在含PdCl2、NiSO4和乙二胺的弱碱性镀液中,于Au电极上用恒电位电沉积Pd—Ni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—Ni电极.扫描电镜以及电化学测试表明,去合金化处理使Pd—Ni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Ni的优先溶出造成Pd的富集.去合金化处理的Pd.Ni电极电催化氧化甲酸的活性明显优于未处理的Pd—Ni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 treat- ment 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.