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Bent crystals can be used to deflect high-energy charged particles for beam extraction and/or beam collimation at accelerator facilities, thanks to the channelling phenomenon. In the present paper, two perfect silicon mono-crystals were bent using two different methods: sandblasting and the application of a carbon fibre composite. In particular, these samples were obtained for the realization of bent crystal prototypes to be used to steer the 7 TeV proton beam of the Large Hadron Collider in the context of the CRYSBEAM project. The two bending methods were selected since they allow a very homogeneous curvature of the crystals to be obtained, which is essential for high channelling efficiency. Moreover, the deformation obtained is self-standing, i.e. there is no need for any external device to keep the samples bent. Self-standing curvature can be useful because the presence of an external bender could be a severe limitation in the collider beam-pipe. The curvature of the samples was measured through high-energy X-ray diffraction at the ID11 beamline of the European Synchrotron Radiation Facility in Grenoble, France. Since the diffraction efficiencies obtained were in good agreement with theoretical expectations, it follows that the manufacturing techniques did not damage the samples, i.e. the crystallographic quality was preserved. Finally, the crystal quality of the sandblasted sample was investigated in detail at the synchrotron source at Karlsruhe Institute of Technology by X-ray white-beam topography. The measurements showed no diffusion of defects from the machined surfaces to the crystal bulk.

In modern gasoline direct injection engines, the fuel is (partially) superheated for a significant proportion of the time during operation. This means that the vapour pressure of the fuel, or at least of many of its components, is higher than the ambient pressure inside the engine during injection. If the excess fuel enthalpy cannot be removed by evaporation at the free surface of the spray, the liquid phase boiling creates new surfaces. This phenomenon is known as flash boiling. Flash-boiling atomization produces smaller droplets and can therefore be beneficial as an additional atomization mechanism. Furthermore, it can reduce the penetration depth of a spray, although it also decreases the stability of fuel sprays. This is manifested in undesired targeting changes, that is, spray contraction due to jet-to-jet interaction. In extreme cases, a complete spray collapse can occur, where a multi-hole or hollow-cone spray contracts towards the spray axis and forms a jet-like structure that increases penetration depth. To understand the relationship between flash-boiling atomization and targeting changes, flash boiling was investigated with a single-hole generic injector without jet-to-jet interaction. In addition to macroscopic spray parameters, this study also focused on the flow field of the spray itself measured using laser Doppler anemometry, as well as the spray-induced flow field of the surrounding gas phase measured using fluorescent particle image velocimetry. The results show a strong radial expansion of the jet directly after nozzle exit, caused by internal flash boiling. It is shown that this expansion is caused by a zone of expanding fuel vapour in the centre of the spray. As a result, the displacement of air after injector opening as well as at the front of the spray is significantly increased, causing a decrease in spray front velocity and penetration depth. The stationary air entrainment, however, is only moderately increased as is the total amount of captured air, since the fuel vapour displaces air in the spray.

Optica 6(9), 1106 - 1109 (2019). doi:10.1364/OPTICA.6.001106, Modern emerging technologies, such as additive manufacturing, bioprinting, and new material production, require novel metrology tools to probe fundamental high-speed dynamics happening in such systems. Here we demonstrate the application of the megahertz (MHz) European X-ray Free-Electron Laser (EuXFEL) to image the fast stochastic processes induced by a laser on water-filled capillaries with micrometer-scale spatial resolution. The EuXFEL provides superior contrast and spatial resolution compared to equivalent state-of-the-art synchrotron experiments. This work opens up new possibilities for the characterization of MHz stochastic processes on the nanosecond to microsecond time scales with object velocities up to a few kilometers per second using XFEL sources., Published by OSA, Washington, DC

Pulsed laser ablation in liquids is a hierarchical multi-step process to produce pure inorganic nanoparticle colloids. Controlling this process is hampered by the partial understanding of individual steps and structure formation. In situ X-ray methods are employed to resolve macroscopic dynamics of nanosecond PLAL as well to analyse the distribution and speciation of ablated species with a microsecond time resolution. High time resolution can be achieved by synchrotron-based methods that are capable of 'single-shot' acquisition. X-ray multicontrast imaging by a Shack-Hartmann setup (XHI) and small angle X-ray scattering (SAXS) resolve evolving nanoparticles inside the transient cavitation bubble, while X-ray absorption spectroscopy in dispersive mode opens access to the total material yield and the chemical state of the ejecta. It is confirmed that during ablation nanoparticles are produced directly as well as reactive material is detected, which is identified in the early stage as Zn atoms. Nanoparticles within the cavitation bubble show a metal signature, which prevails for milliseconds, before gradual oxidation sets in. Ablation is described by a phase explosion of the target coexisting with full evaporation. Oxidation occurs only as a later step to already formed nanoparticles.

This article describes complete characterization of the polygonal dislocation half-loops (PDHLs) introduced by scratching and subsequent bending of an Si(111) crystal. The study is based on the X-ray topo-tomography technique using both a conventional laboratory setup and the high-resolution X-ray image-detecting systems at the synchrotron facilities at KIT (Germany) and ESRF (France). Numerical analysis of PDHL images is performed using the Takagi–Taupin equations and the simultaneous algebraic reconstruction technique (SART) tomographic algorithm.

In this work a double-crystal setup is employed to study compound refractive lenses made of single-crystal diamond. The point spread function of the lens is calculated taking into account the lens transmission, the wavefront aberrations, and the ultra-small-angle broadening of the X-ray beam. It is shown that, similarly to the wavefront aberrations, the ultra-small-angle scattering effects can significantly reduce the intensity gain and increase the focal spot size. The suggested approach can be particularly useful for the characterization of refractive X-ray lenses composed of many tens of unit lenses.A double-crystal setup is used to quantify aberrations and to assess the influence of ultra-small-angle X-ray scattering on the optical properties of a single-crystal diamond compound refractive lens.

In this contribution, we compare the performance of Hartmann masks and inverted Hartmann masks of different periods for phase-sensitive X-ray imaging. The Hartmann masks were gold meshes and the inverted Hartmann masks were arrays of gold pillars, both manufactured by UV lithography and gold electroforming on low-absorbing graphite substrates. We asses masks performance by comparing the visibility and homogeneity of the periodic patterns. Manufactured customized masks exhibit clear periodic patterns and demonstrate visibility values from 30 % to 50 % depending on the setup configuration. Finally, we show the phase contrast imaging with an angular resolution of 1.5 μm and demonstrate that images obtained with an inverted Hartmann mask have superior quality.

Nanotechnology 30(50), 505703 (2019). doi:10.1088/1361-6528/ab40f1, InAs x P1−x nanowires are promising building blocks for future optoelectronic devices and nanoelectronics. Their structure may vary from nanowire to nanowire, which may influence their average optoelectronic properties. Therefore, it is highly important for their applications to know the average properties of an ensemble of the nanowires. Structural properties of the InAs x P1−x -InP core–shell nanowires were investigated using the coplanar x-ray diffraction performed at a synchrotron facility. Studies of series of symmetric and asymmetric x-ray Bragg reflections allowed us to determine the 26% ± 3% of As chemical composition in the InAs x P1−x core, core–shell relaxation, and the average tilt of the nanowires with respect to the substrate normal. Based on the x-ray diffraction, scanning, and transmission electron microscopy measurements, a model of the core–shell relaxation was proposed. Partial relaxation of the core was attributed to misfit dislocations formed at the core–shell interface and their linear density was estimated to be 3.3 ± 0.3 × 104 cm−1., Published by IOP Publ., Bristol

Roman wall fragments dating from 2nd and 3rd centuries AD, from two sites of the Roman province of Germania Superior, near the present day towns of Wossingen (Baden-Wurttemberg) and Mulheim-Karlich (Rheinland-Pfalz), were analyzed with synchrotron-based scanning macro-X-ray fluorescence (SR-MA-XRF) at the FLUO beamline (ANKA Synchrotron Radiation Facility, Karlsruhe Institute of Technology). Lead, iron, copper, calcium, potassium, among other elements, were detected and are correlated with red, blue, yellow and green pigments. In the fragments from Mulheim-Karlich, red has high correlation with Pb (red lead pigment), Fe and Ca were detected in 2 different hues of yellow respectively, and Cu is correlated with the blue pigment. The green pigment investigated in the Wossingen's fragments has high correlation with Fe and K, indicating the use of green earth, and the red pigment is correlated with iron, indicating the use of the red ochre. Synchrotron-based scanning macro-X-ray fluorescence applied in fragments of wall paintings has shown to be a fast, non-destructive and effective technique in the identification and discrimination of the pigments, plaster, different layers and impurities in paintings through the 2D elemental distribution.

We report on the growth and characterization of several sapphire single crystals for the purpose of x-ray optics applications. Structural defects were studied by means of laboratory double-crystal X-ray diffractometry and white beam synchrotron-radiation topography. The investigations confirmed that the main defect types are dislocations. The best quality crystal was grown using the Kyropoulos technique with a dislocation density of 102-103 cm-2 and a small area with approximately 2*2 mm2 did not show dislocation contrast in many reflections and has suitable quality for application as a backscattering monochromator. As a result, a clear correlation between growth rate and dislocation density is observed, though growth rate is not the only parameter impacting the quality.

Enrichment of hydrogels with inorganic particles improves their suitability for bone regeneration by enhancing their mechanical properties, mineralizability, and bioactivity as well as adhesion, proliferation, and differentiation of bone-forming cells, while maintaining injectability. Low aggregation and homogeneous distribution maximize particle surface area, promoting mineralization, cell-particle interactions, and homogenous tissue regeneration. Hence, determination of the size and distribution of particles/particle agglomerates in the hydrogel is desirable. Commonly used techniques have drawbacks. High-resolution techniques (e.g., SEM) require drying. Distribution in the dry state is not representative of the wet state. Techniques in the wet state (histology, µCT) are of lower resolution. Here, self-gelling, injectable composites of Gellan Gum (GG) hydrogel and two different types of sol-gel-derived bioactive glass (bioglass) particles were analyzed in the wet state using Synchrotron X-ray radiation, enabling high-resolution determination of particle size and spatial distribution. The lower detection limit volume was 9 × 10(-5) mm(3) . Bioglass particle suspensions were also studied using zeta potential measurements and Coulter analysis. Aggregation of bioglass particles in the GG hydrogels occurred and aggregate distribution was inhomogeneous. Bioglass promoted attachment of rat mesenchymal stem cells (rMSC) and mineralization.

International audience; Micro-damage mechanisms in a semicrystalline PolyAmide 6 polymer were characterized by in situ synchrotron radiation computed laminog-raphy (SRCL) using compact-tension like specimens with a notch root radius of 0.25 mm. SRCL allows the quantification of cavity nu-cleation, growth and coalescence in flat 2 mm-thick notched specimens with a micrometer resolution in 3D (under conditions of severe stress triaxiality) during the in situ loading. The maximum damage occurred at mid-thickness and was located at a small distance ∼ 200 µm from the notch root. It is shown that damage was distributed in distinct zones, that could be linked to different stress triaxiality states. Penny shaped cracks were found after some loadings. Their diameters were a function of the distance to the notch root: In a layer of about 33 µm no damage was found. In the adjacent 128 µm layer penny-shaped cracks were found with diameters of the order of average spherulite sizes (4-6 µm). In the next region 30-45 µm long cracks were found corresponding to several average spherulite diameters. During propagation, tunnel-like cracks formed ahead of the main crack. Finally, crack initiation location was found to be largely dependent on the roughness of the machined notch surface by comparing two samples with the same loading conditions.

A real-time synchrotron radiation study of the crystalline phase, texture formation and resulting surface roughness during deposition of thin La and LaN films is presented. For LaN, the theoretically predicted metastable wurtzite and zincblende structures were found, while La assumes the expected NaCl structure., Lanthanum and lanthanum nitride thin films were deposited by magnetron sputtering onto silicon wafers covered by natural oxide. In situ and real-time synchrotron radiation experiments during deposition reveal that lanthanum crystallizes in the face-centred cubic bulk phase. Lanthanum nitride, however, does not form the expected NaCl structure but crystallizes in the theoretically predicted metastable wurtzite and zincblende phases, whereas post-growth nitridation results in zincblende LaN. During deposition of the initial 2–3 nm, amorphous or disordered films with very small crystallites form, while the surface becomes smoother. At larger thicknesses, the La and LaN crystallites are preferentially oriented with the close-packed lattice planes parallel to the substrate surface. For LaN, the onset of texture formation coincides with a sudden increase in roughness. For La, the smoothing process continues even during crystal formation, up to a thickness of about 6 nm. This different growth behaviour is probably related to the lower mobility of the nitride compared with the metal. It is likely that the characteristic void structure of nitride thin films, and the similarity between the crystal structures of wurtzite LaN and La2O3, evoke the different degradation behaviours of La/B and LaN/B multilayer mirrors for off-normal incidence at 6.x nm wavelength.

Mineralization of hydrogel biomaterials is desirable to improve their suitability as materials for bone regeneration. In this study, gellan gum (GG) hydrogels were formed by simple mixing of GG solution with bioactive glass microparticles of 45S5 composition, leading to hydrogel formation by ion release from the amorphous bioactive glass microparticles. This resulted in novel injectable, self-gelling composites of GG hydrogels containing 20% bioactive glass. Gelation occurred within 20 min. Composites containing the standard 45S5 bioactive glass preparation were markedly less stiff. X-ray microcomputed tomography proved to be a highly sensitive technique capable of detecting microparticles of diameter approximately 8 μm, that is, individual microparticles, and accurately visualizing the size distribution of bioactive glass microparticles and their aggregates, and their distribution in GG hydrogels. The widely used melt-derived 45S5 preparation served as a standard and was compared with a calcium-rich, sol-gel derived preparation (A2), as well as A2 enriched with zinc (A2Zn5) and strontium (A2Sr5). A2, A2Zn, and A2Sr bioactive glass particles were more homogeneously dispersed in GG hydrogels than 45S5. Composites containing all four bioactive glass preparations exhibited antibacterial activity against methicillin-resistant Staphylococcus aureus. Composites containing A2Zn5 and A2Sr5 bioactive glasses supported the adhesion and growth of osteoblast-like cells and were considerably more cytocompatible than 45S5. All composites underwent mineralization with calcium-deficient hydroxyapatite upon incubation in simulated body fluid. The extent of mineralization appeared to be greatest for composites containing A2Zn5 and 45S5. The results underline the importance of the choice of bioactive glass when preparing injectable, self-gelling composites.

Synchrotron radiation computed laminography (SR-CL) is presented as an imaging method for analyzing the three-dimensional (3D) anatomy of leaves. The SR-CL method was used to provide 3D images of 1-mm² samples of intact leaves at a pixel resolution of 750 nm. The method allowed visualization and quantitative analysis of palisade and spongy mesophyll cells, and showed local venation patterns, aspects of xylem vascular structure and stomata. The method failed to image subcellular organelles such as chloroplasts. We constructed 3D computer models of leaves that can provide a basis for calculating gas exchange, light penetration and water and solute transport. The leaf anatomy of two different tomato genotypes grown in saturating light conditions was compared by 3D analysis. Differences were found in calculated values of tissue porosity, cell number density, cell area to volume ratio and cell volume and cell shape distributions of palisade and spongy cell layers. In contrast, the exposed cell area to leaf area ratio in mesophyll, a descriptor that correlates to the maximum rate of photosynthesis in saturated light conditions, was no different between spongy and palisade cells or between genotypes. The use of 3D image processing avoids many of the limitations of anatomical analysis with two-dimensional sections.

The applications of synchrotron radiation (SR) in medical imaging have become of great use, particularly in angiography, bronchography, mammography, computed tomography, and X-ray microscopy. Thanks to recently developed phase contrast imaging techniques non-destructive preclinical testing of low absorbing materials such as polymers has become possible. The focus of the present work is characterization and examination of UHMWPE-derived materials widely used in medicine, before and after their exposure to SR during such testing. Physical properties, such as wettability, surface energy, IR-spectroscopy, roughness, optical microscopy, microhardness measurements of UHMWPE samples were studied before and after SR. The relationship between a growth of UHMWPE surface hydrophilicity after SR and surface colonization by stromal cells was studied in vitro. Obtained results demonstrate that SR may be used as prospective direction to examine bulk (porous) structure of polymer materials and/or to modify polymer surface and volume for tissue engineering.

In this work, a group of Lu 2 SiO 5 :Tb (LSO:Tb) scintillating layers with a Tb concentration between 8% and 19% were investigated by means of synchrotron and laboratory techniques. The scintillation efficiency measurements proved that the highest light yield is obtained for a Tb concentration equal to 15%. At higher concentration, quenching processes occur which lower the light emission. The analysis of the reciprocal space maps of the (082) (280) and (040) Bragg reflections showed that LSO:Tb epilayers are well adapted on YbSO substrates for all the investigated concentrations. The spatial resolution tests demonstrated the possibility to achieve a resolution of 1 μm with a 6 μm thick scintillating layer.

X-ray phase-contrast microtomography (XPCμT) is a label-free, high-resolution imaging modality for analyzing early development of vertebrate embryos in vivo by using time-lapse sequences of 3D volumes. Here we provide a detailed protocol for applying this technique to study gastrulation in Xenopus laevis (African clawed frog) embryos. In contrast to μMRI, XPCμT images optically opaque embryos with subminute temporal and micrometer-range spatial resolution. We describe sample preparation, culture and suspension of embryos, tomographic imaging with a typical duration of 2 h (gastrulation and neurulation stages), intricacies of image pre-processing, phase retrieval, tomographic reconstruction, segmentation and motion analysis. Moreover, we briefly discuss our present understanding of X-ray dose effects (heat load and radiolysis), and we outline how to optimize the experimental configuration with respect to X-ray energy, photon flux density, sample-detector distance, exposure time per tomographic projection, numbers of projections and time-lapse intervals. The protocol requires an interdisciplinary effort of developmental biologists for sample preparation and data interpretation, X-ray physicists for planning and performing the experiment and applied mathematicians/computer scientists/physicists for data processing and analysis. Sample preparation requires 9-48 h, depending on the stage of development to be studied. Data acquisition takes 2-3 h per tomographic time-lapse sequence. Data processing and analysis requires a further 2 weeks, depending on the availability of computing power and the amount of detail required to address a given scientific problem.

We present the theoretical description of the image formation with the in-line germanium Bragg Magnifier Microscope (BMM) and the first successful phase retrieval of X-ray holograms recorded with this imaging system. The conditions under which the BMM acts as a linear shift invariant system are theoretically explained and supported by the experiment. Such an approach simplifies the mathematical treatment of the image formation and reconstruction as complicated propagation of the wavefront onto inclined planes can be avoided. Quantitative phase retrieval is demonstrated using a test sample and a proof of concept phase imaging of a spider leg is also presented.

In this work, we present preliminary in-line X-ray lensless projection imaging results at a synchrotron facility by using novel solid-state detectors based on non-destructive readout of photoluminescent colour centres in lithium fluoride thin films. The peculiarities of LiF radiation detectors are high spatial resolution on a large field of view, wide dynamic range, versatility and simplicity of use. These properties offered the opportunity to test a broadband X-ray synchrotron source for lensless projection imaging experiments at the TopoTomo beamline of the ANKA synchrotron facility by using a white beam spectrum (3-40 keV). Edge-enhancement effects were observed for the first time on a test object; they are discussed and compared with simulations, on the basis of the colour centre photoluminescence linear response found in the investigated irradiation conditions. (c) 2013 Elsevier Ltd. All rights reserved.

Novel X-ray imaging detectors based on photoluminescence of colour centres in lithium fluoride (LiF) have been proposed and tested for extreme ultraviolet, soft and hard X-rays up to 10 keV. For the first time we present the optical characterisation of LiF crystals and thin films irradiated at the TOPO-TOMO beamline of synchroton light source Anka (Karlsruhe, Germany) in the energy range 6-40 keV for different exposure times. Absorption and photoluminescence spectra were analysed to study the optical response of the LiF-based detectors. High resolved X-ray imaging of commercial test patterns has been obtained on LiF crystals and films by optical readout with a confocal laser scanning fluorescence microscope. © 2012 Elsevier B.V.

High resolution X-ray coplanar (symmetric X-ray diffraction (SXRD) and asymmetric X-ray diffraction (ASXRD)) and non-coplanar diffraction (grazing incidence diffraction (GID)) have been used to investigate the quality of AlGaN epilayers with 20% Al content, grown on sapphire using SiN x interlayers. The measurement of reciprocal space maps (RSM) with higher orders of reflections of SXRD and ASXRD which is readily performed at the synchrotron with high resolution and intensity reveals the presence of several diffraction peaks originating from the occurrence of local differences in the lattice constants. Two distinguishable AlGaN phases having different crystalline parameters were clearly recognized from X-ray data and the corresponding densities of screw dislocations have been determined measured as function of the overgrowth thickness varying from 0.5 μm to 3.5 μm. The variation of the screw and edge type dislocation densities with the overgrowth thickness has been found to follow the scaling law h − n where h is the thickness of the buffer layer.

The characterisation of the microstructure and micromechanical behaviour of paint is key to a range of problems related to the conservation or technical art history of paintings. Synchrotron-based X-ray laminography is demonstrated in this paper to image the local sub-surface microstructure in paintings in a non-invasive and non-destructive way. Based on absorption and phase contrast, the method can provide high-resolution 3D maps of the paint stratigraphy, including the substrate, and visualise small features, such as pigment particles, voids, cracks, wood cells, canvas fibres etc. Reconstructions may be indicative of local density or chemical composition due to increased attenuation of X-rays by elements of higher atomic number. The paint layers and their interfaces can be distinguished via variations in morphology or composition. Results of feasibility tests on a painting mockup (oak panel, chalk ground, vermilion and lead white paint) are shown, where lateral and depth resolution of up to a few micrometres is demonstrated. The method is well adapted to study the temporal evolution of the stratigraphy in test specimens and offers an alternative to destructive sampling of original works of art.

The kinetics of phase transitions during formation of small-scale systems are essential for many applications. However, their experimental observation remains challenging, making it difficult to elucidate the underlying fundamental mechanisms. Here, we combine in situ and real-time synchrotron X-ray diffraction (XRD) and X-ray reflectivity (XRR) experiments with substrate curvature measurements during deposition of nanoscale Mo and Mo1–xSix films on amorphous Si (a-Si). The simultaneous measurements provide direct evidence of a spontaneous, thickness-dependent amorphous-to-crystalline (a–c) phase transition, associated with tensile stress build-up and surface roughening. This phase transformation is thermodynamically driven, the metastable amorphous layer being initially stabilized by the contributions of surface and interface energies. A quantitative analysis of the XRD data, complemented by simulations of the transformation kinetics, unveils an interface-controlled crystallization process. This a–c phas...

Roman mural green pigment painting fragments from three Roman sites in the north of the Roman province Germania Superior: Koblenz Stadtwald Remstecken (KOSR), Weisenthurm “Am guten Mann” (WEIS) and Mendig Lungenkarchen (MELU), dating from second and third centuries AD were analyzed. The experiments were performed nondestructively using synchrotron-based scanning macro-X-ray fluorescence (SR-MA-XRF), synchrotron-based scanning micro-X-ray fluorescence (SR-μ-XRF), synchrotron-based X-ray diffraction (SR-XRD) and Raman spectroscopy. Correlation between SR-MA-XRF, SR-μ-XRF elemental map distributions and optical images of scanned areas was mainly found for the elements Ca, Fe and K. With XRF, Fe and K were identified correlated with green pigment, but in samples from two sites, Mendig Lungenkarchen and Weisenthurm “Am guten Mann”, also Cu was detected in minor concentration. The results of SR-XRD and Raman spectroscopy were limited to one sample from Weisenthurm “Am guten Mann”. In this sample, green earth and calcium carbonate were identified by SR-XRD and, additionally, malachite by Raman spectroscopy.

Nuclear instruments & methods in physics research / A 833, 68 - 76(2016). doi:10.1016/j.nima.2016.07.005, The white beam (∼6–80 keV) available at the TopoTomo X-ray beamline of the ANKA synchrotron facility (KIT, Karlsruhe, Germany) was used to perform edge-enhancement imaging tests on lithium fluoride radiation detectors. The diffracted X-ray image of a microscopic boron fibre, consisting of tungsten wire wrapped by boron cladding, was projected onto lithium fluoride thin films placed at several distances, from contact to 1m. X-ray photons cause the local formation of primary and aggregate colour centres in lithium fluoride; these latter, once illuminated under blue light, luminesce forming visible-light patterns—acquired by a confocal laser scanning microscope—that reproduce the intensity of the X-ray diffracted images. The tests demonstrated the excellent performances of lithium fluoride films as radiation detectors at the investigated photon energies. The experimental results are here discussed and compared with those calculated with a model that takes into account all the processes that concern image formation, storing and readout., Published by Elsevier, Amsterdam

The performance of a recently developed full-field X-ray micro-imaging system based on an in-line Bragg magnifier is reported. The system is composed of quasi-channel-cut crystals in combination with a Medipix single-photon-counting detector. A theoretical and experimental study of the imaging performance of the crystals–detector combination and a comparison with a standard indirect detector typically used in high-resolution X-ray imaging schemes are reported. The spatial resolution attained by our system is about 0.75 µm, limited only by the current magnification. Compared with an indirect detector system, this system features a better efficiency, signal-to-noise ratio and spatial resolution. The optimal working resolution range of this system is between ∼0.4 µm and 1 µm, filling the gap between transmission X-ray microscopes and indirect detectors. Applications for coherent full-field imaging of weakly absorbing samples are shown and discussed.

Titanium beryllide Be12Ti and vanadium beryllide Be12V are considered to be promising materials for advanced neutron multipliers in the helium-cooled breeding blanket of DEMO reactor. A study of the surface layers of oxidized beryllide specimens by means of powder X-ray diffraction technique is presented in this work. The phase composition of the near-to-surface layers of Be12Ti and Be12V specimens was investigated at the Single Crystal Diffraction (SCD) beamline at ANKA synchrotron facility after air-annealing at 800 °C. A high surface sensitivity of measurements was achieved at grazing incidence conditions by varying the incidence angle. Since beryllium has low values of X-ray absorption, the near-surface regions having depths from 2 up to 20 μm were investigated. The main objective of the work is the evaluation of composition of the reactant products which can influence the parameters of retention and release of radiogenic gases.

During the last years the electron beams produced by Laser-Plasma Accelerators were used for the first time to generate synchrotron radiation in an undulator. Both the emittance and especially the energy spread of a laser plasma accelerator beam are significantly larger than the emittance and the energy spread of beams from conventional accelerators. Beams with a high energy spread produce in a conventional undulator photon beams with a high wavelength spread. In this paper a novel modified undulator design is presented which can reduce the energy spread of the photon beam caused by the energy spread of the electron beam. The magnetic concept is analysed in detail by tracking test electrons through the device. An experiment to test this concept is in preparation.

Computed tomography (CT) is a three-dimensional (3D) imaging method which, for compact or prolate (i.e. rather isotropically extended around the rotation axis) specimens, can yield artefact-free reconstructed cross-sections. Laterally extended specimens like plate-like objects, however, are much less amenable to CT since reliable projection data cannot be acquired from angles where the plate is oriented parallel to the irradiation direction. To overcome this drawback, computed laminography (CL) was introduced recently to imaging set-ups at synchrotron storage rings. Here, we report on the first implementation of computed laminography with neutron radiation, showing measurements that were performed at the ANTARES neutron imaging facility at the FRM II research reactor of Technische Universitat Munchen. In general, neutrons are highly interesting probes for imaging since they provide a sensitivity to chemical elements very different from X-rays, yielding complementary information about the specimens investigated. Like for X-ray laminography, we avoid the projection directions where the beam is parallel to the long extensions of the specimen. We accomplish this by tilting of the rotation axis with respect to the transmitted-beam to an angle smaller than 90° (which would be the limiting case of CT) and roughly aligning the specimen's surface normal parallel to this rotation axis. The principles of neutron laminography are introduced and first test experiments are described.

One of the most promising methods of phase-contrast imaging is the Talbot grating interferometry. We report about the optimization of the method for fast imaging, requiring reduced exposure times by keeping sufficient imaging contrast. To do this a new Talbot interferometer working with a broad energy bandwidth beam has been installed at the Topo–Tomo beamline at ANKA. We demonstrate the method with a filtered white beam and without the need of a source grating that is commonly used at moderate-emittance synchrotron sources. Taking advantage of a higher photon flux, the exposure time is significantly reduced. At the same time, images obtained with this setup show a sufficient visibility contrast of 25% on average, which opens the way for new applications in real-time measurements.

In this work an X-ray imaging system based on a recently developed in-line two-dimensional Bragg magnifier composed of two monolithic V-shaped crystals made of dislocation-free germanium is presented. The channel-cut crystals were used in one-dimensional and in two-dimensional (crossed) configurations in imaging applications and allowed measurement of phase-contrast radiograms both in the edge-enhanced and in the holographic regimes. The measurement of the phase gradient in two orthogonal directions is demonstrated. The effective pixel size attained was 0.17 mu m in the one-dimensional configuration and 0.5 mu m in the two-dimensional setting, offering a twofold improvement in spatial resolution over devices based on silicon. These results show the potential for applying Bragg magnifiers to imaging soft matter at high resolution with reduced dose owing to the higher efficiency of Ge compared with Si.

Babcock Noell GmbH (BNG) is completing the fabrication of a 1.5 m long superconducting insertion device for the Karlsruhe Institute of Technology (KIT). The unit is planned to be installed in the ANKA storage ring at the end of 2010 to become the light source of the new beamline NANO for high resolution X-ray diffraction. The period length of the device is 15 mm for a total of 100.5 full periods plus an additional matching period at each end. The key specifications of the system are: a K value higher than 2 for a magnetic gap of 5 mm, the capability of withstanding a 4 W beam heat load and a phase error smaller than 3.5 degrees. The superconducting coils have been qualified by means of a vertical test in liquid helium at CERN and are ready to be installed in the cryostat. This paper describes the main features of the system.

In this contribution we report the results of the training and of the local field measurements performed in a liquid helium bath of the ANKA superconducting undulator. The period length is 15 mm and the coils are 1.5 m long. The key specifications of the system are an undulator parameter K higher than 2 (for a magnetic gap of 5 mm) and a phase error smaller than 3.5 degrees. The superconducting undulator is planned to be installed in the ANKA storage ring by the beginning of 2011 to be the light source of the new beamline NANO for high resolution X-ray diffraction..

Accurate magnetic field measurements are a prerequisite for the characterization and optimization of undulators. The precision for measuring the magnetic properties of conventional, i.e., permanent magnet based insertion devices, has undergone tremendous improvements over the past 10 to 15 years initiating a new era in synchrotron light sources worldwide; a similar break through is now necessary in the field of superconducting insertion devices. In this contribution we describe the planned instrumentation needed to perform magnetic measurements of the local field, and field integrals, of up to 2 m length superconducting undulator coils while in a cold-in-vacuum (helium free) environment.

Superconducting insertion devices (IDs) are very attractive for synchrotron light sources since they offer the possibility to enhance the tuning range and functionality significantly by period length switching. Period length switching can be achieved by employing two or more individually powerable subsets of superconducting coils and reverse the current in a part of the windings. In this contribution we report the first experimental test of this principle demonstrated on a 70 mm NbTi mock-up coil with period tripling, allowing to switch between a 15 mm period length undulator and a 45 mm wiggler (SCUW 15/45).

In order to produce synchrotron radiation of the highest brilliance, third generation synchrotron sources make use of insertion devices (IDs). The state of the art available today for IDs is the permanent magnet technology with magnet blocks placed inside the vacuum (IVU) of the storage ring. Following an initial proposal at SPring-8 [1], the concept of Cryogenic Permanent Magnet Undulators (CPMU) is presently considered as a possible future evolution of in-vacuum undulators [2–5]. Superconducting undulators (SCUs) can reach, for the same gap and period length, even higher fields than CPMU devices, allowing increases in the spectral range and the brilliance. At ANKA we are running a research and development program to develop superconducting IDs. The proof of principle of SCU technology application in a storage ring has been demonstrated at ANKA with a device developed together with the company ACCEL Instr. GmbH and installed in the ANKA storage ring since March 2005 [6].

The efficiency of high-resolution pixel detectors for hard X-rays is nowadays one of the major criteria which drives the feasibility of imaging experiments and in general the performance of an experimental station for synchrotron-based microtomography and radiography. Here the luminescent screen used for the indirect detection is focused on in order to increase the detective quantum efficiency: a novel scintillator based on doped Lu(2)SiO(5) (LSO), epitaxially grown as thin film via the liquid phase epitaxy technique. It is shown that, by using adapted growth and doping parameters as well as a dedicated substrate, the scintillation behaviour of a LSO-based thin crystal together with the high stopping power of the material allows for high-performance indirect X-ray detection. In detail, the conversion efficiency, the radioluminescence spectra, the optical absorption spectra under UV/visible-light and the afterglow are investigated. A set-up to study the effect of the thin-film scintillator's temperature on its conversion efficiency is described as well. It delivers knowledge which is important when working with higher photon flux densities and the corresponding high heat load on the material. Additionally, X-ray imaging systems based on different diffraction-limited visible-light optics and CCD cameras using among others LSO-based thin film are compared. Finally, the performance of the LSO thin film is illustrated by imaging a honey bee leg, demonstrating the value of efficient high-resolution computed tomography for life sciences.

X-ray computed laminography (CL) with synchrotron radiation is used to investigate fracture in carbon fibre–epoxy laminates. CL allows for high-resolution (∼1 μm) imaging of laterally extended objects. Whilst artefacts inherent to CL data reduce image quality compared with computed tomography (CT), imaging regions of interest in large planar samples greatly increases the engineering applicability. High-resolution in situ three-dimensional analysis of structural failure is therefore achievable at levels that would be impossible via CT or any other volume-imaging methods.

The current report covers the establishment of an in situ X-ray diffraction tensile experiment at the synchrotron ANKA located at Forschungszentrum Karlsruhe for probing diffraction signals from nanocrystalline thin films during tensile deformation. Measurements on nanocrystalline palladium films verify the capabilities of the setup.

X-ray detector systems are powerful tools: in combination with tomographic methods they provide volumetric data of samples in a non-destructive manner which is of high interest for, e.g., biology, medicine or materials research. The detector able to provide images with submicrometer spatial resolution frequently consists of a scintillator screen, light microscopy optics and a digital camera. Here, the scintillator converts the X-rays into a visible light image which is projected onto the camera by the light optics. In order to perform high resolution imaging Single Crystal Film (SCF) scintillators 1 mum to 30 mum thin are required due to the limited depth of focus of the microscopy optics. Thin SCFs can be obtained via liquid phase epitaxy (LPE). A drawback is that a detector working with SCFs suffers from low efficiency (2% at 50 keV) owing to their limited thickness. The detective quantum efficiency (DQE) is here mainly limited by the low absorption of X-rays and the light yield in the thin scintillator layer. Performances, i.e absorption, light yield, afterglow of operational systems at the European Synchrotron Radiation Facility (ESRF) using YAG:Ce (Y3Al5O12:Ce), LAG:Eu (Lu3Al5O12:Eu) and GGG:Eu (Gd3Ga5O12:Eu) scintillators will be presented and compared to new LSO:Tb (Lu2SiO5:Tb) scintillators developed in the framework of an European project , . A new concept to improve the efficiency of detection in the 20 keV - 40 keV energy range with 1 mum spatial resolution will be presented. This concept based on multilayer scintillators is realised by the LPE process as well. First results will be illustrated with X-ray images and will demonstrate the absorption efficiency improvement of the X-ray detector. The expected performance is 7 times better than the LAG-based scintillators.

Superconducting insertion devices are very attractive for synchrotron light sources. For a given gap and period length, higher fields can be reached in respect to permanent magnet insertion devices thus permitting to reach higher photon fluxes. A new R&D program has been recently launched at ANKA aiming for the development of the next generation superconducting insertion devices for light sources. A cold bore superconducting undulator (14 mm period length, 100 full periods long) is installed in the ANKA storage ring since three years. This will be replaced by an improved version which shows a more efficient cooling system and a high precision design aiming for reduced field errors. Two additional devices are scheduled. One will allow to electrically switch the period length between 15 mm and 45 mm corresponding to an undulator and a wiggler mode, respectively. The other will be optimized for third generation light sources. It will be capable of tolerating higher beam heat loads up to 6 W while achieving very small field errors. The field error minimization will be obtained through the use of new shimming concepts which will correct inaccuracies due to manufacturing tolerances. This paper describes the technical concepts of the three projects.

The TopoTomo bending magnet beamline at the ANKA synchrotron facility in Karlsruhe (Germany) operates in the hard X-ray regime (above 6 keV). Recently, an X-ray micro-imaging station has been installed at TopoTomo. For typical imaging applications, a filtered white beam or from 2009 on a double-multilayer monochromator is used. In order to optimize the field of view and the resolution of the available indirect pixel detectors, different optical systems have been installed, adapted, respectively, to a large field of view (macroscope) and to high spatial resolution (microscope). They can be combined with different camera systems, ranging from 14-bit dynamic range CCDs to fast CMOS cameras. The spatial resolution can be brought substantially beyond the micrometer limit by using a Bragg magnifier. Due to the moderate flux of the beamline compared to insertion-device beamlines on third generation light sources, special emphasis has been put on the efficiency of the detectors via a dedicated scintillator concept. The layout of the beamline optics makes optimal use of the coherence properties. Thus, absorption contrast, phase-contrast and analyzer-based imaging can be applied. Additionally, white beam synchrotron topography is performed, using digital indirect X-ray pixel detectors as well as X-ray film.

Accurate magnetic field measurements are a prerequisite for the characterization and optimization of undulators. At the synchrotron light source ANKA there is an ongoing R&D program for superconducting insertion devices. Within this program a test stand for precise magnetic field measurements of superconductive coils was designed, built and installed at the Research Center Karlsruhe. Comprehensive magnetic measurements are performed to confirm the magnet design and to detect or correct field imperfections resulting from the manufacturing process. The magnetic field is measured along a fixed direction by Hall probes with a positioning precision of 3 mum. A NbTi undulator prototype with local correction coils was built to verify the performance of the superconductor and the shimming concept. In this contribution we describe the measuring test station and preliminary tests results including the efficiency of the shimming concept.

More than one hundred years ago, Lucien Bull showed, by means of his famous high-speed cinematographic movies of living species, the outstanding scientific value of time-resolved imaging, e.g. to understand the mechanisms behind insect flight [1]. For X-ray imaging, synchrotron light sources offer a photon beam that (i) propagates quasi-parallel, (ii) has fluxes that are higher by orders of magnitude than laboratory sources, and (iii) allows one to exploit more sophisticated contrast modalities. The use of synchrotron light is thus the next step in fast-imaging development: high-speed hard X-ray cineradiography employing phase contrast mechanisms [2,3]. Imaging with X-rays offers the chance to investigate complex kinematics of, for example, feeding and locomotion devices of animals, as the penetrating nature of the radiation reveals internal information.

Superconducting undulators and wigglers are developed for synchrotron light sources, damping rings for linear colliders and polarized positron sources. In an undulator the emitted photons along the trajectory have to interfere. In order to do so the magnetic field in all periods has to be almost identical. The field strength over one or several hundred periods is not allowed to deviate by more than 1%. Translated into mechanical accuracy the position of the wire and the poles has to be more accurate than about 5 over 1 to 2 m. High quality measurement of the field is an essential requirement. In this paper we present two field measuring systems, one is under construction and another one is under design phase at the Forschungszentrum Karlsruhe.

LiNi0.5Mn1.5O4 spinel cathode was studied during the first discharge cycle using combined full field Transmission X-ray Microscopy (TXM) and X-ray Absorption Near Edge Structure Spectroscopy (XANES) techniques to follow the chemical phase transformation as well as the microstructural evolution of cathode materials upon operation within an electrochemical cell. The spatial distribution and electrochemical process of the spinel material with spherical granules of 30 μm and 3 μm crystallite size was investigated. The spectroscopic imaging of the cathode within field of view of 40 × 32 μm(2) and spatial resolution of 40 nm has revealed an increase of the LiNi0.5Mn1.5O4 granule size during lithiation providing an insight into the effect of the particle size and morphology on the electrochemical process. The chemical elemental distribution and the content of the different oxidation states of the two absorbing elements (Ni and Mn) have been determined in operando from the XANES imaging. A gradual increase in the content of the oxidation state Mn(3+) from 8% up to 64% has been recorded during the discharge from 5 V to 2.7 V. The study of the local oxidation reduction behavior of Mn(3+) reveals a reversibility aspect in the local electrochemical reaction of Mn(4+) toward Mn(3+) in areas located in the center of the aggregate as well as in areas closed to the electrolyte. During the discharge process, a mixture of Mn(3+) and Mn(4+) has been detected while only single electron valence states have been found in the case of Ni. Probing the chemical changes during the discharge using two-dimensional XANES reveals spatial differences in the electrochemical activities of the two absorbing elements Ni and Mn.

High resistivity, chromium compensated gallium arsenide (HR-GaAs:Cr) has recently shown to be a promising sensor material for X-ray detectors due to its high resistivity, its fully active volume, the good electron transport properties and good absorption properties for photon energies up to around 40 keV. These properties make this material a favorable candidate for producing sensors for photon counting X-ray imaging detectors. Such detector systems have also gained increasing attention to be used for high flux applications as found at synchrotrons or in medical applications like computed tomography. Whereas other interesting high-Z materials such as CdTe have already been studied under high flux irradiation, the behavior of HR-GaAs:Cr under such conditions has yet to be investigated. In this work, we study the performance of a 500 μm thick GaAs:Cr sensor, bump-bonded to Timepix readout electronics, with a main emphasis laid on the behavior under the irradiation of high X-ray fluxes using a monochromatic synchrotron beam. We find that, at high X-ray fluxes, the detector performance degrades, and that the dislocation network typically present in melt-grown GaAs influences the detection properties due to local variations of the charge transport properties. However, we also demonstrate that the high flux behavior can be substantially improved by optimized chip settings, namely by tuning the Timepix' preamplifier output pulse shape. In this way, the photon counting capabilities of the detector assembly are restored to a certain extent and it is possible to operate the detector assembly at impinging fluxes as high as 1010 s−1mm−2.

Grating-based x-ray differential phase-contrast imaging (DPCI) is capable of acquiring information based on phase-shift and dark-field signal, in addition to conventional x-ray absorption-contrast. Thus DPCI gives an advantage to investigate composite materials with component wise similar absorption properties like soft tissues. Due to technological challenges in fabricating high quality gratings over a large extent, the field of view (FoV) of the imaging systems is limited to a grating area of a couple of square centimeters. For many imaging applications (e.g. in medicine), however, a FoV that ranges over several ten centimeters is needed. In this manuscript we propose to create large area gratings of theoretically any extent by assembling a number of individual grating tiles. We discuss the precision needed for alignment of each microstructure tile in order to reduce image artifacts and to preserve minimum 90% of the sensitivity obtainable with a monolithic grating. To achieve a reliable high precision alignment a semiautomatic assembly system consisting of a laser autocollimator, a digital microscope and a force sensor together with positioning devices was built. The setup was used to tile a first four times four analyzer grating with a size of 200 mm × 200 mm together with a two times two phase grating. First imaging results prove the applicability and quality of the tiling concept.