Hostname: page-component-78c5997874-8bhkd Total loading time: 0 Render date: 2024-11-19T06:34:15.091Z Has data issue: false hasContentIssue false
  • English
  • Français

Possibility of Scanning Electron Microscope Observation and Energy Dispersive X-Ray Analysis in Microscale Region of Insulating Samples Using Diluted Ionic Liquid

Published online by Cambridge University Press:  27 February 2012

Susumu Imashuku ,
Tetsuo Kawakami ,
Long Ze  and
Jun Kawai
Susumu Imashuku*
Affiliation:
Department of Materials Science and Engineering, Kyoto University, Sakyo-ku, Kyoto 606-8501, Japan
Tetsuo Kawakami
Affiliation:
Department of Geology and Mineralogy, Graduate School of Science, Kyoto University, Sakyo-ku, Kyoto 606-8502, Japan
Long Ze
Affiliation:
Department of Materials Science and Engineering, Kyoto University, Sakyo-ku, Kyoto 606-8501, Japan
Jun Kawai
Affiliation:
Department of Materials Science and Engineering, Kyoto University, Sakyo-ku, Kyoto 606-8501, Japan
*
Corresponding author. E-mail: [email protected]
Get access

Abstract

The possibility of scanning electron microscope (SEM) observation and energy dispersive X-ray (EDX) spectrometry analysis in microscale regions of insulating samples using diluted ionic liquid was investigated. It is possible to obtain clear secondary electron images of insulating samples such as a rock and mineral at 5,000 times magnification by dropping 10 μL of 1 wt% of 1-ethyl-3-methylimidazolium acetate (EMI-CH3COO) diluted with ethanol onto the samples. We also obtained EDX spectra of the samples in microscale regions (∼5 μm2) without overlapping EDX spectra of other minerals with different composition. It might be possible to perform quantitative analysis of the samples if a method that does not need standard samples is applied or an X-ray detector sensitive for light elements was attached. The method of dropping 1 wt% EMI-CH3COO diluted with ethanol onto insulating samples is useful for SEM observation, EDX analysis in microscale regions, and the preservation of scarce rock and mineral samples because ionic liquid can be easily removed with acetone.

Keywords

ionic liquidSEMEDXinsulating sampleelectrical chargingmicroscale region
Type
Techniques and Software Development
Information
Microscopy and Microanalysis , Volume 18 , Issue 2 , April 2012 , pp. 365 - 370
Copyright
Copyright © Microscopy Society of America 2012

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Arimoto, S., Sugimura, M., Kageyama, H., Torimoto, T. & Kuwabata, S. (2008). Development of new techniques for scanning electron microscope observation using ionic liquid. Electochim Acta 53, 6228–6234.CrossRefGoogle Scholar
Carlin, R.T., De Long, H.C., Fuller, J. & Trulove, P.C. (1994). Dual intercalating molten electrolyte batteries. J Electrochem Soc 141, L73–L76.CrossRefGoogle Scholar
Deer, W.A., Howie, R.A. & Zussman, J. (1992). An Introduction to the Rock-Forming Minerals. Essex, UK: Longman Scientific & Technical.Google Scholar
Igarashi, S. & Yotsuyanagi, T. (1989). Temperature dependent phase transformation in the homogeneous liquid-liquid extraction with fluorocarbon surfactant. In Symposium on Solvent Extraction, Japanese Association of Solvent Extraction & Nihon Kagakkai (Eds.), pp. 51–54. Sendai, Japan: Japanese Association of Solvent Extraction.Google Scholar
Inoue, M., Suganami, M., Hashimoto, Y., Iyasu, T., Saito, H., Moriguchi, K. & Tanaka, T. (2010). Application of ionic liquid coating method to observation of non-conductive samples by a mobile scanning electron microscope for elementary science education. In 5th International Symposium on Practical Surface Analysis, p. 138. Gyeongju, Japan: The Surface Analysis Society of Japan and The Korean Vacuum Society.Google Scholar
Ishigaki, Y., Nakamura, Y., Takehara, T., Nemoto, N., Kurihara, T., Koga, H., Nakagawa, H., Takegami, T., Tomosugi, N., Miyazawa, S. & Kuwabata, S. (2011a). Ionic liquid enables simple and rapid sample preparation of human culturing cells for scanning electron microscope analysis Microsc Res Tech 74, 415–420.CrossRefGoogle ScholarPubMed
Ishigaki, Y., Nakamura, Y., Takehara, T., Shimasaki, T., Tatsuno, T., Takano, F., Ueda, Y., Motoo, Y., Takegami, T., Nakagawa, H., Kuwabata, S., Nemoto, N., Tomosugi, N. & Miyazawa, S. (2011b). Scanning electron microscopy with an ionic liquid reveals the loss of mitotic protrusions of cells during the epithelial–mesenchymal transition. Microsc Res Tech 74(11), 1024–1031.CrossRefGoogle ScholarPubMed
Ishii, H. & Kawai, J. (2006). SEM-EDX with an SDD X-ray detector installed onto the scanning electron microscope. Adv X-Ray Chem Anal Jpn 37, 281–288 (in Japanese).Google Scholar
Kuwabata, S., Kongkanand, A., Oyamatsu, D. & Torimoto, T. (2006). Observation of ionic liquid by scanning electron microscope. Chem Lett 35, 600–601.CrossRefGoogle Scholar
Kuwabata, S. & Torimoto, T. (2008). Observation of ionic liquid by electron microscopy. J Surf Sci Soc Jpn 28, 322–326 (in Japanese).CrossRefGoogle Scholar
Matsumoto, H. & Matsuda, T. (2002). Photoelectrochemical solar cells using ionic liquid as an involatile electrolyte. Electrochemistry 70, 190–193.CrossRefGoogle Scholar
McEwen, A.B., McDevitt, S.F. & Koch, V.R. (1997). Nonaqueous electrolytes for electrochemical capacitors: Imidazolium cations and inorganic fluorides with organic carbonates. J Electrochem Soc 144, L84–L86.CrossRefGoogle Scholar
Nanjundiah, C., McDevitt, S.F & Koch, V.R. (1997). Differential capacitance measurements in solvent-free ionic liquids at Hg and C interfaces. J Electrochem Soc 144, 3392–3397.CrossRefGoogle Scholar
Okuyama, M., Sato, M. & Akada, M. (2011). Studies on the excavated archaeological textile fibers using room temperature ionic liquid (1)—The utility of ionic liquid for the SEM observation of natural fibers. Sen'is Gakkaishi 67, 47–52 (in Japanese).CrossRefGoogle Scholar
Papageorgiou, N., Athanassov, Y., Armand, M., Bonhôte, P., Pettersson, H., Azam, A. & Grätzel, M. (1996). The performance and stability of ambient temperature molten salts for solar cell applications. J Electrochem Soc 143, 3099–3108.CrossRefGoogle Scholar
Tobishima, S. (2002). Application of ionic liquids as electrolytes in rechargeable cells. Electrochemistry 70, 198–202.CrossRefGoogle Scholar
Ue, M., Takeda, M., Takahashi, T. & Takehara, M. (2002). Ionic liquids with low melting points and their application to double-layer capacitor electrolytes. Electrochem Solid-State Lett 5, A119–A121.CrossRefGoogle Scholar
Wilkes, J.S. & Zaworotko, M.J. (1992). Air and water stable 1-ethyl-3-methylimidazolium based ionic liquids. J Chem Soc Chem Commun 13, 965–967.CrossRefGoogle Scholar
Yamaguchi, H. (2007). Does research on ionic liquid begin from analytical chemistry? Bunseki 608–609 (in Japanese).Google Scholar
Ze, L., Imashuku, S., Ichida, M. & Kawai, J. (2011). SEM observation at high magnification and EDX analysis of insulating sample by diluted ionic liquid. J Surf Sci Soc Jpn 32, 659–663 (in Japanese).CrossRefGoogle Scholar