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Analysis of Kikuchi band contrast reversal in electron backscatter diffraction patterns of silicon
(2010)

We analyze the contrast reversal of Kikuchi bands that can be seen in electron backscatter diffraction (EBSD) patterns under specific experimental conditions. The observed effect can be reproduced using dynamical electron diffraction calculations. Two crucial contributions are identified to be at work: First, the incident beam creates a depth distribution of incoherently backscattered electrons which depends on the incidence angle of the beam. Second, the localized inelastic scattering in the outgoing path leads to pronounced anomalous absorption effects for electrons at grazing emission angles, as these electrons have to go through the largest amount of material. We use simple model depth distributions to account for the incident beam effect, and we assume art exit angle dependent effective crystal thickness in the dynamical electron diffraction calculations. Very good agreement is obtained with experimental observations for silicon at 20 key primary beam energy.

A survey is presented on some characteristic features of meteoritic (Fe,Ni)3P which is an abundant and important minor phase of most iron meteorites. This mineral (named schreibersite/rhabdite) plays a decisive role during the formation of the so-called Widmanstätten pattern. Different transmission as well as scanning electron microscopic techniques have been applied to get more precise information about the real structure of the phosphide crystals, their chemical composition and the metal distribution across the phoshide/ kamacite interface. X-ray crystal structure determinations have been performed for selected (Fe,Ni)3P - cystals from various iron meteorites (Toluca, North Chile, Watson, Orange River, Morasko, Agpalilik, Odessa, Canyon Diablo). These experiments revealed a metal ordering, i.e. for the three non-equivalent metal positions a different substitution of Fe by Ni has been found. The perfection of the brittle (Fe,Ni)3P samples differs appreciably and seems to be dependent on the thermal history of each individual meteorite. Moreover, inside Ni-rich rhabdite crystals small monocrystalline inclusions of CrN (carlsbergite) have been detected.

We demonstrate an approach to overcome Kikuchi pattern misindexing problems caused by crystallographic pseudosymmetry in electron backscatter diffraction (EBSD) measurements. Based on the quantitative comparison of experimentally measured Kikuchi patterns with dynamical electron diffraction simulations, the algorithm identifies the best-fit orientation from a set of pseudosymmetric candidates. Using measurements on framboidal pyrite (FeS2) as an example, we also show the improvement of the orientation precision using this approach.

The visualization of spatially resolved single Orientation data, e.g. collected by electron backscatter diffraction (EBSD) in the scanning electron microscope (SEM), is still a challenge since some Orientation coloring schemes have low color sensitivity, and/or specific color discontinuities. The latter appear even for crystal Orientations which are practically identical and characterized only by a tiny misorientation. Euler angle coloring schemes suffer from their lack of intuitiveness. The inverse pole figure (IPF) coloring that has been widely accepted does not display the real Orientation Information for each measurement point, but only the crystallographic description of a single reference direction. For the representation of the complete Orientation information at least a second IPF Orientation map must be shown which displays the crystallographic description for another reference direction. In this context it must be pointed out that the IPF coloring is also not immune to color discontinuities, which are visible as speckled grains (and usually misinterpreted as erroneous Orientation determinations by EBSD). However, a general analysis of the commonly used color keys shows that color discontinuities are a consequence of the crystal symmetry for 6 of the 11 centrosymmetric Laue groups. This means that the Orientation description is correct, but the representation tool is inappropriate for properly displaying the orientation information.

We demonstrate polarity-sensitive orientation mapping of non-centrosymmetric phases by Electron Backscatter Diffraction (EBSD). The method overcomes the restrictions of kinematic orientation determination by EBSD, which is limited to the centro-symmetric Laue-groups according to Friedel's rule. Using polycrystalline GaP as an example, we apply a quantitative pattern matching approach based on simulations using the dynamical theory of electron diffraction. This procedure results in a distinct assignment of the local orientation according to the non-centrosymmetric point group of the crystal structure under investigation.

We discuss the application of EBSD for the analysis of structural features of magnetite and hematite relevant in the topotactic growth of both phases. The orientation relationships of both phases are investigated using characteristically related sets of Kikuchi patterns, which were collected from topotactically intergrown hematite variants and their parent magnetite crystal grain. We address the hexagonal description of trigonal and cubic phases with respect to crystallographic relationships. The combination of locally resolved EBSD measurements and microstructural investigations thus offers a promising opportunity to evaluate orientation relationships and intergrowth between magnetite and hematite.

We demonstrate the determination of crystal chirality using electron backscatter diffraction (EBSD) in the scanning electron microscope. The chirality of a-quartz as a space-group-dependent property is verified via direct comparison of experimental diffraction features to simulations using the dynamical theory of electron diffraction.

For the description of (single) crystal orientations, e.g. as measured by electron backscatter diffraction (EBSD) & X-ray diffraction (XRD), Euler angles are still generally used to import and export data. However, because of the lack of standard definitions for the unit cell reference settings and specimen axes, several transformation descriptions exist which produce different sets of Euler angles for the same orientation. There is also no recommended region within the minimal Euler orientation space into which orientations should be placed. This is the reason why different sets of Euler angles for the same orientation are generated by the available software packages for indexing EBSD patterns. These issues are reviewed and addressed.
The influence of crystal symmetry in form of chiral (enantiomorphic) groups is discussed, as well as how multiple, but symmetry-equivalent sets of Euler angles can be reduced in order to deliver a unique orientation description. The Euler coloring algorithms applied to EBSD map data is critically discussed. The specific case of cubic symmetry, especially the effect of the three-fold rotation on the Euler space is investigated in more detail for the highest-symmetric chiral group 432. Recommendations for standard settings of the unit cell to orthogonal coordinate system transformation are given which exploit inherent symmetry.