Rietveld refinement using neutron, laboratory X-ray, and synchrotron powder diffraction data of NIST SRM clinker 8488 was performed. Quantitative phase analysis (QPA) results were compared between data, and with other studies. QPA results for the main phases in the clinker were found to be in agreement between the different data used here, and in and other studies, although the QPA of the tricalcium silicate polymorphs was shown to be inconsistent. The QPA results for the tricalcium aluminate phase varied between data types, and the neutron data were unable to distinguish this phase.

The technique of standard addition in combination with powder X-ray diffraction was used to identify and quantify the amount of Ln3+ segregating into secondary phases from Ln3+doped alkaline earth aluminates. Results indicate that Ln3+ ions are more soluble in CaAl2O4 than SrAl2O4 and BaAl2O4, with this being rationalized by the structural details of the A sites. These results indicate that the enhancement of the luminescence afterglow obtained by doping AAl2O4:Eu2+ samples with Ln3+ ions is a result of much lower doping levels than previously thought.

Low energy characteristic X-ray emission from Al2O3 monocrystalline specimens is measured under bombardment of 100 keV Xe+ ions. The electric field influence on emission of the X-rays of constitute elements in the specimens was investigated. The energy dispersive X-ray spectroscopy spectra show that the characteristic X-ray of Al-Kα seems to be depressed by the applied dc voltages, while the peak intensity of O-Kα was not notably influenced. The O-Kα peaks were broadened and the total counts increased as a higher dc bias was applied. It is possible that a dc electric field parallel to the target surface may influence the X-ray emission from it under ion bombardment.

Characterization of materials used in the digital imaging industry has been performed using micro X-ray diffraction (microXRD) techniques. Case studies are described that demonstrate the use of microXRD for identification of phases, texture, and microstructure morphology of components used in imaging applications.

The structural models of three synthetic Al-substituted goethite specimens have been refined from the neutron data, including crystallographic determinations of the Al levels and H positions. The d-I data were calculated for the final models. A relationship between the c unit cell parameter and Al content has been extended to the entire goethite-diaspore solid-solution system, which makes the regression equation procedure simpler and more accurate. A second prospective H site could not be confirmed because of the quality of existing neutron data. However, it is hoped that a further neutron powder diffraction study of a synthetic, fully deuterated goethite material may allow the existence of the site to be demonstrated.

New layered bismuth oxides Bi2(BiCaNa)m−1NbmO3m+3(m=2-4) with the Aurivillius type phase were successfully synthesized. The structures of the compounds have been studied by X-ray powder diffraction and refined by the Rietveld method. Bi2.25Ca0.5Na0.25Nb2O9(m=2) has an orthorhombic crystal structure with lattice constants a=5.4478(1) Å;b=5.4770(2) Å;c=24.883(8) Å, space group A21am (No. 36). Bi2CaNaNb3O12 and Bi2.25Ca0.5Na1.25Nb3O12(m=3) are orthorhombic with Fmmm(No. 69) space group and the unit-cell parameters a=5.4473(7) Å, b=5.4770(3) Å, c=32.722(6) Å and a=5.4574(7) Å, b=5.4884 (3) Å, c=32.711(6) Å, respectively. The structure of Bi2CaNa2Nb4O15(m=4) was found to be orthorhombic with parameters a=5.4584(8) Å, b=5.4833(3) Å, c=40.534(1) Å and was refined in the space group A21am (No. 36).

The lattice parameters of α-alumina have been determined for temperatures in the range 20<T<1050 °C, using the lattice parameter of tungsten as a thermometer and a simple furnace in the diffractometer on the Australian beamline at the Photon Factory, Tsukuba, Japan. It is shown that the accuracy of this technique for measurement of cell parameters at temperatures up to ∼1200 °C is limited at present by uncertainty in the cell parameters of the reference material (i.e., tungsten) at high temperatures. Some problems with the equipment are discussed.

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.

Structural development of BPDA-PPD polyimide thin film has been investigated by in situ grazing incidence X-ray diffraction at the BL24XU beamline of the SPring-8. Optimizing the sample shape, two-dimensional images were measured successfully without sacrificing angle resolution. It has been clearly shown that the crystallization first begins in the in-plane direction, at the curing temperature of 180 °C, in which the periodic structure of the molecular chain axis (c axis) is developed. The crystallization in the surface normal (out-of-plane) direction is observed later, at the curing temperature above 300 °C. A slight increase of the d spacing of the c axis during heating process has been observed, suggesting the stretching of the contracted molecular chain in accordance with the curing process. In the cooling process, the decrease of the d spacings for a and b axes was considerable, which indicates thermal expansion of the crystals at high temperatures. The increases in the peak intensities during the cooling process have been observed, which indicate the d spacing of each axis becomes close to the equilibrium value to produce higher periodicity.

We have fabricated a bifocal miniature toroidal mirror that horizontally and vertically focuses to two different locations to provide a smaller footprint of the beam for grazing-incidence wide-angle scattering (GIWAXS), while at the same time focusing the beam in the horizontal direction on the detector to further enhance the angular resolution. At CHESS we traditionally use glass single-bounce monocapillary optics for a wide range of X-ray experiments to get a fine X-ray beam of 5 to 20 μm. This miniature toroidal mirror was prepared by designing and fabricating an X-ray focusing capillary in which the sagittal and meridional focusing is decoupled and only a quadrant of the accepted annulus is used for focusing the beam. The mirror produced a 120 μm horizontal by 25 μm vertical focus at 50 mm from the tip of the optic and a 44 μm horizontal by 70 μm vertical focus at 150 mm from the tip of the optic.

The α, β, γ, and δ polymorphs of Y2Si2O7 were synthesized using sol-gel and solid-state methods. The structures of the α and γ polymorphs were determined by identification of isostructural rare-earth disilicates, and the structures were refined using Rietveld analysis of X-ray powder diffraction data. The α polymorph crystallizes in space group P1, with a=6.5872(6) Å, b=6.6387(7) Å, c=12.032(1) Å, α=94.501(7)°, β=90.984(8)°, γ=91.771(7)°, and volume=524.16(9) Å3. The γ form is described by space group P21/c, a=4.68824(5) Å, b=10.84072(9) Å, c=5.58219(6) Å, and γ=96.0325(3)°. The anisotropic thermal expansion of each phase was measured using high temperature diffraction up to 1200 or 1400 °C, depending on the stability of the polymorph. The thermal expansion is highly anisotropic for all polymorphs, with the low-expansion direction normal to the long axis of the corner-shared SiO4 tetrahedra.

The crystal structure of the mineral strontiodresserite, (Sr,Ca)Al2(CO3)2(OH)4⋅H2O, from the Francon Quarry, Montreal, Quebec, Canada, has been solved from laboratory powder diffraction data using a combination of charge-flipping and simulated annealing methods. The structure is orthorhombic in space group Pnma with a=16.0990(7), b=5.6133(3), and c=9.1804(4) Å (Z=4) and the framework of the mineral is isostructural with that of dundasite. The strontium has a coordination number of 9 and the carbonate anions form a bridge between the SrO9 polyhedra and AlO6 octahedra. The water molecule lies in a channel that runs parallel to the b axis. An ordered network of hydrogen atoms could be uniquely determined from crystal-chemical principles in the channels of strontiodresserite. Ab initio density functional theory (DFT) energy minimization of the whole structure gave results in full agreement with X-ray refinement results for nonhydrogen atoms. The stability of this model (as well as that of the corresponding model of dundasite) in the proposed Pnma space group was tested by DFT optimization in space group P1 of random small distortions of this structure. This test confirms that both minerals are isostructural, including their hydrogen-bond networks.

Five new derivatives of N-(ω-hydroxyalkyl)-4-chlorophenoxyacetamide [namely, 2-(4-chlorophenoxy)-N-(2-hydroxyethyl) acetamide, 2-(4-chlorophenoxy)-N-(3-hydroxypropyl) acetamide, 2-(4-chlorophenoxy)-N-[1-(hydroxymethyl) propyl] acetamide, 2-(4-chlorophenoxy)-N-(2-hydroxy-1,1-dimethylethyl) acetamide, and 2-(4-chlorophenoxy)-N-{2-[(2-hydroxyethyl) amino] ethyl} acetamide] and one 2-(4-chlorophenoxy) acetohydrazide have been characterized by X-ray powder diffraction. These organic compounds are potential pesticides. New diffraction data including experimental and calculated 2θ peaks positions, values of d, experimental relative peak intensities, and Miller indices as well as unit-cell parameters are reported.

This paper presents a nondestructive measurement technique for the determination of the film thicknesses of Co and SmCo based magnetic films deposited by sputtering on single-crystal silicon (100) substrates. X-ray diffraction of Cu Kα radiation has been used to measure the intensity of the (400) reflection from bare silicon substrates and as attenuated by sputter coated Co and SmCo based films on Si substrates. A four-axis research diffractometer allowed the substrate orientation to be fine adjusted to maximize the (400) diffraction intensity. The thickness of SmCo based films was in a range from 0.05 to 5 μm. Co film thicknesses on Si could be measured to a few tens of nanometers. The accuracy of the thickness measurements depends on the effective mass attenuation coefficient of the film material. For the materials considered, the thicknesses determined by the X-ray attenuation method agree within at least several percent to values determined by other methods.