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Accurate X-ray quantitative analysis in SiC-based ceramics is a difficult task owing to the strong overlap among the Bragg reflections of the different polytypes. In relation to this point, the Rietveld method can be used as a powerful tool in order to solve this problem. In this study we have applied this procedure to determine the weight fractions of the phases in a liquid– phase-sintered SiC sample. It is shown that the consideration of preferred orientation effects is also indispensable to obtain the accurate proportion of the phases.La determinación de las fracciones en peso de las fases mediante difracción de rayos X es enormemente complicada en cerámicos a base de SiC debido al intenso solapamiento entre las reflexiones Bragg de los diferentes politipos. No obstante, el método de Rietveld constituye una herramienta poderosa para resolver este problema. En este trabajo se utiliza el método de Rietveld al objeto de determinar las fracciones en peso de las diferentes fases para una muestra de SiC sinterizado en fase líquida (LPS SiC). Nuestros resultados ponen también de manifiesto la necesidad de incorporar correcciones debidas a orientación preferencial para efectuar un análisis cuantitativo preciso.

In this work, we propose a polymorphic method for the quantitative analysis in zirconia. This procedure uses a square system of equations relating the intensities of a peaks groups set in the diffraction pattern with the weight fractions of the different phases present in the sample. In this system it is used as unknowns, besides the relative abundance of the phases, a group of parameters that incorporates the contribution from the tails of the groups adjacent to the intensity of a selected group. The described procedure has been applied to a simulated diffractogram corresponding to a composition of zirconia of 50% of cubic phase, 25% of tetragonal phase and 25% of monoclinic phase, and also to a sample of zirconia processed by the sol-gel method.En este trabajo se propone un método polimórfico para el análisis cuantitativo de fases en la circona. Este procedimiento emplea un sistema de ecuaciones compatible y determinado que relaciona las intensidades de un conjunto de grupos de picos del espectro de difracción con las fracciones en peso de las diferentes fases presentes en la muestra. En dicho sistema, además de las abundancias relativas de las fases, se utilizan como incógnitas un conjunto de parámetros que dan cuenta de la aportación de las colas de los grupos de picos adyacentes al grupo de picos considerado. Este procedimiento se ha aplicado a un difractograma simulado correspondiente a una circona con 50% de fase cúbica, 25% de fase tetragonal y 25% de fase monoclínica y también a una muestra en polvo de circona fabricada mediante técnicas sol-gel.

The title compound was synthesized in the form of a powder, and was studied by elemental analysis, IR spectroscopy, thermogravimetry and mass spectroscopy. Its crystal structure was then determined by X-ray powder diffractometry, using X-ray diffraction data collected in the reflection Bragg–Brentano geometry. The methodology followed in the present study to resolve the crystal structure consisted of peak indexing, then the use of the Monte-Carlo/parallel tempering search algorithm, and finally Rietveld refinement coupled with difference-Fourier synthesis. We found that the crystals are composed of monoclinic unit cells, with 1.5 molecules in the asymmetric unit and therefore six molecules per unit cell. In addition, we concluded that the complexes adopt a planar conformation, forming trimers created by groups of parallel molecules. [ABSTRACT FROM AUTHOR]

The title copper(II) coordination compound, C18H22CuN8O6S2 {[Cu(NO3)(PyTz)2]NO3}, was synthesized in the form of small crystals unsuitable for structure determination by single-crystal X-ray diffractometry. It was therefore characterized by molecular modelling coupled with X-ray powder diffractometry [monoclinic, space group P21/n, a = 20.695 (7) Å, b = 8.054 (2) Å c = 15.157 (4) Å bb = 112.09 (2)° and Rwp 0.129]. The procedure used to resolve the structure followed direct space methods with a ‘Monte Carlo/parallel tempering’ search algorithm, where the starting configuration was obtained by means of molecular mechanics. A final refinement was performed with the Rietveld method. Bond distances, bond angles and torsion angles were compared with those of similar compounds deposited in the Cambridge Structural Database. [ABSTRACT FROM AUTHOR]

The title compound was synthesized in the form of a powder, and was studied by elemental analysis, IR spectroscopy, thermogravimetry and mass spectroscopy. Its crystal structure was then determined by X-ray powder diffractometry, using X-ray diffraction data collected in the reflection Bragg-Brentano geometry. The methodology followed in the present study to resolve the crystal structure consisted of peak indexing, then the use of the Monte-Carlo/parallel tempering search algorithm, and finally Rietveld refinement coupled with difference-Fourier synthesis. We found that the crystals are composed of monoclinic unit cells, with 1.5 molecules in the asymmetric unit and therefore six molecules per unit cell. In addition, we concluded that the complexes adopt a planar conformation, forming trimers created by groups of parallel molecules.