Polyacrylonitrile films have been spin cast and pyrolyzed to produce thin (500–1500 A˚) carbon films. These films have higher electrical conductivities than films produced by other methods at similar temperatures. The conductivity can be varied by at least four orders of magnitude by changing the pyrolysis temperature. Ultraviolet, infrared, and Raman spectroscopies were used to investigate the chemical structure of the films during different stages of processing.