Hostname: page-component-8448b6f56d-c47g7 Total loading time: 0 Render date: 2024-04-25T04:29:45.335Z Has data issue: false hasContentIssue false
  • English
  • Français

Electron Beam-Induced Carbon Erosion and the Impact on Electron Probe Microanalysis

Published online by Cambridge University Press:  16 November 2018

Mike B. Matthews ,
Stuart L. Kearns  and
Ben Buse
Mike B. Matthews*
Affiliation:
AWE, Aldermaston, Reading, RG7 4PR, UK University of Bristol, School of Earth Sciences, Wills Memorial Building, Queens Road, Clifton, BS8 1RJ, UK
Stuart L. Kearns
Affiliation:
University of Bristol, School of Earth Sciences, Wills Memorial Building, Queens Road, Clifton, BS8 1RJ, UK
Ben Buse
Affiliation:
University of Bristol, School of Earth Sciences, Wills Memorial Building, Queens Road, Clifton, BS8 1RJ, UK
*
Author for correspondence: M. B. Matthews, E-mail: matthm@hotmail.com
Get access

Abstract

Electron beam-induced carbon contamination is a balance between simultaneous deposition and erosion processes. Net erosion rates for a 25 nA 3 kV beam can reduce a 5 nm C coating by 20% in 60 s. Measurements were made on C-coated Bi substrates, with coating thicknesses of 5–20 nm, over a range of analysis conditions. Erosion showed a step-like increase with increasing electron flux density. Both the erosion rate and its rate of change increase with decreasing accelerating voltage. As the flux density decreases the rate of change increases more rapidly with decreasing voltage. Time-dependent intensity (TDI) measurements can be used to correct for errors, in both coating and substrate quantifications, resulting from carbon erosion. Uncorrected analyses showed increasing errors in coating thickness with decreasing accelerating voltage. Although the erosion rate was found to be independent of coating thickness this produces an increasing absolute error with decreasing starting thickness, ranging from 1.5% for a 20 nm C coating on Bi at 15 kV to 14% for a 5 nm coating at 3 kV. Errors in Bi Mα measurement are <1% at 5 kV or above but increase rapidly below this, both with decreasing voltage and increasing coating thickness to 20% for a 20 nm coated sample at 3 kV.

Keywords

carbon erosionlow voltageelectron probe microanalysisthin filmcoating
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 24 , Issue 6 , December 2018 , pp. 612 - 622
Copyright
© Microscopy Society of America 2018 

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.)

Footnotes

Cite this article: Matthews MB, Kearns SL and Buse B (2018) Electron Beam-Induced Carbon Erosion and the Impact on Electron Probe Microanalysis. Microsc Microanal. 24(6), 612–622. doi: 10.1017/S1431927618015398

References

Amman, M, Sleight, JW, Lombardi, DR, Welser, RE, Deshpande, MR, Reed, MA and Guido, LJ (1996) Atomc force microscopy study of electron beam written contamination structures. J Vac Sci Technol B 14(1), 54–62.Google Scholar
Bastin, GF and Heijligers, HJM (1988) Contamination phenomena in the electron probe microanalyzer. In Microbeam Analysis, Newbury DE (Ed.), pp. 325–328. San Francisco, CA: San Francisco Press.Google Scholar
Bearden, JA and Burr, AF (1967) Reevaluation of X-ray atomic energy levels. Rev Mod Phys 39(1), 125–142.Google Scholar
Buse, B and Kearns, SL (2015) Importance of carbon contamination in high-resolution (FEG) EPMA of silicate minerals. Microsc Microanal 20(1), 1–12.Google Scholar
Buse, B, Kearns, SL, Clapham, C and Hawley, D (2016) Decontamination in the electron probe microanalysis with a Peltier-cooled cold finger. Microsc Microanal 22(5), 981–986.Google Scholar
Choi, YR, Rack, PD, Randolph, SJ, Smith, DA and Joy, DC (2006) Pressure effect of growing with electron beam-induced deposition with tungsten hexafluoride and tetraethylorthosilicate precursor. Scanning 28(6), 311–318.Google Scholar
Demers, H, Poirier-Demers, N, Couture, AR, Joly, D, Guilmain, M, De Jonge, N and Drouin, D (2011) Three-dimensional electron microscopy simulation with the CASINO Monte Carlo software. Scanning 33(3), 135–146.Google Scholar
Ennos, AE (1953) The origin of specimen contamination in the electron microscope. Br J Appl Phys 4(4), 101–106.Google Scholar
Ennos, AE (1954) The sources of electron-induced contamination in kinetic vacuum systems. Br J Appl Phys 5(1), 27–31.Google Scholar
Heide, HG (1962) The prevention of contamination without beam damage to the specimen. In Electron Microscopy: Fifth International Congress for Electron Microscopy, Philadelphia, Breese SS (Ed.), pp. A4–A5. New York: Academic Press.Google Scholar
Hren, JJ (1979) Barriers to AEM: Contamination and etching. In Introduction to Analytical Electron Microscopy, Hren JJ, Goldstein JI and Joy D (Eds.), pp. 481–505. New York: Plenum Press.Google Scholar
Isabell, TC, Fischione, PE, O’Keefe, C, Guruz, MU and Dravid, VP (1999) Plasma cleaning and its applications for electron microscopy. Microsc Microanal 5, 126–135.Google Scholar
Kohlmann-von Platen, KT and Bruenger, WH (1996) Electron-beam induced etching of resist with water vapor as the etching medium. J Vac Sci Technol B 14(6), 4262.Google Scholar
Konuma, H (1983) Rate of carbon contamination on copper, iron and aluminum targets in gas flows by an electron microprobe. Mikrochimica Acta 80(1–2), 99–108.Google Scholar
Lobo, CJ, Toth, M, Wagner, R, Thiel, BL and Lysaght, M (2008) High resolution radially symmetric nanostructures from simultaneous electron beam induced etching and deposition. Nanotechnology 19(2), 025303–1-025303-6.Google Scholar
Matthews, MB, Kearns, SL and Buse, B (2018) The accuracy of Al and Cu film thickness determinations and the implications for electron probe microanalysis. Microsc Microanal 24(2), 83–92.Google Scholar
Mitchell, DRG (2015) Contamination mitigation strategies for scanning transmission electron microscopy. Micron 73, 36–46.Google Scholar
Nielsen, CH and Sigurdsson, H (1981) Quantitative methods for electron microprobe analysis of sodium in natural and synthetic glasses. Am Mineral 66(5–6), 547–552.Google Scholar
Pinard, PT (2016) Electron probe microanalysis of carbon containing steels at a high spatial resolution. Thesis, RWTH Aachen University. Available at http://publications.rwth-aachen.de/record/673259/files/673259.pdf (retrieved 8 April, 2018).Google Scholar
Pinard, PT, Schwedt, A, Ramazani, A, Prahl, U and Richter, S (2013) Characterization of dual-phase steel microstructure by combined submicrometer EBSD and EPMA carbon measurements. Microsc Microanal 19(4), 996–1006.Google Scholar
Ranzetta, GVT and Scott, VD (1966) Specimen contamination in electron-probe microanalysis and its prevention using a cold trap. J Sci Instrum 43, 816–819.Google Scholar
Reed, SJB (1975) Electron Microprobe Analysis. Cambridge: Cambridge University Press.Google Scholar
Reimer, L and Tollkamp, C (1980) Measuring the backscattering coefficient and secondary electron yield inside a scanning electron microscope. Scanning 3, 35–39.Google Scholar
Reimer, L and Wachter, M (1978) Contribution to the contamination problem in transmission electron microscopy. Ultramicroscopy 3, 169–174.Google Scholar
Shimojo, M, Mitsuishi, K, Tameike, A and Furuya, K, et al. (2004) Electron induced nanodeposition of tungsten using field emission scanning and transmission electron microscopes. J Vac Sci Technol B 22(2), 742–746.Google Scholar
Silvis-Cividjian, N, Hagen, CW and Kruit, P (2002) The role of secondary electrons in electron-beam-induced-deposition spatial resolution. Microelectron Eng 61–62, 693–699.Google Scholar
Stormer, JC, Pierson, ML and Tacker, RC (1993) Variation of F and Cl X-ray intensity due to anisotropic diffusion in apatite during electron microprobe analysis. Am Mineral 78(5–6), 641–648.Google Scholar
Tanaka, M, Shimojo, M, Han, M, Mitsuishi, K and Furuya, K (2005) Ultimate sized nano-dots formed by electron beam-induced deposition using an ultrahigh vacuum transmission electron microscope. Surf Interface Anal 37(2), 261–264.Google Scholar
Toth, M, Lobo, CJ, Hartigan, G and Ralph Knowles, W (2007) Electron flux controlled switching between electron beam induced etching and deposition. J Appl Phys 101(5), 54309–1-54309–6.Google Scholar
Ueda, K and Yoshimura, M (2004) Fabrication of nanofigures by focused electron beam-induced deposition. Thin Solid Films 464–465, 331–334.Google Scholar
Utke, I, Hoffmann, P and Melngailis, J (2008) Gas-assisted focused electron beam and ion beam processing and fabrication. J Vac Sci Technol B 26(4), 1197.Google Scholar
van Dorp, WF, van Someren, B, Hagen, CW, Kruit, P and Crozier, PA (2005) Approaching the resolution limit of nanometer-scale electron beam-induced deposition. Nano Lett 5(7), 1303–1307.Google Scholar
Waldo, RA (1988) An iteration procedure to calculate film compositions and thicknesses in electron-probe microanalysis. In Microbeam Analysis, Newbury DE (Ed.), pp. 310–314. San Francisco, CA: San Francisco Press.Google Scholar