Biaxial residual stress in a 〈111〉 textured cubic TiN polycrystalline thin film was analyzed by linear least-squares refinement using the method proposed by Yokoyama and Harada [J. Appl. Crystallogr. 42, 185–191 (2009)]. Values of the unstressed (or stress-free) unit-cell parameter a0=4.2332±0.0006 Å and the stress components of σ11=397(88), σ22=401(88), and σ12=−110(100) were obtained. The values of the in-plane stresses σ11 and σ22 presented in the TiN film are practically the same, while σ12 is relatively small. The results obtained in this study confirm that the above theoretical prediction by Yokoyama and Harada can be used to obtain reliable values of stress-free unit-cell parameter and three biaxial stress components of a textured cubic thin film.

New powder X-ray diffraction data of davyne, a member of the cancrinite group of minerals, were collected using a rotating anode diffractometer: the hexagonal cell parameters are a=12.6711(3) Å, c=5.3278(2) Å, volume 740.82(4) Å3 (space group P63). The strongest lines are: 3.658(100), 4.790(73), 3.272(70), 2.112(48), 2.438(22), 2.663(19), 1.781(19), and 4.147(17). The new data provide quantitative intensities improved precision in d-spacings and cover an increased 2θ angular range with respect to PDF 20-379. Measured intensities and a simulated pattern are reported together with crystal-chemical considerations.

The crystal structure of solifenacin hydrogen succinate [C23H27N2O2(HC4H4O4)] has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Solifenacin hydrogen succinate crystallizes in space group P21 (#4) with a = 6.477 03(2), b = 7.830 95(2), c = 23.848 72(7) Å, β = 90.2373(3)°, V = 1209.63(1) Å3, and Z = 2. The hydrogen succinate anions form a chain linked by strong hydrogen bonds parallel to the a-axis. Discrete N–H···O hydrogen bonds lie on the sides of this chain, resulting in a layer parallel to the ab-plane rich in hydrogen bonds. Halfway between these layers the molecules meet in a herringbone packing of aromatic rings. The powder pattern has been submitted to ICDD for inclusion in future releases of the Powder Diffraction File™.

To minimize waste, improve process safety, and reduce costs, modifications were implemented to a method for quantifying gallium in plutonium metal using wavelength dispersive X-ray fluorescence. These changes included reducing sample sizes, reducing ion exchange process volumes, using cheaper reagent grade acids, eliminating the use of HF acid, and using more robust containment films for sample analysis. Relative precision and accuracy achieved from analyzing multiple aliquots from a single parent sample were approximately 0.2 and 0.1%, respectively. The same precision was obtained from analyzing a total of four parent materials, and the average relative accuracy from all the samples was 0.4%, which is within programmatic uncertainty requirements.

The characteristics of the (101) peak of α-quartz and the (104) peak of the NIST SRM 1976 alumina flat plate standard have been measured in dependence of time for 60 h with Cu-Kα1 radiation in Bragg-Brentano geometry with a Philips X’Pert diffractometer equipped with a primary Ge(111) monochromator. It was found that the reproducibility of the peak position and the peak shape falls well in the ±3σ range, whereas the peak intensity strongly depends on the power history of the X-ray generator and the temperature of the diffraction system. The effects on Rietveld refinements are discussed and recommendations are given for optimized data collection.

New X-ray powder data and a refined cell for mellite are presented and evaluated in comparison with the current PDF 28-2001.

Hard turning, i.e., turning hardened steels, may produce the unique “hook” shaped residual stress (RS) profile characterized by surface compressive RS and subsurface maximum compressive RS. However, the formation mechanism of the unique RS profile is not yet known. In this study, a novel hybrid finite element modeling approach based on thermal-mechanical coupling and internal state variable plasticity model has been developed to predict the unique RS profile patterns by hard turning AISI 52100 steel (62 HRc). The most important controlling factor for the unique characteristics of residual stress profiles has been identified. The transition of maximum residual stress at the surface to the subsurface has been recovered by controlling the plowed depth. The predicted characteristics of residual stress profiles favorably agree with the measured ones. In addition, friction coefficient only affects the magnitude of surface residual stress but not the basic shape of residual stress profiles.

The workshop was aimed at demonstrating the uses and methods of analysis of powder diffraction data collected from X-ray sources. There were around 35 participants in the workshop from Chile, Uruguay, Brazil, and Argentine. The participants came from inorganic and organic chemistry, physics, mineralogy and materials science backgrounds, and additionally we had attendees from a local cement company.

The structures of two high-pressure tungsten oxides, previously studied by high-resolution electron microscopy, were confirmed by Rietveld refinement based on X-ray powder diffraction data. The phases have identical stoichiometry, W3O8, and extremely narrow 00l reflections in common. The microstructure of the dominant phase was investigated by means of X-ray powder diffraction pattern decomposition. A Williamson–Hall plot revealed that all lines, except the 00l reflections, were broadened solely due to the crystallite size effect. A cylindrical model is used to describe the average form of the coherently diffracting domains. The height of the cylinder, whose axis is colinear with the crystallographic c parameter of both phases, is considered “infinite,” and the average diameter of the cylinder model is 655(22) Å. A quantitative confirmation is obtained from electron microscopy.

The peak profile shape analysis has been preferentially used in the evaluation of X-ray and synchrotron powder diffraction pattern. However, neutron diffraction facilities of new generation frequently offer the instrumental resolution high enough to efficiently study the effects of broadening of neutron diffraction profiles. The present paper describes the procedure for a detailed evaluation of Bragg peak shape based on the method of transformed model fitting (TMF) which has been recently developed particularly for the treatment of neutron diffraction profiles. Microstructure modeling is performed in the reciprocal space and the convolution of the model with the instrumental resolution curve is fitted to the profiles recorded in the diffraction experiment.

Powder diffraction data are presented for 3,4-methylenedioxymethylamphetamine hydrochloride monohydrate, the hydrated form of MDMA.HCl, the drug of abuse commonly known as Ecstasy. Samples of pure MDMA.HCl were recrystallized from a variety of solvents, and powder diffraction patterns of the resulting products recorded. Data were collected at room temperature using iron-filtered CoKα radiation.

A direct method for determining powder diffraction data from a range of depths is described, where the linear absorption coefficient may vary with depth. A series of traditional data collections with varying angles of incidence are required, and the X-ray diffraction data arising from specific depths will be calculated by the transformation of these measured, angle-dependent spectra. These may then be analysed using any conventional method in order to gain information about characteristics of the sample in question at specific depths. Regularisation techniques have been used to solve the governing Fredholm integral equation to determine the depth-dependent diffractograms. The method has been validated by the use of simulated data having known model profiles, and has also been applied to experimental data from polycrystalline thin film samples.

The ternary compound YAg0.4Ga1.6 has the CaIn2-type structure. The only variable positional parameter z was determined by graphical methods from visual observations of intensities on a Debye-Scherrer pattern. Cu or Ni substitutions for Ag also result in a ternary CaIn2-type structure.

This study focuses on characterization of an (Al,Cr)3Ti alloy processed together with titanium powder by reactive mechanical milling (RMM) to produce an ultrafine grained intermetallic alloy matrix with in situ carbide and hydride phases formed during processing. Observations of X-ray scattering as RMM processing time increases show severe broadening of matrix diffraction peaks, accompanied by the appearance of diffraction peaks resulting from the formation of very small crystallites of TiC and TiH1.92 phases with increasing volume fractions, and finally, increasing background intensity as the crystallite size of the matrix phase decreases to ∼2 nm. Estimates of phase volume fractions were made by the direct comparison method, along with crystallite sizes by Warren–Averbach peak profile analysis. The general increase in background intensities has been attributed to random static displacements of the large fraction of atoms located within the grain boundary regions. Further, it has been concluded that the matrix material with a crystallite size of a few nanometers has about half the atoms in statically displaced positions defining the boundary regions. The results argue that background intensity changes should not be ignored and are useful in interpreting scattering from these nano-scale materials.