Search results for "Diffraction tomography"
showing 10 items of 32 documents
Using FOCUS to solve zeolite structures from three-dimensional electron diffraction data
2013
The programFOCUS[Grosse-Kunstleve, McCusker & Baerlocher (1997).J. Appl. Cryst.30, 985–995] was originally developed to solve zeolite structures from X-ray powder diffraction data. It uses zeolite-specific chemical information (three-dimensional 4-connected framework structure with known bond distances and angles) to supplement the diffraction data. In this way, it is possible to compensate, at least in part, for the ambiguity of the reflection intensities resulting from reflection overlap, and the program has proven to be quite successful. Recently, advances in electron microscopy have led to the development of automated diffraction tomography (ADT) and rotation electron diffraction (R…
Expanding the Variety of Zirconium‐based Inorganic Building Units for Metal–Organic Frameworks
2019
Two new zirconium-based metal-organic frameworks with the composition [Zr6 O4 (OH)4 (OAc)6 (BDC)3 ] (CAU-26) and [Zr5 O4 (OH)4 (OAc)4 (BDC)2 ] (CAU-27) are reported, which were synthesized from acetic acid, a rarely utilized but green and sustainable solvent (BDC2- : 1,4-benzenedicarboxylate). Structure determination aided by automated electron diffraction tomography revealed that CAU-26 is composed of layers of well-known {Zr6 O8 } clusters interconnected by terephthalate ions. In contrast CAU-27 exhibits a three-dimensional structure with a so far unknown type of one-dimensional inorganic building unit (IBU), which can be rationalized as condensed polyhedron-sharing chains of {Zr6 O8 } cl…
Ba 6 P 12 N 17 O 9 Br 3 – A Column‐Type Phosphate Structure Solved from Single‐Nanocrystal Data Obtained by Automated Electron Diffraction Tomography
2011
Oxonitridophosphate Ba6P12N17O9Br3 was synthesized by heating a multicomponent mixture of BaBr2, BaS, phosphoryl triamide and thiophosphoryl triamide in an evacuated and sealed silica-glass ampoule to 750 °C. Ba6P12N17O9Br3 was obtained as the main product as a nanocrystalline powder. The crystal structure was determined ab initio on the basis of electron diffraction data acquired from a single needle-shaped nanocrystal by automated diffraction tomography. Ba6P12N17O9Br3 crystallizes in the hexagonal space group P63/m (no. 176) with unit cell parameters a = 14.654(19), c = 8.255(9) A and Z = 2. Its structure includes triangular, column-shaped anions of ∞1{(P12N17O9)9–}, which are built from…
A multi-technique characterisation of cronstedtite synthetized by iron-clay interaction in a step by step cooling procedure
2013
International audience; The cooling of steel containers in radioactive-waste storage was simulated in a step-by-step experiment from 90 to 40 degrees C. Among newly formed clay minerals observed in run products, cronstedtite was identified by a number of analytical techniques (powder X-ray diffraction, transmission electron microscopy, and scanning electron microscopy). Cronstedtite has not previously been recognized to be so abundant and so well crystallized in an iron-clay interaction experiment. The supersaturation of experimental solutions with respect to cronstedtite was due to the availability of Fe and Si in solution, as a result of the dissolution of iron metal powder, quartz, and m…
Partially Coherent Optical Diffraction Tomography Toward Practical Cell Study
2021
Optical diffraction tomography (ODT) is a computational imaging technique based on refractive index (RI) contrast. Its application for microscopic imaging of weakly absorbing and scattering samples has been demonstrated by using a specially designed holographic microscope with angular scanning of the coherent sample illumination direction. Recently, an alternative low cost technique based on partially coherent sample illumination (PC-ODT), which is compatible with the conventional wide-field transmission microscope, has been established. In this case, the 3D refractive index distribution of the sample is obtained by deconvolution from a single stack of through-focus intensity images. The pe…
Structural Characterization of Organics Using Manual and Automated Electron Diffraction
2010
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.
Structure characterization of hard materials by precession electron diffraction and automatic diffraction tomography: 6H-SiC semiconductor and Ni1+xT…
2012
Using a combination of automated diffraction tomography and precession electron diffraction techniques, quasi-kinematical electron diffraction data sets were collected from intermetallic Ni1+xTe1 embedded nanodomains and ion-thinned specimens of 6H–SiC semiconductor. Cell parameters and space groups were found automatically from the reconstructed 3D diffraction volume. The extracted intensities were used for fast ab initio structure determination by direct methods.
Ab initio structure determination and quantitative disorder analysis on nanoparticles by electron diffraction tomography.
2017
Nanoscaled porous materials such as zeolites have attracted substantial attention in industry due to their catalytic activity, and their performance in sorption and separation processes. In order to understand the properties of such materials, current research focuses increasingly on the determination of structural features beyond the averaged crystal structure. Small particle sizes, various types of disorder and intergrown structures render the description of structures at atomic level by standard crystallographic methods difficult. This paper reports the characterization of a strongly disordered zeolite structure, using a combination of electron exit-wave reconstruction, automated diffrac…
Highly stable and porous porphyrin-based zirconium and hafnium phosphonates – electron crystallography as an important tool for structure elucidation
2018
The Ni-metallated porphyrin-based tetraphosphonic acid (Ni-tetra(4-phosphonophenyl)porphyrin, Ni-H8TPPP) was used for the synthesis of highly porous metal phosphonates containing the tetravalent cations Zr4+ and Hf4+. The compounds were thoroughly characterized regarding their sorption properties towards N2 and H2O as well as thermal and chemical stability. During the synthesis optimization the reaction time could be substantially decreased under stirring from 24 to 3 h in glass vials. M-CAU-30, [M2(Ni-H2TPPP)(OH/F)2]·H2O (M = Zr, Hf) shows exceptionally high specific surface areas for metal phosphonates of aBET = 1070 and 1030 m2 g-1 for Zr- and Hf-CAU-30, respectively, which are very clos…
A new hydrous Al-bearing pyroxene as a water carrier in subduction zones
2011
Abstract A new Hydrous Al-bearing PYroxene (HAPY) phase has been synthesized at 5.4 GPa, 720 °C in the MgO–Al2O3–SiO2–H2O model system. It has the composition Mg2.1Al0.9(OH)2Al0.9Si1.1O6, a C-centered monoclinic cell with a = 9.8827(2), b = 11.6254(2) c = 5.0828(1) A and β = 111.07(1)°. The calculated density is 3.175 g/cm3 and the water content is 6.9% H2O by weight. Its structure has been solved in space group C2/c by the recently developed automated electron diffraction tomography method and refined by synchrotron X-ray powder diffraction. HAPY is a single chain inosilicate very similar to pyroxenes but with three instead of two cations in the octahedral layer, bonded to four oxygens and…