The pore size and volume of activated carbon fiber were increased by steam activation in the presence of iron or magnesium oxide; then, copper, cobalt and silver nitrate was loaded on it, respectively. The pore structures of activated carbon fibers were characterized by nitrogen adsorption (77.4 K); the morphologies and crystal styles of metal particles on surface of activated carbon fibers were observed by SEM and determined by XRD. The result showed that the pore diameter was widened after catalytic activation and the metal oxides were reduced during heat treatment. The adsorption capacity of dichloroethylene was increased with the pore size in 1-10nm; also, the loaded metal particles could markedly improve the adsorption property of dichloroethylene due to the chemical reaction between metal and chlorine atom.