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A newly designed thin-layer STM (TLSTM) technique is presented based on a microfabricated probe combining an electrolytic STM probe with an annular iridium oxide microelectrode operating as a potential-controlled generator or scavenger of H+. This TLSTM configuration can be used to combine in situ STM studies of electrode processes with the simultaneous investigation of H+ flux integrals associated with the electrode reaction. In this paper, the technique is applied to investigate the H+ exchange behaviour of electropolymerised polyaniline films and associated STM-relevant properties in 0.5 M NaClO4 + 10-2 M HClO4. For a polyaniline film kept in the intermediate (emeraldine) oxidation state at 0 mV versus MSE it is shown that its thickness increases due to H+ insertion if the pH is lowered from pH 2 to ca. 1.6, and that its conductivity decreases significantly if the pH is increased from 2 to ca. 12. In a second experiment, where the exchange of H+ at pH 2 is monitored during film oxidation and reduction within the potential range of both redox transfer steps, it is shown that significant exchange of H+ occurs only in the interval of the second (emeraldine/pernigraniline) redox transfer. © 2001 Elsevier Science Ltd. All rights reserved.
Ardemis Anoush Boghossian, Melania Reggente, Mohammed Mouhib, Hanxuan Wang, Charlotte Elisabeth Marie Roullier, Fabian Fischer, Patricia Brandl
Hubert Girault, Andreas Stephan Lesch, Gregorio Bonazza