Zirconium-based compounds, such as ZrO x N y , have been investigated as a cathode of polymer electrolyte fuel cells. ZrO x N y was prepared using radio-frequency ͑rf͒ magnetron sputtering under an Ar + O 2 + N 2 with heating the substrate. The solubility of ZrO x N y deposited at 500°C was less than 5 ϫ 10 −8 mol dm −3 in 0.1 mol dm −3 H 2 SO 4 at 30°C under atmospheric condition, indicating that ZrO x N y had a high chemical stability in acidic media. The effect of the heat-treatment during the film deposition on the catalytic activity for oxygen reduction reaction ͑ORR͒ and the properties of ZrO x N y has been examined. The ORR current density on ZrO x N y deposited at a substrate temperature of 800°C was ϳ30 times greater than that at 50°C. The dependence of both the ORR current density at 0.4 V and the apparent activation energy of the ORR at 0.4 V on the substrate temperature changed near 500°C. The crystalline structure of ZrO x N y also changed near 500°C. In addition, the catalytic activity for the ORR increased with the increasing crystallinity and decreasing ionization potential of the specimens. Therefore, the crystalline structure, the crystallinity, and the ionization potential might affect the catalytic activity for the ORR.