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Development of In Situ Electrochemical Scanning Electron Microscopy with Ionic Liquids as Electrolytes
Authors:Satoshi Arimoto  Daisuke Oyamatsu Dr  Tsukasa Torimoto Prof  Susumu Kuwabata  Prof
Institution:1. Department of Applied Chemistry, Graduate School of Engineering, Osaka University, Suita, Osaka 565‐0871 (Japan), Fax: (+81)6‐6879‐7372;2. JST, CREST, Kawaguchi, Saitama 332‐0012 (Japan);3. Department of Crystalline Materials Science, Graduate School of Engineering, Nagoya University, Nagoya 464‐8603 (Japan), Fax: (+81)52‐789‐5299
Abstract:We report that ionic liquids (ILs) can be observed by electron microscopy without any charging of the liquid. Based on this, we present an in situ electrochemical scanning electron microscopy (in situ ECSEM) system. The key technology that enables in situ ECSEM is that charges can be removed from an IL by grounding it with a Pt wire, even if the IL is in an insulating glass cell. As a first demonstration, we describe the redox reaction of a polypyrrole (PPy) film accompanied by changes in its thickness when it is polarized by the film‐deposited Pt electrode in the IL. Furthermore, energy‐dispersive X‐ray fluorescence (EDX) analysis can be employed for the electrode polarized in the IL. The component analysis by EDX of PPy in an IL containing K+ as a marker, reveals doping of electrolyte cations into the PPy film upon the latter′s reduction and dedoping of cations from the film upon oxidation.
Keywords:conducting materials  electron microscopy  ionic liquids  scanning electron microscopy  X‐ray fluorescence analysis
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