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Neutron Diffraction Experiments (neutron + diffraction_experiment)
Selected AbstractsStructure of Fast Ion Conductors Li3xLa2/3-xTiO3 Deduced from Powder Neutron Diffraction Experiments.CHEMINFORM, Issue 28 2005A. Varez Abstract For Abstract see ChemInform Abstract in Full Text. [source] Growth of large protein crystals by a large-scale hanging-drop methodJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 4 2010Keisuke Kakinouchi A method for growing large protein crystals is described. In this method, a cut pipette tip is used to hang large-scale droplets (maximum volume 200,µl) consisting of protein and precipitating agents. A crystal grows at the vapor,liquid interface; thereafter the grown crystal can be retrieved by droplet,droplet contact both for repeated macroseeding and for mounting crystals in a capillary. Crystallization experiments with peroxiredoxin of Aeropyrum pernix K1 (thioredoxin peroxidase, ApTPx) and hen egg white lysozyme demonstrated that this large-scale hanging-drop method could produce a large-volume crystal very effectively. A neutron diffraction experiment confirmed that an ApTPx crystal (6.2,mm3) obtained by this method diffracted to beyond 3.5,Å resolution. [source] Dependence of small-angle neutron scattering contrast on the difference in thermal expansions of phases in two-phase alloysJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 6 2009Pavel Strunz Theoretical expressions describing small-angle neutron scattering (SANS) contrast dependence on temperature in the region where no phase-composition changes occur were derived for two-phase Ni superalloys. The theory is based on the difference in thermal expansion of the two primary phases, , and ,,. The simulations show that the scattering contrast temperature evolution is significant enough to be considered in in situ SANS experiments with superalloys at elevated temperatures. The simulations performed show that the magnitude of the scattering contrast at room temperature is firmly connected with the particular shape of the scattering contrast temperature dependence. This fact can be used for determination of the scattering contrast without a knowledge of the compositions of the individual phases. The theoretical expressions derived for scattering contrast were proven experimentally on an Ni,Fe-base alloy, DT706. The evolution of lattice parameters of both the matrix and the precipitate phases was obtained from an in situ wide-angle neutron diffraction experiment. The theoretical scattering contrast dependence was then successfully fitted to the measured SANS integral intensity. [source] Disordered misfit [Ca2CoO3][CoO2]1.62 structure revisited via a new intrinsic modulationACTA CRYSTALLOGRAPHICA SECTION B, Issue 2 2008Hervé Muguerra The structure of the thermoelectric lamellar misfit cobalt oxide [Ca2CoO3][CoO2]1.62 was refined again using single-crystal X-ray diffraction data. A new commensurate intrinsic modulation was observed involving a modulation vector orthogonal to the misfit direction (,,0,,,). The five-dimensional superspace group is C2/m(1,0)(,0,)gm and the structure was solved using a commensurate approximation. A new model is given involving an occupation modulation of the split sites of the [CoO] layer. This [CoO] layer can be described by triple chains running along b. The residual disorder along b can then be explained by the assumption of a local ordering with two types of clusters: CoO2 and Co5O4. A powder neutron diffraction experiment confirmed the ordering evidenced by the single-crystal X-ray diffraction study, but was not sufficient by itself to deal with this double modulated scheme. The new intrinsic modulation is destroyed by partial metal substitutions in the [CoO] layer. The structural modifications of this layer directly influence the physical properties which are related to the electronic structure of the [CoO2] layers. [source] Extracting charge density distributions from diffraction data: a model study on ureaACTA CRYSTALLOGRAPHICA SECTION B, Issue 1 2000R. Y. De Vries The quality of the extraction of electron density distributions by means of a multipole refinement method is investigated. Structure factors of the urea crystal have been obtained from an electron density distribution (EDD) resulting from a density function calculation with the CRYSTAL95 package. To account for the thermal motion of the atoms, the stockholder-partioned densities of the atoms have been convoluted with thermal smearing functions, which were obtained from a neutron diffraction experiment. A POP multipole refinement yielded a good fit, R = 0.6%. This disagreement factor is based on magnitudes only. Comparison with the original structure factors gave a disagreement of 0.8% owing to differences in magnitude and phase. The fitted EDD still showed all the characteristics of the interaction density. After random errors corresponding to the experimental situation were added to the structure factors, the refinement was repeated. The fit was R = 1.1%. This time the resulting interaction density was heavily deformed. Repetition with another set of random errors from the same distribution yielded a widely different interaction density distribution. The conclusion is that interaction densities cannot be obtained from X-ray diffraction data on non-centrosymmetric crystals. [source] Solid-State Structures and Properties of Europium and Samarium HydridesEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 18 2010Holger Kohlmann Abstract The structural chemistry of europium and samarium hydrides in the solid state is very rich, ranging from typical ionic hydrides following the hydride-fluoride analogy to complex transition metal hydrides and interstitial hydrides. While crystal structure, electrical, and magnetic properties suggest that europium is divalent in all hydrides investigated so far, samarium is easily transformed to a trivalent oxidation state in its hydrides and shows similarities to other lanthanide(III) hydrides. The problem of neutron absorption of europium and samarium, hampering crystal structure solution and limiting the available structural information, is discussed in detail, and practical solutions for neutron diffraction experiments are given. [source] The ,-to-, Transition in BiFeO3: A Powder Neutron Diffraction StudyADVANCED FUNCTIONAL MATERIALS, Issue 13 2010Donna C. Arnold Abstract High-temperature powder neutron diffraction experiments are conducted around the reported ,,, phase transition (,930,°C) in BiFeO3. The results demonstrate that while a small volume contraction is observed at the transition temperature, consistent with an insulator,metal transition, both the ,- and ,-phase of BiFeO3 exhibit orthorhombic symmetry; i.e., no further increase of symmetry occurs during this transition. The ,-orthorhombic phase is observed to persist up to a temperature of approximately 950,°C before complete decomposition into Bi2Fe4O9 (and liquid Bi2O3), which subsequently begins to decompose at approximately 960,°C. [source] Liquid Rb micrometric droplets confined in paraffin wax: an X-ray absorption spectroscopy studyJOURNAL OF SYNCHROTRON RADIATION, Issue 2 2001Simone De Panfilis We have performed high-quality X-ray absorption measurements on crystalline (c -Rb) and liquid (l -Rb) Rubidium in the range from 15 K to 320 K. Performing a consistent analysis that takes into account the contribution of the medium range structure, we observe that the l -Rb spectrum is compatible with pair correlation function g(r) previously determined by neutron diffraction experiments. Due to the micrometric size of the liquid droplets we were able to observe a slight undercooling down to 290 K. We were also able to study the details of the very strong multielectron excitations channels in terms of resonances, edges and shake-off features at proper theoretical energy values. [source] Magnetic behaviour of synthetic Co2SiO4ACTA CRYSTALLOGRAPHICA SECTION B, Issue 6 2009Andrew Sazonov Synthetic Co2SiO4 crystallizes in the olivine structure (space group ) with two crystallographically non-equivalent Co positions and shows antiferromagnetic ordering below 50,K. We have investigated the temperature variation of the Co2SiO4 magnetic structure by means of non-polarized and polarized neutron diffraction for single crystals. Measurements with non-polarized neutrons were made at 2.5,K (below TN), whereas polarized neutron diffraction experiments were carried out at 70 and 150,K (above TN) in an external magnetic field of 7,T parallel to the b axis. Additional accurate non-polarized powder diffraction studies were performed in a broad temperature range from 5 to 500,K with small temperature increments. Detailed symmetry analysis of the Co2SiO4 magnetic structure shows that it corresponds to the magnetic (Shubnikov) group Pnma, which allows the antiferromagnetic configuration (Gx, Cy, Az) for the 4a site with inversion symmetry (Co1 position) and (0,Cy,0) for the 4c site with mirror symmetry m (Co2 position). The temperature dependence of the Co1 and Co2 magnetic moments obtained from neutron diffraction experiments was fitted in a modified molecular-field model. The polarized neutron study of the magnetization induced by an applied field shows a non-negligible amount of magnetic moment on the oxygen positions, indicating a delocalization of the magnetic moment from Co towards neighbouring O owing to superexchange coupling. The relative strength of the exchange interactions is discussed based on the non-polarized and polarized neutron data. [source] Structure of the defect perovskite Ce1/3NbO3: a redetermination by electron and neutron powder diffractionACTA CRYSTALLOGRAPHICA SECTION B, Issue 2 2000C. Bridges The crystal structure of the defect perovskite Ce1/3NbO3, cerium niobium oxide, has been re-examined by neutron powder and electron diffraction. The results of a powder neutron Rietveld refinement indicate that the structure is monoclinic: space group P2/m with Z = 4, a = 5.5267,(3), b = 7.8824,(2), c = 5.5245,(3),Å, , = 90.294,(1)°, V = 240.67,(2),Å3 at 298,K with ,2 = 2.570. Previous reports have described the Ce1/3NbO3 structure in a smaller (V/2) orthorhombic cell based solely upon X-ray powder diffraction data. The presence of weak reflections in the electron diffraction pattern provides conclusive evidence for a monoclinic superstructure of the orthorhombic cell. While these superlattice reflections are barely detectable with X-ray radiation, they are clearly visible in the neutron diffraction experiments. The superlattice reflections are shown to arise from a tilting of the NbO6 octahedra which results in the reduction of symmetry from orthorhombic to monoclinic. It is also found that the Ce3+ and Nb5+ cations are displaced from the centres of their respective polyhedra to accommodate the bond-valence requirements of the crystal structure. It is likely that distortions of this type are present in other Ln1/3NbO3 and Ln1/3TaO3 defect perovskites. [source] | ||||||||||