Sub-micrometer fibers of polyacrylonitrile were prepared by using electrospinning technique, and thin continuous gold films were coated on the polyacrylonitrile fibers surface through self-catalyzed reduction of chloroauric acid in solution. The conductivities of the metallized fibrous mats were relatively high and increased with the increase of deposited gold amount. When the metallized fibrous mats were thermally treated at higher temperature, the morphology of the gold films on fibers surface changed, and the morphology changes depended on not only the temperature but also the amount of gold deposited on the fibers surface. Porous carbon fibers were obtained when the thermal treated gold-coated fibers were treated with dilute aqua regia. (C) 2008 Elsevier B.V. All rights reserved.