Surface properties of CuCl 2 /activated carbon (AC) catalyst for dimethyl carbonate synthesis were studied by CO-TPD, XRD, SEM and thermogravimetry (TG)/differential scanning calorimetry (DSC) with varying Cu contents. CuCl 2 /AC catalysts were prepared by impregnating AC with CuCl 2 -ethanol solution in the range of Cu content from 2.8 to 18.7wt.%. CuCl 2 .2H 2 O crystalline phase as active sites was gradually increased with an increase in Cu content. Appearance of CuCl 2 .2H 2 O was clearly identified by XRD and SEM. In relatively low Cu contents, 4.6 and 9.9wt.%, CuCl 2 .2H 2 O was not detected in XRD. This indicates the formation of good dispersion of CuCl 2 compounds on activated carbon. However, DSC result revealed that CuCl 2 .2H 2 O was formed in multi-layers for the catalyst with Cu content more than 9.9wt.%, which limit the catalyst activity. This fact was also strongly supported by CO-TPD experiment. The two CuCl 2 /AC catalysts having Cu contents of 4.6 and 9.9wt.% showed no difference in CO adsorption amount in TPD experiments.