Preparation and electrochemical characterization of palladium single crystal electrodes in 0.1 M H{sub}2SO{sub}4 and HClO{sub}4 - Part I: low-index phases

摘要

The electrochemical properties of Pd(111), Pd(100) and Pd(110) single crystal bead electrodes, prepared by a novel electron beam heating and inductive annealing technique, have been characterized in 0.1 M sulfuric acid and 0.1 M perchloric acid by cyclic voltammetry and chronoamperometry. Hydrogen and (hydrogen) sulfate adsorption as well as surface oxidation were found to depend strongly on the crystallographic orientation and the nature of the electrolyte. The combination of charge displacement and voltammetric experiments allowed the determination of the potentials of zero total charge (E{sub}(pztc)) of Pd(111) and Pd(100). The values of E{sub}(pztc) in sulfuric acid were found to be more negative than in perchloric acid. The estimation of E{sub}(pztc) for Pd(110) was hampered by the superposition with hydrogen absorption. The electro-oxidation of irreversible adsorbed carbon monoxide monolayers was studied on the three low-index Pd electrodes. The onset potential of the CO oxidation reaction follows the sequence Pd(100)