Powder diffraction data were collected for a synthetic zinc molybdate of composition Na(OH)Zn2(MoO4)2·2.5H2O. The material is monoclinic, space group C2/m, with a=9.4543(12), b=6.3492(7), c=7.6453(11), β=115.899(13), and V=412.83 Å3.

A natural olivine sample from a mantle peridotite xenolith has been studied by in situ high-temperature powder diffraction. The structure has been successfully refined from powder data at three temperatures (25, 600, and 800 °C) using the Rietveld method. The study shows that the full-profile technique is well suited for the structure analysis of high-temperature powder diffraction data. The results indicate that, in this temperature range, there is no significant ordering of the Fe,Mg cations in the two crystallographically independent octahedral sites. This has implications for the thermodynamic modeling of olivine at upper mantle conditions. The present experiments allowed measurement of the lattice thermal expansion of olivine in the temperature range 25–800 °C, and assessment of the temperature dependence of the isotropic atomic displacement parameters.

Transformation behaviors of the technologically important polycrystalline Ti50.75Ni47.75Fe1.50 shape memory alloy were investigated using differential scanning calorimeter (DSC) and powder diffraction techniques. DSC revealed that there are two-stage (i.e., cubic→trigonal→monoclinic) martensitic phase transformations on cooling and a one-step transformation (monoclinic→cubic) on heating. In situ structural refinement of cubic→trigonal→monoclinic on cooling was carried out using the D1A high-resolution neutron powder diffractometer at the Institut Laue-Langevin Neutrons for Science in Grenoble, France. Results showed that the phases involved during the phase transition are consistent with the differential scanning calorimeter cooling curve, and the refined crystal structure parameters obtained from Rietveld refinements with the generalized spherical harmonic description agreed reasonably well with X-ray single-crystal data. Subsequently, a combined neutron and synchrotron structural refinement for each phase was conducted because the trial refinements initially using only the synchrotron data of trigonal phase yielded a false minimum with a somewhat high goodness-of-fit χ2. Results obtained from the combined neutron and synchrotron data of the cubic, trigonal, and monoclinic phases show that the same minimum goodness-of-fit indices were always obtained.

The deflection (curvature) of embedded single-crystal silicon chips was investigated by rocking curve X-ray diffraction techniques at two significant manufacturing stages in the process chain of printed circuit boards with embedded components. An overview of the curvature deduction by two different approaches was presented: (1) the measurement of the variation of the rocking curve maximum as a function of the lateral sample position along a specific traverse; the slope in such a diagram is then proportional to the corresponding curvature in that direction. (2) The evaluation of the rocking curve width; here the peak width is inversely proportional to the curvature at known beam diameter, diffraction angle, and beam divergence. It was shown that the rocking curve method is applicable to determine the curvature inside single crystalline chips. Furthermore, the method is also suitable to determine the curvature of fully embedded or encapsulated chips. Additionally the absorption of the radiation in the embed medium was quantitatively discussed. The curvature of two different prepared samples was determined at temperatures up to 200 °C in a heating stage attached to the diffractometer device.

Building materials are very complex samples of worldwide importance; hence quantitative knowledge of their mineralogical composition is necessary to predict performances. Rietveld quantitative phase analysis (RQPA) allows a direct measurement of the crystalline phase contents of cements. We highlight in this paper the use of laboratory X-ray powder diffraction (LXRPD) employing high-energy radiation, molybdenum (Mo), for attaining the RQPA of cements. Firstly, we evaluate the accuracy of RQPA employing a commercial calcium sulfoaluminate clinker with gypsum. In addition to MoKα 1 and MoKα 1,2 radiations, Cu and synchrotron patterns are also analyzed for the sake of comparison. Secondly, the assessment of the accuracy of RQPA results obtained using different radiations (synchrotron, Mo, and Cu) and geometries (reflection and transmission) is performed by analyzing two well-known commercial samples. As expected, for LXRPD data, accuracy in the RQPA results improves as the irradiated volume increases. Finally, three very complex aged hydrated cements have been analyzed using MoKα1-LXRPD and Synchrotron-XRPD. The main overall outcome of this work is the benefit for RQPA of using strictly monochromatic MoKα 1 radiation. Best laboratory results arise from MoKα 1 data as the effective tested volume is much increased but peak overlapping is not swelled.

A model for the long awaited crystal structure of metastable NaAlF4 is established from the powder diffraction pattern of a partly disproportionated sample. Orthorhombic, Cmcm, a=3.6121(3), b=14.952(1), c=5.2692(4) Å, Z=4, V=284.58(4) Å3. Sodium atoms are in NaF6 trigonal prisms interconnected by edges in compact layers. AlF6 octahedra are both cis- and trans-corner connected forming a layer structure similar to that observed in the NaNbO2F2 (P21/c) and BaZnF4 (Cmc21) structure types. NaAlF4 is ideally simple and symmetrical, isostructural with BiReO4 (Cmcm), representing the aristotype of the NaMIIIF4 and BaMIIF4 series.

Besides statistical and graphical measures, many structural features can be used to assess the quality of a Rietveld refinement. These include the metric symmetry of the lattice (which can assist in determining the true symmetry and in identifying isostructural compounds), bond distances and angles (which should fall within normal ranges), displacement coefficients, refined stoichiometry, the absolute values of the standard uncertainties of the fractional coordinates, the hydrogen bonding pattern, the presence of approximate symmetry, the presence of unindexed peaks in the pattern, and whether the refinement converges at all. Chemical knowledge can be built into a Rietveld refinement though the use of restraints and rigid bodies. A knowledge of chemical reasonableness proved important in refining the correct structures of [Fe(H2O)6](BF4)2, (Ba1.5Sr0.5)TiO4, and (Ba1.25Sr0.75)TiO4.

The effectiveness of different routes of equal channel angular pressing (A, Bc, and C) is studied for commercially pure copper. The stored energy and the activation energy of recrystallization for the deformed samples were quantified using differential scanning calorimetry and X-ray diffraction line profile analysis. Results of the study revealed that the dislocation density and the stored energy are higher in the case of route Bc deformed sample. The activation energy for recrystallization is lower for route Bc.

X-ray powder diffraction data, unit-cell parameters, and space group for S-2-(methylamino)-2-phenylcyclohexan-1-one hydrochloride, C13H18ClNO, are reported [a = 6.578 (1) Å, b = 13.250 (2) Å, c = 15.096 (2) Å, β = 91.619 (3)°, unit-cell volume V = 1315(1) Å3, Z = 4, and space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurities were observed.

A new polymorph of HfMo2O8 (β-form) is synthesized under high pressure and high temperature conditions. The powder X-ray diffraction (XRD) data could be explained based on a monoclinic lattice (Space Group: C2/c No. 15) with the unit cell parameters as: a=11.415(3), b=7.906(2), c=7.438(2) Å and β=122.37(2)°, V=566.9(2) Å3. The detailed powder XRD data and analysis are reported herein.

New powder X-ray data for cancrinite [ideally Na8Si6Al6O24 (CO3)2·2 H2O] are reported along with in-situ real-time thermal processes recorded using energy dispersive X-ray diffractometry (EDXD). A completely anhydrous phase is obtained after heating the sample up to 600 °C and quickly cooling it to room temperature, as shown by means of both Rietveld analysis and IR spectroscopy. The anhydrous phase does not show any tendency to re-acquire molecular water. During the heating process, at around 450 °C, a peak splitting is observed, possibly due to a reversible phase transition.

The crystal structure of the mullite in a commercial material was refined by the Rietveld method using laboratory X-ray powder diffraction data. In this one refinement, most of the common challenges—including variable stoichiometry (partially occupied sites), multiple impurity phases, amorphous material, constraints, restraints, correlation, anisotropic profiles, microabsorption, and contamination during grinding—are encountered and the thought processes during the refinement are described step-by-step. Interpretation of the refinements includes bulk chemical analysis, chemical composition of the mullite, assessment of the geometry, bond valence sums, the displacement coefficients, crystallite size and microstrain, comparison to similar structures to assess chemical reasonableness, and the nature of the amorphous phase.

Nuclear fuel plates based on a γU-Mo/Al mixture are proposed for research reactors. In this work their thermal behavior in the [425; 550°C] temperature range has been studied mainly by neutron and high energy X-ray diffraction. Even if complementary studies will be necessary, the kinetics of first the growth of the interaction layer between γU-Mo and Al and second of the γU-Mo destabilization have been accurately measured. This basic work should be helpful for defining manufacturing conditions for fuel plates with optimized composition.

The transition metal fluorides KMF3 (M = Mn, Co, and Ni) were synthesized through a simple solution route. The crystal structure, morphology and electrical transport property of the resulting products were investigated. The compound KMF3 crystallizes in a cubic perovskite structure with space group Pm-3m (No. 221). A crystal structure of KMF3 was refined by the Rietveld method based on the X-ray powder diffraction data. The unit-cell parameters are 4.189 46(4), 4.075 58(4), and 4.025 70(2) for KMnF3, KCoF3 and KNiF3, respectively. A metal–insulator transition was observed in temperature-dependent electrical transport characterization in the temperature range from 250 to 280 K for these three compounds, which is considered to be related to spin-exchange in this kind of material.

Five structurally related compounds, TlMgAsO4, TlMgPO4, TlZnAsO4, TlZnPO4, TlZnVO4, have been synthesized by solid-state reaction. Single crystals have been grown by various methods. Space group and unit-cell parameters were determined. Powder diffraction data for each phase are reported.

The NaYF4:Yb3+,Tb3+ (x Yb: 0.20, x Tb: 0.04) materials were prepared by the co-precipitation method. The as-prepared material was washed with and without water and thereafter annealed at 500 °C. This resulted in materials with moderate (with water) and very high (without water) up-conversion luminescence intensity. The structural details causing the differences in luminescence intensity were investigated at room temperature with X-ray powder diffraction and Rietveld analyses. All materials crystallized in the hexagonal form (P63/m, No. 176, Z: 1.5) with a composition very close to stoichimetric. The local structural details revealed microstrains in the rare earth sublattice that were relaxed for the material with very high up-conversion luminescence intensity thus decreasing energy losses and enhancing up-conversion.

The title materials are stuffed cristobalites possessing moderate to extreme pseudosymmetry. On the bases of their X-ray powder diffraction patterns, the Mg, Zn, and Cd compounds had been previously reported as cubic and, more recently, the Zn phase as orthorhombic. Newly measured X-ray powder diffraction data demonstrate that all (including the hitherto unknown Co analog) have the Pca21 structure of Na2BeSiO4 at room temperature, but with a widely variable degree of cubic pseudosymmetry. Observed X-ray diffraction data are in good agreement with those calculated by the Rietveld method using a constrained model with Pca21 M2+/Si site occupancy and pseudocentrosymmetric Pcab atom locations. For the most nearly cubic phase, the Cd compound, there is too little deviation in the pattern from cubic symmetry to support atom coordinate refinement even with the constrained model. In these derivatives of the stuffed cristobalite structure family, M2+ and Si atoms form an ordered tetrahedral array which avoids M2+–O–M2+ connections. Potassium atoms fill all of the intervening large cavity sites.

4-hydroxy-3-methoxyphenyl-4-hydroxycoumarin chalcone (C19H14O6) was synthesized by the Claisen–Schmidt reaction with the condensation of 3-acetyl-4-hydroxycoumarin with 4-hydroxy-3-methoxybenzaldehyde (vanillin). The new compound was characterized by Fourier transform infrared microscopy, UV–vis 1H, and 13C NMR spectroscopy and its crystal structure was ab initio determined from laboratory X-ray powder diffraction data. The crystal structure is monoclinic with unit-cell parameters a = 14.3181(4), b = 8.040 71(9), c = 13.5524(3), β = 100.3559(13)°, V = 1534.84(6) Å3, and space group P21/c.

The crystal structures of LaCo0.5Ni0.5O3−δ and LaCo0.5Fe0.5O3−δ solid solutions, studied by powder X-ray diffraction, were found to be rhombohedral perovskite. The unit cell parameters in the hexagonal setting are a=5.491(6) Å and c=13.231(3) Å for LaCo0.5Fe0.5O3−δ, and a=5.464(4) Å and c=13.125(3) Å for LaCo0.5Ni0.5O3−δ. The space group is R3c (No. 167).

Zn7Sb2O12 is known to adopt an inverse spinel crystal structure, in which Zn2+ occupies the eight tetrahedral positions and Sb5+ and Zn2+ randomly occupy the 16 octahedral positions. Samples of Zn7−xNixSb2O12 (x=0, 1, 2, 3, and 4) were synthesized using a modified polymeric precursor method, known as the Pechini method. The crystal structure of the powders was characterized by Rietveld refinement with X-ray diffraction data. The results show that for x=0, 1, and 2 Ni substitutes for Zn2+ in the octahedral sites, and that for x=3 and 4 it is assumed that Ni2+ replaces Zn2+ ions in both the octahedral and tetrahedral positions. It is also observed for x=3 and 4 the formation of two spinel phases.