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Scanning Microscopy

Abstract

The channelling or Borrmann effect in electron diffraction has been developed into a versatile, high spatial resolution, crystallographic technique with demonstrated applicability in solving a variety of materials problems. In general, either the characteristic x-ray emissions or the electron energy-loss intensities are monitored as a function of the orientation of the incident beam. The technique, as formulated in the planar geometry has found wide applications in specific site occupancy and valence measurements, determination of small atomic displacements and crystal polarity studies. For site occupancy studies, the appropriate orientations in most cases can be determined by inspection and the analysis carried out according to a simple classification of the crystal structure discussed in this paper. Concentration levels as low as 0.1 wt% can be easily detected. The reciprocity principle may be used to advantage in all these studies, if electron energy-loss spectra are monitored, as both the channelling of the incoming beam and the blocking of the outgoing beam are included in the formulation and analysis. The formulation in the axial geometry is an useful alternative, particularly for monatomic crystals. Localization effects are important if, either the experiment is performed in the axial geometry or if low atomic number elements (z<11) are detected. In general, the sensitivity to L-shells is lower compared to K-shell excitations. Other experimental parameters to be considered include temperature of the sample, the acceleration voltage and parallelism of the incident beam. Any detrimental effects of channelling on conventional microanalysis can be minimized either by tilting the crystal to an orientation where no lower order diffraction vectors are excited or by using a convergent probe such that a large range of incident beam orientations are averaged in the analysis.

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