LiCu2O2 crystals grown by spontaneous crystallization from the fluxed melt were studied by powder X-ray diffraction. The phase analysis shows that the applied growth conditions are suitable for preparation of a single-phase compound. The as-grown crystals contain only traces of foreign phases (Li2CuO2, CuO, Cu2O) typical for preparation of the LiCu2O2 compound. Attempts to anneal or quench the as-grown crystals led to two-phase samples containing LiCu2O2 and LiCu3O3. X-ray powder diffraction pattern of a LiCu2O2 crystal is reported and compared with literature data. The crystal structure is orthorhombic, space group Pnma, in agreement with literature data. Lattice parameters of the studied sample are a=5.7286(2) Å, b=2.8588(1) Å, and c=12.4143(3) Å. Time evolution of a diffraction pattern illustrates a slow increase of the secondary-phases contribution assumed to be due to interaction of the powdered crystal with humid air. A brief summary of compounds known in the Li–Cu–O system is included

Powder X-ray diffraction data for methionine sulfoxide, C5H11NO3S, obtained from the commercial amino acid, are presented in this work. Monoclinic cell parameters are: a=15.500 Å; b=3.820 Å; c=13.490 Å; β=97.300 °.

The crystal structure of the layered cadmium hydroxide sulfate Cd4SO4(OH)6.1.5H2O has been solved from X-ray powder diffraction data. The compound crystallizes with hexagonal symmetry, a=9.145(1) Å, c=15.099(3) Å, V=1093.5 Å3, Z=4, space group P63. Due to the unusual environment of one cadmium atom and to the fact that a suitable thin tabular crystal could be found later, a single-crystal X-ray diffraction experiment was also carried out. In both cases the structure was solved applying direct-methods. The refinements converged to the residual factors Rwp=0.152 and RF=0.059 from the powder data and R1=0.058 and wR=0.165 for the single crystal data case. The structure is built from brucite-type layers based on CdO6 octahedra, in which one-seventh of the octahedral sites are empty. Directly above and below these empty sites, two additional octahedrically coordinated Cd atoms are located. The crystal chemistry of the cadmium hydroxide sulfate family is discussed.

Retained austenite is an important characteristic of properly heat-treated steel components, particularly gears and shafts, that will be subjected to long-term use and wear. Normally, either X-ray diffraction or optical microscopy techniques are used to determine the volume percent of retained austenite present in steel components subjected to specific heat-treatment regimes. As described in the literature, a number of phenomenological, experimental, and calculation factors can influence the volume fraction of retained austenite determined from X-ray diffraction measurements. However, recent disagreement between metallurgical properties, microscopy, and service laboratory values for retained austenite led to a re-evaluation of possible reasons for the apparent discrepancies. Broad, distorted X-ray peaks from un-tempered martensite were found to yield unreliable integrated intensities whereas diffraction peaks from tempered samples were more amenable to profile fitting with standard shape functions, yielding reliable integrated intensities. Retained austenite values calculated from reliable integrated intensities were found to be consistent with values obtained by Rietveld refinement of the diffraction patterns. The experimental conditions used by service laboratories combined with a poor choice of diffraction peaks were found to be sources of retained austenite values containing significant bias.

An organic adduct nonlinear optical material m-nitrobenzoic acid⋅diethanolamina (C11H16N2O6) has been characterized by X-ray powder diffraction. Experimental values of 2θ corrected for systematic errors, relative peak intensities, values of d, and the Miller indices of 56 observed reflections are reported. The powder diffraction data have been evaluated, and the figure of merit was found to be F30=57.9 (0.0108, 48). The unit cell parameters were refined by a least-squares fit with a Cc space group and a=22.973(5) Å, b=4.6657(6) Å, c=15.023(3) Å, β =124.45(1)°, V=1327.75 Å3; Z=4, Dx=1.37 g/cm3. The powder diffraction results are in agreement with those obtained from single crystal structure data.

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.

Palmierite (K2Pb(SO4)2) has been prepared via a chemical synthesis method. Intensity differences were observed when X-ray powder data from the newly synthesized compound were compared to the published powder diffraction card (PDF) 29-1015 for Palmierite. Investigation of these differences indicated the possibility of preferred orientation and/or chemical inhomogeneity affecting intensities, particularly those of the basal (00l) reflections. Annealing of the Palmierite was found to reduce the effects of preferred orientation. Electron microprobe analysis confirmed K:Pb:S as 2:1:2 for the for the annealed Palmierite powder. Subsequent least-squares refinement and Rietveld analysis of the annealed powder showed peak intensities very close to that of a calculated Palmierite pattern (based on single crystal data), yet substantially higher than many of the PDF 29-1015 published intensities. Further investigation of peak intensity variation via calculated patterns suggested that the intensity discrepancies between the annealed sample and those found in PDF 29-1015 were potentially due to chemical variation in the K2Pb(SO4)2 composition. X-ray powder diffraction and crystal data for Palmierite are reported for the annealed sample. Palmierite is trigonal/hexagonal with unit cell parameters a=5.497(1) Å, c=20.864(2) Å, space group R-3m(166), and Z=3.

The effects of proper drying and grinding of [Fe(Htrz)3](ClO4)2⋅1.85H2O specimens on the quality of X-ray powder patterns are illustrated (Htrz=1H-1,2,4-Triazole). A procedure is suggested to achieve high-quality, reproducible X-ray powder patterns of the compound. The observed powder diffraction data of the compound are reported together with preliminary indices calculated for a monoclinic system with cell parameters a=15.8160 Å, b=20.6134 Å, c=13.0321 Å, β=103.83° and Volume=4125.633 Å3, with reliability factors: M15=10.4, F15=22.0 (0.0100; 68) and space group P21/m. This compound is very similar to the compound [Cu(Hyetrz)3](ClO4)2⋅3H2O and a comparison is made between the cell parameters of the two compounds

Powder diffraction data and refined unit cell parameters of two palladium borides were determined. For Pd3B (space group Pnma; Fe3C type) it was found that a=0.54602(3) nm, b=0.75596(4) nm, c=0.48417(4) nm and for Pd5B2 (space group C2/c; Mn5C2 type) a=1.27759(12) nm, b=0.49497(5) nm, c=0.54704(4) nm, β=97.049(7)°. Further, it was shown that the position of the principal scattering peak of the amorphous Pd2B fulfils the Nagel–Tauc criterion about glass forming ability.

The structure of the new Y0.8Ca0.2Ba1.8La0.2Cu3Oy (YBLCO) compound was obtained at 298 K from X-ray powder diffraction data and refined by the Rietveld technique. YBLCO has a structure isotypical with YBa2Cu3Oy (YBCO) at room temperature. The crystal data are: Y0.81Ca0.19Ba1.8La0.2Cu3O7.08, Mw=657.69, orthorhombic system, space group Pmmm, a=3.8731(1) Å, b=3.8249(1) Å, c=11.6602(3) Å, V=172.740(13) Å3, Z=1, dx=6.325 g/cm3; the structure was refined with 37 parameters to Rwp=7.66%, Rp=5.86%, and Rexp=5.11% for 2001 data points. Moreover, the proportions of Ca and La were refined to be 0.19 and 0.2, in agreement with the stoichiometric proportion of 0.2.

Two adducts (NH2CH2COOH)3⋅H2BeF4(TGFb) and (NH2CH2COOH)3⋅H2SeO4(TGSe) were obtained and characterized by X-ray powder diffraction. The samples were indexed using the TREOR program [Werner, Z. Kristallogr. Kristallogeom. Kristallphys. Kristallchem. 120, 375–387 (1964)] on a monoclinic unit cell. The lattice parameters of adducts TGFb and TGSe were refined by a least-squares method using the Lattice Constant Refinement Program of the Rikagu software. The refined lattice parameters are a=9.1589(9) Å, b=12.6204(13) Å, c=5.6966(8) Å, β=105.451(9)° for TGFb. The Smith and Snyder figure [Smith and Snyder, J. Appl. Crystallogr. 12, 60–65 (1979)] is F30=39.4(0.0141,54). The refined lattice parameters a=9.5063(11) Å, b=12.8281(10) Å, c=5.8682(7) Å, β=110.353(77)° for TGSe. The Smith and Snyder figure is F30=39(0.0106,73). The powder diffraction results are in agreement with those obtained from single crystal structure data.

Si–SiC composite (reaction bonded SiC) with a submicron SiC microstructure (starting SiC particle size: 0.22 μm) was examined by XRD analysis to determine the amount and phase composition of the secondary SiC formed by the reaction between silicon and carbon during the sintering process. It was found that the secondary SiC has grown onto the original hexagonal α-SiC grains as well as into the porosity of the green body. An increase of 3C–SiC was found within the microstructure after infiltration (from 2.6 wt. % before infiltration to 8.8 wt. % after infiltration) whereas the 4H-ploytype content was reduced. This behavior may be explained by the very small original SiC grains which acted as seeds for disoriented SiC growth and were assumed to force the nonepitaxically deposition of secondary SiC. Solid state and fast transportation processes caused the observed transformation of the SiC. Examinations of the silicon source (infiltrant) after the infiltration procedure showed that most of the carbon was converted to SiC with cubic modification (3C stacking sequence)

Improved powder X-ray diffraction (XRD) data for franzinite, the ten-layer member of the cancrinite group of minerals, were obtained using an automated parallel-beam powder diffractometer with a capillary mount. The cell parameters of franzinite were found to be a=12.8976(3) Å, c=26.5040(8) Å, V=3818.2(2) Å3 in space group P321, while the strongest reflections were at 3.725(100), 3.809(65), 3.562(56), 3.586(55), 2.662(42), 2.150(31) and 3.302(30) Å. The new results include an increased number of indexed peaks, improved figures-of-merit with respect to PDF 30-1170 and intensities validated by Rietveld refinement.

X-ray powder diffraction data for the orthorhombic natural amino acid djenkolic acid, C7H14N2O4S2, is described in this paper. The orthorhombic cell parameters are: a=8.12 Å, b=12.16 Å, and c=5.38 Å

Calcium hydroxyapatite (Ca10(PO4)6(OH)2) whiskers were prepared by using the technique of molten salt synthesis with the fluxing agent of potassium sulphate (K2SO4). A tentative x-ray diffraction (XRD) pattern was suggested for the produced whiskers. Phase purity, composition, and morphology of the whiskers were investigated by powder XRD, inductively coupled plasma-atomic emission spectroscopy, Fourier transform infrared spectroscopy, and scanning electron microscopy, respectively.

Ba0.5Sr0.5TiO(C2O4)2·5H2O, which is used as a precursor for Ba0.5Sr0.5TiO3 (BST), has been characterized by X-ray powder diffraction. In accordance with the known structure of BaTiO(C2O4)2·yH2O, the crystal system was found to be monoclinic with unit cell parameters: a=1.3965(1) nm, b=1.3811(2) nm, c=1.3306(2) nm, and β=92.15(1)°. The space group is P21/n, ρ=2.292(2) g cm−3, and Z=8.

Powder X-ray diffraction data are reported for RE6UO12 (RE=Eu, Gd, and Dy). The powders were prepared by a solution combustion method using urea as fuel. All compositions exhibit a rhombohedral structure with hexagonal unit cell parameters of a=1.012 67 (9) nm, c=0.9601 (1) nm for Eu6UO12; a=1.008 78 (6) nm, c=0.954 24 (7) nm for Gd6UO12; and a=0.998 06 (7) nm, c=0.944 03 (8) nm for Dy6UO12. The diffraction patterns of all the compounds are indexed on the R3¯ space group with Z=3. The a and c values decrease with increasing atomic number of the rare earth ion.