Thermolysis of Cu(NO3)2·3H2O impregnated activated carbon fiber (ACF) was studied by means of XRD analysis to obtain Cu-impregnated ACF. Cu(NO3)2·3H2O was converted into Cu2O around 230℃. The Cu2O was reduced to Cu at 400℃, resulting in ACF-C(Cu). Some Cu particles have a tendency to aggregate through the heat treatment, resulting in the ununiform distribution in ACF. Catalytic decomposition of NO gas has been performed by Cu-impregnated ACF in a column reactor at 400℃. Initial NO concentration was 1300 ppm diluted in helium gas. NO gas was effectively decomposed by 5~10 wt% Cu-impregnated ACF at 400℃. The concentration of NO was maintained less than 200 ppm for 6 hours in this system. The ACF-C(Cu) deoxidized NO to N2 and was reduced to ACF-C(Cu2O) in the initial stage. The ACF-C(Cu2O) also deoxidized NO to N2 and reduced to ACF-C(CuO). This ACF-C(CuO) was converted again into ACF-C(Cu) by heating. There was no consumption of ACF in mass during thermolysis and catalytic decomposition of NO to N2 by copper. The catalytic decomposition was accelerated with increase of the reaction temperature.