液相脉冲放电制备纳米Ni-P合金粉工艺

Synthesis of Ni-P nanopowders via pulse discharging in aqueous solution

  • 摘要: 采用液相脉冲放电技术,通过改变脉冲电压、放电次数、Ni2+浓度、pH值,以及加入稀土添加剂(LaCl3、NdCl3)等途径,研究了制备工艺中各因素对Ni-P合金粉的结构、形貌、粒径以及对Ni2+转化率的影响.结果表明,脉冲能量是影响Ni-P合金粉粒径和Ni2+转化率的主要因素,提高脉冲电压或增加放电次数,Ni-P合金粉平均粒径明显减小,而Ni2+转化率增大.聚焦光束反射测量仪(FBRM)实时监测结果表明,在放电过程中Ni-P合金粉的形核、生长速率显著大于放电结束之后的形核、生长速率.加入LaCl3、NdCl3能使Ni-P合金粉粒径减小,LaCl3质量浓度为0.1g·L·时制得的Ni-P合金粉平均粒径为156nm,NdCl3质量浓度为0.05g·L-1时其平均粒径为72nm.

     

    Abstract: The effects of pulse potential,discharging times,Ni2+ concentration,pH value and rare earth additives(LaCl3,NdCl3) on the conversion ratio of Ni2+ as well as the structure,shape and average diameter of Ni-P nanopowders prepared by pulse discharging in solution were investigated by X-ray diffraction(XRD),field emission scanning electron microscopy(FESEM),and focused beam reflectance measurement(FBRM).It is indicated that discharging energy is the key factor that influences the size of Ni-P nanopowders and the conversion ratio of Ni2+.With the increasing of pulse potential or discharging times,the average diameter of Ni-P nanopowders decreased while the conversion ratio of Ni2+ increased.The real-time monitoring results of FBRM showed that the velocities of nucleating and growing of Ni-P particles during the course of discharging were remarkably higher than those after discharging.The size of Ni-P nanopowders could be reduced by adding LaCl3 or NdCl3 to precursor solution.The average diameters of Ni-P nanopowders were 156 nm at the LaCl3 concentration of 0.1 g·L-1 and 72 nm at the NdCl3 concentration of 0.05 g·L-1,respectively.

     

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