Polyacrylonitrile/pitch nanofibers were prepared by electrospinning as a precursor for a gas sensor material. Pitch nanofibers were properly fabricated by incorporating polyacryloni-trile as an electrospinning supplement component. Polyacrylonitrile/pitch nanofibers were activated with steam at various temperatures followed by subsequent carbonization to make carbon nanofibers with a highly conductive graphitic structure. Steam activation was effec-tive in facilitating gas adsorption onto the carbon nanofibers due to the increased surface area. The carbon nanofibers activated at 800°C had a larger surface area and a lower micro pore fraction resulting in a higher variation in electrical resistance for improved CO gas sensing properties.