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.

A Pd-Ni alloy film was electrodeposited on Au disc electrode at a constant potential from a weakly basic bath containing PdCl2,NiSO4 and ethylenediamine.The as-deposited film was then subjected to potential cycling in a perchloric acid solution for surface dealloying treatment.The dealloyed Pd-Ni film electrode was examined for the electrocatalytic oxidation of formic acid,and compared with the as-deposited one as well as a Pd film electrode.The FE-SEM and electrochemical measurements on the Pd-Ni films revealed that the dealloying treatment caused a surface roughening and an increase in specific surface reaction area.The ICP-AES and XPS analyses demonstrated that the preferential dissolution of Ni in the dealloying treatment led to a Pd-rich outer layer in the resultant Pd-Ni film.The electrocatalysis measurements indicated that the dealloyed Pd-Ni electrode is superior to the as-deposited Pd-Ni as well as the Pd electrode in terms of the electro-oxidation of formic acid.