This study introduces a novel approach for producing CeO2-ZrO2 powder through an electrochemical route. To this end, nanocrystalline CeO2-ZrO2 powder was coprecipitated electrochemically by the cathodic electrogeneration of hydroxyl ion from an aqueous ammonium nitrate electrolyte. The powder was deposited potentiostatically in a quiescent solution at room temperature onto a stainless steel inverted shaft-disk electrode. The average crystallite size was 5 +/- 1 nm determined from transmission electron microscopy. The powder composition, measured by X-ray fluorescence, was 18 mol % ZrO2 (82 mol clo CeO2) and a single phase of cubic structure was verified by X-ray diffraction. The ultrafine particle size, composition, and crystallinity that the mixture exhibits are requisites for use as a catalyst or as a desulfurization sorbent.