A practical description of the mathematics required to implement the hexagonal grid and spiral trace pole figure data collection schemes is presented. Applying the concepts of stereographic and equal area projections with geometry, spreadsheets were created to calculate the angular settings of the goniometer. Using the generated settings, the hexagonal grid and spiral trace schemes were programmed into the existing X-ray software and employed to collect data for a sample of aluminum foil. The resulting (111) pole figures were similar to those collected with the conventional 5°χ×5°ϕ grid. The hexagonal grid has been shown by others to reduce the number of data points and time needed to complete a pole figure, while providing equal area sampling. Although not optimized, the spiral method was also investigated as another alternative to the 5°χ×5°ϕ grid.

MgB2 superconductors were synthesized at high pressure and high temperature (HPHT) using pure Mg and B as raw materials. The effects of the experimental conditions such as pressure and temperature on phase evolution were studied using X-ray diffraction (XRD), scanning electron microscope (SEM), and DC magnetization techniques. Results showed that high pressure and high temperature are two important factors for synthesizing the MgB2 phase. Stable MgB2 can be most effectively obtained in a pressure-temperature region from 3 to 6 GPa and between the melting points of Mg up to 1100 to 1300 °C. MgB2 starts to decompose into MgB4 at higher temperatures and pressures. The decomposition temperature of MgB2 increases with increasing pressure. The superconducting transition temperature Tc(bulk) was measured to be 38.0 to 38.8 K for MgB2 prepared at 900 to 1000 °C under 3 GPa. The larger grains and better crystalline perfection contribute to the higher Tc(bulk) and the narrower ΔT.

The engineering of strained semiconductor materials represents an important aspect of the enhancement in CMOS device performance required for current and future generations of microelectronic technology. An understanding of the mechanical response of the Si channel regions and their environment is key to the prediction and design of device operation. Because of the complexity of the composite geometries associated with microelectronic circuitry, in situ characterization at a submicron resolution is necessary to verify the predicted strain distributions. Of the measurement techniques commonly used for strain characterization, synchrotron-based X-ray microbeam diffraction represents the best nondestructive method to provide spatially resolved information. The mapping of strain distributions in silicon-on-insulator (SOI) features induced by overlying silicon nitride structures and embedded heteroepitaxial features adjacent to SOI device channels are presented. The interaction regions of the SOI strain were observed to extend large distances from the SOI/stressor interfaces leading to significant overlap in the strain distributions at technically relevant dimensions. Experimental data were also compared to several mechanical models to assess their validity in predicting these strain distributions.

Four sol-gel TiO2 powders have been prepared from titanium tetraisopropoxide. The calcined powders are then characterized by X-ray diffraction. Cell parameters are extracted using two Rietveld refinement programs (FULLPROF and MAUD) leading to close values and indicating a contraction of the a (or b) cell parameter and an expansion of the c cell parameter of the anatase phase with temperature. Crystallite size and microstrain are highly dependent not only on the sol synthesis but also on the diffraction line profile analysis (LPA) models (i.e., Williamson-Hall, Thomson-Cox-Hastings, Dehlez et al., and log-normal size distribution) employed. Discrepancies are then observed for the phase transformation critical size, the activation energy of grain growth, and the microstrain stored potential energy according to the LPA approach used to calculate the microstructural parameters.

Synchrotron-based X-ray microbeam measurements were performed on silicon-on-insulator (SOI) features strained by adjacent shallow-trench isolation (STI). Strain engineering in microelectronic technology represents an important aspect of the enhancement in complementary metal-oxide semiconductor device performance. Because of the complexity of the composite geometry associated with microelectronic circuitry, characterization of the strained Si devices at a submicron resolution is necessary to verify the expected strain distributions. The interaction region of the SOI strain extended the SOI film thickness from the STI edge at least 25 times. Regions of 65-nm-thick SOI less than 3 μm wide exhibited an overlap in the strain fields because of the surrounding STI. Microbeam mapping of arrays containing submicron SOI features and embedded STI structures revealed the largest out-of-plane strains because of the close proximity of superimposed strain distributions induced by the STI.

The crystal structure of skutterudite-related phase IrGe1.5Se1.5 has been refined by the Rietveld method from laboratory X-ray powder diffraction data. Refined crystallographic data for IrGe1.5Se1.5 are a=12.0890(2) Å, c=14.8796(3) Å, V=1883.23(6) Å3, space group R3 (No. 148), Z=24, and Dc=8.87 g/cm3. Its crystal structure can be derived from the ideal skutterudite structure (CoAs3), where Se and Ge atoms are ordered in layers perpendicular to the [111] direction of the original skutterudite cell. Weak distortions of the anion and cation sublattices were also observed.

Total reflection X-ray fluorescence analysis (TXRF) is a method for qualitative and quantitative analysis of trace elements. In general TXRF is known to allow for linear calibration typically using an internal standard for quantification. For small sample amounts (low ng region) the thin film approximation is valid neglecting absorption effects of the exciting and the detected radiation. However, for higher total amounts of samples deviations from the linear relation between fluorescence intensity and sample amount have been observed. The topic of the presented work is an investigation of the parameters influencing the absorption phenomenon. Samples with different total amounts of arsenic have been prepared to determine the upper limit of sample mass where the linear relation between fluorescence intensity and sample amount is no longer guaranteed. It was found that the relation between fluorescence intensity and sample amount is linear up to ∼100 ng arsenic. A simulation model was developed to calculate the influence of the absorption effects. Even though the results of the simulations are not satisfying yet it could be shown that one of the key parameters for the absorption effect is the density of the investigated element in the dried residues.

Corrections are made to two equations and one table value in “Thermal expansion of anatase and rutile between 300 and 575 K using synchrotron powder X-ray diffraction” [Powder Diffr. 22, 352–357 (2007)].

The growth of precipitates in a deformed Cu–Ni–Si alloy with an aging treatment and the rearrangement of dislocations were investigated using small-angle X-ray scattering method and XRD line-profile analysis. The small-angle X-ray scattering method was used for characterizing the growth behavior of the precipitates. The results showed that the precipitates grew gradually to a few nanometers in radius when aged under the condition that the alloy exhibited a maximum of the hardness due to precipitation hardening. The growth rate rose from the onset of the overaging, where the hardness started to decrease. The line-profile analysis of copper-based alloy diffraction peaks using modified Williamson–Hall and modified Warren–Averbach procedures yielded a variation in the dislocation densities of the alloy as a function of the aging time. The dislocation density of the alloy before the aging treatment was estimated to be 1.7×1015 m−2 and its high value was held up to the peak-aging time. With the onset of the overaging, however, the dislocation density distinctly decreased by about 1 order of magnitude indicating that a large amount of the dislocations rearranged to release the alloy from the high dislocation-density state. The results suggest that the massive rearrangement of dislocations was accompanied with coarsening of the precipitates.

A general least-squares technique for X-ray diffraction line broadening analysis has been developed. The technique can be used to determine single, double, and triple line broadening effects caused by small particle sizes, microstrain, stacking faults, or all three presented in a closed-packed hexagonal nanomaterial. The technique was applied to characterize the microstructure of β-Ni(OH)2, a negative electrode material in nickel-metal hydride (NiMH) batteries. Double line broadening effects caused by both small crystallite sizes and stacking faults in β-Ni(OH)2 were detected and analyzed. Triple line broadening effects caused simultaneously by small crystallite sizes, microstrain, and stacking faults were detected in β-Ni(OH)2 after activation and charge-discharge cycle tests. The triple line broadening effects were found to be selective and most pronounced for diffraction lines with h−k=3n±1. The broadening effects were larger when l=even, but smaller when l=odd. The shape and the average size of the crystallites, microstrain, and stacking fault probability in β-Ni(OH)2 changed dramatically after activation and charge-discharge cycles. The method was also applied to characterize and investigate the microstructure of nano ZnO materials. Results indicate that no selective broadening appears in the XRD patterns of the nano ZnO materials. The average crystallite sizes were different slightly, and the stacking fault probabilities differed significantly with different dopants.

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.

X-ray powder diffraction data for CuGa0.15In0.85Se2 and CuGa0.50In0.50Se2 are reported. Indexing of the X-ray diffraction powder pattern and the Rietveld refinement confirmed that these compounds crystallize in the tetragonal crystal system, with space group I-42d (No. 122) and lattice parameters of a=5.7528(2) Å and c=11.5225(3) Å for CuGa0.15In0.85Se2 and a=5.6847(1) Å and c=11.2817(1) Å for CuGa0.50In0.50Se2. The CuGaxIn1−xSe2 system presents the chalcopyrite type crystal structure (CuFeS2) and corresponds to two stacked zinc-blende unit cells. The metal atoms Cu, In, and Ga are regularly ordered in the unit cell. Every Se atom is tetrahedrally bonded to two Cu and two In and Ga atoms.

The status of the solid materials and mineralogical and petrological results of the Stardust mission to comet 81P/Wild 2 are presented. This mission became the first successful sample-return mission since the Apollo project. This time the challenges were much less related to the availability of state-of-the-art analytical capabilities. Still, dedicated tools had to be developed to manipulate the samples that were all firmly embedded in the tracks they made when decelerating in the silica aerogel tiles of the collector. The comet particles were loosely bonded aggregates that shed their grains along the entire length of these tracks. It appears that most of the original comet minerals survived but interactions of debris with melted aerogel occurred and new minerals were made, adding to the incredibly, and unanticipated, diversity of the comet minerals, including some that so far were known only in meteorites. The latter alone showed that transport distances in the solar nebula extended all the way out to beyond Pluto into the Kuiper Belt of icy, comet-like, bodies. The full extent of the scientific yield of this mission is still unknown, promising but stressing current models of the formation of solar systems.

The Rietveld method is increasingly used for amorphous portion determination. This article describes the quantification of amorphous portions using an internal standard in a formal mathematical way. From a set of basic assumptions and postulations, equations for the amorphous portion quantification, the optimum amount of internal standard, and the slope of the amorphous portion calculation formula were derived. With this tool set, the influence of the method principle on the analytical uncertainty is discussed. It is shown that the amount of internal standard has a strong influence on the precision of the amorphous portion determination. A poor choice can make the determination impossible, while a clever choice can enhance the precision compared to the precision of the Rietveld refinement.

Fiber diffraction data have been obtained from Narcissus mosaic virus, a potexvirus from the family Flexiviridae, and soybean mosaic virus (SMV), a potyvirus from the family Potyviridae. Analysis of the data in conjunction with cryo-electron microscopy data allowed us to determine the symmetry of the viruses and to make reconstructions of SMV at 19 Å resolution and of another potexvirus, papaya mosaic virus, at 18 Å resolution. These data include the first well-ordered data ever obtained for the potyviruses and the best-ordered data from the potexviruses, and offer the promise of eventual high resolution structure determinations.