Abstract: Nano PtPb anode catalyst supported on carbon fiber was prepared by the technology of electro-spinning combined with sintering; the catalyst was characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM). The results showed that the nano catalyst is well dispersed on the skeleton of vesicular carbon fiber with a particle size of 3.05 nm; the catalytic efficiency is significantly improved by pre-oxidation at 300 ℃and carbonization at 800 ℃. The catalyst activity in ethanol oxidation was evaluated through cyclic voltammogram (CV) and electrochemical impedance spectroscopy (EIS). The results indicated that the catalyst has better resistance against poisoning; over it, the maximum current density is 125 mA/cm² and the charge transfer resistance is reduced by 60% in comparison with that over the catalyst carbonized at 700 ℃.