Activated carbon fibers were prepared from the petroleum isotropic pitch and organometallic compounds. The metals were dispersed uniformly in the ACFs. The specific surface area and pore size distributions of metal containing ACFs were measured. The mesopores of ACFs were developed by Co, Ni, and Mn metals addition, and the catalytic reactivity of ACFs' SOx removal was increased by adding Ni and Pd metals. It was found that the mesopores did not work forthe improvement of catalytic reactivity of ACFs' SOx removal with the blank experiment using the metal removed ACFs.