Ni-Fe/Al2O3 catalyst for partial oxidation of methane was prepared first by glow discharge plasma treatment following by calcinations thermally. Such prepared catalyst exhibits better performance over the catalyst prepared without such plasma treatment. The conversion of methane and the selectivity of CO and H2 over the plasma treated catalyst are 97.44, 100 and 100% at 875℃, while, at the same temperature, they are 90.09, 97.28 and 97.09%, respectively, over the catalyst prepared without plasma treatment. At the same methane conversion, the reaction temperature with the plasma treated Ni-Fe/Al2O3 is at least 80℃ lower. TEM characterization shows that the catalytically active species after plasma treatment are still highly dispersed on the support. In addition, the plasma treated Ni-Fe/Al2O3 catalyst also possesses better anti-carbon deposit ability.