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Pt–Fe/C catalysts were prepared by a modified polyol synthesis method in an ethylene glycol (EG) solution, and then were heat-treated under H2/Ar (10 vol.%) at moderate temperature (300 °C, Pt–Fe/C300) or high temperature (900 °C, Pt–Fe/C900). As comparison, Pt–Fe/C alloy catalyst was prepared by a two-step method (Pt–Fe/C900B). X-ray diffraction (XRD) and transmission electron microscopy (TEM) images show that particles size of the catalyst increases with the increase of treatment temperatures. Pt–Fe/C300 catalyst has a mean particle size of 2.8 nm (XRD), 3.6 nm (TEM) and some Pt–Fe alloy was partly formed in this sample. Pt–Fe/C900B catalyst has the biggest particle size of 6.2 nm (XRD) and the best Pt–Fe alloy form. Cyclicvoltammetry (CV) shows that Pt–Fe/C300 has larger electrochemical surface area than other Pt–Fe/C and the highest utilization ratio of 76% among these Pt-based catalysts. Rotating disk electrode (RDE) cathodic curves show that Pt–Fe/C300 has the highest oxygen reduction reaction (ORR) mass activity (MA) and specific activity (SA), as compared with Pt/C catalyst in 1.0 M HClO4. However, Pt–Fe/C catalyst does not appears to be a more active catalyst than Pt/C for ORR in 1.0 M HClO4 + 0.1 M CH3OH. Pt–Fe/C300 exhibits higher ORR activity and better performance than other Pt–Fe/C or Pt/C catalysts when employed for cathode in direct methanol single cell test, the enhancement of the cell performance is logically attributed to its higher ORR activity, which is probably attributed to more Pt0 species existing and Fe ion corrosion from the catalyst. [Copyright &y& Elsevier]