磷化镍微纳米材料的水热合成与表征

Hydrothermal Synthesis and Characterization of Nickel Phosphide Micro/Nano-Materials

以无毒的红磷代替白磷作为磷源,以硝酸镍为镍源,利用水热合成法成功实现了磷化镍的温和制备。考察了磷和镍物质的量比、水热温度、水热反应时间和溶剂体系对磷化镍晶相组成及其形貌的影响。结果表明,在水热温度120℃,水热时间12h,原料初始磷和镍物质的量比为6时即可得到纯净的六方相的Ni_2P。磷和镍物质的量比增加有利于四方相结构的Ni_(12)P_5向六方相结构的Ni_2P转变,而温度升高则有利于Ni_2P向Ni_(12)P_5转变,通过控制磷和镍物质的量比和水热温度可以实现磷化镍的相态和形貌的可控合成。反应时间和乙二醇-水体系中溶剂体积比的变化,并未改变磷化镍的组成,但对产物的结晶度有一定影响。

Nickel phosphide catalysts were successfully synthetized by using non-toxic red phosphorus instead of white phosphorus and nickel nitrate as raw materials with water as solvent at a low temperature by hydrothermal method.The influence of several factors in the process of synthesis was studied,including molar ratio of P/Ni,hydrothermal reaction temperature,reaction time and different solvent system.The results showed that the pure hexagonal nickel phosphide（Ni2P）could be successfully prepared under the initial P/Ni mole ratio of 6and the reaction temperature of 120 ℃ and the reaction time of 12 h.Increasing ratio the initial P/Ni mole,pure tetragonal nickel phosphide（Ni（12）P5）could be transformed into pure hexagonal nickel phosphide（Ni2P）,while increasing the temperature,Ni2P could be gradually transformed into Ni（12）P5.With reaction time prolonging,or the solvent volume ration in water- glycol system changed,Ni2P phase could be obtained as well,but the crystallinity of products was changed.