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Electropolymerization of trans-[RuCl2(vpy)4] complex—EQCM and Raman studies

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Abstract

The electropolymerization of trans-[RuCl2(vpy)4] (vpy=4-vinylpyridine) on Au or Pt electrodes was studied by cyclic voltammetry, electrochemical quartz crystal microbalance (EQCM) technique, and Raman spectroscopy. Cyclic voltammetry of the monomer at a microelectrode shows the typical Ru(III/II) and Ru(IV/III) waves, together with the vinyl reduction waves at −1.5 and −2.45 V and adsorption wave at −0.8 V. Electrodeposition on EQCM technique performed under potential cycling between −0.9 and −2.0 V revealed that the polymerization proceeded well in advance of the vinyl reduction waves. At potentials more positive than −0.9 V, soluble oligomers were deposited irreversibly on the electrode during the oxidative sweep. The film also showed reversible mass changes due to the oxidation and accompanying ingress of charge-balancing anions and solvent into the film. In contrast, potentiostatic growth of the polymer at −1.6 V was slower because the oligomeric material was lost completely from the electrode. Unreacted vinyl groups were detected by in situ Raman spectroscopy for films grown at −0.7, −0.9, and −1.6 V but were absent when the polymerization was carried out at −2.9 V vs Ag/Ag+.

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Acknowledgements

The authors are grateful to Laboratório de Espectroscopia Molecular (LEM-IQUSP) for the use of the Raman equipment (Renishaw Raman System 3000). LKN acknowledges CAPES/ProDoc for the grant, NSG acknowledges CNPq Edital Universal 01/2002, and MCEB acknowledges CAPES-Brazilian Research Council for financial support.

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Authors and Affiliations

  1. Depto. de Química, Universidade Federal de Mato Grosso do Sul, Av. Senador Filinto Muller 1555, CxP:549, 79070-900, Campo Grande, MS, Brazil

    Merlin C. E. Bandeira

  2. School of Chemistry, University of St. Andrews, St. Andrews, Fife, Scotland, KY169ST, UK

    Joseph A. Crayston

  3. Depto. de Química-CFM, Campus Trindade, Universidade Federal de Santa Catarina, 88040-900, Florianópolis, SC, Brazil

    Norberto S. Gonçalves, Lúcia K. Noda & César V. Franco

  4. Chemistry Department, University of Glasgow, Glasgow, Scotland, G12 8QQ, UK

    Andrew Glidle

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  1. Merlin C. E. Bandeira
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  2. Joseph A. Crayston
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  3. Norberto S. Gonçalves
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  4. Lúcia K. Noda
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  6. César V. Franco
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Correspondence to Merlin C. E. Bandeira.

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Bandeira, M.C.E., Crayston, J.A., Gonçalves, N.S. et al. Electropolymerization of trans-[RuCl2(vpy)4] complex—EQCM and Raman studies. J Solid State Electrochem 11, 231–239 (2007). https://doi.org/10.1007/s10008-005-0093-8

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  • DOI: https://doi.org/10.1007/s10008-005-0093-8

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