The method of high-energy total elastic X-ray scattering to determine the atomic structure of nanocrystalline, highly disordered, and amorphous materials is presented. The current state of the technique, its potential, and limitations are discussed with two successful studies on the pressure induced phase transition in mackinawite (FeS) and the high-pressure behavior of liquid gallium.

Crystal structures of (NH4)2KWO3F3 at 298 K and 113 K were solved from X-ray powder diffraction data and refined by the Rietveld technique. The compound is isostructural with elpasolite K2NaAlF6 at room temperature with space group Fm-3m, a=8.95850(5) Å, V=718.961(7) Å3, Z=4, Dx=3.363 g/cm3, and MW=364.02. The structure was refined over 18 parameters to Rwp=12.6%, Rp=10.9%, Rexp=5.03%, and RB=3.27% from 40 independent reflections. (NH4)2KWO3F3 was transformed upon cooling to a ferroelastic monoclinic phase with space group P21/n, a′=6.3072(3) Å, b′=6.3028(3) Å, c′=8.9882(3) Å, β′=90.242(2)°, V=357.30(3) Å3, Z=2, and Dx=3.383 g/cm3. The low-temperature structure at 113 K was refined over 28 parameters to Rwp=20.9%, Rp=21.3%, Rexp=12.5%, and RB=6.93% from 453 independent reflections.

High-precision unit-cell parameters for the TiO2 polymorphs anatase and rutile at temperatures between 300 and 575 K have been determined using Rietveld analysis of synchrotron powder XRD data. Polynomial models were used to express the tetragonal unit-cell parameters as a function of absolute temperature, with a (anatase)=1.759 37×10−8×T2+6.418 16×10−6×T+3.779 84, c (anatase)=6.6545×10−8×T2+4.0464×10−5×T+9.4910, V (anatase)=2.237 58×10−6×T2+1.027 77×10−3×T+135.602, a (rutile)=−6.636 42×10−11×T3+1.005 01×10−7×T2−1.009 9310−5×T+4.586 34, c (rutile)=−4.115 50×10−11×T3+6.405 94×10−8×T2+4.675 61×10−7T+2.951 81, and V (rutile)=−2.7790×10−9×T3+4.2386×10−6×T2−3.3551×10−4×T+62.100. The polynomial expressions were used to calculate linear (α) and volume (β) thermal expansion coefficients of anatase and rutile between 300 and 575 K. At 298.15 K, these values were αa=4.46943×10−6 K−1, αc=8.4283×10−6 K−1, and β=17.3542×10−6 K−1 for anatase, and αa=6.99953×10−6 K−1, αc=9.36625×10−6 K−1, and β=28.680×10−6 K−1 for rutile.

Nanocrystallized oxide precursors of colored (oxy)nitrides related to the system Yb-(Zr-W)-O have been successfully prepared using a chimie douce process—the amorphous citrate route. The process involves first a formation of fine and homogeneous powdered solids obtained by calcination at 600 °C, a temperature much lower than that of the conventional solid-state method. At this stage, the X-ray diffraction patterns exhibit large line broadening effects. Finally, two well-crystallized and pure quaternary oxides have been readily obtained by heating and under annealing conditions at 850 and 900 °C for 12 h. For one of the patterns, all the X-ray diffraction lines can be easily indexed to a cubic phase with the fluorite structure conforming to the Fm3m space group [Yb2Zr1.21W0.41O6.65◻1.35 called C-phase: a=5.1864(2) Å]. The second phase adopts the sheelite-type structure [Yb2ZrWO8 called T-phase: space group I41/a, a=5.1584(5), and c=10.8246(6) Å]. By taking into account the present compositions determined by EDS measurements, Rietveld structure refinements produce final RB factors of 0.015 and 0.044, and Rwp factors of 0.069 and 0.089, respectively. In order to characterize the microstructure of the materials (crystallite size and lattice distortion) at the nanometer scale, a study based on diffraction line broadening analysis applying the whole pattern refinement method was also undertaken with confidence. The results show smooth angular variations of the values of FWHMs, indicating that the microstructural properties are isotropic for the cubic and tetragonal oxides. More precisely, the results indicate that whatever the profile fitting approach used (“profile matching” procedure and Rietveld method), the reliability factors Rwp are systematically better with a combined size strain than with zero strain considerations. The strain magnitudes observed for the C-phase-850 °C as well as for the T-phase-900 °C should be viewed as realistic strain.

We report on the use of a microcalorimeter X-ray detector with a transition edge sensor in an electron probe to perform quantitative analysis. We analyzed two bulk samples of multielement glasses that have been previously characterized by chemical methods for use as standard reference materials. The spectra were analyzed against standards using three different correction schemes. In one of the standards, the reference line was easily resolved despite its proximity within 45 eV of another line. With the exception of direct measurements of oxygen (a particularly challenging element), the results are in agreement with the certified characterization to better than 1% absolute or 8% relative. This demonstrates the potential of microcalorimeter detectors as replacements for conventional energy dispersive detectors in applications requiring high energy resolution.

Polycrystalline TiN/SiNx multilayer coatings were deposited by reactive magnetron sputtering from Ti and Si targets. Interfaces, structures, and mechanical properties of the multilayers were characterized using X-ray reflectivity (XRR), X-ray diffraction (XRD), and nanoindentation analyses. Results showed that substrate bias voltage had a significant influence on the structures and mechanical properties of the multilayer coatings, in which sharp interfaces are responsible for an enhancement of mechanical properties of the multilayer coatings. The maximum hardness occurs at the −80 V coating with the sharpest interface and the strongest [200] preferred orientation.

The diffraction pattern of nanocrystalline Ce0.9Zr0.1O2 was analyzed by whole powder pattern modeling, a recently proposed method for the study of line broadening. The main result in this typical case of study—the crystalline domain size distribution—matches closely the corresponding information obtained by transmission electron microscopy. Further information on nature and content of lattice defects is also discussed.

The growth temperature dependence of the InN film’s crystalline quality is reported. InN films are grown on sapphire substrates from 570 to 650 °C with low-temperature GaN buffers by metalorganic vapor phase epitaxy (MOVPE). The X-ray rocking curves and reciprocal space mappings of the symmetric reflection (0 0 0 2) and asymmetric reflection (1 0 1 2) are measured with high resolution X-ray diffraction. The results indicate that the crystallinity is sensitive to the growth temperature for MOVPE InN. At growth temperature 580 °C, highly crystalline InN film has been obtained, for which the full-width-at-half-maxima of (0 0 0 2) and (1 0 1 2) rocking curves are 24 and 28 arcmin, respectively. The crystalline quality deteriorates drastically when the growth temperature exceeds 600 °C. Combined with the carrier concentration and mobility, the approach to improve the quality of InN film by MOVPE is discussed.

A short history of the developments of the successive dichotomy method for powder pattern indexing is presented. In the first computer powder indexing programs (P1 and P2), only high lattice symmetries, down to orthorhombic, were considered [Louër and Louër, J. Appl. Crystallogr. 5, 271–275 (1972)]. Later on, an extension to the monoclinic symmetry was reported in DICVOL, including a partition of the volume space to first search solutions with smaller unit cell volumes [Louër and Vargas, J. Appl. Crystallogr. 15, 542–545 (1982)]. However, CPU times were slow in some monoclinic examples. A thorough mathematical analysis resulted in a significant optimization of the CPU times [Boultif and Louër, J. Appl. Crystallogr. 24, 987–993 (1991)]. Simultaneously, the method is extended to triclinic lattices. The stages of development of the various versions of the DICVOL program are described, with a particular emphasis on DICVOL91 (Boultif and Louër, 1991) and DICVOL04 [Boultif and Louër, J. Appl. Crystallogr. 37, 724–731 (2004)]. This article is written to testify to and emphasize the major role played by Daniel Louër, who introduced the successive dichotomy method and continued to its evolution and optimization over almost 40 years.

X-ray powder diffraction technique and the Rietveld refinement method have been used successfully for the qualitative and quantitative analyses of Pingguo bauxite from Guangxi, China. Qualitative phase analysis shows that the Pingguo bauxite contains diaspore (AlOOH), hematite (Fe2O3), goethite (FeOOH), anatase (TiO2), and kaolinite (Al2(Si2O5)(OH)4). Quantitative Rietveld refinement shows that the weight concentrations of diaspore, goethite, hematite, anatase, and kaolinite for the Pingguo bauxite are 71.9(4)%, 7.0(8)%, 11.3(7)%, 6.5(6)%, and 3.3(9)%, respectively.

X-ray powder diffraction data collected for the complex silver(I) cyclamate [Ag(C6H12NO3S)] are reported. This material was obtained from a stoichiometric mixture of sodium cyclamate and AgNO3. The analysis of the data using the Le Bail method showed that the complex has monoclinic symmetry (space group C2/c). The unit cell parameters are a=31.85852(16) Å, b=6.25257(6) Å, c=8.46165(7) Å, and β=95.7651(5)°.

The versatility of confocal micro X-ray fluorescence (MXRF) in analyzing thin films on semiconductor wafers is demonstrated. Unlike conventional MXRF, confocal MXRF can depth profile sample layers and reduce spectral background. Nondestructive quantification of the silicon dioxide concentration in hafnium silicate thin films is an example of one application demonstrating the advantage of confocal MXRF. Additionally, the growth of titanium nitride films on various high-k gate dielectric substrates was analyzed with confocal MXRF due to its ability to detect sub-nm film thickness changes.

A new compound Th0.9Ce0.1SiO4, iso-typic to zircon, was prepared by heating predried ThO2, CeO2, and SiO2 (in the mole ratio 0.9:0.10:1.0) by a two-step heating protocol. The polycrystalline sample obtained was characterized by Rietveld refinement of the observed neutron diffraction data with the starting model of tetragonal ThSiO4. It has a body centered tetragonal structure with space group I41∕amd and four formula units per unit cell. The unit-cell parameters are a=7.1238(4) Å and c=6.3186(95) Å. The RP, Rwp, and Re factors are 7.77%, 10.9%, and 4.85%, respectively. The incorporation of about 10 mol % cerium was used to stabilize the tetragonal modification of ThSiO4.

The painting materials and drawing techniques of a pair of two-panel folding screens entitled Red and White Plum Blossoms by Ogata Korin, a national treasure in Japan, were investigated directly and nondestructively by XRF, X-ray radiography, and high resolution digital imaging. Several assumptions were made about the materials used in the red and white plum trees drawn on the right and left screens, respectively, and the river drawn at the center. By the present investigation, the materials used for the paintings were revealed, and some of them contradicted what have been previously believed.