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Non-Destructive Chemical-State Analysis of Thin Films and Surface Layers (1-1000 nm) by Low-Energy Electron-Induced X-ray Spectroscopy (LEEIXS)

Published online by Cambridge University Press:  06 March 2019

Angeli K. Gyani
Affiliation:
Chemistry Department, Queen Mary College, Mile End Road, LONDON El 4NS, U.K.
Phillip McClusky
Affiliation:
Chemistry Department, Queen Mary College, Mile End Road, LONDON El 4NS, U.K.
David S. Urch
Affiliation:
Chemistry Department, Queen Mary College, Mile End Road, LONDON El 4NS, U.K.
M. Charbonnicr
Affiliation:
Dépanement de Chimic appliquéc et Génie chimique CNRS. URA 417, Université Claude Bernard-Lyon I, 43 Boulevard du 11 novembre 1918. F-69622 VILLEURBANNE, Cedex FRANCE
F. Gaillard
Affiliation:
Dépanement de Chimic appliquéc et Génie chimique CNRS. URA 417, Université Claude Bernard-Lyon I, 43 Boulevard du 11 novembre 1918. F-69622 VILLEURBANNE, Cedex FRANCE
M. Romand
Affiliation:
Dépanement de Chimic appliquéc et Génie chimique CNRS. URA 417, Université Claude Bernard-Lyon I, 43 Boulevard du 11 novembre 1918. F-69622 VILLEURBANNE, Cedex FRANCE
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Abstract

The penetration depth of 1-12 keV electrons in most materials is less than one micron and the characteristic soft x-rays that are produced can be used to identify the elements present in the surface. Varying the energy of the incident electron beam enables the depth of analysis to be controlled.

Soft x-rays often exhibit large 'chemical effects' (changes in peak profile and peak position) which can he correlated with chemical changes. A study of such effects for each element present in the sample surface, as a function of electron-beam energy, can in some cases, permit changes in the chemical state (valency - coordination number-spin state etc.) to be determined as a function of depth.

Such analyses can be carried out either in a conventional x-ray spectrometer in which the x-ray tube has been replaced by a gas-discharge source, or in a spectrometer in which the sample is bombarded with electrons from a normal electron gun. In this paper these techniques are outlined and some applications reviewed:- the analysis of oxide layers on aluminium and steel, the analysis of aluminium-nitride layers produced by MOCVD on gallium arsenide, the analysis of silica fiims (with added boron and phosphorus oxides) on silicon and the analysis of zinc-oxide films on glass.

Type
Research Article
Copyright
Copyright © International Centre for Diffraction Data 1989

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References

1. Romand, M., Bador, R., Charbonnier, M. and Gaillard, F., Surface and Near Surface Chemical Characterization by Low-Energy Electron Induced X-ray Spectrometry [LEE1XS]: A Review, X-Ray Spectrometry. 16: 7 [1987].Google Scholar
2. Gaillard, F. and Romand, M., Applications de la spectrometrie d‘Emission de rayons - X [LEEIXS]à l'etude des materiaux isolants. Cas de quelques oxydes metalliques, Le Vide, les Couches Minces. supp. to Vol 243: 231 [1988].Google Scholar
3. Urch, D. S., X-ray Emission Spectroscopy, in: ‘Electron Spectroscopy - Theory. Techniques and Applications‘, Brundie, G. R. and Baker, A. D., eds: Academic Press, London, 3: 1 [1979].Google Scholar
4. Horn, R. and Urch, D. S., Chemical Effects in the X-ray emission spectra of sulphur, Spectro chimica Acta B. 42: 1177 [1987].Google Scholar
5. Day, D. E., Determining the Coordination Number of aluminiumions by X-ray emission spectroscopy. Nature, 200: 649 [1963].Google Scholar
6. Urch, D. S., The origin and intensities of low energy satellite lines in X-ray emission spectra : a molecular orbital interpretation, J. Phys. C-Solid St. Phys. 3: 1275 [1970].Google Scholar
7. Urch, D. S. and Wood, P. R., The determination of the valency of manganese in minerals by x-ray fluorescence spectroscopy, X-ray Snectroscopy. 7: 9 [1978].Google Scholar
8. Slater, R. A. and Urch, D. S., The origin of the Kβ' satellite peak in the X-ray fluorescence spectra of iron compounds : a correlation with magnetic susceptibility, J. Chem. Soc. Chem. Comm., 564 [1972].Google Scholar
9. Feldman, C., Range of 1-10keV electrons insolids, Phys. Rev., 117: 2, 455 [1960].Google Scholar
10. Charbonnier, M., Romand, M. and Gaillard, F., Theoretical experimental aspects of lowenergy electron induced spectroscopy, Analusis, 16[supp to #9-10]: 17[1988].Google Scholar
11. Szasz, A. and Kojnok, J., 'soft X-ray emission depth profile analysis :SXDA, App. Surf. Sci., 24: 34 [1985].Google Scholar
12. Esinail, E. I., Nichnlis, C. J. and Urch, D. S.. The detection of light elements by x-ray emission spectroscopy with use of low energy satellite peaks, Analyst. 98: 725 [1973].Google Scholar
13. Luck, S., “X-ray fluorescence spcctroscopy at long wavelengths : elemental and chcmical state analysis“. Ph.D. Thesis, London University, U.K.[1989].Google Scholar
14. Andermann, G., reported by Worthy, W. ‘X-ray technique may provide new way to study surfaces, films, Chem. & Ind. News. 63 # 14 : 28[1985].Google Scholar
15. Willis, J. E., characterization of thin-films amples using X-ray fluorescence. Adv. X-ray Analysis. Vol. 33 [1990].Google Scholar
16. Powell, C. J., Cross-sections for ionisation of inner-shell electrons by electrons, Rev. Mod. Phys., 48: 33 [1976].Google Scholar