The carbon monoxide coupling reaction on supported metal catalysts Pd/Al2O3 and Pd-Fe/Al2O3 was used to study the characteristics of the catalyst under different conditions. The results indicated that the catalytic activation temperature influenced the catalytic activity and that there was an optimum activation temperature. The characteristics of effective coupling catalysts were found to be smaller surface areas and bigger pores, for example the alpha-phase of aluminum oxide. X-ray photoelectron spectroscopic analysis results show that the catalytic reaction of CO coupling occurs via a redox mechanism.