NiCu-carbon nanofibers (CNFs) composite was introduced as electrocatalyst for methanol oxidation. Nanofibers (NFs) were synthesized by calcination of electrospun nanofiber mats composed of nickel (II) acetate tetrahydrate, Copper (II) acetate monohydrate, and polyvinyl alcohol (PVA) in the argon/hydrogen atmosphere at 700 • C for 2 hr. The introduced NFs showed a very good ectrocatalytic activity for methanol oxidation as compared tothat of Ni nanoparticles (NPs) and NiCNFs. As the current densities ∼110 mA/Cm 2 , 85 mA/Cm 2 , and 60 mA/Cm 2 for NiCuCNFs nanocomposite, NiCNFs, and Ni NPs, respectively, were obtained.Energy, like water is one of the most important daily needs for the human beings to survive. New energy source draws immediate attention as the conventional energy sources deplete. Direct alcohol fuel cells (DAFCs) are believed a promised candidates for energy producing devices. 1 Among of them, direct methanol fuel cells (DMFCs) are very attractive due to their low cost, performance at the room temperature, and use liquid methanol as fuel. Moreover, methanol has a high energy density enabling it to be easily stored and distributed. 2,3 In DMFCs, aqueous methanol is electrooxidized to carbon dioxide and water on the surface of highly active anode consisting of precious platinum-based materials. 4 However, they face a major challenge in commercialization of the fuel cells due to their highly cost. 5 Moreover, they are poisoned by the adsorption of CO or CHO species that form during the methanol oxidation. 2 Thus, huge effort has been expended to replace Pt-based materials. Recently, transition metals due to their low cost and ease of preparation are used as alternatives for precious metals in DMFCs. Especially, the use of bimetallic nanoalloy for catalytic chemical reaction has been thought to be useful owing to the formation of new properties dissimilar from monometallic. 6,7 Generally, alloy nanomaterials have featured binding properties with reactants in contrary to those of monometallic metal catalysts. 7 Among alloy nanomaterials, nickel copper nanoalloy has been used in electrooxidation of alcohols and other organics. 8,9 However, nude nanoalloy suffers from corrosion during methanol electrooxidation.Electrooxidtion of methanol is a combination of electrochemical reaction and adsorption of reactants on the anode surface. Carbon nanostructures with ordered graphite-like structure have been incorporated in many recently reported as electrocatalytic materials in fuel cells Due to their high adsorption capacity, electrical properties, chemical stability and corrosion resistance. 2,4,10 Accordingly, covering NiCu nanoalloy with nano-carbon might be enhancing corrosion resistance and methanol electrooxidation. Among nanostructures, NFs have been extensively applied in a wide variety of applications ranging from catalysts and photocatalysts to biological and medical application. As compared to nanoparticles, nanofibers have a large axial ratio that faciles electrons transfer, an important factor in elec...