scholarly journals Atomic-level elastic strain measurement of amorphous materials by quantification of local selected area electron diffraction patterns

Author(s):  
Christian Ebner ◽  
Rohit Sarkar ◽  
Jagannathan Rajagopalan ◽  
Christian Rentenberger
IUCrJ ◽  
2020 ◽  
Vol 7 (3) ◽  
pp. 490-499
Author(s):  
Marcus Gallagher-Jones ◽  
Karen C. Bustillo ◽  
Colin Ophus ◽  
Logan S. Richards ◽  
Jim Ciston ◽  
...  

Nanocrystallography has transformed our ability to interrogate the atomic structures of proteins, peptides, organic molecules and materials. By probing atomic level details in ordered sub-10 nm regions of nanocrystals, scanning nanobeam electron diffraction extends the reach of nanocrystallography and in principle obviates the need for diffraction from large portions of one or more crystals. Scanning nanobeam electron diffraction is now applied to determine atomic structures from digitally defined regions of beam-sensitive peptide nanocrystals. Using a direct electron detector, thousands of sparse diffraction patterns over multiple orientations of a given crystal are recorded. Each pattern is assigned to a specific location on a single nanocrystal with axial, lateral and angular coordinates. This approach yields a collection of patterns that represent a tilt series across an angular wedge of reciprocal space: a scanning nanobeam diffraction tomogram. Using this diffraction tomogram, intensities can be digitally extracted from any desired region of a scan in real or diffraction space, exclusive of all other scanned points. Intensities from multiple regions of a crystal or from multiple crystals can be merged to increase data completeness and mitigate missing wedges. It is demonstrated that merged intensities from digitally defined regions of two crystals of a segment from the OsPYL/RCAR5 protein produce fragment-based ab initio solutions that can be refined to atomic resolution, analogous to structures determined by selected-area electron diffraction. In allowing atomic structures to now be determined from digitally outlined regions of a nanocrystal, scanning nanobeam diffraction tomography breaks new ground in nanocrystallography.


2019 ◽  
Author(s):  
Marcus Gallagher-Jones ◽  
Karen C. Bustillo ◽  
Colin Ophus ◽  
Logan S. Richards ◽  
Jim Ciston ◽  
...  

AbstractNanocrystallography has transformed our ability to interrogate the atomic structures of proteins, peptides, organic molecules and materials. By probing atomic level details in ordered sub-10 nm regions of nanocrystals, approaches in scanning nanobeam electron diffraction extend the reach of nanocrystallography and mitigate the need for diffraction from large portions of one or more crystals. We now apply scanning nanobeam electron diffraction to determine atomic structures from digitally defined regions of beam-sensitive peptide nanocrystals. Using a direct electron detector, we record thousands of sparse diffraction patterns over multiple crystal orientations. We assign each pattern to a specific location on a single nanocrystal with axial, lateral and angular coordinates. This approach yields a collection of patterns that represent a tilt series across an angular wedge of reciprocal space: a scanning nanobeam diffraction tomogram. From this diffraction tomogram, we can digitally extract intensities from any desired region of a scan in real or diffraction space, exclusive of all other scanned points. Intensities from multiple regions of a crystal or from multiple crystals can be merged to increase data completeness and mitigate missing wedges. Merged intensities from digitally defined regions of two crystals of a segment from the OsPYL/RCAR5 protein produce fragment-based ab-initio solutions that can be refined to atomic resolution, analogous to structures determined by selected area electron diffraction. In allowing atomic structures to now be determined from digitally outlined regions of a nanocrystal, scanning nanobeam diffraction tomography breaks new ground in nanocrystallography.


Author(s):  
R. Herrera ◽  
A. Gómez

Computer simulations of electron diffraction patterns and images are an essential step in the process of structure and/or defect elucidation. So far most programs are designed to deal specifically with crystals, requiring frequently the space group as imput parameter. In such programs the deviations from perfect periodicity are dealt with by means of “periodic continuation”.However, for many applications involving amorphous materials, quasiperiodic materials or simply crystals with defects (including finite shape effects) it is convenient to have an algorithm capable of handling non-periodicity. Our program “HeGo” is an implementation of the well known multislice equations in which no periodicity assumption is made whatsoever. The salient features of our implementation are: 1) We made Gaussian fits to the atomic scattering factors for electrons covering the whole periodic table and the ranges [0-2]Å−1 and [2-6]Å−1.


Minerals ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 206 ◽  
Author(s):  
James Hower ◽  
Dali Qian ◽  
Nicolas Briot ◽  
Eduardo Santillan-Jimenez ◽  
Madison Hood ◽  
...  

Fly ash from the combustion of eastern Kentucky Fire Clay coal in a southeastern United States pulverized-coal power plant was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). TEM combined with elemental analysis via energy dispersive X-ray spectroscopy (EDS) showed that rare earth elements (REE; specifically, La, Ce, Nd, Pr, and Sm) were distributed within glassy particles. In certain cases, the REE were accompanied by phosphorous, suggesting a monazite or similar mineral form. However, the electron diffraction patterns of apparent phosphate minerals were not definitive, and P-lean regions of the glass consisted of amorphous phases. Therefore, the distribution of the REE in the fly ash seemed to be in the form of TEM-visible nano-scale crystalline minerals, with additional distributions corresponding to overlapping ultra-fine minerals and even true atomic dispersion within the fly ash glass.


The selected area electron diffraction patterns from a crystal containing a stacking fault have been observed to exhibit a number of unusual features. In some cases a periodic intensity distribution about the Bragg spot, in other cases streaking. By applying Kirchhoff’s theory of diffraction and using the dynamical theory of electron diffraction this intensity distribution around the Bragg spots in the electron diffraction patterns from stacking faults has been calculated. The calculated intensity distributions compare favourably with experiment. A similar calculation has also been carried out to predict the intensity distribution around Bragg spots in the selected area electron diffraction patterns from a crystal containing a grain boundary.


2010 ◽  
Vol 18 (4) ◽  
pp. 22-28
Author(s):  
William F. Tivol

One of the capabilities of electron microscopes is to obtain diffraction patterns, which can be analyzed to give information about the structure of the specimen. This brief review discusses some of the technical considerations in using electron diffraction patterns for structural analysis. The technique of selected-area electron diffraction uses diffraction obtained from a limited region of the specimen.


Author(s):  
N. Güven ◽  
R.W. Pease

Selected area electron diffraction (SAD) patterns of beidellite exhibit fine structure in the form of nonradial streaks and extra spots between the normal Laue spots. The streaks form a regular network as shown in Figure 1A andvery clearly after a long exposure, in Fig. IB. These streaks do not pass through the origin and they are not symmetrical with respect to the reciprocal lattice points. Therefore they cannot be caused by finite crystallite size. The distribution of the streaks suggests a strong anisotropy in the beidellite structure as they are restricted to the directions parallel to [11], [11], and [02]. However, there are no streaks along the actual [11], [11] and [02] directions. In general terms, these linear streaks are explained by the presence of ‘continuous sheets’ or ‘walls’ of intensity in reciprocal space. These intensity 'walls' are associated with a linear chain of scatterers in the crystal in the direction perpendicular to the intensity sheets. Such linear scatterers may be produced by small shifts of certain atoms due to thermal motion, isomorphic substitutions, distortions, or other lattice imperfections.


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