Activated carbon fibers were prepared from stabilized PAN-based fibers by chemical activation using hydroxides at different concentrations. The experimental data showed variations in specific surface area, microstructure, pore size distribution, and amounts of iodine adsorbed by the activated carbon fibers. Specific surface area of about 2244m2/g and iodine adsorption of 1202mg/g were obtained in the KOH 1.5M. However, the use of NaOH in the activation process rather than KOH and using the same time/ temperature profiles resulted in a carbon with a much lower surface area. KOH is a more developed pore structure than NaOH, which means that KOH is a better activation agent in producing ACF than NaOH.