Chemical deposition of ultrafine gold and palladium particles into poly(3,4-ethylenedioxythiophene) matrix has yielded the metal-containing polymer composites. Their structure has been studied as affected by duration of reduced polymer immersion into the metal salts solution, and by concentration of the latter. Morphology features of the composite films (size and concentration of metal particles) have been elucidated by scanning and transmission electron microscopy. The mixed clusters have been formed predominantly in the course of preparation of bimetal composite films via sequential deposition of gold and palladium; the isolated palladium clusters nucleate slower due to the gold-palladium alloys formation. Longer deposition of the metals leads to increase in the nanoparticles size and their concentration in the composite. Properties of the prepared materials have been demonstrated using the model electrochemical reactions.In recent years a new trend in development of electrode materials has emerged: modification of conductive polymers with nanosized particles of metals and their compounds. Such hybrid organicinorganic materials are especially interesting due to the advantageous functional properties of the highly disperse nanostructured matter incorporated into the conductive matrix [1][2][3][4][5][6][7]. In general, such composites exhibit properties combining those typical of the conductive polymer constituting the matrix and those of the incorporated metal nanoparticles.We have previously demonstrated [8][9][10][11] that redox interaction between the reduced form of poly(3,4-ethylenedioxythiophene) (PEDOT) and ions of electropositive metals (palladium or gold) can be applied to produce metal nanoparticles at the polymer surface and inside its pores. We have investigated electrochemical behavior of the PEDOT/Pd and PEDOT/Au composite films [8-10] and morphology of the PEDOT/Pd films [11]. Morphology of the PEDOT/Au films has not been studied in detail in the above-cited papers.Here we report new data on morphology of the PEDOT/Au films and possibility of the Au-Pd mixed metal clusters formation. The bimetal Au-Pd particles are extremely interesting: catalytic properties of the mixed particles have been demonstrated to be enhanced as compared to those of the corresponding individual particles [12][13][14][15]. For example, thin palladium films on gold support are more active towards oxygen reduction than pure palladium and gold [14,15]; the effect is caused by the formation of Pd-Au alloys at the interface.The composites prepared in this work are applicable in electroanalysis as micro-and nanoelectrode assemblies, the incorporated metal particles acting as electrodes in the electrochemical process, and the conductive polymer behaves as the integrating conducting matrix. When metal nanoparticles are deposited onto the surface of carbon or metal electrodes, the former are agglomerated to form larger structures, whereas the polymer matrix can stabilize the nano-particles to prevent the aggregation. This approach ...