Carbon/CdS coaxial nanofibers (NFs) have been prepared using polyacrylonitrile (PAN)/CdS composite NFs as precursors. The synthesis strategy involves immersing the as-spun PAN fibers into cadmium acetate aqueous solution, followed by reaction with H2S gas and carbonization. SEM and TEM showed the morphology of the obtained coaxial NFs. The structures were examined by XRD, FT-IR and Raman spectra. The NFs displayed photoluminescence and conductive properties which were characterized by room-temperature photoluminescent spectra and standard four-probe method. (C) 2007 Elsevier B.V. All rights reserved.