This paper describes the preparation of Ni/Pt/CNFs via electrospinning technology, carbonization process, and chemical reduction method. The structure and composition of Ni/Pt/CNFs were characterized with X-ray diffraction, Raman spectroscopy, nitrogen adsorption isotherms, and X-ray photoelectron. spectroscopy. Meanwhile, the morphology was analyzed with scanning electron microscopy and transmission electron microscopy. The electrochemical performance was evaluated by oxygen reduction reaction (ORR), cyclic voltammetry and chronopotentiometry. The results indicated that Pt and Ni nanoparticles were completely reduced in the experimental process and homogeneously distributed on the nanofibers with the average diameters of 3.8 and 17.8 nm, respectively. In addition, the Ni-50/Pt/CNEs catalyst showed excellent electrocatalytic performance for ORR. and superior specific and mass activities for methanol oxidation (the maximum current density is ca. 10.9 mA cm(-2)) and exhibited a slightly slower current decay over time; better than the reference samples which indicated a higher tolerance to CO-like intermediates.