Two compounds with compositions around n=14 and n∼5.4 (n=Bi/Mo molar ratio) have been prepared by solid-state reaction with five heating/grinding cycles at 800 °C. The lattice constants of both compounds can be related to the fluorite-type structure of δ-Bi2O3. Bi14MoO24 has been indexed as an orthorhombic pseudotetragonal (√2×√2×1) superstructure: a=7.812 (±0.005) Å, b=7.762 (±0.005) Å, c=5.7716 (±0.0007) Å (but a+b=15.5750±0.0020). For orthorhombic (3×5×3) Bi38Mo7O78: a=16.8236 (±0.0027) Å, b=28.6182 (±0.0045) Å, c=16.9082 (±0.0027) Å.

A full-pattern fitting procedure based on the Rietveld method was applied to electron diffraction ring patterns of a two-phase system, exhibiting the co-presence of zinc sulfide (sphalerite) and zinc oxide (Wurtzite). Bright and dark field (DF) images reveal the presence of micrometric aggregates, composed of quasi-spherical nanosized crystallites. These conventional transmission electron microscopy imaging methods provide a general morphological characterization of the specimens although, in the present case, they are not suitable for a detailed characterization of the microstructural features of the analyzed samples. Owing to the overlap and broadening of the diffraction rings of the two phases, DF images cannot provide a satisfactory picture of the individual crystallites of each single phase. To overcome this limit, the mentioned Rietveld approach was applied to model the electron diffraction data. The crystalline domain size and relevant shapes for both phases were successfully evaluated using the proposed methodological approach. The excellent results obtained in the microstructural characterization of the nanostructured multiphase samples demonstrate the capability of this technique, that may represents a fully quantitative method for the routine characterization of crystalline nanomaterials.

A general least-squares technique for X-ray diffraction line broadening analysis has been developed. The technique can be used to determine single, double, and triple line broadening effects caused by small particle sizes, microstrain, stacking faults, or all three presented in a closed-packed hexagonal nanomaterial. The technique was applied to characterize the microstructure of β-Ni(OH)2, a negative electrode material in nickel-metal hydride (NiMH) batteries. Double line broadening effects caused by both small crystallite sizes and stacking faults in β-Ni(OH)2 were detected and analyzed. Triple line broadening effects caused simultaneously by small crystallite sizes, microstrain, and stacking faults were detected in β-Ni(OH)2 after activation and charge-discharge cycle tests. The triple line broadening effects were found to be selective and most pronounced for diffraction lines with h−k=3n±1. The broadening effects were larger when l=even, but smaller when l=odd. The shape and the average size of the crystallites, microstrain, and stacking fault probability in β-Ni(OH)2 changed dramatically after activation and charge-discharge cycles. The method was also applied to characterize and investigate the microstructure of nano ZnO materials. Results indicate that no selective broadening appears in the XRD patterns of the nano ZnO materials. The average crystallite sizes were different slightly, and the stacking fault probabilities differed significantly with different dopants.

The biaxial stress and thermal expansion of multilayer doped-aluminosilicate environmental barrier coatings were measured in situ during cooling using microfocused high-energy X-rays in transmission. Coating stresses during cooling from 1000 °C were measured for as-sprayed and thermally cycled samples. In the as-sprayed state, tensile stresses as high as 75 MPa were measured in the doped-aluminosilicate topcoat at 375 °C, after which a drop in the stress occurred accompanied by through-thickness cracking of the two outermost layers. After thermally cycling the samples, the stress in the topcoat was reduced to approximately 50 MPa, and there was no drop in stress upon cooling. This stress reduction was attributed to a crystallographic phase transformation of the topcoat and the accompanying change in thermal expansion coefficient. The addition of a doped aluminosilicate to the mullite layer did not lower the stress in the topcoat, but may offer increased durability due to an increased compressive stress.

The thermal behavior and decomposition reaction of Prussian blue (PB) (Fe43+[Fe2+(CN)6]3·xH2O) was studied under inert atmosphere of argon by simultaneous thermogravimetry and differential scanning calorimetry, from room temperature up to 900 °C, with a heating rate of 5 K min−1. Parallel to the thermogravimetric measurements, the thermal process was monitored by in situ X-ray powder diffraction (XRD) technique under nitrogen atmosphere. The thermogravimetric data show six steps, corresponding to different stages of the decomposition reaction; comparable results are also obtained by in situ XRD. In addition, a set of PB samples heated up to selected temperatures (190, 300, 370, 540, 680, and 790 °C) were ex situ analyzed by powder XRD and Mössbauer spectroscopy. It is found that PB exhibits a negative thermal expansion prior to the water release from its crystalline lattice. Above 300 °C, the decomposition is based on the release of cyanogen gas from the PB structure. At 370 °C, a cubic iron cyanide compound is formed, while at higher temperatures several iron carbides were found. The subsequent thermal treatment of these carbides leads to the formation of metallic iron and graphite.

In pursuit of design and characterisation of Cu adsorbing in thin films, we present data from a large variety of Cu-K edge X-ray Absorption Near Edge Spectroscopy (XANES) spectra obtained from organic and inorganic standards. Additionally, we have explored the impact of beam damage inducing redox alterations. Polymer nanoparticles were tested against films to produce higher concentration samples while maintaining high surface area to bulk effects. Spectra from nanoparticles were highly comparable to thin films of ~8 nm thickness, implying comparable contributions by surface effects on copper association. Finally, we observed no impact on Cu XANES spectra from vitrification with dimethyl sulfoxide to produce amorphous frozen, hydrated samples. The spectra should act as a valuable resource in assisting the design of experiments and identification of copper associations.

The crystal structure of a new compound Li2Mg2(WO4)3 has been determined by means of X-ray powder diffraction. Li2Mg2(WO4)3 belongs to the orthorhombic system, with space group Pnma and the lattice parameters are: a = 5.1129 Å, b = 10.462 A, and c = 17.612 Å at room.temperature. Its measured density is Dm = 5.48 g/cm3, and each unit cell contains four formula weights.

Two-dimensional proportional detectors with their faster data collection, large dynamic range, and more available information than point or linear proportional detectors make them ideal for microdiffraction analysis. The unique capabilities of these detectors coupled with a rotating anode source, capillary optics, and a variety of accessories allow for a wide range of applications.

A wide range of transition metal oxide solid solutions have been prepared and characterised using powder X-ray diffraction (MnxCo1−xFe2O4, FexCo1−xFe2O4, NixCo1−xFe2O4, FeFexCr2−xO4, MnFexCr2−xO4, MnxFe1−xCr2O4, MnxFe1−xFe2O4, NixFe1−xFe2O4). Calibration curves have been obtained relating oxide composition to unit cell parameter or d spacing. From these curves it is possible to identify the composition of oxides formed on steel surfaces in varied industrial environments. Even when poor diffraction patterns are obtained and little sample is available, an estimate of composition can be made.

Crystal data and results of structure refinements for ScPO4 are reported. The material is tetragonal, I41/amd, with a = 6.5787(2) Å, c = 5.7963(2) Å, Vd = 250.86(2) Å3, Z = 4, Dx = 3.704 Mg/m3. Intensity data were obtained from a Stoe transmission type diffractometer equipped with a position sensitive detector. CuKα1 radiation, λ = 1.5405981 Å was employed. Silicon, SRM 640b (a = 5.43094 Å) was used as an internal standard. The structure was refined by the Rietveld method by aid of three different programs.

Single crystals and powder samples of Ca2Bi5O5and Ca4Bi6O13have been synthesized and studied using single crystal X-ray diffraction as well as X-ray and neutron powder diffraction. Unit cell dimensions were calculated using a least squares analysis that refined to a δ2θof no more than 0.03°. A triclinic cell was found with space group , a = 10.1222(7), b = 10.1466(6), c = 10.4833(7) Å. α= 116.912(5), β= 107.135(6) and γ= 92.939(6)°, Z = 6 for the Ca2Bi2O5compound. An orthorhombic cell was found with space group C2mm, a = 17.3795(5), b = 5.9419(2) and c = 7.2306(2) Å, Z = 2 for the Ca4Bi6O13compound.

X-ray powder diffractograms from fcc crystals containing high concentration (more than 1%) of planar defects [deformation stacking faults (SF), double deformation SF, twin boundaries (TB)] have been simulated by Monte Carlo method in kinematic approach. It was shown that the characteristics of powder diffraction peak profiles (except peaks with indexes H00) dependent nonmonotonically on PD concentration, during which peak maximums stay in Bragg positions. An addition point to emphasize is that an appearance of TB only in the crystal not affects on position of all peaks. Several types of PD to be occurred simultaneously in the crystal influence on powder diffractograms additively. Peculiarities of the powder diffraction pattern inherent in different types of PD have been revealed to permit predominant PD type to be found with a high degree of accuracy based on experimental data.

Powder X-ray diffraction was used to monitor the solvent-free synthesis of two-dimensional (2D) metal–organic frameworks (MOFs) via mechanochemical methods. For four isophthalic acid-based, alkoxide-functionalized organic ligands, optimal milling times were found to vary from 12 to 48 min. This work confirms that mechanochemical synthesis routes can be utilized to afford highly-crystalline, 2D MOFs.

Weight fractions of four dominant phases (C3S, C2S, C4AF, and C3A) present in five industrial clinkers were estimated by a series of neutron and X-ray Rietveld refinements. Calculated powder patterns were derived from the structural data for monoclinic and triclinic C3S, monoclinic C2S, orthorhombic C4AF, cubic C3A and MgO. Neutron diffraction data were collected with the high resolution E9 diffractometer (BENSC) using two different wavelengths, X-ray diffraction data with a high resolution transmission diffractometer. Elemental composition of the samples obtained by ESEM/EDX technique were in a good agreement with the data delivered by the producers. Convergence of the refinements was remarkably different for X-ray and for neutron data. Several refinements were not completed due to numerical instabilities. Neutron refinements were found to be more stable than X-ray, but there was not any notable difference in the final estimated phases’ compositions. Calculated absolute deviates of phases’ weight fractions were mostly within ±10%, which for the less abundant phases corresponded to relative deviations within ±50%. © 2004 International Centre for Diffraction Data.

The Rietveld method based on X-ray diffraction (XRD) technology has been commonly applied for the quantitative analysis of crystalline minerals in organic-rich rocks. The presence of organic matter, however, has interference in varying degree to the quantitative result. In this work, the mixed samples of organic matter and crystalline minerals at given proportions were prepared to investigate the effect of organic matter on the Rietveld quantitative analysis of crystalline minerals in coal gangue. The relative standard deviation (RSD) and absolute error (AE) were used to evaluate the precision and accuracy of the quantitative result. The results showed that the presence of organic matter led to a reduction in the precision and accuracy. It was attributed in part to the presence of organic matter, which can produce a background noise in the XRD pattern, especially in the region of 5–30° (2θ). Further results showed that the interference in this region increased with the increase in the organic matter content. The RSD and AE were within the range of 10% and 2%, respectively, when the organic matter content is <30 wt%. Based on this, an approximate method for the Rietveld quantitative analysis of crystalline minerals in coal gangue was established.

Aluminum borate (9Al2O3·2B2O3) whiskers were chemically synthesized in potassium sulphate flux by using the starting chemicals of aluminum sulphate and boric acid. The synthesis temperature of 1075 °C was found to be the optimum with respect to whisker morphology. A tentative X-ray diffraction (XRD) pattern was suggested for the whiskers produced after heating at 1150 °C. The product purity, phase composition, and whisker morphology were investigated by XRD, energy dispersive X-ray spectroscopy, and scanning electron microscopy, respectively.

The crystal structure of Tl4V2O7 is solved ab-initio from powder diffraction data collected in Debye-Scherrer geometry using an Inel X-ray Position Sensitive Detector. The structure has been determined from Rietveld analysis in space group ml, Z = 1, with a = 5.9388(2)Å and c = 7.7322(3)Å. The structure of Tl4V2O7 is built up from isolated V2O7 groups aligned along the trigonal c axis. Thallium atoms alternate along a 3-fold axis. The presence of stereochemically active lone pairs is demonstrated and their positions are calculated using a self-consistent electrostatic model. The influence of sample absorption is briefly discussed and the results are compared with those obtained in Bragg-Brentano geometry using flat-plate specimen.

Solid lipid nanoparticles (SLNs) were characterized by differential scanning calorimetry (DSC) and powder diffraction. The DSC thermograms showed a slight reduction in the melting point of lipid matrix and a broadening of its melting peak, indicating an increased number of lattice defects in SLNs. X-ray powder diffraction data also revealed a slightly broader reflection for SLNs and the presence of X-ray peaks of the all-trans retinoic acid (RA) crystals outside of the lipid matrix of SLNs without stearylamine (STE). These data suggest the presence of an extensive association of ion pairing components (RA and STE), and indicate that the utilization of some specific types of compounds containing amine groups is an interesting approach to improve the encapsulation efficiency of RA in SLNs. The formation of the ion pairing is an interesting alternative for RA encapsulation in SLNs, improving the benefits obtained by the drug incorporation in lipid matrix (increased stability, controlled release, and targeting effect), which are important for the topical treatment of acne.

New X-ray powder data for CaWO4 (synthetic scheelite) are presented and compared with the current PDF patterns and with a calculated pattern.

Indexed X-ray powder diffraction data are reported for the semiconducting compound Ba2Cl2Cu3O4. The structure was refined by the Rietveid technique on the basis of the space group I4/mmm. Refined unit cell dimensions are a = 5.5156(1) Å, c = 13.8221(3) Å, V = 420.49 Å3Dx = 4.74 g/cm3, F30 = 129(0.0075,30), M20 = 121, Rp = 6.58, Rwp = 8.66, and RB = 4.49.