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Passivation of nanoscale zerovalent iron hinders its efficiency in water treatment, and loading another catalytic metal has been found to improve the efficiency significantly. In this study, Cu/Fe bimetallic nanoparticles were prepared by liquid-phase chemical reduction for removal of hexavalent chromium (Cr(VI)) from wastewater. Synthesized bimetallic nanoparticles were characterized by transmission electron microscopy, Brunauer–Emmet–Teller isotherm, and X-ray diffraction. The results showed that Cu loading can significantly enhance the removal efficiency of Cr(VI) by 29.3% to 84.0%, and the optimal Cu loading rate was 3% (wt%). The removal efficiency decreased with increasing initial pH and Cr(VI) concentration. The removal of Cr(VI) was better fitted by pseudo-second-order model than pseudo-first-order model. Thermodynamic analysis revealed that the Cr(VI) removal was spontaneous and endothermic, and the increase of reaction temperature facilitated the process. X-ray photoelectron spectroscopy (XPS) analysis indicated that Cr(VI) was completely reduced to Cr(III) and precipitated on the particle surface as hydroxylated Cr(OH)3 and CrxFe1−x(OH)3 coprecipitation. Our work could be beneficial for the application of iron-based nanomaterials in remediation of wastewater. [ABSTRACT FROM AUTHOR]