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Decontamination in the Electron Probe Microanalysis with a Peltier-Cooled Cold Finger

Published online by Cambridge University Press:  05 October 2016

Ben Buse ,
Stuart Kearns ,
Charles Clapham  and
Donovan Hawley
Ben Buse*
Affiliation:
School of Earth Sciences, University of Bristol, Bristol, BS8 1RJ, UK
Stuart Kearns
Affiliation:
School of Earth Sciences, University of Bristol, Bristol, BS8 1RJ, UK
Charles Clapham
Affiliation:
School of Earth Sciences, University of Bristol, Bristol, BS8 1RJ, UK
Donovan Hawley
Affiliation:
School of Earth Sciences, University of Bristol, Bristol, BS8 1RJ, UK
*
*Corresponding author.[email protected]
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Abstract

A prototype Peltier thermoelectric cooling unit has been constructed to cool a cold finger on an electron microprobe. The Peltier unit was tested at 15 and 96 W, achieving cold finger temperatures of −10 and −27°C, respectively. The Peltier unit did not adversely affect the analytical stability of the instrument. Heat conduction between the Peltier unit mounted outside the vacuum and the cold finger was found to be very efficient. Under Peltier cooling, the vacuum improvement associated with water vapor deposition was not achieved; this has the advantage of avoiding severe degradation of the vacuum observed when warming up a cold finger from liquid nitrogen (LN2) temperatures. Carbon contamination rates were reduced as cooling commenced; by −27°C contamination rates were found to be comparable with LN2-cooled devices. Peltier cooling, therefore, provides a viable alternative to LN2-cooled cold fingers, with few of their associated disadvantages.

Keywords

electron probe microanalysisanticontaminationPeltier coolingcold fingercarbon contamination
Type
Instrumentation and Techniques Development
Information
Microscopy and Microanalysis , Volume 22 , Issue 5 , October 2016 , pp. 981 - 986
Copyright
© Microscopy Society of America 2016 

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References

Ash, G.S. (1998). Cryogenic pumps. In Handbook of Vacuum Science and Technology, Hoffman, D.M., Singh, B. & Thomas III, J.H. (Eds.), pp. 149–182. San Diego, CA and London: Academic Press.Google Scholar
Bastin, G.F. & Heijligers, H.J.M. (1986). Quantitative electron probe microanalysis of carbon in binary carbides. X-Ray Spectrom 15, 135–141.CrossRefGoogle Scholar
Bastin, G.F. & Heijligers, H.J.M. (1988). Contamination phenomena in the electron probe microanalyzer. In Microbeam Analysis, Newbury, D.E. (Ed.), pp. 325–328. San Francisco, CA: Scan Francisco Press, Inc.Google Scholar
Bastin, G.F. & Heijligers, H.J.M. (2011). Quantitative Electron Probe Microanalysis of Boron, Carbon, Nitrogen and Oxygen. The Netherlands. ISBN 978-94-6228-222-3.Google Scholar
Borile, F. & Garulli, A. (1978). Modifications to an electron microprobe to aid in the determination of low atomic number elements. X-Ray Spectrom 7, 124–131.Google Scholar
Buse, B. & Kearns, S. (2015). Importance of carbon contamination in high-resolution (FEG) EPMA of silicate minerals. Microsc Microanal 21, 594–605.Google Scholar
Campbell, A.J. & Gibbons, R. (1966). Specimen contamination in the electron microprobe. In The Electron Microprobe, McKinley, T.D., Heinrich, K.F.J. & Wittry, D.B. (Eds.), pp. 75–82. New York and London: John Wiley & Sons, Inc.Google Scholar
Castaing, R. & Descamps, J. (1954). Sur la contamination des échantillons dans le microanalyseur à sonde électronique. C R Acad Sci 238, 1506–1508.Google Scholar
Ennos, A.E. (1954). The sources of electron-induced contamination in kinetic vacuum systems. Br J Appl Phys 5, 27–31.CrossRefGoogle Scholar
Fourie, J.T. (1976). Contamination phenomena in cryopumped TEM and ultra-high vacuum field-emission STEM systems. Scan Electron Microsc 1976/1, 53–60.Google Scholar
Hart, R.K., Kassner, T.F. & Maurin, J.K. (1970). The contamination of surfaces during high-energy electron irradiation. Philos Mag 21, 453–467.Google Scholar
Heide, H.G. (1963). The prevention of contamination without beam damage to the specimen. In Proceedings of the Fifth International Congress on Electron Microscopy, Breese, S.S. (Ed.), pp. A4. New York: Academic Press.Google Scholar
Heide, H.G. & Urban, K. (1972). A novel specimen stage permitting high-resolution electron microscopy at low temperatures. J Phys E 5, 803–808.Google Scholar
Hirsch, P., Kässens, M., Püttmann, M. & Reimer, L. (1994). Contamination in a scanning electron microscope and the influence of specimen cooling. Scanning 16, 101–110.CrossRefGoogle Scholar
Honig, R.E. & Hook, H.O. (1960). Vapor pressure data for some common gases. RCA Rev 21, 360–368.Google Scholar
Hsu, C.C., Walsh, A.J., Nguyen, H.M., Overcashier, D.E., Koning-Bastiann, H., Bailey, R.C. & Nail, S.L. (1996). Design and application of a low-temperature peltier-cooling microscope stage. J Pharm Sci 85, 70–74.Google Scholar
Komoda, T. & Morito, N. (1960). Experimental study on the specimen contamination in electron microscopy. J Electron Microsc 9, 77–80.Google Scholar
Merlet, C. & Llovet, X. (2012). Uncertainty and capability of quantitative EPMA at low voltage—A review. IOP Conf Ser Mater Sci Eng 32, 012016.Google Scholar
Ong, P.S. (1966). Reducing carbon contamination. In X-Ray Optics and Microanalysis, Castaing, R., Deschamps, P. & Philibert, J. (Eds.), pp 181–192. Paris: Hermann.Google Scholar
Ranzetta, G.V.T. & Scott, V.D. (1964). Electron-probe microanalysis of low atomic number elements. Br J Appl Phys 15, 263–274.CrossRefGoogle Scholar
Ranzetta, G.V.T. & Scott, V.D. (1966). Specimen contamination in electron-probe microanalysis and its prevention using a cold trap. J Sci Instrum 43, 816–819.Google Scholar
Reed, S.J.B. (1975). Electron Microprobe Analysis. Cambridge: Cambridge University Press.Google Scholar
Swaroop, B. (1973). Carbon and case depth determination in steel by electron microprobe. Rev Sci Instrum 44, 1387–1389.CrossRefGoogle Scholar
Yamashita, T., Tanaka, Y., Yagoshi, M. & Ishida, K. (2016). Novel technique to suppress hydrocarbon contamination for high accuracy determination of carbon content in steel by FE-EPMA. Sci Rep 6, 29825.Google Scholar