Preparation and time-resolved in situ reflection spectra of bilayer electrodes with polythiophene outer layers.

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Bilayer electrodes, Pt/poly-1/polythiophene [1: tris(4-vinyl-4′-methyl-2,2′-bipyridine)ruthenium(II) perchlorate], where polythiophene is derived from poly(3-methylthiophene) [poly(3-methyl-2,5-thienylene), abbreviated as PMeT] and poly(2,2′-bithiophene) [poly(2,2′-dithienyl-5,5′-ene), abbreviated as PBT], have been prepared. Electropolymerizations of MeT and BT at Pt/poly-1 occur at the platinum electrode surface, followed by phase separation of the polymer components which results in the bilayer structure. Significant imbalance, observed between charge densities involved in the cathodic and anodic waves of the cyclic voltammogram for Pt/poly-1/PBT, is explained as being due to the positive charge leakage from the PBT layer to the platinum substrate through the 2+/3+ redox level of the intervening poly-1 during the potential sweep in the negative direction. This charge leakage is ascribed to the consequence of the closely located oxidation potential of PBT to that of the 2+/3+ of poly-1 (E°′=+0.875 V vs. Ag/Ag+). Time-resolved in situ reflection spectra taken at Pt/poly-1/PMeT immersed in electrolytic solutions give evidence for the mediated redox reactions of PMeT by the poly-1 layer. The spectral changes strongly suggest the transient occurrence of polarons during the doping process.
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