Thin film libraries of Ta x Ni y C 1−x−y ͑0.1 Ͻ x Ͻ 0.5,0 Ͻ y Ͻ 0.9͒ and Ta 1−x−y Ni x C y ͑0.1 Ͻ x Ͻ 0.18,0.82 Ͻ y Ͻ 0.86͒ were prepared combinatorially by dc magnetron sputtering. The as-sputtered Ta x Ni y C 1−x−y libraries with x Ͼ 0.2 showed good stability in 1.0 M H 2 SO 4 at 80°C, which indicates that good passivation against corrosion is provided by the Ta component in the ternary. The electrocatalytic activities of the Ta x Ni y C 1−x−y ͑0.1 Ͻ x Ͻ 0.5,0 Ͻ y Ͻ 0.9͒ and Ta 1−x−y Ni x C y ͑0 Ͻ x Ͻ 0.18,0.82 Ͻ y Ͻ 0.86͒ libraries before and after heat-treatment toward the oxygen reduction reaction were studied in 0.1 M. HCIO 4 solution using the rotating disk electrode technique. The heat-treated Ta x Ni y C 1−x−y ͑0.1 Ͻ x Ͻ 0.5,0 Ͻ y Ͻ 0.9͒ libraries showed obvious electrocatalytic activity while the same libraries before heat-treatment did not. The catalytic activity of the libraries improved with increasing Ni content. The best catalytic activity was found near Ta 0.26 Ni 0.73 ͑Ta 0.26 Ni 0.73 C 0.01 ͒ in the heated Ta x Ni y C 1−x−y ͑0.1 Ͻ x Ͻ 0.5,0 Ͻ y Ͻ 0.9͒ libraries and near Ni 0.16 C 0.83 ͑Ta 0.01 Ni 0.16 C 0.83 ͒ in the heated Ta 1−x−y Ni x C y ͑0 Ͻ x Ͻ 0.18,0.82 Ͻ y Ͻ 0.86͒ library. The results suggest that the heat-treatment and the Ni component play important roles in the electrocatalytic activity of this ternary system.Polymer electrolyte membrane fuel cells ͑PEMFCs͒, as a promising energy conversion device for transportation, stationary, and portable applications, have attracted a lot of attention due to their high energy densities, low operating temperatures, and lack of emissions. 1-3 The high cost of PEMFC is one of the limiting factors for their commercialization. The development of non-noble metal catalysts for reduction of oxygen at the cathode of the PEMFC could lead to significant cost reduction. Non-noble metal catalysts such as organometallic complexes, 4-6 pyrolyzed carbon-supported metal salts, 7,8 pyro1yzed carbon-supported N 4 -metal macrocycles, [9][10][11][12][13]