Acquisition and evaluation procedure to improve the accuracy of SAED. Issue 2 (7th September 2022)

• Record Type: Journal Article
• Authors: Czigány, Zsolt; Kis, Viktória Kovács
• Is Part Of: Microscopy research and technique. Volume 86:Issue 2(2023)
• Page Start: 144
• Page End: 156
• Publication Date: 2022-09-07
• Subjects: aberration corrected TEM -- bioapatite -- evaluation procedure -- precision -- reproducibility -- SAED; Electron microscopy -- Technique -- Periodicals; Microscopy -- Periodicals; Microscopy -- Technique -- Periodicals; 502.825
• DOI: 10.1002/jemt.24229
• Languages: English
• ISSNs: 1059-910X

Abstract

Abstract: The achievement of this work is that fine tuning of experimental and evaluation parameters can improve the absolute accuracy and reproducibility of selected area electron diffraction (SAED) to 0.1% without using internal standard. Due to the proposed procedure it was possible to reach a reproducibility better than 0.03% for camera length between sessions by careful control of specimen height and illumination conditions by monitoring lens currents. We applied a calibration specimen composed of nanocrystalline grains free of texture and providing narrow diffraction rings. Refinements of the centre of the diffraction pattern and corrections for elliptic ring distortions allowed for determining the ring diameters with an accuracy of 0.1%. We analyze the effect of different error sources and reason the achieved absolute accuracy of the measurement. Application of the proposed evaluation procedure is inevitable in case of multicomponent nanocomposites or textured materials and/or having close diffraction rings where application of automated procedures is limited. The achieved accuracy of 0.1% without internal standard is approaching that of routine laboratory XRD, and reduction of instrumental broadening due to the elaborated evaluation procedure allows for separation of close reflections, provides more reliable ring width and thus improved input parameters for further nanostructure analysis as demonstrated on dental enamel bioapatite. Abstract : The improved reproducibility and accuracy of electron diffraction patterns without internal standard allows for reliable detection of 0.05 Å shift of peak positions and distinction and intensity analysis of 8 and 15 pixels wide diffraction rings separated by 12 pixels in case of dental enamel bioapatite.