Abstract
We report a new electrochemical route for fabricating molybdenum and vanadium mixed oxyhydroxide films on Au electrode from Keggin-type vanadium-substituted polymolybdophosphate. The process involves a potentiodynamic reduction of aqueous 9-molybdo(VI)-3-vanadophosphosphate(V) ([PMo 9V 3O 40] 6−) in the potential region between 0 and −0.7 V versus Ag/AgCl. The resulting Mo V oxyhydroxide film electrode gave a stable redox behavior in Na 2SO 4 electrolyte of pH 3. X-ray photoelectron spectroscopy revealed that this results from oxidation/reduction of Mo 5+/Mo 6+ in the film which accompanies extraction/insertion of protons for charge compensation. The deposited V ions remained in the film upon repetitive potential cycling without affecting their oxidation state. Voltammetric data in the presence of sodium nitrite showed electrocatalytic activity of the Mo V oxyhydroxide toward the electroreduction of nitrite.
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