0000000001301399
AUTHOR
Andrew Stewart
Automated Diffraction Tomography: A New Era for Electron Crystallography
Extended abstract of a paper presented at Microscopy and Microanalysis 2011 in Nashville, Tennessee, USA, August 7–August 11, 2011.
Solution synthesis of nanoparticular binary transition metal antimonides
The preparation of nanoengineered materials with controlled nanostructures, for example, with an anisotropic phase segregated structure or a regular periodicity rather than with a broad range of interparticle distances, has remained a synthetic challenge for intermetallics. Artificially structured materials, including multilayers, amorphous alloys, quasicrystals, metastable crystalline alloys, or granular metals, are mostly prepared using physical gas phase procedures. We report a novel, powerful solution-mediated approach for the formation of nanoparticular binary antimonides based on presynthesized antimony nanoparticles. The transition metal antimonides M-Sb (M = Co, Ni, Cu(2), Zn) were …
Structure solution with automated electron diffraction tomography data: different instrumental approaches
Summary Over the past few years automated electron diffraction tomography has become an established technique for structure solution of nano-crystalline material. The intentional choice of an arbitrary tilt axis and thus, the use of nonoriented diffraction patterns (off-zone acquisition) together with fine equidistant sampling of the reciprocal space result in high quality intensity data sets. Coupling automated electron diffraction tomography with electron beam precession (Vincent & Midgley, 1994) enables sampling of intensities between the static slices of reciprocal space and therefore enhances the quality of intensity data further; relatively complex structures have been solved using 3D…
ChemInform Abstract: Solution Synthesis of Nanoparticular Binary Transition Metal Antimonides.
The transition metal antimonides MSb with M: Co, Ni, and Zn and Cu2Sb with particle sizes ranging from 20 to 60 nm are prepared using presynthesized antimony nanoparticles and activated metal nanoparticles as precursors.
Structural Characterization of Organics Using Manual and Automated Electron Diffraction
In the last decade the importance of transmission electron microscopic studies has become increasingly important with respect to the characterization of organic materials, ranging from small organic molecules to polymers and biological macromolecules. This review will focus on the use of transmission electron microscope to perform electron crystallography experiments, detailing the approaches in acquiring electron crystallographic data. The traditional selected area approach and the recently developed method of automated diffraction tomography (ADT) will be discussed with special attention paid to the handling of electron beam sensitive organic materials.
Structural and electronic properties ofβ-FeSi2nanoparticles: The role of stacking fault domains
We use conventional and aberration-corrected transmission electron microscopy (TEM) and ab initio calculations to investigate the structural and electronic properties of \ensuremath{\beta}-FeSi${}_{2}$ nanoparticles, which are a promising material for photovoltaic applications due to a band gap of 1 eV and a high absorption coefficient. The nanoparticles have average sizes of \ensuremath{\sim}20 nm, form aggregates, and are prepared by gas-phase synthesis. Amorphous SiO${}_{x}$ shells with thicknesses of \ensuremath{\sim}1.7 nm around \ensuremath{\beta}-FeSi${}_{2}$ cores are identified on individual nanoparticles using electron energy-loss spectroscopy, while stacking fault domains in the …
“Ab-initio” structure solution of nano-crystalline minerals and synthetic materials by automated electron tomography
Most of the newly discovered mineral phases, as well as many new synthesized industrial materials, appear only in the form of nano crystals, with a size not sufficient for single-crystal x-ray structure analysis. The development of techniques able to investigate the structure of nano crystalline materials is therefore one of the most important frontiers of crystallography. The most widespread technique providing relatively fast and well consolidated routes for structure analysis of bulk materials is x-ray powder diffraction (XRPD). Nevertheless, XRPD suffers from intrinsic 1-dimension reduction of information that greatly limits its applicability in presence of peak broadening and overlappi…
Application of clustering techniques to electron-diffraction data: determination of unit-cell parameters.
A new approach to determining the unit-cell vectors from single-crystal diffraction data based on clustering analysis is proposed. The method uses the density-based clustering algorithm DBSCAN. Unit-cell determination through the clustering procedure is particularly useful for limited tilt sequences and noisy data, and therefore is optimal for single-crystal electron-diffraction automated diffraction tomography (ADT) data. The unit-cell determination of various materials from ADT data as well as single-crystal X-ray data is demonstrated.
Nanorings and rods interconnected by self-assembly mimicking an artificial network of neurons
[EN] Molecular electronics based on structures ordered as neural networks emerges as the next evolutionary milestone in the construction of nanodevices with unprecedented applications. However, the straightforward formation of geometrically defined and interconnected nanostructures is crucial for the production of electronic circuitry nanoequivalents. Here we report on the molecularly fine-tuned self-assembly of tetrakis-Schiff base compounds into nanosized rings interconnected by unusually large nanorods providing a set of connections that mimic a biological network of neurons. The networks are produced through self-assembly resulting from the molecular conformation and noncovalent intermo…
CCDC 936468: Experimental Crystal Structure Determination
Related Article: Martha V. Escárcega-Bobadilla, Gustavo A. Zelada-Guillén, Sergey V. Pyrlin, Marcin Wegrzyn, Marta M.D. Ramos, Enrique Giménez, Andrew Stewart, Gerhard Maier, Arjan W. Kleij|2013|Nat.Commun.|4|2648|doi:10.1038/ncomms3648
CCDC 936469: Experimental Crystal Structure Determination
Related Article: Martha V. Escárcega-Bobadilla, Gustavo A. Zelada-Guillén, Sergey V. Pyrlin, Marcin Wegrzyn, Marta M.D. Ramos, Enrique Giménez, Andrew Stewart, Gerhard Maier, Arjan W. Kleij|2013|Nat.Commun.|4|2648|doi:10.1038/ncomms3648
CCDC 936467: Experimental Crystal Structure Determination
Related Article: Martha V. Escárcega-Bobadilla, Gustavo A. Zelada-Guillén, Sergey V. Pyrlin, Marcin Wegrzyn, Marta M.D. Ramos, Enrique Giménez, Andrew Stewart, Gerhard Maier, Arjan W. Kleij|2013|Nat.Commun.|4|2648|doi:10.1038/ncomms3648