AbstractA tantalum electrode on which polypyrrole (PPy) had been previously formed by electropolymerization was galvanostatically electrolyzed in an aqueous solution of 0.01 wt phosphoric acid. This process contains the irreversible oxidation of a PPy film, the decomposition of solvent, and the formation of Ta2O5by the reaction of OH−coming through the PPy film, with Ta electrodes. A three layer‐structure (PPy/Ta2O5/Ta) was confirmed by electron spectroscopy for chemical analysis (ESCA). A PPy film containing CIO4−as dopant PPy(CIO4−) was significantly deteriorated in comparison with PPy(TsO−) at the electrolysis. Therefore, the (PPy(TsO−)/Ta2O5/Ta) system showed better electrical characteristics as a capacitor than the (PPy(CIO4−)/Ta2O5/Ta) system showed better electrical characteristics as a capacitor than the (PPy(ClO4−)/T
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