In order to establish a desirable method for NO reduction, selective catalytic reduction (SCR) of NO by urea-CeO2/ACF and urea-CeO2-CuO/ACF was carried out at room temperature. The experimental results showed that 10% urea-9% CeO2/ACF could yield the highest NO conversion of 85% among the series of urea-CeO2/ACF prepared. When urea-CeO2-CuO/ACF was compared with urea-CeO2/ACF, it achieved higher NO conversion to a certain degree with the addition of CuO, which was attributed to the synergistic effect between cerium and copper. The effect of the mass ratio of CeO2 and CuO was also observed. The desirable mass ratio of CeO2 and CuO was 1:1, which yielded about 90% NO conversion when ACF was loaded with 10% urea. Furthermore, the influence of O2 concentration and NO concentration was also observed. In this study, NO conversion increased with increasing O2 concentration. In addition, some samples were further characterized by BET, X-ray diffraction, X-ray photoelectron spectroscopy and Fourier transform infrared methods.