College of Chemistry and Materials Science, Anhui Key Laboratory of Functional Molecular Solids, Anhui Normal University, Wuhu, 241000, PR China.
Nanoscale. 2011 Jan;3(1):196-200. doi: 10.1039/c0nr00727g. Epub 2010 Nov 3.
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.
在本文中，我们通过在不同温度和时间下选择不同的表面活性剂，采用简便的水热路线成功地合成了具有可控相的纳米尺寸的磷化镍颗粒。通过 X 射线粉末衍射（XRD）图谱和 XRD 数据的 Rietveld 精修确定了所获得产物的相。通过（高分辨率）透射电子显微镜（HR/TEM）和场发射扫描电子显微镜（FESEM）对产物的形貌进行了表征。实验表明，当无毒红磷和氯化镍二水合物作为起始原料，在 160°C 下分别使用聚乙烯吡咯烷酮（PVP，30 K）、十二烷基苯磺酸钠（SDBS）、十六烷基三甲基溴化铵（CTAB）或聚乙二醇 10000（PEG-10000）作为表面活性剂，并反应 10 小时时，可以制备出纯 Ni2P 相。然而，当选择丙烯酰胺（AM）作为表面活性剂时，通过将反应时间延长至 20 小时或在 160°C 下反应 10 小时，提高反应温度至 180°C，可以制备出纯 Ni12P5 相。此外，实验表明，纯 Ni2P 相具有比纯 Ni12P5 相更强的光催化降解能力。
