Angle-resolved infrared spectroelectrochemistry, a new technique based on attenuated total reflectance (ATR), allows in situ depth profiling at the electrode/electrolyte interface. Varying the angle of incidence of the infrared beam at the sensing surface of the ATR element allows various depths from the electrode surface to be sampled. This technique was used to study the structure of hydrated nickel oxide films. In the reduced state, both a and ß nickel hydroxides were found, indicating the presence of the a phase at the metal/film interface and the ß phase at the film/solution interface. A sandwich-type structural model for the hydrated nickel oxide is proposed: it has an open structure at the top surface and a more compact structure at the electrode/film interface. The spectra of the film after its transformation into the oxidized state showed the presence of nickel oxyhydroxide. Both the reduced and oxidized forms were found to contain water in the film structure.
Electrochromic thin films of polyaniline were prepared by electropolymerization of aniline from an acidic aqueous solution on platinum and conducting glass surfaces. An in situ FTIR spectroelectrochemical technique was used to investigate structural changes of the film during oxidation and reduction. Coloring (oxidation) and bleachin~ (reduction) of the film were shown to be associated with the deprotonation and protonation of the film. It was detected that the N--H stretching band around 2970 cm 1 decreased as the film was gradually oxidized.
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