In a recent report, ozone was produced with high efficiency in perchloric acid on an anode coated with antimony-doped tin oxide. We report here that high current efficiency can be enhanced if trace amounts of a second dopant, nickel, is present. The effect of composition of the coating in terms of Ni:Sb:Sn was carefully analyzed. The optimum Ni: Sb: Sn ratio, determined to be 1: 8: 500, was determined giving a corresponding ozone generation current efficiency of over 30% at room temperature. The highest current efficiency was observed at an optimum operating potential of 2.2 V vs Ag/AgCl. Electrolytic generation of ozone in perchloric acid, sulfuric acid, and phosphoric acid at different concentrations was also studied and compared. In 0.1 M H2SO4, the ozone concentration reached 34 mg/L and a current efficiency of 36.3% could be achieved. This is about the highest current efficiency ever reported for electrolytic generation of ozone in an aqueous medium at room temperature. (c) 2005 The Electrochemical Society.