The determination of rotation axis in the rotation electron diffraction technique.

Methods to determine the rotation axis using the rotation electron diffraction technique are described. A combination of rotation axis tilt, beam tilt, and simulated experimental diffraction patterns with nonintegers zone axis has been used. Accurate knowledge of the crystallographic direction of the incident beam for deducing the excitation error of reflections simultaneously near Bragg positions is essential in quantitative electron diffraction. Experimental patterns from CoP3 are used as examples.

Geometry determination and refinement in the rotation electron diffraction technique.

The necessary parameters (rotation axis, incident electron beam direction and beam tilt path) in order to describe the diffraction geometry in the Rotation Electron Diffraction (RED) method during data collection are determined and refined. These parameters are prerequisites for the subsequent calculations of excitation errors, sg, for zero (ZOLZ) or higher order Laue zones (HOLZ) reflections. Comparison with simulated results, for a CoP3 thermoelectric crystal, shows excellent agreement between the two approaches -calculated and simulated. In addition to their determination, a thorough refinement methodology for the incident electron beam direction and beam tilt path has been applied, too, based on Kikuchi lines of HOLZ reflections. Incorporation of the refined excitation error values can be considered both in theoretical calculations for diffracted beam intensities, based on the Bloch wave method, as well as in deducing integrated intensities from experimental rocking curves. The methodology described in this study is quite indispensable, as it forms an essential step for performing dynamical calculations in RED, enabling thus enhanced accuracy in structural parameter clarification. The latter is especially important in the case of thermal factors refinement for e.g. thermoelectrics, which are imperative for material properties' evaluation.