Search results for "Powder diffraction"
showing 10 items of 243 documents
X-ray powder diffraction study of monoclinic V4+-ZrO2 solid solutions obtained from gels
2003
Abstract Rietveld refinement of six monoclinic V x Zr 1− x O 2 solid solutions, with x =0, 0.01, 0.02, 0.05, 0.075 and 0.1, prepared by heating dried gel precursors at 1300°C in air atmosphere, has been characterized using X-ray powder diffractometer data. The present results confirm that crystal structure of these solid solutions contain V 4+ (Zr 4+ ) cations surrounded by seven oxygens, four at a distance between 2.13 and 2.28 A (referred as to O(2) in the tetrahedrally coordinated oxygens) and other three at a distance between 2.03 and 2.20 A (denoted as O(1) in the triangularly coordinated oxygens). The trends in the lattice parameter variation of V x Zr 1− x O 2 solid solutions specime…
Structure determination of three polymorphs of xylazine from laboratory powder diffraction data
2014
The crystal structures of three xylazine hydrochloride [N-(2,6-dimethylphenyl)-5,6-dihydro-4H-1,3-thiaz-2-amine hydrochloride] polymorphsA,ZandXhave been solved from powder diffraction data and refined using Rietveld refinement. Data were obtained with Cu Kα radiation. All polymorphs were found to have structures withZ′ = 1 andZ= 4. All the structures determined contained strong hydrogen bonds between the amino groups and chloride anions. The crystal structures of formsAandXfeatured π–π stacking interactions.
Cerium effect on the phase structure, phase stability and redox properties of Ce-doped strontium ferrates
2006
Nanostructured perovskite-type Sr1−aCeaFeO3−x, (0⩽a<0.15) powders have been prepared by citrate–nitrate smoldering auto-combustion. Their phase structure and stability, surface and morphological properties, reduction behavior and interaction with oxygen have been investigated by X-ray Powder Diffraction combined with Rietveld Analysis, 57Fe Mossbauer and X-ray Photoelectron Spectroscopies, N2-adsorption method, Temperature Programmed Reduction and Oxidation experiments. Our results reveal that citrate–nitrate auto-combustion method is effective in obtaining single phase Sr1−aCeaFeO3−x. The Sr1−aCeaFeO3−x structure is cubic only for a⩾0.06, while for a<0.06 remains tetragonal. Moreover, for …
Synchrotron powder-diffraction study of the spin transition compound [Fe(bpp)2](NCS)2·2H2O and soft X-ray-induced structural phase conversion
2008
Abstract We have studied the high spin and low spin structural phases of the two-step spin transition compound [Fe(bpp) 2 ](NCS) 2 ·2H 2 O (bpp: 2,6-bis(pyrazol-3-yl)pyridine) of different sample history with X-ray synchrotron ( λ ∼ 0.32 A) powder diffraction at different temperatures as well as with usual X-ray ( λ ∼ 1.54 A) powder diffraction at room temperature by performing rapid repeated scans at regular intervals of time. A structural phase transition occurs only during the first step of the spin transition. Time dependent interconversions of the two crystallographic phases have been observed at room temperature for this material. The results indicate that a soft X-ray (Cu-K α )-ind…
XRMA analysis and X-ray diffraction analysis of dental enamel from human permanent teeth exposed to hydrogen peroxide of varying pH
2019
Background This in vitroinvestigation shows how 3.3% H2O2, at different pH-values affects the enamel. Material and Methods A number of fifteen human premolars were used. The enamel of the coronal half in six of the teeth, were exposed by H2O2. Nine teeth were prepared to enamel powder. The enamel was exposed to 3.3% H2O2, at six different pH-values (pH range 4.5 - 7.0). Analyses of the topography of enamel performed by scanning electron microscope (SEM) and the chemical composition of enamel by X-ray microanalysis (XRMA). X-ray powder diffraction (XRD) analysed the crystallinity in enamel powder. Results The exposure to H2O2 at pH5.5 resulted in a decrease of O in the exposed enamel, and ch…
The conversion from cellulose I to cellulose II in NaOH mercerization performed in alcohol–water systems: An X-ray powder diffraction study
2007
Abstract The slurry-mercerization (SM) processes in 2-propanol–water and 2-propanol–ethanol–water and wet-mass-mercerization (WMM) process in ethanol–water solvents are investigated. Based on X-ray diffraction measurements in the earlier reports, we have derived a mathematical method to evaluate more exactly the conversion of cellulose I (CI) to cellulose II (CII) and used it to survey the effects of different alkali treatments on cellulose crystals. This method is very useful when the crystal system changes in a certain set of experiments are compared with each other. The optimal alcohol concentration in SM processes was found to be 80–92 w/w-% in 2-propanol–water solution, 85–90 w/w-% in …
Crystal structure determination of a new LaPO4 phase in a multicomponent glass ceramic via 3D electron diffraction
2022
Abstract A glass ceramic from the MgO–Al2O3–SiO2 system containing additives of ZrO2, TiO2, La2O3 and P2O5 was investigated. Via x-ray powder diffraction (XRPD) and Transmission electron microscopy(TEM) the crystalline phases present could be identified as MgAl2O4 (Spinel), orthorhombic ZrTiO4 and a polymorph of LaPO4 with a previously unknown crystal structure. The crystal structure of this LaPO4 phase was solved ab initio via 3D ED Data. The polymorph occurs in a distorted barite structure type in the same space group (P21/n) as the stable monazite type polymorph, however the density is higher and the La has a higher coordination number. Furthermore the LaPO4 is present in a spinodal reli…
Interface charge density matching as driving force for new mesostructured oxovanadium phosphates with hexagonal structure, [CTA]xVOPO4·zH2O
1999
Hexagonal mesostructured mixed-valence oxovanadium phosphates [CTA]xVOPO4·zH2O, in short ICMUV-2, have been synthesized through a S+I- cooperative mechanism using cationic surfactant (cetyltrimethylammonium, CTAB) rodlike micelles as a template. On the lines of the hypothesis that the driving force leading to the formation of mesostructured solids is the charge density matching at the interface between the supramolecular−organic and supramolecular−inorganic moieties, the self-assembling process between CTA+ micelles and VOPO4q- planar anions can be thought of as consequence of the adequate adjustment of the metal mean oxidation state. X-ray powder diffraction and TEM techniques show that th…
Impact of the use of sterically congested Ir(III) complexes on the performance of light-emitting electrochemical cells
2018
International audience; The synthesis, structural and optoelectronic characterization of a family of sterically congested cyclometalated cationic Ir(iii) complexes of the form [Ir(C^N)2(dtBubpy)]PF6 (with dtBubpy = 4,4′-di-tert-butyl-2,2′-bipyridine and C^N = a cyclometalating ligand decorated at the 4-position of the pyridine ring and/or the 3-position of the phenyl ring with a range of sterically bulky substituents) are reported. This family of complexes is compared to the unsubstituted analogue complex R1 bearing 2-phenylpyridinato as cyclometalating ligand. The impact of sterically bulky substituents on the C^N ligands on both the solid state photophysics and light-emitting electrochemi…
An X-ray powder diffraction study of lanthanum–strontium ferromanganites
2001
Abstract Various lanthanum–strontium ferromanganites (La 1− x Sr x )(Mn 1− y Fe y )O 3± δ (LSMF) with x =0.2, 0.5 and 0.7 and y =0.2, 0.5 and 0.8 were prepared by a glycine–nitrate combustion route and conditioned into two different oxygenation states which are likely to be encountered in cathode materials for solid oxide fuel cells (SOFC). Crystal symmetries for both the low and the fully oxygenated states were determined by X-ray diffractometry. Most perovskite compositions crystallized in either cubic or rhombohedral symmetry with the exception of La 0.5 Sr 0.5 Mn 0.2 Fe 0.8 O 3± δ , where a transition from rhombohedral to cubic occurred in going from the full to the low oxygenation stat…