Search results for "precession electron diffraction"
showing 10 items of 14 documents
"Ab initio" structure solution from electron diffraction data obtained by a combination of automated diffraction tomography and precession technique
2009
Using a combination of our recently developed automated diffraction tomography (ADT) module with precession electron technique (PED), quasi-kinematical 3D diffraction data sets of an inorganic salt (BaSO(4)) were collected. The lattice cell parameters and their orientation within the data sets were found automatically. The extracted intensities were used for "ab initio" structure analysis by direct methods. The data set covered almost the complete set of possible symmetrically equivalent reflections for an orthorhombic structure. The structure solution in one step delivered all heavy (Ba, S) as well as light atoms (O). Results of the structure solution using direct methods, charge flipping …
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…
Structure of the new mineral sarrabusite, Pb5CuCl4(SeO3)4, solved by manual electron-diffraction tomography.
2012
The new mineral sarrabusite Pb5CuCl4(SeO3)4 has been discovered in the Sardinian mine of Baccu Locci, near Villaputzu. It occurs as small lemon–yellow spherical aggregates of tabular crystals (< 10 µm) of less than 100 µm in diameter. The crystal structure has been solved from and refined against electron diffraction of a microcrystal. Data sets have been measured by both a manual and an automated version of the new electron-diffraction tomography technique combined with the precession of the electron beam. The sarrabusite structure is monoclinic and consists of (010) layers of straight chains formed by alternating edge-sharing CuO4Cl2 and PbO8 polyhedra parallel to the c axis, which sha…
Structural insights into M2O-Al2O3-WO3 (M = Na, K) system by electron diffraction tomography.
2015
TheM2O–Al2O3–WO3(M= alkaline metals) system has attracted the attention of the scientific community because some of its members showed potential applications as single crystalline media for tunable solid-state lasers. These materials behave as promising laser host materials due to their high and continuous transparency in the wide range of the near-IR region. A systematic investigation of these phases is nonetheless hampered because it is impossible to produce large crystals and only in a few cases a pure synthetic product can be achieved. Despite substantial advances in X-ray powder diffraction methods, structure investigation on nanoscale is still challenging, especially when the sample i…
Atomic structure solution of the complex quasicrystal approximant Al77Rh15Ru8 from electron diffraction data
2014
The crystal structure of the novel Al77Rh15Ru8phase (which is an approximant of decagonal quasicrystals) was determined using modern direct methods (MDM) applied to automated electron diffraction tomography (ADT) data. The Al77Rh15Ru8E-phase is orthorhombic [Pbma,a= 23.40 (5),b= 16.20 (4) andc= 20.00 (5) Å] and has one of the most complicated intermetallic structures solved solely by electron diffraction methods. Its structural model consists of 78 unique atomic positions in the unit cell (19 Rh/Ru and 59 Al). Precession electron diffraction (PED) patterns and high-resolution electron microscopy (HRTEM) images were used for the validation of the proposed atomic model. The structure of the E…
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.
Charoite, as an example of a structure with natural nanotubes
2012
Charoite from the Murun massif in Yakutiya, Russia (Vorob’ev 2008) was investigated using automated electron diffraction tomography (ADT) (Kolb et al. 2007, 2008; Mugnaioli et al. 2010) and precession electron diffraction (PED) (Mugnaioli et al. 2010, 2009), which allowed to determine the structure of charoite for the first time. The structure was solved ab initio in space group P21/m by direct methods using a fully kinematic approach. The least squares refinements with 2878 reflections F(hkl) >4s F converged to unweighted/weighted residuals R 1/wR 2 • 0.173/0.21 (Rozhdestvenskaya et al. 2010).
Electron Diffraction Reinvestigation of CdCr<sub>2</sub>Se<sub>4</sub> and ZnCr<sub>2-x</sub>V<sub>x</su…
2013
Crystal structure of two spinel single crystals CdCr2Se4 and ZnCr2-xVxSe4 have been reinvestigated using automated electron diffraction tomography method with beam precession. 3D reciprocal space have been reconstructed base on recorded tilt series. For both samples crystal structure was refined and the cubic symmetry with space group Fd-3m was confirmed. No additional electron potential has been located beside occupied atom sites.
A multi-technique, micrometer- to atomic-scale description of a synthetic analogue of chukanovite, Fe-2(CO3)(OH)(2)
2014
International audience; A synthetic analogue of chukanovite Fe-2(CO3)(OH)(2) is formed during experimental work on iron-clay interactions simulating the cooling of containers in radioactive waste repositories. Despite its small size and the mixture with other minerals it is undoubtedly identified by X-Ray Diffraction, Fourier Transform Infrared Spectroscopy, Scanning Electron Microscopy and Transmission Electron Microscopy. For the first time, the structural characterisation of a synthetic chukanovite is carried out thanks to the combination of Automated Diffraction Tomography and Precession Electron Diffraction. Refinement results and comparison with literature data show that the structure…
Towards automated diffraction tomography: Part I—Data acquisition
2007
Abstract The ultimate aim of electron diffraction data collection for structure analysis is to sample the reciprocal space as accurately as possible to obtain a high-quality data set for crystal structure determination. Besides a more precise lattice parameter determination, fine sampling is expected to deliver superior data on reflection intensities, which is crucial for subsequent structure analysis. Traditionally, three-dimensional (3D) diffraction data are collected by manually tilting a crystal around a selected crystallographic axis and recording a set of diffraction patterns (a tilt series) at various crystallographic zones. In a second step, diffraction data from these zones are com…