It is demonstrated that a complex X-ray characterization of semiconductor films epitaxially grown on metal oxide buffer layers and Si(111) substrates is possible using laboratory-based equipment. This is demonstrated with epi-germanium on Pr2O3 as buffer material. Pole figure measurements prove that epi-Ge layers are nearly single crystalline with exactly the same in-plane orientation (type A) as the Si(111) substrate, while the lattice of the oxide layer is 180° rotated around the [111] surface normal (type B). Only a small fraction (less than 0.6 vol %) of the epi-Ge exhibits type B rotation twins. The main structural defects are microtwin lamellas lying in {111} planes 70.5° inclined to the wafer surface. The different in-plane orientation of the Si substrate and epi-Ge on one side and the Pr2O3 buffer layer on the other side allows a very sensitive analysis of strain and defects even for a 10-nm oxide layer buried under a 100-nm Ge. The epi-Ge layers are nearly fully relaxed and the Pr2O3 buffer layer is compressively strained. Due to the existing defects the Ge (111) planes are tilted in a characteristic pattern relative to the Si substrate.

The nucleation of dislocations at indents in silicon following rapid thermal annealing (RTA) has been examined by X-ray diffraction imaging (topography). For indentation loads below 200 mN, no slip bands were generated from the indent sites following RTA at 1000 °C under spike conditions. Upon plateau annealing at 1000 °C, slip dislocations were propagated from some indents but not all. Slip was also observed from edge defects not associated with indentation. For 500-mN indentation load, large scale dislocation sources were generated from the indent sites propagating on two of the four {111} slip planes. These dislocations multiplied into macroscopic-scale slip bands. A significant change in morphology was observed in the 60° dislocation segments after the screw segment reached the rear surface of the wafer. Dislocations changed line direction and in some cases appeared to leave the Peierls trough during glide.

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.

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.

The evolution of internal stresses in oxide scales growing on polycrystalline Fe3Al alloy in atmospheric air at 700 °C was determined using in situ energy-dispersive synchrotron X-ray diffraction. Ex situ texture analyses were performed after 5 h of oxidation at 700 °C. Under these conditions, the oxide-scale thickness, as determined by X-ray photoelectron spectroscopy, lies between 80 and 100 nm. The main phase present in the oxide scales is α-Al2O3, with minor quantities of metastable θ-Al2O3 detected in the first minutes of oxidation, as well as α-Fe2O3. α-Al2O3 grows with a weak (0001) fiber texture in the normal direction. During the initial stages of oxidation the scale develops, increasing levels of compressive stresses which later evolve to a steady state condition situated around −300 MPa.

Strain field distribution in a naval platform under dry-dock conditions is complex and represents the cumulative response from residual stress (“locked in” during fabrication of materials and formation of the structure) and static loading stress (e.g., dry-dock loading). The magnitude and distribution of stress fields are a significant concern for the Canadian Navy, where the superposition of applied stresses on residual stresses may adversely affect the performance, safe operational envelope, and service life of naval platforms. Stress analysis was conducted on Canada’s VICTORIA Class submarines using a portable miniature X-ray diffractometer (mXRD) under dry-dock conditions. This paper introduces the concept of “residential stress” as it applies to submarine platforms and discusses the methodology for performing stress analysis with a portable mXRD. The evolution of residential stress during routine pressure hull repairs to Canada’s VICTORIA Class submarines is discussed. In particular, the recent replacement of the diesel exhaust hull and back-up valves on one of the submarines, as well as a pressure hull plate extraction-insertion-weld procedure on another, is discussed.

New XRD total pattern fitting software MSTRUCT was used to study the microstructure of magnetron-deposited TiO2 thin films. MSTRUCT is an extension of the FOX program for structure determination from powder diffraction data. MSTRUCT makes corrections for refraction and absorption, residual stress, and preferred orientation that are necessary for thin-film analysis using the parallel-beam geometry and an asymmetric detector scan with small angles of incidence. The program also corrects for crystallite size broadening in terms of log-normal distribution, two models of strain (phenomenological and dislocation models), as well as the influence of stacking faults in the most common cubic and hexagonal structures. The microstructure results obtained by this study show that during crystallization of the amorphous TiO2 films, tensile stresses were generated resulting in anisotropic shifts of diffraction peaks. This was confirmed by in situ crystallization and direct stress measurements. The consideration of the stress effect in terms of the weighted Reuss-Voigt model improved the fits significantly. The stresses were found to depend systematically on the TiO2 film thickness, and their values determined by total pattern fitting agree well with the values measured directly by XRD stress analysis.

Verification tests of the forward modeling technique for near-field high energy X-ray diffraction microscopy are conducted using two simulated microstructures containing uniformly distributed orientations. Comparison between the simulated and reconstructed microstructures is examined with consideration to both crystallographic orientation and spatial geometric accuracy. To probe the dependence of results on experimental parameters, simulated data sets use two different detector configurations and different simulated experimental protocols; in each case, the parameters mimic the experimental geometry used at Advanced Photon Source beamline 1-ID. Results indicate that element orientations are distinguishable to less than 0.1°, while spatial geometric accuracy is limited by the detector resolution.

A single-pulse X-ray diffraction (XRD) diagnostic has been developed for the investigation of shocked material properties on a very short time scale. The diagnostic, which consists of a 37-stage Marx bank high-voltage pulse generator coupled to a needle-and-washer electron beam diode via coaxial cable, produces line-and-bremsstrahlung X-ray emission in a 40 ns pulse. The molybdenum anode produces 0.71 Å characteristic Kα lines used for diffraction. The X-ray beam passes through a pinhole collimator and is incident on the sample with an approximately 2 mm×5 mm spot and 1° full width at half maximum angular divergence. Coherent scattering from the sample produces a Debye-Scherrer diffraction pattern on an image plate located at 75 mm from the polycrystalline sample surface. An experimental study of the polycrystalline structures of zirconium and tin under high-pressure shock loading has been conducted with single-pulse XRD. The experimental targets were 0.1-mm-thick foils of zirconium and tin using 0.4-mm-thick vitreous carbon back windows for shock loading, and the shocks were produced by either Detasheet or PBX-9501 high explosives buffered by 1-mm-thick 6061-T6 aluminum. The diffraction patterns from both shocked zirconium and tin indicated a phase transition into a polymorphic mix of amorphous and new solid phases.

The electrochemical reaction behavior of a commercial Li-ion battery (LiFePO4-based cathode, graphite-based anode) has been measured via in situ neutron diffraction. A multivariate analysis was successfully applied to the neutron diffraction data set facilitating in the determination of Li bearing phases participating in the electrochemical reaction in both the anode and cathode as a function of state-of-charge (SOC). The analysis resulted in quantified phase fraction values for LiFePO4 and FePO4 cathode compounds as well as the identification of staging behavior of Li6, Li12, Li24, and graphite phases in the anode. An additional Li-graphite phase has also been tentatively identified during electrochemical cycling as LiC48 at conditions of ∼5% to 15% SOC.

This paper presents a nondestructive measurement technique for the determination of the film thicknesses of Co and SmCo based magnetic films deposited by sputtering on single-crystal silicon (100) substrates. X-ray diffraction of Cu Kα radiation has been used to measure the intensity of the (400) reflection from bare silicon substrates and as attenuated by sputter coated Co and SmCo based films on Si substrates. A four-axis research diffractometer allowed the substrate orientation to be fine adjusted to maximize the (400) diffraction intensity. The thickness of SmCo based films was in a range from 0.05 to 5 μm. Co film thicknesses on Si could be measured to a few tens of nanometers. The accuracy of the thickness measurements depends on the effective mass attenuation coefficient of the film material. For the materials considered, the thicknesses determined by the X-ray attenuation method agree within at least several percent to values determined by other methods.

We have fabricated a bifocal miniature toroidal mirror that horizontally and vertically focuses to two different locations to provide a smaller footprint of the beam for grazing-incidence wide-angle scattering (GIWAXS), while at the same time focusing the beam in the horizontal direction on the detector to further enhance the angular resolution. At CHESS we traditionally use glass single-bounce monocapillary optics for a wide range of X-ray experiments to get a fine X-ray beam of 5 to 20 μm. This miniature toroidal mirror was prepared by designing and fabricating an X-ray focusing capillary in which the sagittal and meridional focusing is decoupled and only a quadrant of the accepted annulus is used for focusing the beam. The mirror produced a 120 μm horizontal by 25 μm vertical focus at 50 mm from the tip of the optic and a 44 μm horizontal by 70 μm vertical focus at 150 mm from the tip of the optic.

We have demonstrated that structures down to 150 nm can be visualized in X-ray projection images using nanofocus X-ray sources. Due to their unlimited depth of focus, they do not possess a limit on the specimen size. This is essential for three-dimensional tomographic imaging of samples with a diameter larger than a few microns. Further simulation studies have shown that optimization of the detector response curve and switching from a reflective X-ray target to a transmission target should allow us to reach sub-100-nm resolutions.

Due to the extraordinary beam characteristics of the new PETRA III synchrotron, i.e., the high brilliance, the extremely low emittance of 1 nm rad, and the high fraction of coherent photons even in the hard X-ray range, the imaging beamline (IBL) at PETRA III will provide state of the art imaging and tomography capabilities with resolution well into the nanometer range. Novel applications of tomographic techniques allow for high speed in situ measurements as well as highest spatial and density resolutions. Additionally, the highly coherent beam enables the application of phase contrast methods in an exceptional way. Since the focus is on the energy range between 5 and 50 keV, the IBL will among others be ideally suited for microtomography and nanotomography on small engineering materials science samples as well as for studying soft matter, bones, medical implants, and biomatter.

This paper presents Monte Carlo simulations considering all stages of the creation process of two-dimensional projections in a computed tomography (CT) device: excitation of angle dependent X-ray spectra within the X-ray tube using results from a previous study [Chyba et al. (2008). Powder Diffr. 23, 150–153]; interaction of these X-rays and secondary photoelectrons with a simple inhomogeneous sample; and interaction of X-rays and photoelectrons with the components (thin layers) of a matrix scintillation detector. The simulations were carried out by using custom software running on up to 50 nodes of a computer cluster. Comparative calculations were also made by using the software package MCNP [Booth et al. (2003). MCNP—A general Monte Carlo N-particle transport code, Report LAUR 03-1987, Los Alamos National Laboratory, Los Alamos, NM]. Tube spectra were calculated with algorithms proposed by Ebel [(2006). Adv. X-Ray Anal. 49, 267–273]. Measurements for the chosen setup made with an available CT device were in relatively good agreement with calculated results. It was shown that good knowledge of the tube spectra is of importance, but most differences between resulting projections and measurements are caused by uncertainties concerning detector response due to light yield of the scintillator and to internal scattering effects within the thin detector layers which lead to spreading of a detected point signal within the detector matrix into neighboring matrix elements.

Micro-X-ray fluorescence (μ-XRF) is a rapidly evolving analytical technique which allows visualising the trace level metal distributions within a specimen in an essentially nondestructive manner. At second generation synchrotron radiation sources, detection limits at the sub-parts per million level can be obtained with micrometer resolution, while at third generation sources the spatial resolution can be better than 100 nm. Consequently, the analysis of metals within biological systems using micro- and nano-X-ray fluorescence imaging is a quickly developing field of research. Since X-ray fluorescence is a scanning technique, the elemental distribution within the sample should not change during analysis. Biological samples pose challenges in this context due to their high water content. A dehydration procedure is commonly used for sample preparation enabling an analysis of the sample under ambient temperature conditions. Unfortunately, a potential change in elemental redistribution during the sample preparation is difficult to verify experimentally and therefore cannot be excluded completely. Creating a cryogenic sample environment allowing an analysis of the sample under cryogenic condition is an attractive alternative but not available on a routine basis. In this article, we make a comparison between the elemental distributions obtained by micro-SR-XRF within a chemically fixed and a cryogenically frozen Daphnia magna, a model organism to study the environmental impact of metals. In what follows, we explore the potential of a dual detector setup for investigating a full ecotoxicological experiment. Next to conventional 2D analysis, dual detector X-ray fluorescence cryotomography is illustrated and the potential of its coupling with laboratory absorption micro-CT for investigating the tissue-specific elemental distributions within this model organism is highlighted.