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液相脈沖放電制備納米Ni-P合金粉工藝

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

  • 摘要: 采用液相脈沖放電技術,通過改變脈沖電壓、放電次數、Ni2+濃度、pH值,以及加入稀土添加劑(LaCl3、NdCl3)等途徑,研究了制備工藝中各因素對Ni-P合金粉的結構、形貌、粒徑以及對Ni2+轉化率的影響.結果表明,脈沖能量是影響Ni-P合金粉粒徑和Ni2+轉化率的主要因素,提高脈沖電壓或增加放電次數,Ni-P合金粉平均粒徑明顯減小,而Ni2+轉化率增大.聚焦光束反射測量儀(FBRM)實時監測結果表明,在放電過程中Ni-P合金粉的形核、生長速率顯著大于放電結束之后的形核、生長速率.加入LaCl3、NdCl3能使Ni-P合金粉粒徑減小,LaCl3質量濃度為0.1g·L·時制得的Ni-P合金粉平均粒徑為156nm,NdCl3質量濃度為0.05g·L-1時其平均粒徑為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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