In order to produce a polyaniline graphite oxide nano-composite, electro-polymerization of aniline was performed within the graphite oxide layers via electrochemical treatment of aniline-intercalated graphite oxide in the supporting electrolyte. It was found that graphite oxide has special electro-active properties. Therefore, electrochemical polymerization of aniline was performed on a Pt substrate in the presence of graphite oxide that had been dispersed in the electrolyte solution by the cyclic voltammetric method. Formation of polyaniline within the layers of graphite oxide occurred during electro-polymerization. This mechanism affects the polyaniline morphology and leads to the formation of well-defined concrete microstructures differing from the pure graphite oxide. Moreover, the results of the thermogravimetric analysis showed that graphite oxide and the polyaniline graphite oxide nano-composite electrodeposited on the Pt substrate have different weight loss behaviors. This confirms that intercalation of the polyaniline improved the oxidation stability of graphite oxide, along with the fact that the polyaniline graphite oxide nano-composite was successfully synthesized by an electrochemical method.