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This work has focused on the development of metallic amorphous microparticulated alloys of composition Ni59Nb40Pt0.6Cu0.4 and Ni59Nb40Pt0.6Cu0.2Sn0.2, obtained by mechanical alloying (MA), for use as anodes in direct alcohol fuel cells (DAFCs). The addition of copper modifies the electronic properties of platinum due to its special electronic configuration (3d104s1), demonstrating a better performance for ethanol/bioethanol electro‐oxidation. Ni59Nb40Pt0.6Cu0.4 alloy provides higher current densities than Ni59Nb40Pt0.6Cu0.2Sn0.2 alloy. In spite of tin significantly improving the tolerance to different adsorbed species such as CO, its presence does not improve the electro‐oxidation reaction due to limit the distribution of platinum atoms by the ligand effect, avoiding the final oxidation to CO2. In both alloys higher current densities were obtained for bioethanol electro‐oxidation than ethanol, due mainly to the presence of acetaldehyde, formic acid and another organic compounds (ppb), which may contribute to improvement of catalytic results.