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Ultrathin films of graphite–polymer composites, which are required for sensors applications, are the target of the work reported here. The preparation and characterization of ultrathin films composed of self‐assembled graphite oxide (GO) platelets and polyelectrolytes are described, followed by the in situ reduction of GO to a conductive graphite‐like state (G) by chemical and electrochemical methods. Particular attention is paid to the non‐conductive to conductive transition that occurs on reduction and the behavior of incorporated CdS particles.