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The electrosynthesis of polythiophene films from thiophene, 2, 2 ′ :5, 2″-terthiophene,3-methylthiophene and 3-bromothiophene monomers were investigated using different electrochemical techniques. The stability and electrical conductivity of the prepared films were studied. The most stable polythiophene film was obtained using galvanostatic technique in acetonitrile solvent and TBAPF6 as supporting electrolyte at 5°C, except in case of electropolymerization of 3-bromothiophene the most stable film was obtained potentiodynamically. The relaxation kinetics of the films were extensively studied. It was found that a very thin film would hardly show the slow relaxation. Also by using TBAPF6 as electrolyte, the most sensitive film was obtained, which has the lowest relaxation. The relaxation time is sharply affected by increasing the donner number of the solvent used and also by temperature.