Search results for "Powder diffraction"
showing 10 items of 243 documents
ChemInform Abstract: X-Ray Powder Structure Determination and Thermal Behavior of a New Modification of Pb(II) Selenite.
2010
The crystal structure of a new polymorphic form of lead(II) selenite (PbSeO3) was solved directly from conventional X-ray powder diffraction data. Direct methods and Rietveld refinement techniques were used for the structure determination. The compound crystallizes in the monoclinic space group P21/c (no. 14) with cell dimensions a = 9.1587(1) A, b = 8.0902(1) A, c = 8.7932(1) A, β = 103.032(1)°, and V = 634.76(2) A3. The final refinement gave background excluded Rp = 6.22%, Rwp = 8.81%, and RB = 2.16% by using 45 structural and 15 profile parameters with 10 atoms in an asymmetric unit. The three-dimensional structure consists of 9-coordinated lead atoms, which are linked by three bidentate…
Dehydration of detomidine hydrochloride monohydrate
2010
The thermodynamic stability of detomidine hydrochloride monohydrate has been evaluated on the basis of phase transition kinetics in solid state. A method free of empirical models was used for the treatment of kinetic data, and compared to several known solid state kinetic data processing methods. Phase transitions were monitored by powder X-ray diffraction (PXRD) and thermal analysis. Full PXRD profiles were used for determining the phase content instead of single reflex intensity measurements, in order to minimize the influence of particle texture. We compared the applicability of isothermal and nonisothermal methods to our investigation of detomidine hydrochlorine monohydrate dehydration.
Quasi-hydrostatic X-ray powder diffraction study of the low- and high-pressure phases of CaWO4 up to 28 GPa
2014
We have studied CaWO4 under compression using Ne as pressure-transmitting medium at room temperature by means of synchrotron X-ray powder diffraction. We have found that CaWO4 beyond 8.8 GPa transforms from its low-pressure tetragonal structure (scheelite) into a monoclinic structure (fergusonite). The high-pressure phase remains stable up to 28 GPa and the low-pressure phase is totally recovered after full decompression. The pressure dependence of the unit-cell parameters, as well as the pressure volume equation of state, has been determined for both phases. Compared with previous studies, we found in our quasi-hydrostatic experiments a different behavior for the unit-cell parameters of th…
Complex high-pressure polymorphism of barium tungstate
2012
We have studied BaWO 4 under compression at room temperature by means of x-ray diffraction and Raman spectroscopy. When compressed with neon as a pressure-transmitting medium (quasihydrostatic conditions), we found that BaWO 4 transforms from its low-pressure tetragonal structure into a much denser monoclinic structure. This result confirms our previous theoretical prediction based on ab initio calculations that the scheelite to BaWO 4-II transition occurs at room temperature if kinetic barriers are suppressed by pressure. However, our experiment without any pressure- transmitting medium has resulted in a phase transition to a completely different structure, suggesting nonhydrostaticity may…
Structural and vibrational study of cubic Sb2O3under high pressure
2012
We report an experimental and theoretical study of antimony oxide (Sb${}_{2}$O${}_{3}$) in its cubic phase (senarmontite) under high pressure. X-ray diffraction and Raman scattering measurements up to 18 and 25 GPa, respectively, have been complemented with ab initio total-energy and lattice-dynamics calculations. X-ray diffraction measurements do not provide evidence of a space-group symmetry change in senarmontite up to 18 GPa. However, Raman scattering measurements evidence changes in the pressure coefficients of the Raman mode frequencies at 3.5 and 10 GPa, respectively. The behavior of the Raman modes with increasing pressure up to 25 GPa is fully reproduced by the lattice-dynamics cal…
Crystallographic changes and thermal properties of lanthanum?strontium ferromanganites between RT and 700 �C
2005
Abstract X-ray powder diffraction was used to determine the crystallographic changes between room temperature (RT) and 700 °C of the (La 0.8 Sr 0.2 )(Mn 1− y Fe y )O 3± δ perovskites with y =0.2, 0.5, 0.8, 1 which can be considered as possible cathode materials for the ITSOFCs. For y =0.2, the rhombohedral symmetry was preserved in the whole temperature range. For y =1, a transition from orthorhombic to rhombohedral symmetry occurred at 290 °C. The compounds with y =0.5 and 0.8 were found to be diphasic at RT by combination of both rhombohedral and orthorhombic symmetries. They became only rhombohedral at 80 and 160 °C, respectively. This reversible transition is discussed in terms of iron …
Exploring the high-pressure behavior of the three known polymorphs of BiPO4: Discovery of a new polymorph
2015
We have studied the structural behavior of bismuth phosphate under compression. We performed x-ray powder diffraction measurements up to 31.5 GPa and ab initio calculations. Experiments were carried out on different polymorphs: trigonal (phase I) and monoclinic (phases II and III). Phases I and III, at low pressure (P < 0.2-0.8 GPa), transform into phase II, which has a monazite-type structure. At room temperature, this polymorph is stable up to 31.5 GPa. Calculations support these findings and predict the occurrence of an additional transition from the monoclinic monazite-type to a tetragonal scheelite-type structure (phase IV). This transition was experimentally found after the simultaneo…
Synthesis and processing of nanocrystalline tungsten carbide: Towards cemented carbides with optimal mechanical properties
2011
Abstract Nanocrystalline tungsten carbide has been obtained by reduction/carburization at low temperature from precursors obtained by freeze-drying of aqueous solutions. Nanocrystalline WC powders with a adequate content of carbon were mixed with submicrometric Cobalt powder (12 wt.%), obtained by same synthesis method, and sintered in vacuum furnace. The cemented carbides fabricated from experimental powders were compared with both commercial ultrafine and nanocrystalline WC-12Co mixtures consolidated by the same route. The synthesised powders were characterized by X-ray powder diffraction, elemental analysis and scanning and high resolution transmission electron microscopy. On the other h…
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…
The interplay of crystallization kinetics and morphology during the formation of SnO2 nanorods: snapshots of the crystallization from fast microwave …
2011
A microwave-assisted reaction pathway to rutile SnO2nanorods was investigated. The microwave-treatment significantly reduces the reaction time compared to standard hydro-/solvothermal techniques. By moving the overall process into a shorter time slot, the growth and crystal formation during the reaction could be monitored via snapshots by trapping the intermediates through quenching. To gain a better insight into the template-free growth of one-dimensional (1D) nanostructures, a parameter-dependent (various temperatures/pressures and times were investigated) study was carried out. For all materials, the phase purity and crystallite sizes were determined by X-ray powder diffraction (XRD). Th…