In this paper, we employed a facile hydrothermal route to successfully synthesize nanosized nickel phosphide particles with controlled phases via selecting different surfactants at different temperatures and times. The phases of the as-obtained products were determined by X-ray powder diffraction (XRD) patterns and Rietveld refinement of XRD data. The morphologies of the products were characterized by (high resolution) transmission electron microscopy (HR/TEM) and field emission scanning electron microscopy (FESEM). Experiments indicated that pure Ni2P phase could be prepared when nontoxic red phosphorus and nickel dichloride were used as starting materials in the presence of polyvinylpyrrolidone (PVP, 30 K), sodium dodecylbenzene sulfonate (SDBS), cetyltrimethylammonium bromide (CTAB) or polyethylene glycol 10000 (PEG-10000) at 160 °C for 10 h. When acrylamide (AM) was selected as the surfactant, however, pure Ni12P5 phase could be prepared by prolonging the reaction time to 20 h at 160 °C, or enhancing the reaction temperature to 180 °C for 10 h. Furthermore, the experiments indicated that the pure Ni2P phase possessed a stronger photocatalytic degradation ability than the pure Ni12P5 phase.
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