Search results for "Powder diffraction"
showing 10 items of 243 documents
High-pressure/high-temperature phase diagram of zinc
2018
The phase diagram of zinc (Zn) has been explored up to 140 GPa and 6000K, by combining optical observations, x-ray diffraction, and ab initio calculations. In the pressure range covered by this study, Zn is found to retain a hexagonal close-packed (hcp) crystal symmetry up to the melting temperature. The known decrease of the axial ratio (c/a) of the hcp phase of Zn under compression is observed in x-ray diffraction experiments from 300K up to the melting temperature. The pressure at which c/a reaches root 3 (approximate to 10GPa) is slightly affected by temperature. When this axial ratio is reached, we observed that single crystals of Zn, formed at high temperature, break into multiple pol…
The role of electron diffraction in zeolite structure determination
2006
Because electron diffraction can sample individual microcrystals, it is clear that this single crystal method can facilitate, in at least two ways, structure determination for inorganic materials, such as zeolites, that are preferentially microcrystalline. First, in a qualitative application, three-dimensional tilts of individual small crystals, to map the reciprocal lattice, greatly facilitates unit cell and space group determination when powder diffraction indexing programs fail. If incoherent multiple scattering leads to violation of systematic absences, these absences can be restored by collection of precession diffraction patterns based on the Vincent-Midgley method [1], as demonstrate…
Automated electron diffraction tomography - a new tool for nano crystal structure analysis
2011
Automated electron Diffraction Tomography (ADT) comprises an upcoming method for “ab intio” structure analysis of nano crystals. ADT allows fine sampling of the reciprocal space by sequential collection of electron diffraction patterns while tilting a nano crystal in fixed tilt steps around an arbitrary axis. Electron diffraction is collected in nano diffraction mode (NED) with a semi-parallel beam with a diameter down to 50 nm. For crystal tracking micro-probe STEM imaging is used. Full automation of the acquisition procedure allowed optimisation of the electron dose distribution and therefore analysis of highly beam sensitive samples. Cell parameters, space group and reflection intensitie…
Ab Initio Structure Determination of Vaterite by Automated Electron Diffraction
2012
tion that is fundamental for understanding material properties. Still, a number of compounds have eluded such kinds of analysis because they are nanocrystalline, highly disordered, with strong pseudosymmetries or available only in small amounts in polyphasic or polymorphic systems. These materials are crystallographically intractable with conventional Xray or synchrotron radiation diffraction techniques. Single nanoparticles can be visualized by high-resolution transmission electron microscopy (HR-TEM) up to sub�ngstrom resolution, [2] but obtaining 3D information is still a difficult task, especially for highly beam-sensitive materials and crystal structures with long cell parameters. Elec…
On the existence of a pyrochlore-type phase in the system Bi2O3–TiO2
1995
The existence of a bismuth titanate in the range between Bi 2 Ti 4 O 11 (Bi 2 O 3 . 4 TiO 2 ) and Bi 4 Ti 3 O 12 (2 Bi 2 O 3 . 3 TiO 2 ) has been investigated by X-ray diffraction of samples prepared by solid state reactions. For reaction temperatures above 1100 °C and a starting composition Bi 2 O 3 . 2 TiO 2 there appeared additional lines which could be attributed to a cubic face-centred cell with a = 10.354 A. A multiphase Rietveld analysis based on X-ray powder diffraction data confirmed the structural model of a pyrochlore for this compound. There is evidence that this phase belongs to the group of defect pyrochlores with a Bi 3+ -deficiency resulting in a composition of Bi 1.833 Ti 2…
Isomerism in [MCl2(ERR‘)2] (M = Pd, Pt; E = S, Se; R, R‘ = Me, Ph)
2006
A series of thioether and selenoether complexes [MCl2(EPh2)2] and [MCl2(SMePh)2] (M = Pt, Pd; E = S, Se) have been prepared and characterized to explore the isomerism of the complexes in solution and in the solid state. The NMR spectroscopic information indicates that only one isomer is present in solution in case of the palladium complexes, while two isomers are formed in the case of most platinum complexes. Single-crystal X-ray structures of trans-[PdCl2(SPh2)2] (1t), trans-[PdCl2(SePh2)2] (2t), cis-[PtCl2(SePh2)2] (4c), trans-[PdCl2(SMePh)2] (5t), and trans-[PtCl2(SMePh)2] (7t) are reported and have been used as starting points for the X-ray powder diffraction structure determinations us…
Cation Distribution in a Titanium Ferrite Fe2.75Ti0.25O4Measured byin-SituAnomalous Powder Diffraction Using Rietveld Refinement
1998
Many ferrites contain different cations with various valence states and location in the spinel structure. In compounds such as these, only a combination of different techniques such as Mussbauer spectroscopy, IR analysis, and thermogravimetry allows the distribution of cations to be obtained. For very complicated distributions, the mathematical decomposition of derivative thermogravimetric curves (DTG) leading to quantitative distribution is uncertain. In this paper, we present an alternative technique based on resonant diffraction. The anomalous scattering of each cation in the crystalline material is used to determine its amount and position by Rietveld refinement. Since the energy for su…
Structure solution of zeolites by automated electron diffraction tomography - Impact and treatment of preferential orientation
2014
Abstract In this paper the reliability of structure solution of nano-crystalline porous compounds with preferred orientation based on automated electron diffraction tomography (ADT) is discussed. It will be shown that the limitations of the data acquisition geometry can be overcome by completing the missing diffraction data with additional diffraction information. Apart from different ways of sample preparation, data merging with either additional ADT data sets or intensities derived from X-ray powder diffraction comprise an effective way to improve the accuracy of the structure solution.
Applications of automated diffraction tomography (ADT) on nanocrystalline porous materials
2013
Abstract Many porous materials, both inorganic and hybrid organic–inorganic, can only be synthesized as nanocrystals. X-ray powder diffraction delivers one-dimensional data from the overall sample and is therefore often limited by peak overlap at low or medium resolution and by peak broadening. Thus, structure solution of materials with large unit cells and low symmetry, disorder or pseudosymmetry, or available only in polyphasic systems, turns out to be problematic or even impossible. Electron diffraction allows collecting three-dimensional structure information from nanocrystalline materials, but is traditionally biased by low completeness of the diffraction data, dynamical scattering and…
Structural characterization of carane derivative stereoisomers - Potent local anesthetics
2002
The paper reports on structural investigation and phase analysis of a newly synthesized potent local anesthetic with chiral molecular structure. Absolute structure and absolute configuration on four chiral centres was determined using microcrystalline single-crystal difracti on with anomalous scattering of X-ray radiation azimuthal scan technique. Phase analysis for new compound (K P23SS) and its epimer (K P23 RS) was carried out using classical and synchrotron radiation powder difraction. Enantiopurity of the bulk material was verifed for both isomers by comparison of experimental and simulated high- resolution powder difraction diagrams. The presence of two new polymorphic phases of K P23…