Shot peening was conducted on [100]- and [111]-oriented monocrystalline nickel-based superalloy samples to study the effect of crystal orientation on the distributions of the residual stress and evolution of microstructures in the deformation layers on the sample surfaces as a function of the coverage up to 400%. The XRD results show that the orientation randomizations and the values of compressive residual stress in the [111]-oriented samples are relatively higher than those in the [001]-oriented samples. Moreover, the residual-stress distribution in each sample is anisotropic, and the residual stress is maximum along the 〈110〉 direction. This phenomenon can be explained by the anisotropic properties of a single-crystal alloy and mechanism of the dislocation slip in the plastic deformation layers. Line profile analysis was also used to obtain microstructural information of the samples.

This work aims to investigate the hydration behavior and structural properties of two dioctahedral smectites with contrasting location charge (beidellite SbId-1 and montmorillonite SWy-2) according to the nature of the bivalent compensator heavy metal cations (i.e. Hg (II), Ni (II), Ba (II) and Mg (II)). This study is achieved using XRD profile modeling approach based on the simulation of the 00l reflection which allowed us to determine structural characteristics along the c* axis related to the nature, abundance, size, position and organization of exchangeable cation and water molecule in the interlamellar space along the c* axis. The obtained results show that a heterogeneous hydration behavior is systematically observed in all studied samples and the structural models, used to fit samples with tetrahedral charge, are more heterogeneous than smectite with an octahedral sheets substitution. In the case of exchanged beidellite specimen, the proposed models are described by a mixed layer structure with variable abundance containing respectively, dehydrated (0W), mono-hydrated (1W) and bihydrated (2W) layers. Whereas, in the case of the montmorillonite, the absence of 0W hydration state is noted.

The application of powder X-ray diffraction (PXRD) for the detection and quantification of low levels of a solid-state chemical impurity, BrettPhos oxide, in an active pharmaceutical ingredient is discussed. It is demonstrated that with appropriate methodology and experimentation, the impurity levels of as low as 0.07% w/w could be detected reliably and limit of quantification of 0.10% w/w could be achieved by PXRD, using a laboratory X-ray source. Method development, validation, and benchmarking using conventional high-performance liquid chromatography are presented in the manuscript highlighting the robustness and reproducibility of such measurements.

Quantitative X-ray diffraction (XRD) analysis is performed on 172 samples mainly containing paleosol sections of Unayzah and Basal Khuff clastics taken from the core of one well drilled by Saudi Aramco. Quantitative XRD bulk mineralogical determination is achieved using the Rietveld refinement method whereas quantitative XRD clay mineralogical determination of clay-size fraction is obtained using the reference intensity ratio method. The XRD results indicate that the samples from paleosol sections consist mainly of quartz and feldspar (microcline and albite) as framework constituents. Cement minerals include dolomite, hematite, anhydrite, siderite, gypsum, calcite, and pyrite. Clay minerals are important constituents in paleosols. The XRD results show that clay minerals in the samples are illite, mixed-layer illite/smectite, kaolinite, and chlorite. No discrete smectite is present in the samples. The clay mineral associations in these samples of paleosol sections can be classified into three types: Type I predominantly consists of illite and a mixed layer of illite/smectite; Type II of kaolinite; and Type III of illite and a mixed layer of illite/smectite, but also significant amounts of kaolinite. The change of clay mineral association type with sample depth can indicate the change of paleoclimate and paleoenvironment. For example, kaolinite usually forms under strongly leaching conditions such as abundant rainfall, good drainage, and acid waters. Therefore, XRD mineralogical data of paleosol sections are important for petroleum geologists to study paleoclimate and paleoenvironment and to predict the reservoir quality of the associated rock formations.

A compilation has been made of the X-ray powder diffraction patterns of the high Tc superconductor and related phases in the systems of Ba-R-Cu-O, Sr-R-Cu-O and Ca-R-Cu-O, where R = yttrium and lanthanides. In addition to the patterns of compounds found in these systems, other related compounds included are cation substitution products of the high Tc phases of Ba2RCu2O6+x, potential reaction products with different types of sample containers, and selected thin-film substrates. The International Centre for Diffraction Data/Powder Diffraction file (ICDD/PDF) coverage includes Sets 1 to 41. A cross correlation of these phases with those reported in Phase Diagrams For Ceramists (PDFC), has also been completed. Results of these efforts are tabulated.

The crystal structure of tin (II) sulphate, SnSO4, was obtained by Rietveld refinement using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data. The structure was refined in space group Pbnm. The unit-cell parameters for SnSO4 are a = 7.12322(1), b = 8.81041(1), c = 5.32809(1) Å, and V = 334.383(1) Å3. The average 〈Sn–O〉 [12] distance is 2.9391(4) Å. However, the Sn2+cation has a pyramidal [3]-coordination to O atoms and the average 〈Sn–O〉 [3] = 2.271(1) Å. If Sn is considered as [12]-coordinated, SnSO4 has a structure similar to barite, BaSO4, and its structural parameters are intermediate between those of BaSO4 and PbSO4. The tetrahedral SO4 group has an average 〈S–O〉 [4] = 1.472(1) Å in SnSO4. Comparing SnSO4 with the isostructural SrSO4, PbSO4, and BaSO4, several well-defined trends are observed. The radii, rM, of the M2+(=Sr, Pb, Sn, and Ba) cations and average 〈S–O〉 distances vary linearly with V because of the effective size of the M2+cation. Based on the trend for the isostructural sulphates, the average 〈Sn–O〉 [12] distance is slightly longer than expected because of the lone pair of electrons on the Sn2+cation.

The dependence of polymer properties on their processing history can be used advantageously. Polyethylene terephthalate (PET), a semi-crystalline polymer, exhibits a microstructure reliant on process and thermal history. PET undergoes strain-induced crystallization, making it sensitive to mechanical stretching. As the level of crystallinity in PET governs its mechanical behavior, it is necessary to quantify the effect of crystallinity and molecular orientation for efficient use. The present research is focused on an approach that will aid in correlating the stretch ratio of PET films to the percent crystallinity and mechanical properties. PET films with different local stretch ratios were obtained through bi-axially stretching injection-molded cylinders of increasing thickness and weight. Percent crystallinity of the PET films with different stretch ratios was measured using X-ray diffraction. Film samples were marked with respect to the stretch directions for measuring their longitudinal (primary stretch direction) and transverse mechanical properties. Local molecular orientation in the form of pole figures was mapped using the (100) plane corresponding to the PET lattice. This will help in linking the physical sample directions and processing to the molecular orientation. Associating the mechanical properties with molecular alignment helps in designing production processes that realize the material's structural potential.

Legislation in the United States and Canada requires labelling of products containing ≥ 0.1 wt.% crystalline silica. Kaolin clays are used in a variety of industries and usually contain low levels of total (i.e., respirable plus non-respirable) quartz, even after beneficiation. X-ray diffraction procedures have been developed here which are suitable for the quantification of total quartz in commercial kaolins with accuracy sufficient to satisfy the legislation. Separation and analysis of the respirable fraction is not addressed in this paper; however, the procedures described would be applicable to such samples if sufficient were available. Use of the 50.1° 2θrather than the 26.6° 26 (CuKα) quartz peak avoids most of the potential problems of overlap with reflections from other accessory minerals. It is shown that profile fitting techniques and optimised experimental procedures allow the determination of quartz in bulk samples to ± 0.03 wt.% (95% confidence) at the 0.1 wt.% level, and ± 0.1 wt.% at the 1.0 wt.% level, with tolerable data collection times.

High-quality powder X-ray diffraction data for a well-characterised natural sample of natrolite (Na2Al2Si3O10.2H2O, space group Fdd2, Z = 8) are presented. Refined cell parameters were a = 18.2984±0.0007 Å, b = 18.6502±0.0008 Å, and c = 6.5589±0.0003 Å. The sample was characterised using thermogravimetric techniques (to determine water content), EPMA and ICP-MS (to determine composition). Available data suggest that the crystal matches the expected stoichiometry of natrolite. Our powder data show close similarity with the proposed structure of natrolite using the Rietveld method, giving R values of 8.54%, and suggest that preferred orientation is not present in the sample.

Complete sets of correction factors for absorption and air scattering effects in X-ray powder diffraction are reported. Both symmetrical reflection and transmission techniques are considered and boundary conditions to be tested for any given value of scattering angles are listed. This may prove particularly useful on coding computer programs for correction of raw intensity data files. Effects of interstitial volume on correction for absorption and subtraction of air scattering were investigated. For samples of high interstitial volume, like loosely packed powders or aerogels, the contribution from air trapped inside the specimen is significant and leads to expressions of the air scattering correction factors different from those commonly reported in the literature.

Single crystals of rhombohedral bismuth tri-iodide grown by physical vapor transport are possible candidates for room-temperature detectors. Previously reported, low angle reflections in X-ray diffraction patterns of various BiI3 starting powders are attributed to the BiI3 structure from Rietveld analysis. Accordingly, the lattice parameters of stoichiometric BiI3 are determined as a0=7.5192±0.0003 Å and c0=20.721±0.004 Å at room temperature. It also appears that lattice parameter determination using Rietveld refinement can lead to significant errors if experimental aberrations are present and their nature and magnitude are unknown. A modified internal standard technique is applied to the data set prior to Rietveld refinement for more reliable lattice parameter determination.

A variable frequency ferroelectric polarisation measurement system has been designed and built at the UK's Diamond Light Source. The electric field induced phase transitions in Pb(Zr1−xTix)O3 (PZT) have been used to test the facility via in-situ measurements of electric polarisation and XRD. Stroboscopic and real time data collection methods on polycrystalline samples were employed as a function of frequency to determine the dynamic ferroelectric response. The system has been shown to deliver XRD patterns of good statistical quality measured over 40 points of a ferroelectric PE loop. The system is now available on station I11 as a user facility at the Diamond Light Source.

The structures and powder X-ray reference diffraction patterns of the “natural superlattice” series Bi1−x Pbx OCuSe (x = 0, 0.02, 0.04, 0.06, 0.08, and 0.10) have been investigated. As the ionic radius of Pb2+ is greater than that of Bi3+, the unit-cell volume of Bi1−x Pbx OCuSe increases progressively from x = 0 to 0.1, namely, from 137.868(5) to 139.172(11) Å3, as expected. The structure of Bi1−x Pbx OCuSe is built from [Bi2(1−x)Pb2x O2]2(1−x)+ layers normal to the c-axis alternating with [Cu2Se2]2(1−x)− fluorite-like layers. Pb substitution in the Bi site of Bi1−x Pbx OCuSe leads to the weakening of the “bonding” between the [Bi2(1−x)Pb2x O2]2(1−x)+ and the [Cu2Se2]2(1−x)− layers. Powder patterns of Bi1−x Pbx OCuSe were submitted to be included in the Powder Diffraction File.

Synchrotron powder diffraction data from beamline 08B1-1 at the Canadian Light Source have been used to examine the structure of curcumin, a prime component of the Asian spice turmeric. Rigid body refinement, with the application of restraints on distances and angles, was performed with the Rietveld software package GSAS yielding monoclinic lattice parameters of a = 12.6967(1) Å, b = 7.198 52(3) Å, c = 19.9533(2) Å, and β = 95.1241(6)° (C21H20O6, Z = 4, and space group P2/n). The refinement was compared with a recent single-crystal structure and ab initio results obtained with density functional theory calculations.

A new micro-X-ray flourescence (XRF) instrument was developed in combination with an atomic force microscope (AFM). A small pinhole of 5 or 10 μm was made on the AFM cantilever. The center of the micro-X-ray beam generated by a polycapillary X-ray lens was passed through the pinhole. The present experiment demonstrated that the size of the original X-ray beam of 48 μm produced by the polycapillary lens was reduced to about 10 μm. This instrument enables both observation of the surface morphology by the AFM and elemental analysis by micro-XRF.

The synthesis and X-ray powder diffraction data for the long-known CaSiF6 and CaSiF6·2H2O species are reported. Their crystal structures have been determined from laboratory powder diffraction data by simulated annealing and full-profile Rietveld refinement methods. CaSiF6·2H2O was found to crystallize in the monoclinic P21/n space group with unit-cell parameters: a = 10.48107(9), b = 9.18272(7), c = 5.72973(5) Å, β = 98.9560(6)°, V = 544.733(8) Å3, and Z = 4. The crystal structure of CaSiF6·2H2O, eventually found to be isomorphous with SrSiF6·2H2O (but not with the Mg analogue—a hexahydrate phase), contains centrosymmetric [Ca(μ-H2O)2Ca]4+ dimers, interconnected by hexafluorosilicate anions, in a dense 3D framework. The crystal structure is completed by a further water molecule, terminally bound to the Ca2+ ion, which, consequently, attains a F5O3 octacoordination. Thermodiffractometric measurements allowed the determination of the linear and volumetric thermal expansion coefficients of CaSiF6·2H2O, which showed a minor contraction, along a, on heating. CaSiF6 is trigonal, space group R-3, a = 5.3497(3), c = 13.5831(11) Å, V = 336.66(5) Å3, and Z = 3, and isomorphous with several other species of MIIAIVF6 or MIAVF6 formulation, among which several silicates, germanates, and stannates.

The structures of anhydrous nickel, niobium, and tantalum chlorides have been investigated in situ in acidic and basic ionic liquids (ILs) of 1-methyl-3-ethylimidazolium chloride (EMIC)/AlCl3 with X-ray absorption spectroscopy (XAS). The coordination of NiCl2 changes from tetrahedral in basic solution to octahedral in acidic solution. The NiCl2 is a strong Lewis acid in that it can induce the AlCl3 to share its chlorides in the highly acidic IL, forming a structure with six near Cl− ions and eight further distant Al ions which share the chloride ions surrounding the Ni2+. When Nb2Cl10, a dimer, is added to the acidic or basic solution, the dimer breaks apart and forms two species. In the acid solution, two trigonal bipyramids are formed with five equal chloride distances, while in the basic solution, a square pyramid with four chlorides forming a square base and one shorter axial chloride bond. Ta2Cl10 is also a dimer and divides into half in the acidic solution and forms two trigonal bipyramids. In the basic solution, the dimer breaks apart but the species formed is sufficiently acidic that it attracts two additional chloride ions and forms a seven coordinated tantalum species.

X-ray powder diffraction investigation of the new high temperature polymorphs beta- and gamma-CaTeO3 and gamma- and delta-CaTe2O5 and picnometric measurements of the room temperature phases of the two compounds have been carried out. The study led to the elucidation of their unit cell structures and assignment of entirely new lattice types and parameters to the room temperature phases of CaTeO3 and CaTe2O5 in contrast and supersession to the existing structural information. The results are as follows: CaTeO3 has only one stable phase at room temperature and temperatures up to 882 °C, i.e., α- and has a triclinic unit cell with a=4.132±0.003 Å, b=6.120±0.006 Å, c=12.836±0.013 Å, α=121.80°, β=99.72°, γ=97.26°. The first high temperature phase stable between 882 and 894 °C, i.e., β-CaTeO3, has a monoclinic lattice: a=20.577±0.007 Å, b=21.857±0.009 Å, c=4.111±0.002 Å, β=96.15°, while the next phase stable above 894 °C, i.e., γ-CaTeO3, has a hexagonal unit cell with parameters: a=14.015±0.0001 Å, c=9.783±0.001 Å, c/a=0.698. CaTe2O5 has one stable phase at temperatures up to 802 °C, i.e., α-CaTe2O5 with a monoclinic lattice and parameters: a=9.069±0.002 Å, b=25.175±0.007 Å, c=3.366±0.001 Å, β=98.29 °. The first high temperature phase stable in the range 802–845°, i.e., β-CaTe2O5, is monoclinic with unit cell parameters: a=4.146±0.001 Å, b=5.334±0.002 Å, c=6.105±0.002 Å, β=98.362 °; the next higher temperature phase stable over 845–857 °C, i.e., γ-CaTe2O5, has an orthorhombic unit cell with: a=8.638±0.001 Å, b=9.291±0.001 Å, c=7.862±0.001 Å and the highest temperature solid phase stable above 857 °C, i.e., δ-CaTe2O5 has a tetragonal unit cell with a=5.764±0.000 Å, c=32.074±0.020 Å, c/a=5.5637.

Time-resolved synchrotron powder diffraction was used to follow the thermal transformation of cement-asbestos. Thermal transformation of asbestos fibers into nonfibrous crystalline phases is a promising solution for the elimination of these hazardous minerals. Time resolution offered by the use of an imaging plate detector with a high-brightness X-ray source allowed for the observation of metastable phases, commonly not detectable with conventional instrumentation. In addition, the use of a closed capillary as a sample holder mimicked the real, novel industrial reactor where cement-asbestos slates are sealed in a tunnel kiln. The changing gas atmosphere in the closed system was shown to affect the final composition of the recrystallized product. This study demonstrates the importance of advanced powder diffraction techniques in this field of applied research.

The formation and decomposition of silico-ferrite of calcium and aluminium (SFCA) and SFCA-I iron ore sinter bonding phases have been investigated using in situ synchrotron and laboratory X-ray diffraction (XRD) and neutron diffraction (ND). An external standard approach for determining absolute phase concentrations via Rietveld refinement-based quantitative phase analysis is discussed. The complementarity of in situ XRD and ND in characterising sinter phase formation and decomposition is also shown, with the volume diffraction afforded by the neutron technique reducing errors in the quantification of magnetite above ~1200 °C. Finally, by collecting 6 s laboratory XRD datasets and using a heating rate of 175 °C min−1, phase formation and decomposition have been monitored under heating rates more closely approximating those encountered in industrial iron ore sintering.