Preparation of silica-supported nickel molybdenum phosphides by temperature-programmed reduction technique

Silica supported nickel molybdenum phosphides (NiMoP/SiO2) were successfully prepared by temperature-programmed reduction (TPR) reaction of phosphorous-impregnated nickel molybdenum oxides (NiMoO4) precursors with hydrogen at relatively low temperatures (530-590 degrees C) and characterized by Fourier transform-infrared spectrometry (FT-IR), X-ray diffraction (XRD), Electron probe microanalysis (EPMA) and Temperature-programmed reduction reaction (TPR). The process of solid transformation and properties of materials prepared from ammonium hydrogen phosphate (AMP)-impregnated samples were compared with those of phosphide made from phosphoric acid (PAC)-impregnated samples. Results show that the formation of a single NiMoP phase on silica significantly depends on reduction rates, phosphorous sources and phosphorous loadings. A single phase of NiMoP on SiO2 was particularly promoted at a below 5 degrees C/min of reduction rate and the starting molar ratio of Ni/Mo/P=1/1/1. A single phase of crystalline NiMoP on silica was produced from AMP-impregnated samples, while other phases of MoP, Ni2P, or NiMoP2 were appeared from PAC-impregnated samples with loading. The new phase of NiMoP2 was occurred with increasing phosphorous loading (above Ni/Mo/P=1/1/2.5) as a result of facilitated contact on the surface between the Ni-Mo bimetallic component and the phosphorous reagent.