Electrodeposition of porous Co layers and their conversion to electrocatalysts for methanol oxidation by spontaneous deposition of Pd

Electrocatalysts for methanol oxidation were prepared through a two stage deposition process: porous cobalt layers were deposited, by cathodic reduction of Co2+ ions, and then modified by spontaneous deposition of Pd. A basic sulphate solution and a mildly acid chloride solution were compared as media for the electrodeposition of Co. Deposits with the highest surface roughness were obtained in the chloride solution, at large current densities. Pd was deposited onto the Co porous layers by immersing them in acid deaerated PdCl2 solutions, at open circuit. The Pd loading and the Pd surface area were estimated by UV-visible spectroscopy and by cyclic voltammetry, respectively. The Pd-modified Co electrodes were tested as anodes for methanol oxidation and compared to the similarly prepared Pd-modified Ni electrodes. The former exhibited better stability of performance and higher methanol oxidation peak currents per unit Pd mass, ca. 200 A g−1.