International
Tables for Crystallography Volume C Mathematical, physical and chemical tables Edited by E. Prince © International Union of Crystallography 2006 |
International Tables for Crystallography (2006). Vol. C. ch. 2.4, p. 80
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The electron wavelengths normally used to obtain powder patterns from thin films of polycrystalline materials lie in the range 8 × 10−2 to 2 × 10−2 Å (20 to 200 kV accelerating voltages). The maximum scattering angles () observed are usually less than 10−1 rad.
Patterns are usually recorded on flat photographic plates or films and a small-angle approximation is applied. For a camera length L, the distance from the specimen to the photographic plate in the absence of any intervening electron lenses, the approximation is made that, for a diffraction ring of radius r, or the interplanar spacing, d, is given by For a scattering angle of 10−1 rad, the error in this expression is 0.5%. A better approximation, valid to better than 0.1% at 10−1 rad, is The `camera constant' may be obtained by direct measurement of L and the accelerating voltage if there are no electron lenses following the specimen.
Direct electronic recording of intensities has great advantages over photographic recording (Tsypursky & Drits, 1977).
In recent years, electron diffraction patterns have been obtained most commonly in electron microscopes with three or more post-specimen lenses. The camera-constant values are then best obtained by calibration using samples of known structure.
With electron-optical instruments, it is possible to attain collimations of 10−6 rad so that for scattering angles of 10−1 rad an accuracy of 10−5 in d spacings should be possible in principle but is not normally achievable. In practice, accuracies of about 1% are expected. Some factors limiting the accuracy of measurement are mentioned in the following sections. The small-angle-scattering geometry precludes application of any of the special camera geometries used for high-accuracy measurements with X-rays (Chapter 2.3 ).
References
Tsypursky, S. I. & Drits, V. A. (1977). The efficiency of the electronometric measurement of intensities in electron diffraction structural studies. Izv. Akad. Nauk SSSR Ser. Phys. 41, 2263–2271. [In Russian.]Google Scholar