Search results for "Powder diffraction"
showing 10 items of 243 documents
Properties of new low melting point quaternary ammonium salts with bis(trifluoromethanesulfonyl)imide anion
2010
Eight new monocationic quaternary ammonium (QA) salts with the bis(trifluoromethanesulfonyl)imide (TFSI) anion were prepared by metathesis using our previously reported QA halides as precursors. New salts were characterized both in liquid and solid state using 1 H and 13 C NMR techniques, mass spectroscopy and elemental analysis together with X-ray diffraction and thermoanalytical methods. In addition, residual water content, viscosity and conductivity measurements were made for three of the roomtemperature ionic liquids (RTILs). The crystal structures of three compounds were determined by X-ray single crystal diffraction. Powder diffraction was used to study the crystallinity of the solid …
Synthesis, characterization and thermal properties of nine quaternary dialkyldiaralkylammonium chlorides
2006
Abstract Nine R 2 R 2 ′ N + Cl − (R=benzyl, 2-methylbenzyl, 3-methylbenzyl, 4-methylbenzyl, 2-phenylethyl or 3-phenylpropyl; R′=ethyl or methyl) quaternary dialkyldiaralkylammonium chlorides were synthesized by treating dimethylformamide or diethylformamide with non-substituted or substituted arylalkyl (aralkyl) halide in the presence of sodium carbonate. The 1H NMR, 13C NMR spectroscopy, mass spectroscopy and elemental analysis were used to characterize the synthesized products. The crystal structures of six compounds were determined by X-ray single crystal diffraction. Four of the compounds crystallized in monoclinic space groups C2/c and P21/c (or P21/n), one in triclinic space group P−1…
Rietveld Refinement of Tetragonal V4+–ZrO2 Solid Solutions Obtained from Gels by X-ray Powder Diffraction
2002
Abstract The crystal structure of three tetragonal V x Zr 1− x O 2 solid solutions, with x =0.025, 0.05, and 0.075, prepared by heating dried gel precursors at 450°C in air atmosphere, have been determined by Rietveld refinement on the basis of powder X-ray powder diffractometer data. They contain V 4+ cations surrounded by eight oxygens, four at a distance between 2.079 and 2.093 A and another four at longer distances between 2.369 and 2.348 A. The estimation of the crystal average oxygen position from the X-ray lattice parameter of V x Zr 1− x O 2 conform with the relationship proposed by Howard et al. ( J. Am. Ceram. Soc. 81, 241 (1998)).
Quantitative Phase Analysis of Mixtures of Three Components using Rietveld and Rius Standardless Methods. Comparative Results
2000
Eight samples, supplied by the Commission on Powder Diffraction of the International Union of Crystallography, through the Round Robin on quantitative phase analysis, were analized using standardless methods. Samples were mixtures of corundum, zincite and fluorite in different ratios. The Rietveld method, using the DBW 3.2 and FULLPROF software, and the Rius method, using MENGE-PC software, were used. Results obtained agree well with the real composition supplied (a posteriori) by the IUCr.
Towards a revisitation of vesuvianite-group nomenclature: the crystal structure of Ti-rich vesuvianite from Alchuri, Shigar Valley
2016
Vesuvianite containing 5.85 wt% TiO2from an Alpine-cleft-type assemblage outcropped near Alchuri, Shigar Valley, Northern Areas, has been investigated by means of electron microprobe analyses, gas-chromatographic analysis of H2O, X-ray powder diffraction, single-crystal X-ray structure refinement,27Al NMR,57Fe Mössbauer spectroscopy, IR spectroscopy and optical measurements. Tetragonal unit-cell parameters are:a= 15.5326 (2),c= 11.8040 (2) Å, space groupP4/nnc. The structure was refined to finalR1= 0.031,wR2= 0.057 for 11247I> 2σ(I). A general crystal-chemical formula of studied sample can be written as follows (Z= 2):[8–9](Ca17.1Na0.9)[8]Ca1.0[5](Fe2+0.44Fe3+0.34Mg0.22)[6](Al3.59Mg0.41)…
Effect of annealing temperature on persistent luminescence of Y3Al2Ga3O12:Cr3+ co-doped with Ce3+ and Pr3+
2021
Abstract Y3(Al,Ga)5O12 (YAGG) materials doped with Ce3+, Cr3+ and Pr3+ were synthesized by using a modified Pechini method and subsequently annealed in air at selected temperatures between 900 and 1500 °C. According to X-ray powder diffraction (XRPD) and transmission electron microscopy (TEM) analyses, the particles and size distributions become large and broad, respectively, due to sintering and agglomeration at high annealing temperatures. Based on infrared (FTIR) spectra and calculation of multi-phonon de-excitation probabilities, the high energy O–H vibrations are not causing significant multi-phonon de-excitation of the emitting 5d level of Ce3+ if the annealing temperature is above 90…
Luminescent P-Chirogenic Copper Clusters
2013
P-chirogenic clusters of the cubanes [Cu4I4L4] (L = chiral phosphine) were prepared from (+)- and (-)-ephedrine with L = (S)- or (R)-(R)(Ph)(i-Pr)P (with R = CH3 (seven steps) or C17H35 (10 steps)) with e.e. up to 96%. The X-ray structure of [Cu4I4((R)-(CH3)(Ph)(i-Pr)P)4] confirmed the cubane structure with average Cu···Cu and Cu···I distances of 2.954 and 2.696 Å, respectively. The cubane structure of the corresponding [Cu4I4((S)-(CH3)(Ph)(i-Pr)P)4] was established by the comparison of the X-ray powder diffraction patterns, and the opposite optical activity of the (S)- and (R)-ligand-containing clusters was confirmed by circular dichroism spectroscopy. Small-angle X-ray scattering patterns…
X-ray-diffraction study of the crystal structures and orientational glass state ofAr1−x(N2)xsolid solutions
1990
Solid solutions of ${\mathrm{Ar}}_{1\mathrm{\ensuremath{-}}\mathit{x}}$(${\mathrm{N}}_{2}$${)}_{\mathit{x}}$ have been investigated by x-ray powder diffraction in the range 0.5x1.0, 8T60 K, and under hydrostatic pressures up to 2200 bars. The structural hcp-cubic (Pa3) phase transition is identified as a martensitic transformation with a wide transformation hysteresis. For x0.8 and T30 K the solid solutions show the orientational glass state, which is characterized by a superposition of inhomogeneous and homogeneous lattice strains. The inhomogeneous component is described by the random-field model. The homogeneous component corresponds to an orthorhombic distortion of the hcp lattice. Two …
Neutron-diffraction study of end-for-end ordering in commensurate submonolayers of carbon monoxide physisorbed on the graphite basal plane
1997
The head-tail (dipolar) ordering in commensurate submonolayer films of carbon monoxide adsorbed on graphite recently observed in heat-capacity measurements for T < 5.18 K has been investigated by neutron diffraction. It will be shown that the experimental results are consistent with an end-for-end ordered commensurate herringbone structure.
Synthetic Pathways for New Tubular Transition Metal Hydroxo- and Fluoro-Selenites: Crystal Structures ofM12(X)2(SeO3)8(OH)6(M=Co2+,Ni2+;X= OH−)
1996
The dumortierite-family structuresM12X2(SeO3)8(OH)6(M= Co2+and Ni2+;X= OH−and F−) have been synthesized. The crystal structures of the hydroxo-derivatives have been refined from X?ray powder diffraction data in the space groupP63mc(Z= 1) witha= 12.887(3) A andc= 4.981(4) A (M= Co2+,X= OH−or F−) anda= 12.704(5) A andc= 4.925(6) A (M= Ni2+,X= OH−or F−). Application of the Partial Charge Transference Model allows the understanding of the selenite derivatives crystal chemistry.