Developing stable, highly active, and economical non-precious metal catalysts for the oxygen evolution reaction (OER) has been highly demanded in the new energy field since it can meet the industrial demands of large-scale electrocatalytic water splitting. A novel FeP/Ni2P/Fe0.64Ni0.36/C (FeNiP–FeNi–C) nanofiber was prepared by electrospinning and high-temperature phosphating. Notably, the good dispersion of FeP, Ni2P, and FeNi alloy nanoparticles in the nanocarbon fiber greatly increased the number of electroactive sites, and the synergistic effect between the FeP/Ni2P heterogeneous interface and FeNi alloy significantly improved the inherent activity of each site. Moreover, the carbon nanofibers enhanced the long-term durability of the catalyst by preventing the corrosion of the FeP, Ni2P, and FeNi alloy particles. Therefore, the optimal FeNiP–FeNi–C catalyst revealed exceptionally high OER activity, with overpotentials of 364 mV and 236 mV at 50 mA cm−2 and 10 mA cm−2 respectively, and the slope of Tafel of 61.00 mV·dec−1. This catalyst performs significantly better than commercial RuO2 catalysts in alkaline electrolytes. The results of this study offer a novel perspective for the mass production of non-precious metal OER high-efficiency electrocatalysts.
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