Development of new techniques for scanning electron microscope observation using ionic liquid

• Published in: Electrochimica acta Vol. 53; no. 21; pp. 6228 - 6234
• Main Authors: Arimoto, Satoshi, Sugimura, Masaharu, Kageyama, Hitoshi, Torimoto, Tsukasa, Kuwabata, Susumu
• Format: Journal Article Conference Proceeding
• Language: English
• Published: Oxford Elsevier Ltd 01.09.2008; Elsevier
• Subjects: Chemistry; Condensed matter: structure, mechanical and thermal properties; Electrochemistry; Electrodeposition; Electron, ion, and scanning probe microscopy; Electronic conductivity; Energy dispersive X-ray fluorescence analysis; Exact sciences and technology; General and physical chemistry; In situ electrochemical scanning electron microscope observation; Ionic liquid; Physics; Scanning electron microscope; Structure of solids and liquids; crystallography; Study of interfaces; Transmission, reflection and scanning electron microscopy(including ebic); In situ electrochemical scanning electron microscope observation; Electronic conductivity; Scanning electron microscope; Energy dispersive X-ray fluorescence analysis; Ionic liquid; Scanning electron microscopy; In situ; Dispersive spectrometry; Surface structure; Electrodes; Conducting polymers; Silver; Energy dispersion; Medium effect; Platinum; Transition elements; Morphology; Electrodeposition; X radiation; X ray fluorescence spectrometry; Polypyrroles; Electrochemical reaction; Application
• ISSN: 0013-4686; 1873-3859
• DOI: 10.1016/j.electacta.2008.01.001

Based on our previous discovery that ionic liquid (IL) can be observed by a scanning electron microscope (SEM) without charging the liquid, we have developed several novel techniques for SEM observation. Coating of insulating sample with IL is useful for providing electronic conductivity to the samples like metal or carbon coating by vacuum vapor deposition. In this case, dilution of the IL with appropriate volatile solvent like alcohol is effective for coating thin layer of IL on the sample. As a biological sample, seaweed including IL was attempted to be observed by SEM. A seaweed leaf swollen by water was put in an IL bath and the bath was put in an outgassed desiccator to replace water in the seaweed leaf with IL. The resulting sample gave a SEM image of the swollen seaweed whose thickness was several times larger than dried one. Furthermore, the introduction of the IL in vacuum chamber allowed us to develop the in situ electrochemical SEM observation system. Using this system, we observed changes in polypyrrole film thickness caused by the redox reaction of the film and the electrochemical deposition of silver and its oxidative dissolution. It was also found that the energy dispersive X-ray fluorescence (EDX) analysis was available even for the electrode polarized in IL.