The aim of this study is to analyze the mechanics of a new class of metal/ceramic composites on a mesoscopic length scale. These composites are produced by melt infiltration of porous ceramic preforms produced by freeze casting and subsequent sintering. This production route has a high application potential since it offers a cost-effective way to obtain composites with ceramic content in the 30 to 70 vol. % range. The as-produced material exhibits a hierarchical domain structure with each domain composed of alternating layers of metallic and ceramic lamellae. Residual stresses present in all phases of the composite produced by infiltrating alumina preforms with a eutectic aluminum-silicon alloy have been measured. Integral as well as spatially resolved measurements were carried out on single-domain samples at the high-energy, energy-dispersive diffraction (EDDI) beamline at the synchrotron radiation source BESSY (Berlin, Germany). Results show that strongly fluctuating residual stresses are introduced by the production process, which can be rationalized by taking into account the thermal expansion mismatch of alloy and preform.

To establish standard working practices and further understanding of the application of X-ray fluorescence (XRF) spectroscopy to works of art and cultural heritage materials, a series of round-robin tests have been conducted biannually since 2002. In 2008 the round-robin explored the application of XRF to the study of paintings on canvas. Thirteen samples, consisting of both modern and traditional pigments on canvas, were distributed to 25 participating institutions for analysis. The samples were designed to explore common challenges encountered in the XRF analysis of painted works including peak overlaps, sum peaks, layering/shielding effects, detection of low-Z pigments, and modern pigments. The results from representative samples highlighting each topic are discussed.

Co(II) complexes with benzoic acid and ternary complexes with ligands benzoic acid and histidine/aspartic acid have been synthesized and characterized using various spectroscopic methods. On the basis of infrared, UV-visible spectra, and magnetic data the complexes were found to be having octahedral polymeric geometry. X-ray powder diffraction results show that the crystal systems of Co(II)-Ben and Co(II)-Ben-Hist complexes are triclinic with lattice constants a=15.58 Å, b=11.92 Å, c=4.33 Å, α=96.08°, β=104.68°, γ=88.46°, and V=774.15 Å3 and a=18.88 Å, b=17.01 Å, c=15.13 Å, α=93.15°, β=89.41°, γ=100.71°, and V=4768.75 Å3, respectively. The Co(II)-Ben-Asp complex is orthorhombic with lattice constants a=21.57 Å, b=15.06 Å, c=11.40 Å. α=β=γ=90°, and V=3703.38 Å3.

The room temperature powder pattern of lapatinib ditosylate monohydrate (active ingredient in Tykerb used to treat refractory breast cancer) was indexed and the cell from the single crystal X-ray diffraction structure was refined using the experimental capillary data. Unit-cell parameters for the orthorhombic compound with space group Pbca refined from powder diffraction data are a=9.6850±0.0009 Å, b=29.364±0.003 Å, and c=30.733±0.003 Å, α=β=γ=90°, z=8, V=8740.1 Å3. Values of 2θ, d, I, and Miller indices are reported.

The results from a third structure determination by powder diffractometry (SDPD) round robin are discussed. From the 175 potential participants having downloaded the powder data, nine sent a total of 12 solutions (8 and 4 for samples 1 and 2, respectively, a tetrahydrated calcium tartrate and a lanthanum tungstate). Participants used seven different computer programs for structure solution (ESPOIR, EXPO, FOX, PSSP, SHELXS, SUPERFLIP, and TOPAS), applying Patterson, direct methods, direct space methods, and charge flipping approach. It is concluded that solving a structure from powder data remains a challenge, at least one order of magnitude more difficult than solving a problem with similar complexity from single-crystal data. Nevertheless, a few more steps in the direction of increasing the SDPD rate of success were accomplished since the two previous round robins: this time, not only the computer program developers were successful but also some users. No result was obtained from crystal structure prediction experts.

Four matrix-phase crystallographic directions of IN718 are investigated by in situ tensile tests using neutron diffraction. The elastic diffraction constants for all directions measured are compared to theoretical values calculated by the Kröner model. The differences between the microscopic and the macroscopic material response are given. The accumulation of microstrains in the different crystallographic directions is discussed. A comparison between the results of a single phase material (ingot IN718) and two differently thermal treated multiphase materials is presented.

Sauropod dinosaurs were typically one magnitude larger than any other living or extinct terrestrial animal. This sheer size of the sauropod leads to scale effects in their biology and physiology that still are inadequately understood. The only remnants of the sauropods are their fossilized bones. These fossilized bones have sustained burial for some hundred million years and thus may have experienced significant diagenetic changes. These diagenetic changes often do not affect bone preservation on the histological level, but may lead to significant alterations of the bone microstructure. Here the influence of diagenesis on the microstructure of fossilized sauropod bones using femur cross section of Brachiosaurus brancai that was excavated in the Tendaguru beds in Tanzania is investigated. The element distribution in this dinosaur bone is studied by a combination of micro-X-ray-fluorescence (μ-XRF) using synchrotron radiation and energy dispersive X-ray analyses (EDX) in the scanning electron microscope. These techniques reveal quantitative values of the element concentration at a macroscopic level combined with qualitative information at high spatial resolution of the distribution of Ca, Co, Cr, V, Pb, U, Sr, Y, and As in the fossil bones. This allows a differentiation between the remnants of the original bone apatite and pore filling minerals and also a visualization of damage, e.g., cracks introduced by diagenetic processes.

X-ray powder diffraction data for three new bismuth yttrium ytterbium oxide compounds synthesized by solid-state reaction method are reported. The unit-cell dimensions were determined from X-ray diffraction method using Cu Kα radiation and evaluated by indexing programs. The cubic δ-Bi2O3 phase was identified to be the sole crystalline phase in Bi0.82Y0.09Yb0.09O1.5, Bi0.82Y0.12Yb0.06O1.5, and Bi0.82Y0.06Yb0.12O1.5 with lattice constants of a=5.5110(3), 5.5154(2), and 5.5113(2) Å, respectively.

We have developed a convenient and effective XRF analysis procedure for trace amount of K, Ca, V, Mn, Fe, Ni, Cu, Zn, Cd, and Pb in environmental waters by using a preconcentration using the natural polymer (agar). The thin agar film was prepared by drying a homogeneous agar gel after mixing the aqueous sample solution with the agar powder. XRF analysis of the preconcentrated thin agar films containing trace metals showed a good repeatability because agar films were homogeneous enough. SB (signal to noise) ratios of the XRF intensity of the analytes were improved drastically. The linear calibration curves of K, Ca, V, Mn, Fe, Ni, Cu, Zn, Cd, and Pb showed a good linearity within the calibration ranges. The lower limits of detection (LLD) were 1.4 μg/mL for K, 0.26 μg/mL for Ca, 0.088 μg/mL for V, 0.029 μg/mL for Mn, 0.11 μg/mL for Fe, 0.016 μg/mL for Ni, 0.030 μg/mL for Cu, 0.017 μg/mL for Zn, 0.20 μg/mL for Cd, and 0.066 μg/mL for Pb, respectively. The proposed preconcentration method was applied to several environmental water samples.

An additional statistical calibration for the Bruker D8 Discover microdiffractometer is necessary to obtain accurate reproducible 2θ data for cell-refinement work. This new approach uses a graphical mapping method of the 2θ error versus the location of a selected diffraction peak on the detector surface to describe the separate roles of different calibration procedures (rebiasing, flood field, and spatial corrections) and parameters (sample-to-detector distance, x-y center coordinate) in minimizing the error. Optimized parameters are used to obtain the lowest achievable Δ2θ with this setup. Intensity error relative to the position of the diffracted line on the detector was found to be consistent at up to 20% and could not be reduced using any of the investigated techniques and parameters.

The neutron diffraction technique was applied to measure strain distributions in a rebar in a reinforced concrete. At first, absorption coefficients of several kinds of concrete with different compounding ratios of water, cement, and aggregate were measured, and it was confirmed that the absorption coefficient of concrete was affected by the amounts of water and aggregate. In addition, it was also clarified by measuring strain change of the rebar under tensile loading that accuracy of the strain measurement in the rebar in the reinforced concrete was not affected by the neutron absorption by the concrete. Second, the size of the anchorage zone was evaluated by measuring strain distributions in the rebar under pull-out loading. The length of the anchorage zone measured by neutron diffraction was shorter than that measured by strain gauges. Moreover, detailed strain distributions in the rebar around cracks in the concrete were measured under tensile loading, and it was confirmed that the bond condition between rebar and concrete around cracks could be evaluated using the neutron diffraction technique.

This manuscript describes the construction, testing, and use of a simple side-loading air-tight specimen holder for use with Bruker X-ray powder diffractometers.

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.

We have used synchrotron X-ray diffraction experiments to measure the strain field introduced by a hydride blister grown on a section of a pressure tube from a CANDU nuclear reactor. After charging the tube section with a homogeneous hydrogen concentration of 300 wt ppm, the blister was produced by creating a small cold spot on its surface (∼200 °C), while the bulk was kept at a temperature of 338 °C over a period of 1008 h. The blister studied here is ellipsoidal in shape, with its long axis along the tube axial direction. The experiments were performed on the wiggler beam line ID15 at the European Synchrotron Radiation Facility (ESRF) using a polychromatic beam of high-energy X-rays (60 to 300 keV). Unlike conventional X-ray diffraction, in this mode the scattering angle is fixed and the diffracted beam is discriminated on the basis of the photon energy. The results show that the blister is composed by two crystallographic phases (δ-ZrH and α-Zr), with volume fractions varying with position. The maximum stresses appear at the blister-matrix interfaces. Near the tube outer surface, we found large compressive stresses of (−450±90) MPa along the blister long axis, and tensile stresses (+320±90) MPa along the tube hoop direction. The main uncertainty in these stresses results from the uncertainty in the elastic constants of the hydride phase. Large strains and broad peaks were observed for this phase, which were explained by a rather low Young’s modulus (35 GPa) for the hydride. The results are compared with finite element simulations found in the literature.