To prepare zero-valent iron with excellent adsorptive and reducible properties, activated carbon was used in this experiment as a load, and modified with metal modification to obtain activated carbon-supported Ni/Fe bimetallic particles by electro-deposition. Ni/Fe-AC BPs were characterized by FESEM, EDS, and BET analyzer, and the Cr(Ⅵ) removal rate was used as the performance evaluation index. The results of single factor preparation test showed that the optimum deposition solution ratio was ferric sulfate 400 g/L, nickel sulfate 80 g/L, boric acid 40 g/L and manganese sulfate 60 g/L. The optimum electro-deposition conditions were current density 0.45 A/cm², temperature 40℃ and electrodeposition 10 min. Under these conditions, the removal rate of hexavalent chromium was as high as 100%. FESEM, EDS and XRD confirmed that the preparation of nickel-iron bimetallic particles was successful, and the prepared materials were flocculent and uniformly dispersed. The comparison tests of BET and AC, Fe-AC, Ni/Fe-AC BPs for chromium removal showed that the specific surface area of Ni/Fe-AC BPs was 47.6% smaller than AC, but the removal rate of Cr (VI) was 100%, while the adsorption rate of AC was only 5.43%. Therefore, Ni/Fe-AC BPs have a good catalytic reduction performance.