This paper reports the results of an investigation of the preparation and characterization of carbon-supported ternary PtVFe electrocatalysts. The catalysts were prepared by assembly of pre-synthesized PtVFe nanoparticles onto carbon support. The size, composition, and metal loading on carbon support were controllable. The carbon-supported PtVFe nanoparticles were further processed by thermal treatment, which were optimized for achieving effective shell removal and alloy formation. The structure and morphology of the catalysts were characterized using several techniques, including TEM, DCP-AES, FT-IR, TGA, and XRD. The catalysts were also examined for their intrinsic kinetic activities towards oxygen reduction reaction (ORR). The results have shown that the ternary catalysts are highly active for electrocatalytic ORR. Implications of our findings to applications in fuel cell catalysis are also discussed. (c) 2006 Elsevier Ltd. All rights reserved.