采用方波脉冲方法，在钯镍合金电解液中成功地电化学沉积出镍原子含量分别为12.0%、16.4%和22.6%的钯镍合金纳米颗粒. 钯镍合金纳米颗粒为球状，粒径50 ~ 80 nm. 随钯镍合金生长电位负移，合金的镍含量提高，其纳米颗粒大小基本相似但纳米颗粒数目增多，交联度提高和真实活性面积增大. 钯镍合金纳米颗粒镍含量提高，在硫酸溶液中其氢弱吸附峰电流增大. 钯镍合金纳米颗粒电极的甲酸电催化氧化活性较好，随合金纳米颗粒的镍含量提高和交联度增加，合金纳米颗粒电极的甲酸电催化氧化稳定性更高.

The Pd-Ni alloy nanoparticles with nickel atomic contents of 12.0%, 16.4% and 22.6% were successfully electrodeposited from a Pd-Ni alloy electrolyte by square wave pulse plating. The alloy nanoparticles were in the spherical shape with a diameter of 50 ~ 80 nm. As the growth potential of the alloy was negatively shifted, the nickel content of the alloy was increased, and the size of the nanoparticles was almost the same, whereas the number, the degree of crosslinking and the real active area of the nanoparticles were increased. As the nickel content of the alloy nanoparticles increased, the peak current for weakly adsorbing hydrogen was increased. The alloy nanoparticles electrodes were shown in a good electrocatalytic oxidation activity to formic acid. The electrocatalytic oxidation stability of the alloy nanoparticles was increased by the increases of the number and the degree of crosslinking.