The new diffraction patterns of the low- and high-temperature phases of Li0.87Hf2.032(PO4)3 and LiSn2(PO4)3 are given and indexed on the basis of a structure refinement from neutron powder data using Rietveld method. The two isotypic compounds present a reversible phase transition: triclinic (LT, space group P1¯) ⇄ rhombohedral (HT, space group R3¯c) which proceeds by topotactic distortion of the structural skeleton.

An improved method to correct observed shift and asymmetric deformation of diffraction peak profile caused by the axial-divergence aberration in Bragg–Brentano geometry is proposed. The method is based on deconvolution–convolution treatment applying scale transform of abscissa, Fourier transform, and cumulant analysis of an analytical model for the axial-divergence aberration. The method has been applied to the powder diffraction data of a standard LaB6 powder (NIST SRM660a) sample, collected with a one-dimensional Si strip detector. The locations, widths and shape of the peaks in the deconvolved–convolved powder diffraction data have been analyzed. The finally obtained whole powder diffraction pattern ranging from 10° to 145° in diffraction angle has been simulated by the Pawley method applying a symmetric Pearson VII peak profile model to each peak with ten background, two peak-shift, three line-width, and two peak-shape parameters, and the Rp value of the best fit has been estimated at 4.4%.

In this work we report the synthesis and structural characterization of the elpasolite Cs2NaTbCl6, belonging to the space group Fm3m. The synthesis is by solid state reaction, in controlled atmosphere. By means of thermal analysis (DTA/TGA), the best crystallization temperatures were obtained: 772.2 °C for 2 hours. Structural studies are carried out by means of DRX-powder diffraction and application of the Rietveld profiles refinement method, for the 32 diffraction lines analyzed. The following crystallographic parameters are obtained: a0=10.7636 (Å), Z=4, M=660.44, V=1247.0 (Å)3, Dx=3.519, and Dexp=3.52±0.01.

In this work we present results of X-ray diffraction using powder method, on natural alexandrite samples from Minas Gerais State (Brazil), as a function of a sequence of annealing. From these measurements we determine lattice parameters before (a=9.405 Å, b=5.471 Å, c=4.409 Å) and after annealing, and its structure is confirmed as orthorhombic. Measurements done after an annealing of 15 minutes at 700 °C and for 5 hours at 1000 °C indicate the migration of atoms present in the sample through different phases, which were also identified by Microprobe Analysis (WDS). However we have verified that such migration does not modify the structure. X-ray diffraction measurements have been carried out in conjunction with optical absorption in the UV–Vis as a function of annealing.

Rigid bodies provide a way to simplify the model used in a crystallographic refinement by removing parameters that describe degrees of freedom that are unlikely to change based on chemical experience. The GSAS software package provides a powerful implementation of rigid bodies that allows for refinement of classes of bond lengths, grouping of bodies to further reduce parameterization and where atomic motion can be described from group displacement parameters (TLS) representation. However, use of rigid bodies in GSAS is complex to learn and time-consuming to perform. This paper describes how the rigid body definition process has been simplified and extended through implementation in the EXPGUI interface to GSAS.

A complete set of d spacings, intensities, and h, k, l indexes for Ti2AlN has been determined from X-ray powder diffraction. The lattice parameters are a=2.989(2) Å, c=13.614(5) Å; in good agreement with previous work. The new set of results comprises seven reflections not present in the current Ti2AlN PDF card No. 18-70. Furthermore, a new set of relative intensities are reported that are in better agreement with the calculated values than they are with those listed in the PDF card.

Two XRD specimen holders we designed for use with highly radioactive specimens are described. An injection mold was fabricated to allow inexpensive production of one of the holders. These holders are suitable for single-time use. The ease of use and disposable nature of this holder resulted in a dramatic reduction in personnel exposure and an uncontaminated diffraction unit. A second holder, based on the design of the first, is used to obtain XRD patterns from powders where preferred orientation is an issue and from clays. Both holders result in negligible background, since the specimen is essentially levitated in the X-ray beam. This is a benefit over other methods, such as collodion, that introduce significant background to the XRD pattern.

A well-crystallized sample of powdered KCl has been distributed among several laboratories in order to test the reproducibility of the lattice parameter measurement on different X-ray powder diffraction instruments. The precision of the determined unit-cell dimension is in the 10−5 Å range, while the discrepancies among the results from different laboratories using the same numerical analysis are at least one order of magnitude higher. It is shown that if different numerical analyses, including full pattern refinement, are used, values differing in the third decimal digit are obtained for the same data set.

The General Structure Analysis System (GSAS)-II software package is a fully developed, open source, crystallographic data analysis system written almost entirely in Python. For powder diffraction, it encompasses the entire data analysis process beginning with 2-dimensonal image integration, peak selection, fitting and indexing, followed by intensity extraction, structure solution and ultimately Rietveld refinement, all driven by an intuitive graphical interface. Significant functionality of GSAS-II also can be scripted to allow it to be integrated into workflows or other software. For protein studies, it includes restraints on bond distances, angles, torsions, chiral volumes and coupled torsions (e.g. Ramachandran Φ/Ψ angles) each with graphical displays allowing visual validation. Each amino acid residue (and any ligands) can be represented by flexible rigid bodies with refinable internal torsions and optionally fully described TLS thermal motion. The least-squares algorithm invokes a Levenberg-Marquart minimization of a normalized double precision full matrix via Singular Value Decomposition providing fast convergence and high stability even for a large number of parameters. This paper will focus on the description of the flexible rigid body model of the protein and the details of the refinement algorithm.

Kesterite-type compound semiconductors, containing copper and zinc, have photovoltaic properties depending on cation distribution in the crystal structure. Anomalous diffraction allows discrimination of isoelectronic cations, in principle allowing a straightforward determination of site occupation factors from data collected at multiple energies close to the X-ray absorption edges of copper and zinc. However, extremely strong correlation between structural parameters precludes this. We present a recipe based on the direct dependency between refined occupation factors and atomic scattering power, which allows to lift the correlations and to detect issues of individual diffraction patterns or assumptions in the model, thereby allowing for reliable quantitative analysis of the Cu/Zn distribution.

Internal stresses and textures of electroplated copper films (t=2, 8, 15, 30, 45, and 60) electrodeposited on Al substrates were studied using X-ray diffraction techniques. Results show that the stresses in the films are tensile. The 8 to 60 μm thick films have (220) fiber texture, in good agreement with strain energy minimization calculation. Results also show that a further rotational alignment of the fiber-textured grains was developed, and small amounts of the fiber-textured grains have their (2, −2, 0) planes aligned parallel to the flow direction of the electrodeposited currents. The degree of the rotation alignment increases with film thickness. Values of stress and the degree of texture of copper films were found to be adjustable using an ultrasound technique. Internal stress and the degree of the (220) texture decrease significantly by applying an ultrasound treatment during the electrodeposition process.

We report precision X-ray powder-diffraction (XRD) data of single phase pure Ti2ZrAl. Ti2ZrAl samples were prepared by an arc melting method and annealed at 1000 °C for 30 days. XRD analysis was carried out on these samples and it was found that Ti2ZrAl has a DO19 structure (space group P63/mmc, No. 194). The lattice parameters are found to be a=5.961±0.001 Å and c=4.793±0.001 Å.

As is well known from literature, the grinding process, which is an unavoidable step in sample preparation, may strongly modify the physical properties of chrysotile through amorphisation. The aim of this work is to establish the proper milling time to apply to the samples before an accurate X-ray powder diffraction quantitative analysis. We have used the RIR (reference intensity ratio) analytical method, based on the measurement of the ratio I/Is between the intensity of the strongest line of an analyte and the intensity of the analytical peak of a standard material, when they are thoroughly mixed 50:50 by weight. We have studied how the RIR value changes as a function of the milling time of the sample and how the accuracy of this quantitative method is affected.

Algorithms are presented to correct intensities affected by divergence slit attenuation in the low 2θ region of Bragg–Brentano powder diffractometers with rectangular sample holders. The intensity loss below a limiting angle 2θ1 occurs when the X-ray beam cross section exceeds the sample surface at decreasing angles. For identification purposes, the observed intensities can be scaled up to values comparable with intensities unaffected by divergence slit effects.

The reflection shift δ2Θ caused by a radial shift δr of the sample away from its tangential position at the focusing circle is examined for grazing incidence diffraction and grazing excidence diffraction. Experimental results for residual strain/stress evaluation on thin films using a Bragg–Brentano diffractometer with a grazing incidence equipment are presented. Grazing excidence diffraction is less sensitive to δr than grazing incidence diffraction.

The structure transitions and phase relationships of DyFe3−xAlx compounds have been investigated by X-ray powder diffraction. Our XRD results show that each of the compounds with x≤0.45 crystallizes in the rhombohedral PuNi3-type structure with space group R3¯m and Z=9; for the 0.8≤x<1.0 compounds, each has a hexagonal structure of the CeNi3 type with space group P63/mmc and Z=6; and each of the samples with 0.45<x<0.8 is a two-phase mixture of the PuNi3- and CeNi3-type structures. The calculated XRD intensities of the DyFe3−xAlx compounds with x=0.2, 0.33, 0.4, and 0.45 indicate that Dy occupies the 3a and 6c sites, Fe and Al distribute randomly on the 18h site, and the 3b and 6c sites are exclusively occupied by Fe, which agrees well with those of our experimental XRD patterns. The XRD intensities of the DyFe3−xAlx compounds with x=0.8 and 1.0 have also been calculated and found to agree with the experimental results with Dy on the 2c and 4f sites, Fe and Al at the 12k site, and Fe at the 2a, 2b, and 2d sites. In the two-phase region with x=0.45–0.8, the values of unit-cell parameters and phase compositions are linearly dependent on the value of x, indicating that the two phases are constituted by the same composition x with different stacking arrangements. This abnormal two-phase equilibrium is further confirmed by the structural analysis of the DyFe2.33Al0.67 (or x=0.67) sample. The samples with x=1.1 and 1.2 were also analyzed, and each found to be a mixture of more than two phases.

A unique file structure and search algorithm have been developed for the purpose of obtaining matches between experimental electron diffraction and qualitative energy dispersive X-ray compositional data from an unknown crystalline phase and the reference data in the JCPDS Powder Diffraction File. The reference data for over 32,000 inorganic compounds from sets 1–33 were compressed and stored in binary format as bit pattern maps. The entire data set and searching programs require less than 4 Mbyte and retain the precision appropriate for electron diffraction analysis. The search algorithm, written in both RT-11 FORTRAN and Flextran, is based on pattern matching between bit maps obtained for the unknown and reference compounds for both composition and diffraction data. Special attention is given to double diffraction effects commonly encountered in electron diffraction analysis. The programs run on an interactive basis on a microcomputer dedicated to the X-ray energy dispersive spectrometer on an analytical electron microscope. A typical search takes about 15 seconds to run and extracts about 10–15 different compounds.

A new single-phase copper chromate compound was successfully synthesized by a hydrothermal method and characterized by XRD, SEM, TGA, and XRF analysis. The experimental XRD pattern was analyzed by automatic indexing and the compound was found to be monoclinic with space group P21/a and unit-cell parameters of a=10.1829(11) Å, b=4.9516(6) Å, c=7.2899(7) Å, and β=103.64(1)°. The chemical formula of the copper chromate compound determined by XRF and TGA was determined to be (NH4)1.5Cu2Cr2O8(OH)1.5⋅H2O. XRD results also showed that the synthesized compound decomposed into CuCr2O4 and CuO after being calcined at 600 °C.

The solvent-free conversion of N-carbamoyl-L-proline to hydantoin-L-proline by direct heating at 470 K is reported. A reaction mechanism is proposed based on a nucleophilic intramolecular substitution reaction involving both the lone pair of the NH2 group and the carboxylic acid group of the N-carbamoyl-L-proline. The DSC and TGA experiments show rising of the baselines of the curves prior to melting and decomposition given evidence of the onset of the thermal reaction. NMR experiments were used to identify the product of the reaction, hydantoin-L-proline, whose crystal structure was obtained from X-ray synchrotron powder diffraction data collected on the solidified melt. This compound displays a crystal packing directed by hydrogen bonds forming a layered structure pile up along the c direction.

Crystalline silica is known for its health hazards, and since 1997 has been listed as Group 1, Carcinogenic to Humans, by the International Agency for Research on Cancer. This issue is particularly important in the industrial environment, and there is still no method that allows quantification of the different polymorphs of crystalline silica. Many analytical methods have been proposed, and the major problem in almost all cases is attributable to the very large variety of matrixes encountered. This study evaluates the potential of X-ray diffraction techniques and an automated Rietveld analysis in order to overcome this problem and to adapt the quantitative analysis of quartz, the most prevalent crystalline silica polymorph, to routine analysis in the health and safety environment. Matrix simulations are done and many parameters are optimized. Sample preparation, the acquisition program, pattern treatment, and Rietveld refinement are evaluated, and a general procedure is determined. Automation of Rietveld refinement leads to a significant reduction in analysis time, but cannot be applied to every type of sample.