Least-squares analysis on the diffraction intensity values certified for NIST SRM676a and SRM1976c α-Al2O3 (corundum) have shown that the intensities of SRM1976c can be simulated by the March-Dollase preferred orientation model along the (001)-direction. Diffraction intensities of randomly oriented corundum crystallites have been calculated from electron density data obtained by conventional and density functional theory (DFT) calculations, on the assumption of independent and similar atomic displacements for Al and O atoms. The results of DFT calculations support that the strongest peak of randomly oriented α-Al2O3 crystalline powder should be 113-reflection, though the intensities simulated by DFT calculations are not closer to NIST SRM676a intensities than those expected for a fully ionized model ${\rm Al}_2^{3 + } {\rm O}_3^{2-}$. Diffraction data of two types of relatively fine (nominally 2–3 μm and ca 0.3 μm) α-Al2O3 powder have been collected and processed by a deconvolutional treatment (DCT). Integrated peak intensities extracted from the DCT data by an individual peak profile fitting method also support that the 113-reflection is the strongest reflection of randomly oriented α-Al2O3 crystalline powder.

Pb–Zr–Ti–O (PZT) perovskites span a large solid-solution range and have found widespread use due to their piezoelectric and ferroelectric properties that also span a large range. Crystal structure analysis via Rietveld refinement facilitates materials analysis via the extraction of the structural parameters. These parameters, often obtained as a function of an additional dimension (e.g., pressure), can help to diagnose materials response within a use environment. Often referred to as “in-situ” studies, these experiments provide an abundance of data. Viewing structural changes due to applied pressure conditions can give much-needed insight into materials performance. However, challenges exist for viewing/presenting results when the details are inherently three-dimensional (3D) in nature. For PZT perovskites, the use of polyhedra (e.g., Zr/Ti–O6 octahedra) to view bonding/connectivity is beneficial; however, the visualization of the octahedra behavior with pressure dependence is less easily demonstrated due to the complexity of the added pressure dimension. We present a more intuitive visualization by projecting structural data into virtual reality (VR). We employ previously published structural data for Pb0.99(Zr0.95Ti0.05)0.98Nb0.02O3 as an exemplar for VR visualization of the PZT R3c crystal structure between ambient and 0.62 GPa pressure. This is accomplished via our in-house CAD2VR™ software platform and the new CrystalVR plugin. The use of the VR environment enables a more intuitive viewing experience, while enabling on-the-fly evaluation of crystal data, to form a detailed and comprehensive understanding of in-situ datasets. Discussion of methodology and tools for viewing are given, along with how recording results in video form can enable the viewing experience.

Dimethyl carbonate (DMC) is an important industrial solvent but is additionally a common component of liquid lithium-ion battery electrolytes. Pure DMC has a melting point of 277 K, so encountering solidification under outdoor climatic conditions is very likely in many locations around the globe. Even eutectic, ethylene carbonate:dimethyl carbonate commercial LiPF6 salt electrolyte formulations can start to solidify at temperatures around 260 K with obvious consequences for their performance. No structures for crystalline DMC are currently available which could be a hindrance for in situ battery studies at reduced temperatures. A time-of-flight neutron powder diffraction study of the phase behavior and crystal structures of deuterated DMC was undertaken to help fill this knowledge gap. Three different orthorhombic crystalline phases were found with a previously unreported low-temperature phase transition around 50–55 K. The progression of Pbca → Pbcm → Ibam space groups follow a sequence of group–subgroup relationships with the final Ibam structure being disordered around the central carbon atom.

X-ray fluorescence (XRF) is frequently used to measure layer thickness in the micrometer range. But also X-ray diffraction (XRD) can be used in a comparable way and offers the benefit to differentiate coating layers by their crystal structure. Thus, the thickness of different oxide layers of the same element can be determined, e.g., FeO, Fe3O4, and Fe2O3 on Fe-substrate. An approach for such measurement is discussed. Furthermore, with a suitable sample stage, a spatially resolved coating thickness map can be measured in a nondestructive way. Applications and validations of the presented XRD method for the measurement of the thickness of zinc coatings on steel are given and compared with results from XRF, glow-discharge optical emission spectroscopy, and optical micrographs. In addition, the methodology was tested and validated using XRF reference standards and iron nitride and iron oxide layers.

Quantitative phase analysis (QPA) of slags is complex due to the natural richness of phases and variability in sample composition. The number of phases frequently exceeds 10, with certain slag types (EAF, BOF, blends, stainless) having extreme peak overlap, making identification difficult. Another convolution arises from the variable crystallite sizes of phases found in slag, as well as the mixture of crystalline and amorphous components specific to each slag type. Additionally, polymorphs are common because of the complexity of the steelmaking and slag cooling processes, such as the cation-doped calcium aluminum silicate (Ca3Al2O6, C3A, Z = 24) supercell in LMF slag. References for these doped variants may not exist or in many cases are not known in advance, therefore it is incumbent on the analyzer to be aware of such discrepancies and choose the best available reference. All issues can compound to form a highly intricate QPA and have prevented previous methods of QPA from accurately measuring phase components in slag. QPA was performed via the internal standard method using 8 wt% ZnO as the internal standard and JADE Pro's Whole Pattern Fitting analysis. For each phase, five variables (lattice parameters, preferred orientation, scale factor, temperature factor, and crystallite size) must be accounted for during quantitation, with a specific emphasis on not refining crystallite sizes for iron oxides and trace phases as they are inclined to over-broaden and interact with the background to improve the goodness of fit (R/E value). Preliminary investigations show somewhat reliable results with the use of custom file sets created within PDF-4+ specifically targeted toward slag minerals to further regulate and normalize the analysis process. The objective of this research is to provide a standard protocol for collecting data, as well as to update methodologies and databases for QPA, to the slag community for implementation in a conventional laboratory setting. Currently, Whole Pattern Fitting “Modified” Rietveld block refinement coupled with the addition of a ZnO internal standard gives the most accurate QPA results, though further research is needed to improve upon the complex issues found in this study of the QPA of slags.

X-ray diffraction in the Bragg-Brentano configuration (“XRD”) is a very established method. However, experimental evidence concerning its significant information depth, i.e. microstructure components from which maximum depth can affect the information evaluated from the acquired diffraction pattern, are scarce in the scientific literature. This depth is relevant to all XRD measurements performed on compact samples, especially layered composites and samples showing a crystallographic texture evolution. This article provides experimentally determined upper and lower limits to the significant information depth: XRD patterns acquired from a compact crystal layer through a layer of compact, amorphous glass indicate that the significant information depth of XRD using Cu Kα1 and Kα2 radiation is very likely larger than 48 μm, but smaller than 118 μm, in a material of the composition Mg2Al4Si5O18 with a density of ca. ~2.6 g/cm3. The depth of 48 μm correlates to the depth larger than the layer of material from which 90% of the reflected X-rays originate at 2Θ = 25.8°.

The crystal structure of encorafenib, C22H27ClFN7O4S, has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional theory techniques. Encorafenib crystallizes in space group P21 (#4) with a = 16.17355(25), b = 9.52334(11), c = 17.12368(19) Å, β = 89.9928(22)°, V = 2637.50(4) Å3, and Z = 4. The crystal structure consists of alternating layers of stacked halogenated phenyl rings and the other parts of the molecules perpendicular to the a-axis. One molecule participates in two strong N–H⋯N hydrogen bonds (one intra- and the other intermolecular), which are not present for the other molecule. The intermolecular hydrogen bonds link molecule 2 into a spiral chain along the b-axis. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

The dichloro-dioxide-(4,4′-dimethyl-2,2′-bipyridyl)-molybdenum (VI) complex was prepared from molybdenum(VI)-dichloride-dioxide and 4,4′-dimethyl-2,2′-bipyridyl in CH2Cl2 obtaining a clear green solution. The molybdenum complex was precipitated using ethyl ether, separated by filtration and the light green solid washed with ethyl ether. The XRPD pattern for the new compound showed that the crystalline compound belongs to the monoclinic space group P21/n (No.14) with refined unit-cell parameters a = 12.0225(8) Å, b = 10.3812(9) Å, c = 11.7823(9) Å, β = 103.180(9)°, unit-cell volume V = 1431.79 Å3, and Z = 4.

X-ray powder diffraction data, including unit cell parameters and space group assignment, for the ESP15228 species of C19H34O5 formula, are here reported [a = 6.0434(6), b = 12.2543(6), c = 14.0285(8) Å, α = 86.584(3), β = 85.707(10), γ = 78.801(5)°, V = 1015.2(1) Å3, Z = 2, ρcalc = 1.152 g cm−3, and space group P-1]. All measured lines were indexed and no detectable impurities were observed.

A new ternary compound Al0.931Ni1.069Sc5 has been synthesized and studied by means of the X-ray powder diffraction technique. Al0.931Ni1.069Sc5 crystallizes in the hexagonal crystal system with the Al5Co2 structure type, space group P63/mmc, with a = 8.8287(3) Å, c = 8.6959(4) Å, Z = 4 and V = 587.00 Å3, ρcalc = 3.538 g/cm3.