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Carbon film electrodes were prepared by pyrolysis of photoresists on silicon wafers at temperatures ranging from 600 to 1100°C. The physical properties of the carbon films were characterized by scanning and transmission electron microscopies, thermal gravimetric analysis, and four-point probe electrical resistivity measurements. The electrochemical properties of the carbon films were investigated by cyclic voltammetry to observe the kinetics of the Fe(CN)/Fe(CN) redox couple. The carbon film electrodes prepared at temperatures 700°C showed electrochemical behavior similar to that of glassy carbon. Better electrocatalytic behavior was obtained with carbon films prepared at the higher pyrolysis temperatures, which is attributed to different film compositions at different pyrolysis temperatures. The electrochemical properties of the carbon film electrodes are very stable, exhibiting reproducible behavior even after storing at room temperature in air for 3 months.