A composite thin film of the novel electroactive fullerene-palladium (C₆₀-Pd) polymer and single-wall carbon nanotubes, which were non-covalently modified by 1-pyrenebutiric acid (pyr-SWCNTs), was electrochemically prepared under multi-scan cyclic voltammetry (CV) conditions and its conductive, capacitance and visco-elasitic properties investigated. The film was prepared by using a mixed C₆₀, pyr-SWCNTs, and palladium acetate solution of either mixed acetonitrile : toluene (1 : 4, v : v) or 1,2-dichlorobenzene solvent. A tetrabutylammonium salt, like 0.1 M (TBA)ClO₄ or (TBA)PF₆, was used as a supporting electrolyte. Mass changes of the deposited composite film were measured in situ by piezoelectric microgravimetry with the use of an electrochemical quartz crystal microbalance. The quartz crystal resonators with their electrodes coated by either the C₆₀-Pd or C₆₀-Pd/pyr-SWCNTs composite film were transferred to a blank supporting electrolyte solution, i.e., 0.1 M (TBA)ClO₄ or (TBA)PF₆ in acetonitrile, and current, resonance frequency changes, and dynamic resistance changes vs. scanned potential were simultaneously recorded in different potential ranges. Each polymer revealed electrochemical activity at potentials more negative than ca. -0.7 V. Both cathodic and anodic currents for the C₆₀-Pd/pyr-SWCNTs films were almost twice as high as those for the C₆₀-Pd films. The presence of pyr-SWCNTs in the polymer causes an increase of the electrode capacitance, as manifested by increased CV current. For the potential range 0 to -1.2 V changes of both resonance frequency and dynamic resistance are almost the same for the C₆₀-Pd and C₆₀-Pd/pyr-SWCNTs films. Distinct differences are seen, however, for potentials exceeding -1.2 V. That is, frequency rapidly decreases when the potential reaches the -1.2 V value in the negative excursion. However, this decrease is three times smaller for the C₆₀-Pd/pyr-SWCNTs film than that for the C₆₀-Pd film. This decrease of frequency is accompanied by the increase of dynamic resistance. Changes of dynamic resistance for the C₆₀-Pd film are three times larger than those for the C₆₀-Pd/pyr-SWCNTs film. This behavior suggests that for potentials more negative than -1.2 V the C₆₀-Pd/pyr-SWCNTs film is more rigid than the C₆₀-Pd film. Moreover, redox conductivity of the C₆₀-Pd films doped with pyr-SWCNTs is higher than that of the undoped C₆₀-Pd films. The redox conductivity values, determined from the highest slopes of the rising portions of cathodic CV curves in the range ca. -0.6 to -0.8 V, are 0.92 and 1.48 mS for the film of the C₆₀-Pd and the C₆₀-Pd/pyr-SWCNTs composite, respectively. In the Raman spectrum for the C₆₀-Pd/pyr-SWCNTs film there are peaks characteristic both for pyr-SWCNTs (radial breathing modes, RBM) and C₆₀-Pd indicating that, indeed, pyr-SWCNTs are incorporated into the film during electropolymerization of C₆₀-Pd. Moreover, the RBM peaks for the pyr-SWCNTs film are deconvoluted in the spectrum of the composite due to different extent of aggregation of pyr-SWCNTs.

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