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In situ synchrotron far infrared micro-spectroelectrochemistry with a grazing angle objective |
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| Authors: | F Hahn Y-L Mathis A Bonnefont F Maillard CA Melendres |
| Institution: | aUMR 6503, CNRS – Université de Poitiers, 40 avenue du Recteur Pineau, F-86022 Poitiers, France bSynchrotron Light Source ANKA/Institute for Synchrotron Radiation (ISS), Forschungszentrum Karlsruhe, P.O. Box 3640, D-76021 Karlsruhe, Germany cLaboratoire d’Electrochimie et de Chimie Physique du Corps Solide, UMR 7177, CNRS/ULP, 4 rue Blaise Pascal, B.P. 1032, F-67070 Strasbourg, France dLaboratoire d’Electrochimie et de Physico-chimie des Matériaux et des Interfaces, UMR 5631 CNRS/INPG/UJF, 1130, rue de la piscine, BP75 – F-38402 Saint Martin d’Hères, France eThe SHD Institute – 216 F Street, PMB 114, Davis, CA 95616, USA |
| Abstract: | We demonstrate the use of a grazing angle objective attachment to carry out in situ far infrared micro-spectroelectrochemistry at a copper electrode on a nano-scale. A thin-layer spectrochemical cell made out of Teflon was used, fitted with a 20-μm thick Mylar window; the working electrode was 500 μm in diameter. Measurements were carried out in 0.1 M NaOH solution as a function of applied potential between –1.4 and 0 V vs a Hg/Hg2SO4 reference electrode. Spectra were obtained with excellent signal to noise ratio for the surface oxide film, formed on copper electrochemically with less than 1 nL of active solution volume. The surface film at 0 V was about 130 nm thick and consisted mainly of CuO, with possibly some Cu(OH)2 also present. This interpretation is consistent with previous works and thermodynamic calculations. The technique should be useful in other investigations and the further development of electrochemical surface science. |
| Keywords: | Far infrared spectromicroscopy Electrochemistry Oxide film on copper |
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