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Developing low-cost electrocatalysts for the nitrate reduction reaction (NO3RR) with superior performance is of great significance for wastewater treatment. Herein, we synthesized bimetal Cu/Fe nanoparticles encased in N-doped carbon nanofibers (Cu/Fe@NCNFs) through simple electrospinning followed by a pyrolysis reduction strategy. Metallic copper is beneficial for reducing nitrate to nitrite, and the existence of Fe is conducive to convert nitrate and nitrite into nitrogen. Additionally, the nitrogen-doped carbon nanofibers also facilitate the adsorption of nitrate, and the continuous and complete fiber structure enhances the stability of the catalyst and prevents the corrosion of the active sites. Therefore, the synergetic effect of bimetal Cu/Fe and N-doped carbon fiber plays a key role in promoting the efficiency of nitrate reduction. The obtained Cu/Fe@NCNF catalyst exhibits a satisfactory nitrate conversion efficiency of 76%, removal capacity of 5686 mg N g−1 Cu/Fe and nitrogen selectivity of 94%.