在含PdC l2、N iSO4和乙二胺的弱碱性镀液中,于Au电极上用恒电位电沉积Pd-N i合金薄膜,后经酸性溶液中循环伏安法处理,得到去合金化的Pd-N i电极.扫描电镜以及电化学测试表明,去合金化处理使Pd-N i镀膜表面微观粗糙度增加,比表面积增大;ICP-AES和XPS分析证实合金表层N i的优先溶出造成Pd的富集.去合金化处理的Pd-N i电极电催化氧化甲酸的活性明显优于未处理的Pd-N i电极和多晶Pd电极. Pd-Ni alloy thin films were electropositively deposited on Au electrodes in Pd-Ni alloy containing PdCl 2, NiSO 4 and ethylenediamine and then subjected to cyclic voltammetry in acidic solution to obtain de-alloying Of Pd-Ni electrode.The scanning electron microscopy and electrochemical tests showed that the micro-roughness of Pd-Ni coating surface increased and the specific surface area increased with de-alloying treatment.The preferential dissolution of Ni on alloy surface was confirmed by ICP-AES and XPS analysis Resulting in the enrichment of Pd.The electrocatalytic oxidation of formic acid to the Pd-Ni electrode to alloying treatment was significantly better than the untreated Pd-Ni electrode and the polycrystalline Pd electrode.