The Interactive Data Language has been used to produce a software program capable of advanced three-dimensional visualizations of pole figure and θ-2θ data. The data can also be used to calculate quantitative properties such as strain level and to minimize the peak-height texture effects in individual θ-2θ scans. The collection of the large data sets necessary for the analyses is facilitated by use of a position sensitive detector or area detector.

The low-cycle fatigue behavior of a cobalt-based superalloy was studied in situ using neutron–diffraction experiments. The alloy exhibited stress-induced formation of a hexagonal-close-packed (hcp) phase within its parent face-centered-cubic (fcc) phase at ambient temperature under strain-controlled fatigue conditions with a total strain range, Δε=2.5%. The (101) hcp peak was first observed during the 12th fatigue cycle under the given conditions following a period during which no hcp phase was detected. Subsequently, the intensity of the hcp peaks increased as fatigue progressed. Furthermore, within a single fatigue cycle, the intensity of the (101) hcp peak decreased during the compression half-cycle and increased again when the specimen was subjected to a subsequent tensile strain. The result suggests that the fcc to hcp transformation is partially reversible within one fatigue cycle.

Synthesis and structure of two phosphates belonging to the ternary Sb2O5-Fe2O3-P2O5 system are reported. Structures of both SbV1.50FeIII0.50(PO4)3 and (SbV0.50FeIIIe0.50)P2O7 phases, obtained by solid state reaction in air atmosphere at 950 °C and 900 °C, respectively, were determined at room temperature from X-ray powder diffraction using the Rietveld method. Sb1.50Fe0.50(PO4)3 phosphate belongs to the Nasicon-type structure with R32 space group. Hexagonal cell parameters are ahex.=8.305(1) Å and chex.=22.035(2) Å. Rietveld refinement results show a 2-2 ordered distribution, along the c-axis, of X(1) and X(2) sites (crystallographic formula [Sb0.88Fe0.12]X(1)[Fe0.38Sb0.62]X(2)(PO4)3) in the Nasicon framework. (Sb0.50Fe0.50)P2O7 is isotypic with β-SbP2O7 pyrophosphate [Pna21 space group; a=7.865(1) Å, b=15.699(2) Å, c=7.847(1) Å]. Its crystal structure is built up from corner-shared SbO6 or FeO6 octahedra and P2O7 groups (two group types). Each P2O7 group shares its six vertices with three SbO6 and three FeO6 octahedra, and each octahedra is connected to six P2O7 groups. A quasi 1-1 ordered distribution, along the b-axis, of Sb5+ and Fe3+ ions in the pyrophosphate framework are observed.

Drilling a hole in the blade of a vibrating spatula makes a simple tool for both handling and filling capillary tubes. It is especially useful for filling capillaries with air-sensitive samples in a glove box.

Neutron diffraction provides a direct probe for the ordering of spins from unpaired electrons in materials with magnetic properties. The ordering of the spins can be modeled in many cases by adding spin directions to standard crystallographic models. This requires, however, that crystallographic space groups be extended by addition of a “color” attribute to symmetry operations, which determines if the operation maintains or flips the direction of a magnetic spin. Rietveld analysis provides a mechanism for fitting magnetic structure models to powder diffraction data. The general structure and analysis system (GSAS) software suite is commonly used for Rietveld analysis and includes the ability to compute magnetic scattering. Different approaches are commonly used within GSAS to create models that include magnetism. Three equivalent but different approaches are presented to provide a tutorial on how magnetic scattering data may be modeled using differing treatment of symmetry. Also discussed is how magnetic models may be visualized. The commands used to run the GSAS programs are summarized within, but are shown in great detail in supplementary web pages.

The equation ε(φ, ψ, hkl)=Fij(φ, ψ, hkl)σij can be directly deduced from Hooke’s law. It is shown that the matrix Fij(φ, ψ, hkl) which is usually called X-ray elastic factors, behaves as a second rank tensor. Since this behaviour is the only criterion for the question of whether or not it is a tensor, the F-matrix must be regarded as a second rank tensor. This allows us to make some statements about the structure of the F-matrix on the basis of Neumann’s principle, to find relationships among F-matrices in different measurement directions, and to apply the methods and strategies for the measurement of a second rank tensor. All this is shown in a few examples. It is further shown that a consistent use of the F-matrix can replace all methods for data evaluation which makes use of linear regressions and, in addition, avoids all difficulties and disadvantages of these methods. One of these disadvantages is that the sin2 ψ-method, as well as its derivatives, is generally not correct least square fits of the measured data. This is also shown in an example. The more complicated cases with stress or constitution gradients in the range of the probed volume or stress measurement after plastic deformation are not discussed.

The X-ray Rietveld refinement technique was used to determine the structure and prepare X-ray powder reference patterns for the phases R2Cu9Ti12O36 (R=Nd, Sm, Eu, Gd, Dy, Ho, Y, Er, Tm, Yb, and Lu). R2Cu9Ti12O36 belongs to the perovskite-related [AC3](B4)O12 family of structures, which are cubic with space group Im3. The lattice parameters of the R2Cu9Ti12O36 series range from a=7.377 57(2) Å, V=401.550(3) Å3 for R=Lu to a=7.399 87(3) Å, and V=405.202(4) Å3 for R=Nd. The trend of these lattice parameters parallels the “lanthanide contraction.” In the structure, R occupies the larger icosahedral A site of the ideal ABO3 perovskite structure, while Ti occupies the distorted octahedral B site. The Jahn-Teller cation Cu occupies the C site. The twelve oxygens surrounding Cu are arranged as three mutually perpendicular rectangles of different size. The smallest and largest rectangles are nearly squares. One-third of the R site is vacant, and the chemical formula can be written as [R2∕3X1∕3Cu3](Ti4)O12, where X=vacancy. The X-ray powder patterns of R2Cu2Ti12O36 have been submitted to ICDD for inclusion in the Powder Diffraction File (PDF).

Cognitive deficits are repeatedly described with Pb exposure, but little is known about the distribution of lead in brain. To determine the local distribution of lead (Pb) and other trace elements, X-ray fluorescence spectroscopy measurements have been performed, using a microbeam setup and highest flux synchrotron radiation. Experiments have been carried out at ID-22, ESRF, Grenoble, France. The installed microprobe setup provides a monochromatic beam (16 keV) from an undulator station focused by Kirkpatrick-Baez X-ray optics to a spot size of 5 μm×3 μm. Brain slices from frontal cortex, thalamus, and hippocampus have been investigated (20 μm thickness, imbedded in paraffin and mounted on kapton foils). In general no significant increase in fluorescence intensities could be detected in one of the investigated brain compartments. Pb and other (trace) elements such as S, Ca, Fe, Cu, Zn, and Br could be detected in all samples and showed strong inhomogeneities within the analysed areas. While S, Ca, Fe, Cu, Zn, and Br could be clearly assigned to brain vessel structures (blood vessels, plexus choroidei), Pb was very inhomogeneously distributed. The local distribution of the detected elements in various brain structures will be discussed.

One of the main threats to human health from heavy metals is associated with the exposure to lead (Pb). In vivo X-ray fluorescence analysis (XRF) of human bone is a widely used technique to determine the total Pb body burden. The intention of this work was to study the feasibility of in vivo L-shell XRF measurements of Pb in bone using X-ray tubes as excitation sources. Parameter studies using direct tube excitation with various anode materials (Mo and W) and filters as well as different secondary targets and low-Z polarizers were performed with regard to the lowest limits of detection (LLD) achievable for Pb in bone matrix. A breakthrough for the development of a portable spectrometer was achieved by using an air-cooled low-power (50 W) Pd anode X-ray tube, Mo secondary target, and a Peltier-cooled silicon drift detector. LLDs for Pb in bone were determined from measurements on a plaster-of-paris standard without overlying tissue equivalent material and found to be around 0.6 μg∕g.

A novel synthesis method of fibrillar trimolybdates with the use of Ag2Mo3O10∙2H2O as a precursor has been used successfully to synthesize methylammonium trimolybdate, (CH3NH3)2Mo3O10∙H2O. The crystal structure of this compound was determined by X-ray powder diffraction method and refined by the Rietveld method. The compound is orthorhombic, space group Pnma (62), with a=11.241(3), b=7.585(1), and c=15.516(4) Å. The redetermined crystal structure of the precursor and the structure of the title compound are compared and discussed.

The crystal structure of the perovskite phase KCaF3 has been redetermined at 4.2 and 300 K using powder neutron diffraction collected at the highest resolution. At both temperatures the phase was found to be orthorhombic in space group Pnma, with lattice parameters a=0.622 879(5) nm, b=0.870 031(7) nm, c=0.611 210(5) nm at 4.2 K, and a=0.621 488(6) nm, b=0.876 360(8) nm, c=0.616 481(6) nm at 300 K. The CaF6 octahedron is regular at both temperatures with octahedral rotations of 9.6° and 13.2° for the in-phase and anti-phase tilts, respectively, at 4.2 K. No evidence was found to support the recent revision of the space group from Pnma to the monoclinic space group B21∕m.

Round and spiral-shaped coil springs enable various peening angles that correspond to the surface location, and the directional shot angles may lead to a nonuniform residual stress on the coil spring surface. It is commonly known that a material under directional deformation exhibits a nonlinear 2θ-sin2ψ diagram (ψ split) due to the triaxial stress state. In this study, the residual stress distributions of spring materials deformed by shot peening at different angles were measured, and the microstructure for carbide precipitates was examined using a field-emission scanning electron microscope (FE-SEM). The nonlinearity in the 2θ-sin2ψ diagram for the shot peening samples was revealed. The extent of the ψ split increased with increasing shot peening angles, and was dependent not only on the mass fraction of carbide particles but also on the size distribution of the carbide particles.

Detailed structural properties of La1−xBaxCoO3 (LBCO) have been investigated by means of X-ray powder diffraction and Rietveld analysis. A structural phase transformation from R3c to Pm3m at x=0.30–0.35 has been detected based on a comparison between the refinements of R3c and Pm3m. The Co–O bond length of the CoO6 octahedron expanded rapidly with increasing Ba content when x<0.1, and then it leveled off and kept constant at 0.1⩽x⩾0.35, where the Co–O–Co bond angle reaches 180°. The Co–O bond length expansion resumed with increasing Ba content beyond x=0.35.

X-ray powder diffraction data and unit cells parameters for a monoclinic variety of the popular herbicide 2-chloro-N-(pyrazol-1-ylmethyl) acetyl-2′, 6′-xylidide, commonly known as metazachlor, butisan, and butichlor, is presented [a=7.306(3) Å, b=17.824(9) Å, c=10.728(3) Å, β=98.46(4)°, space group P21/c, cell volume=1381.82 Å3, Z=4]. The four strongest peaks (Irel>25) at 8.87, 7.19, 4.57, and 4.45 Å are quite distinctive, thus X-ray powder diffraction provides a quick, simple, and definitive method of identifying this form of material from other commercially available herbicide products.

We present a review of the application of diffraction stress∕strain analysis to small volumes. For cases in which the material properties and∕or the stress state are not homogeneous, traditional approaches may yield erroneous stress results. On the other hand, with proper care, relevant mechanical information about the system can be obtained. Through the use of conventional and synchrotron-based X-ray methods, we can determine the amount of strain transfer between thin film features that possess heterogeneous stress distributions and the underlying substrate. Two examples of such studies are presented. The resulting data are used to assess the validity of several models often used to predict the mechanical behavior in thin film∕substrate composites.