology and surface chemical compositions of the as-prepared sample were characterized by X-ray diffraction, scanning electron microscope and X-ray photoelectron spectroscopy techniques, respectively. Its catalytic activity for the hydrogen evolution from water was investigated under visible light irradiation ( λ ≥ 420 nm) with fluorescein sodium as the photosensitizer and triethanolamine as the sacrificial electron donor, respectively. The results indicated that the Ni _(12) P _(5) sample showed high catalytic activity (10?760 μmol h ~(?1) g ~(?1) , TOF = 9.3 h ~(?1) ) and good stability (15 h) in the present system. The electrochemical results revealed that Ni _(12) P _(5) had a high cathodic current and small charge transfer resistance, which further suggested Ni _(12) P _(5) indeed could efficiently catalyze the evolution of hydrogen.
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