Search results for " diffraction"
showing 10 items of 896 documents
Caracterización mineralógica de materias primas cerámicas por métodos cuantitativos de difracción de rayos x
2002
[ES] El objetivo de este trabajo es la caracterización de fases minerales presentes en materias primas utilizadas en la industria cerámica. Para ello se utilizan dos métodos cuantitativos basados en la difracción de rayos X, el método de Rietveld y un método sin estándar. Los resultados obtenidos por difracción rayos X de estos materiales policristalinos se comparan con los correspondientes análisis químicos y la composición normativa calculada. La precisión y reproducibilidad de los resultados obtenidos, en concordancia con los del análisis químico, son una de las más importantes ventajas de la difractometría cuantitativa que facilitan su utilización en la industria cerámica en el control …
High-resolution physisorption techniques for the characterization of adsorbents and catalysts
1991
Abstract High-resolution physisorption techniques performed in the continuous volumetric mode have been developed to investigate the surface and pore structure properties of porous solids. Physisorption data on well-defined microporous solids (zeolites and aluminophosphates) provide novel information on the mechanism of micropore filling, the behavior of the adsorbed phase and the pore structure of the adsorbent. The combination of physisorption with high-resolution analytical techniques such as calorimetry and neutron diffraction further expands our knowledge and understanding of physisorption processes. The results are not only important for fundamental research but can be applied in the …
Evidence of noncentrosymmetry of human tooth hydroxyapatite crystals
2014
Herein, we investigate human single hydroxyapatite crystals (enamel and dentine) by convergent-beam electron diffraction (CBED) and automated electron-diffraction tomography (ADT). The CBED pattern shows the absence of the mirror plane perpendicular to the c axis leading to the P63 space group instead of the P63 /m space group considered for larger-scale crystals, this is confirmed by ADT. This experimental evidence is of prime importance for understanding the morphogenesis and the architectural organization of calcified tissues.
Hydroxo Hydrido Complexes of Iron and Cobalt (Sn−Fe−Sn, Sn−Co−Sn): Probing Agostic Sn⋅⋅⋅H−M Interactions in Solution and in the Solid State
2000
Bis(toluene)iron 9 reacts with Lappert's stannylene [Sn[CH(SiMe3)2]2] (4) to form the paramagnetic bis-stannylene complex [[(eta6-toluene)Fe-Sn-[CH(SiMe3)2]2]2] (10). Compound 10 reacts with H2O to form the hydroxo hydrido complex [(eta6-C7H8)(mu-OH)(H)-Fe-[Sn[CH(SiMe3)2]2]2] (12) in high yield; its solid-state structure has been elucidated by X-ray and neutron diffraction analysis. In agreement with the 1H NMR results, 12 contains a hydridic ligand whose exact coordination geometry could be determined by neutron diffraction. The 1H and 119Sn NMR analysis of 12 suggested a multicenter Sn/Sn/H/Fe bonding interaction in solution, based on significantly large values of J(Sn,H,Fe) = 640+/-30 Hz…
Solution synthesis of nanoparticular binary transition metal antimonides
2011
The preparation of nanoengineered materials with controlled nanostructures, for example, with an anisotropic phase segregated structure or a regular periodicity rather than with a broad range of interparticle distances, has remained a synthetic challenge for intermetallics. Artificially structured materials, including multilayers, amorphous alloys, quasicrystals, metastable crystalline alloys, or granular metals, are mostly prepared using physical gas phase procedures. We report a novel, powerful solution-mediated approach for the formation of nanoparticular binary antimonides based on presynthesized antimony nanoparticles. The transition metal antimonides M-Sb (M = Co, Ni, Cu(2), Zn) were …
The Boson Peak of Amyloid Fibrils: Probing the Softness of Protein Aggregates by Inelastic Neutron Scattering
2014
Proteins and polypeptides are characterized by low-frequency vibrations in the terahertz regime responsible for the so-called "boson peak". The shape and position of this peak are related to the mechanical properties of peptide chains. Amyloid fibrils are ordered macromolecular assemblies, spontaneously formed in nature, characterized by unique biological and nanomechanical properties. In this work, we investigate the effects of the amyloid state and its polymorphism on the boson peak. We used inelastic neutron scattering to probe low-frequency vibrations of the glucagon polypeptide in the native state and in two different amyloid morphologies in both dry and hydrated sample states. The dat…
Pressure-induced magnetic switching and linkage isomerism in K0.4Fe4[Cr(CN)6]2.8 x 16 H2O: X-ray absorption and magnetic circular dichroism studies.
2008
The effect of applied pressure on the magnetic properties of the Prussian blue analogue K0.4Fe4[Cr(CN)6]2.8 x 16 H2O (1) has been analyzed by dc and ac magnetic susceptibility measurements. Under ambient conditions, 1 orders ferromagnetically at a critical temperature (T(C)) of 18.5 K. Under application of pressure in the 0-1200 MPa range, the magnetization of the material decreases and its critical temperature shifts to lower temperatures, reaching T(C) = 7.5 K at 1200 MPa. Pressure-dependent Raman and Mossbauer spectroscopy measurements show that this striking behavior is due to the isomerization of some Cr(III)-C[triple bond]N-Fe(II) linkages to the Cr(III)-N[triple bond]C-Fe(II) form. A…
New insights in the formation of silanol defects in silicalite-1 by water intrusion under high pressure.
2010
International audience; The "water-silicalite-1" system is known to act as a molecular spring. The successive intrusion-extrusion cycles of liquid water in small crystallites (6 × 3 × 0.5 μm(3)) of hydrophobic silicalite-1 were studied by volumetric and calorimetric techniques. The experiments displayed a decrease of the intrusion pressure between the first intrusion-extrusion cycle and the consecutive ones, whereas the extrusion pressures remained unchanged. However, neither XRD studies nor SEM observations revealed any structural and morphological modifications of silicalite-1 at the long-range order. Such a shift in the value of the intrusion pressure after the first water intrusion-extr…
High-pressure and high-temperature X-ray diffraction studies of scheelite BaWO4
2009
International audience; We carried out high-pressure (HP) and high-temperature (HT) in situ ADXRD synchrotron measurements in barium tungstate (BaWO4 ) up to 7.5 GPa and 800 K. Coexistence of the scheelite and fergusonite structures was found beyond 7 GPa, both at room temperature and HT, suggesting a polymorphism zone in the P –T phase diagram. The experiments are complemented by thermodynamic calculations within the quasi-harmonic approximation. At ambient pressure, a volume thermal expansivity of 9.5 × 10− 6 K−1 was obtained for scheelite BaWO4 . At HP, the thermal expansivity of the fergusonite doubles that of scheelite. Theoretical equation of state curves at HP and HT are also present…
A structural investigation of titanium dioxide photocatalysts
1991
Abstract A study of the structure and the morphology of a titanium dioxide photocatalyst (Degussa P25) reveals multiphasic material consisting of an amorphous state, together with the crystalline phases anatase and rutile in the approximate proportions 80 20 . Transmission electron microscopy provides evidence that some individual particles are a mixture of the amorphous state with either the anatase phase or with the rutile phase, and that some particles, which are mostly anatase, are covered by a thin overlayer of rutile which manifests its presence by the appearance of Moire fringes. The photocatalytic activity of this form of titanium dioxide is reported as being greater than the activi…