Microporous carbon materials with high specific surface area are well known to have good characteristics as a hydrogen storage media. In this study, electrospun carbon materials were chemically activated for development of pore structure with high specific surface area. To investigate and optimize the hydrogen storage system, the effects of specific surface area and micropore volume were studied with a view to increase the capacity of hydrogen adsorption. Even though specific surface area affects the capacity of hydrogen storage, micropore volume is an important factor. To compare activated electrospun carbon fibers with other carbon materials, activated electrospun carbon fibers have better effects for hydrogen adsorption.