Abstract: Bimetallic Ni-Fe/γ-Al₂O₃ catalyst and monometallic Ni/γ-Al₂O₃, Fe/γ-Al₂O₃ catalysts were prepared by wet impregnation method; they were characterized by XRD, N₂ physisorption, H₂-TPR, H₂-TPD and TPSR. The activity of these catalysts in CO methanation was investigated in a fixed-bed continuous flow reactor. A significant Ni-Fe interaction is observed in the bimetallic Ni-Fe/γ-Al₂O₃ catalyst; Ni-Fe alloy is formed during reduction, which can promote the adsorption of hydrogen. Under the reaction conditions of 0.5% CO, GHSV of 5000h^-1 and atmosphere pressure, the bimetallic Ni-Fe/γ-Al₂O₃ catalyst exhibits high catalytic activity; CO can be completely converted into methane at 220℃.