A facile method for the preparation of thin-film carbonelectrodes by electron beam evaporation onto highlydoped silicon is presented. The physical and electrochemical properties of these films both before and afterpostdeposition pyrolysis are investigated. Raman spectroscopy establishes the amorphous structure of thenonpyrolyzed carbon films and confirms the formation ofgraphitic carbon after pyrolysis at 1000 °C. Scanning forcemicroscopy reveals the root-mean-square roughness ofnonpyrolyzed films to be ∼1 Å, while pyrolyzed filmsexhibit an increased roughness of ∼4 Å. The electrochemical behavior of the electrodes resembles glassycarbon, with measured heterogeneous electron-transferrate constants among the highest measured for thincarbon films. These carbon film electrodes will potentiallyfind applications in such fields as molecular electronicsand scanning probe microscopy of adsorbed species.