Abstract
There are three phenomena produced by the interaction of a high-energy electron beam (100–1000 keV) with a thin specimen that can be used to provide chemical information in the analytical (transmission) electron microscope (AEM or ATEM). The origin of the most widely used of these, the characteristic X-ray spectrum, is explained in section 2.2.2 and quantification of the X-ray signal in the AEM follows procedures that are modifications of those used in electron probe microanalysis (EPMA).
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References
Allen, S.M. (1981) Foil thickness measurement from convergent-beam diffraction patterns. Phil. Mag., A43, 325–35.
Barber, D.J. (1993) Preparation of rock, mineral, ceramic and glassy materials, in Procedures in Electron Microscopy (eds A.W. Robards and A.J. Wilson), Wiley, Chichester, 1140 p
Bishop, H.E. (1974) Recent instrumental developments in microanalysis. in Advances in Analysis of Microstructural Features by Electron Beam Techniques, Metals Soc., London, pp. 1–18.
Boswell, E., Reece, M.J. and Gee, M.G. (1992) Preparation of hard particle powders for examination in the transmission electron microscope. J. Microsc., 167, 123–6.
Budd, P.M. and Goodhew, P.J. (1988) Eight Element Analysis in the Transmission Electron Microscope: WEDS and EEES, Oxford University Press/Royal Microscopical Society, 73 pp.
Buseck, P.R. and Self, P. (1992) Electron energy-loss spectrometry (EELS) and electron channelling (ALCHEMI), in Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy (ed. P.R. Buseck), Mineralogical Society of America, Washington, pp. 141–80.
Champness, P.E. (1987) Convergent beam electron diffraction. Mineral. Mag., 51, 33–48.
Champness, P.E. and Devenish (1990) Elemental mass loss in silicate minerals during X-ray analysis. Trans. Roy. Microsc. Soc., 1, 177–80.
Cliff, G. and Kenway, P.B. (1982) The effects of spherical aberration in probe-forming lenses on probe size, image resolution and X-ray spatial resolution in scanning transmission electron microscopy, in Microbeam Analysis — 1982 (ed. K.F.J. Heinrich), pp. 107–10.
Cliff, G. and Lorimer, G.W. (1975) The quantitative analysis of thin specimens. J. Microsc., 103, 203–7.
Cliff, G. and Lorimer, G.W. (1992) AEM: from microns to atoms, Proc. 50th Ann. EMSA Meeting, pp. 1464–5.
Cliff G. Powell D.J. Pilkington R. et al. (1984) X-ray microanalysis of second phase particles in thin foils in Electron Microscopy and Analysis 1983 (ed. P. Doig) Inst. Phys. Bristol p. 63–6
Cooke, C.J. and Duncumb, P. (1969) Performance analysis of a combined electron microscope and microprobe analyser ‘EMMA’, in Proc 5th Intl. Congr. on X-ray optics and Microanalysis (eds G. Mollenstedt and K.H. Gaukler), pp. 245–7.
Devenish, R.W. and Champness, P.E. (1993) The rate of mass loss in silicate minerals during X-ray analysis, Proc 13th Intl. Congr. on X-ray optics and microanalysis, Manchester, 1992, Inst. Physics, London and Bristol, p. 233–6.
Duncumb, P. (1966) Precipitation studies with EMMA-4 — A combined electron microscope and X-ray analyser, in The Electron Microprobe (eds T.D. McKinley, K.F.J. Heinrich and D.B. Wittry), Wiley, New York
Egerton, R.F. (1981) Values of K-shell partial cross-sections for electron energy-loss spectrometry. J. Microsc., 123, 333–7.
Egerton, R.F. (1986) Electron Energy Loss Spectroscopy, Plenum Press, New York, 410 pp.
Goldstein, J.I., Costley, J.L., Lorimer, G.W. and Reed, S.J.B. (1977) Quantitative X-ray analysis in the electron microscope, in SEM/77 (ed. O. Johari), IITRI, Chicago, pp. 315–24.
Goldstein, J.I., Lyman, C.E. and Williams, D.B. (1989) The wavelength-dispersive spectrometer and its proposed use in the analytical electron microscope. Ultramicroscopy, 28, 162–4.
Goldstein, J.I. and Williams, D.B. (1992) X-ray microanalysis and electron energy loss spectrometry in the analytical electron microscope: review and future directions. Microbeam Anal., 1, 29–53.
Griffin, B.J. and Johnson, A.W.S. (1992) Experiences with HPGe EDS detectors on a Philips EM430 and a JEOL 6300 FESEM, Proc 50th Ann. Meeting EMSA, pp. 1232–3.
Horita, Z., Sano, T. and Nemoto, M. (1987) Simplification of X-ray absorption correction in thin-sample quantitative microanalysis. Ultramicroscopy, 21, 271–6.
Horita, Z., Sano, T. and Nemoto, M. (1989) Energy dispersive X-ray microanalysis in the analytical electron microscope. ISIJ International, 29, 179–90.
Horita, Z., Takeshi, S. and Nemoto, M. (1986) An extrapolation method for the determination of Cliff-Lorimer k AB factors at zero thickness. J. Microsc, 143, 215–31.
Hunt, J.A. and Williams, D.B. (1991) Electron energy-loss spectrum-imaging. Ultramicroscopy. 38, 47–73.
Joy, D.C. and Maher, D.M. (1977) Sensitivity limits for thin specimen X-ray analysis. Scanning Electron Microscopy, 1, 325–33.
Joy, D.C., Romig, A.D. and Goldstein, J.I. (eds) (1986) Principles of Analytical Microscopy. Plenum, New York.
Kelly, P.M., Jostens, A., Blake, R.G. and Napier, J.G. (1975) Determination of foil thickness by scanning transmission electron microscopy. Phys. Stat. Sol., A31, 771–9.
Leapman, R.D. and Newbury, D.E. (1992) Trace element analysis of transition elements and rare earths by parallel EELS. Proc. 50th Ann. Meeting EMSA, pp. 1250–1.
Lee, S.Y. and Jackson, M.L. (1975) Micaceous occlusions in kaolinite observed by ultramicrotomy and high resolution electron-microscopy. Clays and Clay Minerals, 34, 125–9.
Livi, K.J.T. and Veblen, D.R. (1987) ‘Eastonite’ from Easton. Pennsylvania: a mixture of phlogopite and a new form of serpentine. Amer. Mineral., 72, 113–25.
Lorimer, G.W. (1987) Quantitative X-ray microanalysis of thin specimens in the transmission electron microscope; a review. Mineral Mag., 51, 49–60.
Lorimer, G.W., Cliff, G., Champness, P.E. et al. (1984) In situ X-ray microanalysis of second phase particles in thin foils, in Analytical Electron Microscopy — 1984 (eds D.B. Williams and D.C. Joy), San Francisco Press, San Francisco, pp. 153–
Malis, T., Cheng, S.C. and Egerton, R.F. (1988) EELS log-ratio technique for specimenthickness measurement in the TEM. J. Electron Microsc. Technique, 8, 193–200.
McGill, R.J. and Hubbard, F.H. (1981) Thin film k-value calibration for low atomic number elements using silicate standards, in Quantitative Microanalysis with High Spatial Resolution (eds G.W. Lorimer, M.H. Jacobs and P. Doig), Metals Society, London, pp. 30–
Michael, J.R., Williams, D.B., Klein, C.F. and Ayer, R. (1990) The measurement and calculation of the X-ray spatial resolution obtained in the analytical electron microscope. J. Microsc, 147, 289–303.
Morris, P.L., Ball, M.D. and Statham, P.J. (1980) The correction of thin foil microanalysis data for X-ray absorption effects, in Electron Microscopy and Analysis 1979 (ed. T. Mulvey), Inst. Phys., Bristol, p. 413–6.
Mory, C. and Colliex, C. (1989) Elemental analysis near the single-atom detection level by processing sequences of energy-filtered images. Ultramicroscopy, 28, 2339–46.
Nicholson, W.A.P., Gray, C.C., Chapman, J.N. and Robertson, B.W. (1982) Optimising thin film X-ray spectra for quantitative analysis. J. Microsc, 125, 25–40.
Nockolds, C., Nasir, M.J., Cliff, G. and Lorimer, G.W. (1980) X-ray fluorescence correction in thin foil analysis and direct methods for foil thickness measurement, in Electron Microscopy and Analysis 1979 (ed. T. Mulvey), Institute of Physics, Bristol, pp. 417–20.
Nord, G.L. Jr (1982) Analytical electron microscopy in mineralogy; exsolved phases in pyroxenes. Ultramicroscopy. 8, 109–20.
Peacor, D.R. (1992) Analytical electron microscopy: X-ray analysis, in Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy (ed. P.R. Buseck), Mineralogical Society of America, Washington, pp. 113–40.
Porter, D.A. and Westengen, H. (1981) STEM microanalysis of intermetallic phases in an Al-Fe-Si alloy, in Quantitative Microanalysis with High Spatial Resolution (eds G.W. Lorimer, M.H. Jacobs and P. Doig), Metals Society, London, pp. 94–100.
Rae, D.A., Scott, V.D. and Love, G. (1981) Errors in foil thickness measurement using contamination spot method, in Quantitative Microanalysis with High Spatial Resolation (eds G.W. Lorimer, M.H. Jacobs and P. Doig), Metals Society, London, pp. 57–62.
Reed, S.J.B. (1982) The single scattering model and spatial resolution in X-ray analysis of thin foils. Ultramicroscopy, 7, 405–9.
Rietmeijer, F.J.M. and Champness, P.E. (1982) Exsolution structures in calcic pyroxenes from the Bjerkreim-Sokndal lopolith, SW Norway. Mineral. Mag., 45, 11–24.
Romig, A.D. and Goldstein, J.L. (1980) Determination of the Fe-Ni and Fe-Ni-P phase diagrams at low temperatures (700 to 300°C). Metall. Trans., 11A, 1151–9.
Shau, Y.-H., Feather, M.E., Essene, E.J. and Peacor, D.R. (1991) Genesis and solvus relations of submicroscopically intergrown paragonite and phengite in a blueschist from northern California. Contrib. Mineral. Petrol., 106, 367–78.
Sheridan, P.J. (1989) Determination of experimental and theoretical k ASi factors for a 200-kV analytical electron microscope. J. Electron Microsc. Technique, 11, 41–61.
Spence J.C.H. (1988) Techniques closely related to high-resolution electron microscopy in High Resolution Transmission Electron Microscopy (eds P.R. Buseck J.M. Cowley and L. Eyling) Oxford University Press p. 190–243
Titchmarsh, J.M. (1989) Comparison of high spatial resolution in EDX and EELS analysis. Ultramicroscopy, 28, 347–51.
Van Cappellen, E. (1990) The parameterless correction method in X-ray microanalysis. Micro. Microanal. Microstruct., 1, 1–22.
Van Cappellen, E., Van Dyck, D., Van Landuyt, J. and Adams, F. (1984) A parameterless method to correct for X-ray absorption and fluorescence in thin film microanalysis. J. Phys. Colloq. Fr., 45, C2, 411–14.
van der Pluijm, B.A., Lee, J.H. and Peacor, D.R. (1988) Analytical electron microscopy and the problem of potassium diffusion. Clays and Clay Minerals, 36, 498–504.
Westwood, A.D., Michael, J.R. and Notis, M.R. (1992) Experimental determination of lightelement k-factors using the extrapolation technique: oxygen segregation in aluminium nitride. J. Microsc., 167, 287–302.
Williams, D.B. (1984) Practical Analytical Electron Microscopy in Materials Science, Philips Electronic Instruments Inc., Mahwah, New Jersey. 153 p
Williams, D.B. (1986) Standardised definitions of X-ray analysis performance criteria in the AEM, in Microbeam Analysis — 1986 (eds A.D. Romig and W.F. Chambers), pp. 443–8.
Wood, J.E., Williams, D.B. and Goldstein, J.I. (1984) Experimental and theoretical determination of k AFe factors for quantitative X-ray microanalysis in the analytical electron microscope. J. Microsc., 133, 255–74.
Zaluzec, N.J. (1992) Current performance limits for XEDS in the AEM. Proc. 50th Ann. Meeting EMSA, pp. 1466–7.
Zemyan, S.M. and Williams, D.B. (1991) X-ray analysis of heavy elements by use of L and K series lines, in Microbeam Analysis — 1991 (ed. D.G. Howitt), pp. 134–6.
Zemyan, S.M. and Williams, D.B. (1992) Peak-to-background measurements on a 300 kV TEM/STEM. Proc. 50th Ann. Meeting EMSA, pp. 1236–7.
Ziebold, T.O. (1967) Minimum detectability limits in electron probe microanalysis. Anal. Chem., 39, 858–63.
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Champness, P.E. (1995). Analytical electron microscopy. In: Potts, P.J., Bowles, J.F.W., Reed, S.J.B., Cave, M.R. (eds) Microprobe Techniques in the Earth Sciences. The Mineralogical Society Series, vol 6. Springer, Boston, MA. https://doi.org/10.1007/978-1-4615-2053-5_3
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DOI: https://doi.org/10.1007/978-1-4615-2053-5_3
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