TY - JOUR A1 - Schob, D. A1 - Sagradov, I. A1 - Roszak, R. A1 - Sparr, H. A1 - Franke, R. A1 - Ziegenhorn, M. A1 - Kupsch, Andreas A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Experimental determination and numerical simulation of material and damage behaviour of 3D printed polyamide 12 under cyclic loading N2 - The material and damage behaviour of additively manufactured polyamide 12 under cyclic loading was characterized by cyclic tests and microstructure analysis by using microscopy, X-ray refraction, and computed tomography. The results were used to determine parameters for the viscoplastic material model by Chaboche and a damage model by Gurson-Tvergaard-Needleman. The temperature was monitored during the experiments and the self-heating effect was observed. By including this effect, a higher accuracy could be achieved with the results of mechanical experiments. KW - 3D printing Polyamide 12 KW - Chaboche model KW - GTN model KW - Material and damage behaviour KW - X-ray refraction KW - Computed tomography PY - 2020 DO - https://doi.org/10.1016/j.engfracmech.2019.106841 SN - 0013-7944 VL - 229 SP - 106841-1 EP - 106841-13 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-50557 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rack, A. A1 - Riesemeier, Heinrich A1 - Zabler, S. A1 - Weitkamp, T. A1 - Müller, Bernd R. A1 - Weidemann, Gerd A1 - Modregger, P. A1 - Banhart, J. A1 - Helfen, L. A1 - Danilewsky, A.N. A1 - Gräber, H.G. A1 - Heldele, R. A1 - Mayzel, B. A1 - Goebbels, Jürgen A1 - Baumbach, T. ED - Stuart R. Stock, T1 - The high-resolution synchrotron-based imaging stations at the BAMline (BESSY) and TopoTomo (ANKA) N2 - The BAMline at the BESSY light source in Berlin and the TopoTomo beamline at the ANKA synchrotron facility in Karlsruhe (both Germany) operate in the hard X-ray regime (above 6 keV) with similiar photon flux density. For typical imaging applications, a double multilayer monochromator or a filtered white beam is used. In order to optimise 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 16-bit dynamic range slow-scan CCDs to fast CMOS cameras. The spatial resolution can be brought substantially beyond the micrometer limit by using a Bragg magnifier. The moderate flux of both beamlines compared to other 3rd generation light sources is compensated by a dedicated scintillator concept. For selected applications, X-ray beam collimation has proven to be a reliable approach to increase the available photon flux density. Absorption contrast, phase contrast, holotomography and refraction-enhanced imaging are used depending on the application. Additionally, at the TopoTomo beamline digital white beam synchrotron topography is performed, using the digital X-ray pixel detectors installed. KW - Microtomography KW - Non-destructive evaluation KW - Coherent imaging KW - X-ray refraction KW - X-ray phase contrast KW - Synchrotron-CT KW - Synchrotron instrumentation KW - Scintillator KW - Bragg magnification KW - Holotomography KW - X-ray topography PY - 2008 DO - https://doi.org/10.1117/12.793721 SN - 0277-786X VL - 7078 SP - 70780X-1 - 70780X-9 AN - OPUS4-18296 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mouiya, M. A1 - Martynyuk, M. A1 - Kupsch, Andreas A1 - Laquai, R. A1 - Müller, Bernd R. A1 - Doyen, N.T. A1 - Tamraoui, Y. A1 - Serrano-Munoz, Itziar A1 - Huger, M. A1 - Kachanov, M. A1 - Bruno, Giovanni T1 - The stress–strain behavior of refractory microcracked aluminum titanate: The effect of zigzag microcracks and its modeling N2 - The stress–strain behavior of ceramics, such as aluminum titanate, has certain features that are unusual for brittle materials—in particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the sharp increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and are attributed to microcracking. Here we compare different degrees of stress–strain nonlinearity of aluminum titanate materials and quantitatively model them. We use advanced mechanical testing to observe the mechanical response at room and high temperature; electron microscopy, and X-ray refraction radiography to observe the microstructural changes. Experiments show that two types of microcracks can be distinguished: (i) microcracks induced by cooling from the sintering temperature (due to heterogeneity and anisotropy of thermal expansion), with typical sizes of the order of grain size, and (ii) much larger microcracks generated by the mechanical loading. The two microcrack types produce different effects on the stress–strain curves. Such microcracks and the features of the stress–strain behavior depend on the density of the cooling-induced microcracks and on the distribution of grain sizes. They are modeled analytically and numerically. KW - Hystersis KW - Nonlinear stress-strain curve KW - Refractory KW - Stiffness KW - X-ray refraction PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-580517 DO - https://doi.org/10.1111/jace.19325 SN - 1551-2916 VL - 106 SP - 6995 EP - 7008 PB - Wiley-Blackwell CY - Oxford [u.a.] AN - OPUS4-58051 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schob, D. A1 - Roszak, R. A1 - Sagradov, I. A1 - Sparr, H. A1 - Ziegenhorn, M. A1 - Kupsch, Andreas A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Experimental determination and numerical simulation of material and damage behaviour of 3D printed polyamide 12 under quasi-static loading N2 - In order to characterise the material and damage behaviour of additively manufactured polyamide 12 (PA12) under quasi-static load and to implement it in a numerical model, experiments under quasi-static load as well as microstructural investigations were carried out. Selective laser sintering (SLS) was used as the manufacturing process. For the classification of the material behaviour, quasi-static cyclic tests with holding times as well as tensile tests were performed. X-ray refraction and computed tomography (CT) were used to investigate the damage behaviour. The Chaboche model, which has already been applied for metallic materials under thermomechanical loading, served as the basis for the selection of the numerical material model. The same procedure was used for the selection of the damage model, where the Gurson–Tvergaard–Needleman (GTN) model was chosen, which was already used for porous metallic materials. The Chaboche model shows very good agreement with experimental results. Furthermore, the coupling with the GTN model allows a very good modelling of the damage behaviour. Finally, it could be shown that the selected models are suitable to simulate the material and damage behaviour of 3D printed PA12. KW - Polyamide 12 KW - 3D printing KW - Viscoplastic KW - Chaboche model KW - Damage KW - GTN model KW - X-ray refraction KW - Computed tomography PY - 2019 DO - https://doi.org/10.24423/aom.3162 SN - 0373-2029 VL - 71 IS - 4-5 SP - 507 EP - 526 PB - IPPT PAN - Polish Academy of Sciences, Institute of Fundamental Technological Research CY - Warsaw AN - OPUS4-49409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Cooper, R.C. A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Wheeler, M. A1 - Hentschel, Manfred P. A1 - Staude, Andreas A1 - Pandey, A. A1 - Shyam, A. A1 - Bruno, Giovanni T1 - Stress-induced microcrack density evolution in β-eucryptite ceramics: Experimental observations and possible route to strain hardening N2 - In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measure the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. The mechanisms proposed would allow the development of a strain hardening route in ceramics. KW - Beta-eucryptite KW - Microcracked ceramics KW - X-ray refraction KW - Tensile load KW - Strain hardening KW - Synchrotron KW - BAMline KW - Computed Tomography KW - CT PY - 2018 UR - http://www.sciencedirect.com/science/article/pii/S1359645417308881 DO - https://doi.org/10.1016/j.actamat.2017.10.030 SN - 1359-6454 SN - 1873-2453 VL - 144 IS - Supplement C SP - 627 EP - 641 PB - Elsevier B.V. AN - OPUS4-43024 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Harwardt, Michael A1 - Hentschel, Manfred P. A1 - Illerhaus, Bernhard A1 - Goebbels, Jürgen A1 - Bamberg, J. A1 - Heutling, F. T1 - Micro Crack Characterization of Metal Matrix Composites by 3D-Refraction-Computed-Tomography T2 - 16th World Conference on Nondestructive Testing CY - Montreal, Canada DA - 2004-08-30 KW - NDE KW - X-ray refraction KW - Composites KW - MMC PY - 2004 SP - 9 pages PB - International Committee for Non-Destructive Testing CY - Montreal AN - OPUS4-5486 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Soares, A.P. A1 - Baum, D. A1 - Hesse, B. A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Zaslansky, P. T1 - Scattering and phase-contrast X-ray methods reveal damage to glass fibers in endodontic posts following dental bur trimming N2 - Objectives. There is concern that the integrity of fiberglass dental posts may be affected by chairside trimming during treatment. We hypothesize that hard X-ray methods of phase contrast-enhanced micro-CT (PCE-CT) and synchrotron based X-ray refraction (SXRR) can reliably identify and help characterize the extent of damage. Methods. Fiberglass posts were imaged both as manufactured and following trimming with a diamond bur. Each of the posts was imaged by SXRR and by PCE-CT. Datasets from PCE-CT were used to visualize and quantify 2D and 3D morphological characteristics of intact and of damage-affected regions caused by trimming. Results. The SXRR images revealed fiber inhomogeneities from manufacturing with a significant increase in internal surfaces in sample regions corresponding to damage from trimming. PCE-CT volumes unveiled the micromorphology of single fibers in the posts and some damage in the trimmed area (e.g. fractures, splinters and cracks). Area, perimeter, circularity, roundness, volume and thickness of the glass fibers in the trimmed area were statistically different from the control (p < 0.01). Significance. The integrity of single fibers in the post is critical for bending resistance and for long-term adhesion to the cement in the root canals. Damage to the fibers causes substantial structural weakening across the post diameter. Glass fragments produced due to contact with the dental bur may separate from the post and may significantly reduce bond capacity. The above mentioned synchrotron-based imaging techniques can further facilitate assessment of the structural integrity and the appearance of defects in posts (e.g. after mechanical load). KW - Fiberglass composite KW - Fiber reinforced dental post KW - X-ray refraction KW - Phase contrast-enhanced micro-CT KW - Non-destructive testing PY - 2021 DO - https://doi.org/10.1016/j.dental.2020.10.018 SN - 0109-5641 VL - 37 IS - 2 SP - 201 EP - 211 PB - Elsevier Inc. AN - OPUS4-52071 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Harwardt, Michael A1 - Hentschel, Manfred P. A1 - Illerhaus, Bernhard A1 - Goebbels, Jürgen T1 - Synchrotron Refraction CT and Synchrotron Bragg Magnification CT for NDE N2 - X-ray refraction topography techniques are based on ultra-small angle scattering by micro-structural elements causing phase-related effects such as refraction and total reflection at a few minutes of arc as the refractive index of X-rays is nearly unity. The refraction contrast is several times higher than “true absorption” and results in images of cracks, pores and fibre debonding separations below the spatial resolution of the detector. In most cases the investigated inner surface and interface structures correlate to mechanical properties. For the exploration of micro structured materials the refraction technique has been improved by a 3D Synchrotron Refraction Computed Tomography test station. The specimen is placed in an X-ray beam between two single crystals, which suppresses all sample scattering. In addition, an asymmetric cut second crystal can magnify the image up to 50 times revealing nano meter resolution. The technique is an alternative to other attempts on raising the spatial resolution of CT machines. KW - X-ray refraction KW - Diffraction Enhanced Imaging (DEI) KW - Bragg magnification KW - Synchrotron radiation KW - Computed Tomography (CT) KW - Metal Matrix Composites (MMC) KW - Lightweight materials KW - Aerospace PY - 2008 DO - https://doi.org/10.1784/insi.2008.50.6.316 SN - 0007-1137 VL - 50 IS - 6 SP - 316 EP - 319 PB - British Institute of Non-Destructive Testing CY - Northampton AN - OPUS4-18001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Goebbels, Jürgen A1 - Müller, Bernd R. A1 - Riesemeier, Heinrich A1 - Weidemann, Gerd ED - Mazal, P. T1 - Special Solutions for CT-Investigations with Synchrotron Radiation T2 - 2nd International Workshop of NDT Experts CY - Prague, Czech Republic DA - 2003-10-06 KW - Computed Tomography KW - Synchrotron radiation KW - X-ray refraction KW - Metal matrix composites KW - Porosity PY - 2003 SN - 80-2142475-3 SP - 91 EP - 97 PB - Univ. of Technology CY - Brno AN - OPUS4-2876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Hentschel, Manfred P. A1 - Lange, Axel A1 - Müller, Bernd R. T1 - X-ray dark field imaging N2 - A new kind of enhanced contrast X-ray imaging of weakly absorbing materials in dark field mode is presented. Samples such as plastics and biological tissue are a perpetual challenge for radiographic imaging. Recent innovative approaches such as Diffraction Enhanced Imaging (DEI), “phase contrast”, grating interferometry (Talbot-Lau), or Refraction Enhanced Imaging (REI) have in common that they yield enhanced contrast based on deflected X-rays. Here, we introduce a REI modification, which works with a slightly bent single crystal reflecting in Bragg geometry. The samples are placed upstream of the thin crystal within a parallel synchrotron beam. The crystal’s curvature creates a dark-field stripe in the transmission image, similar to the inverse of a Darwin-Prins rocking curve of plane crystals. The reflection condition is met better or worse as a steady function of incidence position. Refracted beam portions of sample interfaces appear bright on black stripes. The entire image is finally synthesized by multiple dark-field stripes. The technique is an alternative to the mentioned techniques. We demonstrate the technique’s advantage by examples of biological and technical microstructures. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - X-ray refraction KW - Refraction enhanced imaging (REI) KW - Phase contrast KW - Radiology KW - Soft matter radiography PY - 2014 SN - 978-80-214-5018-9 SP - 1 EP - 7 AN - OPUS4-31971 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Harwardt, Michael A1 - Hentschel, Manfred P. T1 - Synchrotron-based micro-CT and refraction-enhanced micro-CT for non-destructive materials characterisation N2 - X-ray computed tomography is an important tool for non-destructively evaluating the 3-D microstructure of modern materials. To resolve material structures in the micrometer range and below, high brilliance synchrotron radiation has to be used. The Federal Institute for Materials Research and Testing (BAM) has built up an imaging setup for micro-tomography and -radiography (BAMline) at the Berliner storage ring for synchrotron radiation (BESSY). In computed tomography, the contrast at interfaces within heterogeneous materials can be strongly amplified by effects related to X-ray refraction. Such effects are especially useful for materials of low absorption or mixed phases showing similar X-ray absorption properties that produce low contrast. The technique is based on ultra-small-angle scattering by microstructural elements causing phase-related effects, such as refraction and total reflection. The extraordinary contrast of inner surfaces is far beyond absorption effects. Crack orientation and fibre/matrix debonding in plastics, polymers, ceramics and metal-matrix-composites after cyclic loading and hydro-thermal aging can be visualized. In most cases, the investigated inner surface and interface structures correlate to mechanical properties. The technique is an alternative to other attempts on raising the spatial resolution of CT machines. KW - Refraction KW - Computed tomography KW - NDE KW - Ti-MMC KW - Lightweight materials KW - Metal matrix composites KW - Synchrotron radiation KW - X-ray refraction PY - 2009 DO - https://doi.org/10.1002/adem.200800346 SN - 1438-1656 VL - 11 IS - 6 SP - 435 EP - 440 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-20564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Müller, Bernd R. A1 - Kupsch, Andreas T1 - Characterizing damage evolution in metal matrix composites with X-ray refraction topography and in situ tensile loading N2 - In this study a metal-matrix-composite with aluminum matrix and Al2O3 particles was investigated with x-ray refraction topography and in-situ tensile loading. It could be observed that after reaching a certain load the specific surface increased steadily. However, the classical radiographs taken for comparison show no damage in the sample. T2 - 8th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 07.12.2016 KW - X-ray refraction KW - Metal matrix composites KW - In-situ loading KW - Synchrotron PY - 2016 AN - OPUS4-39113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Harwardt, Michael A1 - Hentschel, Manfred P. A1 - Illerhaus, Bernhard A1 - Goebbels, Jürgen A1 - Bamberg, J. A1 - Heutling, F. T1 - Refraction computed tomography - Application to metal matrix composites N2 - Erstmals wurden MMCs mit Hilfe der Interface-Kontrast verstärkenden Röntgen-Refraktions-Technik in Kombination mit der 3D-CT-Technik untersucht. Die Methode der Röntgen-Refraktions-Topography sowie der Röntgen-Refraktions-Tomography wurden in den letzten Jahren speziell für die zerstörungsfreie Charakterisierung von Leichtbau-Hochleistungs-Werkstoffen wie Verbund-Werkstoffen und Keramiken entwickelt. Die Technik basiert auf der Refraktion von Röntgenlicht an Grenzflächen zwischen Bereichen unterschiedlicher Elektronendichte wie z.B. Faser- und Matrix-Werkstoff. Auf Grund der kurzen Röntgen-Wellenlänge hat der Brechungsindex einen Wert dicht bei eins, sodass der Streuwinkel nur wenige Bogenminuten beträgt. Der Vorteil der kurzen Wellenlänge besteht jedoch darin, dass Poren und Risse detektiert werden können, deren Größe im Nanometerbereich liegen. Damit kann die Refraktions-Technik zum besseren Verständnis von Mikro- und Submikro-Strukturen in der Materialwissenschaft eingesetzt werden. Mit der hier vorgestellten Refraktions-CT wurden Ermüdungsmechanismen an MMCs, bestehend aus SiC-Faser verstärktem Titan (Ti6242) untersucht. Die Messungen wurden am Röntgen-Messplatz der BAM (BAMline) am Synchrotron-Speicherring-BESSY in Berlin Adlershof durchgeführt. KW - X-ray refraction KW - Computed tomography PY - 2004 DO - https://doi.org/10.3139/120.100592 SN - 0025-5300 VL - 46 IS - 6 SP - 314 EP - 319 PB - Carl Hanser Verlag CY - München AN - OPUS4-5870 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - de Andrade Silva, F. A1 - Williams, J. J. A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. A1 - Portella, Pedro Dolabella A1 - Chawla, N. T1 - Three-dimensional microstructure visualization of porosity and Fe-rich inclusions in SiC particle-reinforced Al alloy matrix composites by X-ray synchrotron tomography N2 - Microstructural aspects of composites such as reinforcement particle size, shape, and distribution play important roles in deformation behavior. In addition, Fe-rich inclusions and porosity also influence the behavior of these composites, particularly under fatigue loading. Three-dimensional (3-D) visualization of porosity and Fe-rich inclusions in three dimensions is critical to a thorough understanding of fatigue resistance of metal matrix composites (MMCs), because cracks often initiate at these defects. In this article, we have used X-ray synchrotron tomography to visualize and quantify the morphology and size distribution of pores and Fe-rich inclusions in a SiC particle-reinforced 2080 Al alloy composite. The 3-D data sets were also used to predict and understand the influence of defects on the deformation behavior by 3-D finite element modeling. KW - Synchrotron radiation KW - X-ray tomography KW - X-ray refraction KW - Analyser based imaging KW - Metal matrix composite (MMC) KW - Fatigue PY - 2010 DO - https://doi.org/10.1007/s11661-010-0260-0 SN - 1073-5623 SN - 1543-1940 VL - 41 IS - 8 SP - 2121 EP - 2128 PB - The Minerals, Metals and Materials Society CY - Warrendale AN - OPUS4-21629 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. A1 - Harbich, Karl-Wolfram A1 - Lange, Axel A1 - Schors, Jörg T1 - X-ray refraction topography for non-destructive evaluation of advanced materials T2 - 15th World Conference on Non-Destructive Testing (WCNDT) CY - Roma, Italy DA - 2000-10-15 KW - X-ray refraction PY - 2000 UR - http://www.ndt.net/article/wcndt00/papers/idn257/idn257.htm SN - 1435-4934 VL - 5 IS - 11 SP - 1 EP - 7(?) PB - NDT.net CY - Kirchwald AN - OPUS4-871 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rack, A. A1 - Zabler, S. A1 - Müller, Bernd R. A1 - Riesemeier, Heinrich A1 - Weidemann, Gerd A1 - Lange, Axel A1 - Goebbels, Jürgen A1 - Hentschel, Manfred P. A1 - Görner, Wolf T1 - High resolution synchrotron-based radiography and tomography using hard X-rays at the BAMline (BESSY II) N2 - The use of high brilliance and partial coherent synchrotron light for radiography and computed tomography (CT) allows to image micro-structured, multi-component specimens with different contrast modes and resolutions up to submicrometer range. This is of high interest for materials research, life science and non-destructive evaluation applications. An imaging setup for microtomography and radiography installed at BESSY II (a third generation synchrotron light source located in Berlin, Germany) as part of its first hard X-ray beamline (BAMline) can now be used for absorption, refraction as well as phase contrast — dedicated to inhouse research and applications by external users. Monochromatic synchrotron light between 6 keV and 80 keV is attained via a fully automated double multilayer monochromator. For imaging applications the synchrotron beam transmitted by the sample is converted with a scintillator into visible light. By use of microscope optics this luminescence image is then projected onto, e.g., a CCD chip. Several scintillating materials are used in order to optimise the performance of the detector system. Different optical systems are available for imaging ranging from a larger field of view and moderate resolutions (macroscope — up to 14 mm x 14 mm field of view) to high resolution (microscope — down to 0.35 μm pixel size), offering magnifications from 1.8× to 40×. Additionally asymmetric cut Bragg crystals in front of the scintillator can be used for a further magnification in one dimension by a factor of about 20. Slow and fast cameras are available, with up to 16 bit dynamic range. We show the suitability of the setup for numerous applications from materials research and life science. KW - Microtomography KW - Non-destructive evaluation KW - Synchrotron instrumentation KW - Coherent imaging KW - X-ray refraction KW - Phase contrast KW - Holotomography KW - Synchrotron-CT KW - Scintillator KW - Bragg magnification PY - 2008 DO - https://doi.org/10.1016/j.nima.2007.11.020 SN - 0168-9002 SN - 0167-5087 VL - 586 IS - 2 SP - 327 EP - 344 PB - North-Holland CY - Amsterdam AN - OPUS4-17738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. ED - Czichos, Horst T1 - Micro-diagnostics: X-ray and synchrotron techniques N2 - Beyond classical X-ray techniques are used for the purpose of preferably short-term applications, but some supplementary X-ray and synchrotron techniques for higher resolution microdiagnostics take advantage of scattering effects. In contrast to directly imaging methods their resolution is only limited by the diffraction limit of the X-ray wavelength, far below the atomic dimensions. These techniques of scanning topography and refraction synchrotron tomography may permit the systematic diagnostics for finding and exploiting structure/property relations like correlations among atomic, nano and microstructures with macroscopic properties. Their basic advantage over microscopic techniques is their potential for the non-destructive characterisation of materials, far from invasive sample treatments. They combine scattering and spatial resolution. KW - X-ray KW - X-ray refraction KW - X-ray refraction topography KW - X-ray refraction tomography KW - X-ray scattering KW - USAXS KW - Wide angle X-ray scattering KW - WAXS KW - Interfaces KW - Inner surface density KW - Diffraction enhanced imaging KW - DEI KW - Synchrotron radiation KW - Synchrotron refraction computed tomography KW - SRCT KW - Fibre orientation KW - X-ray diffraction microscopy PY - 2013 SN - 978-3-642-25849-7 SN - 978-3-642-25850-3 DO - https://doi.org/10.1007/978-3-642-25850-3_14 IS - Chapter 14 SP - 287 EP - 300 PB - Springer CY - Berlin Heidelberg AN - OPUS4-27746 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Müller, Bernd R. A1 - Trappe, Volker A1 - Goebbels, Jürgen A1 - Hickmann, Stefan A1 - Grasse, Fabian T1 - Non-destructive characterization of composites: from small scale to complex component testing - a challenge T2 - International Symposium on NDT in Aerospace CY - Hamburg, Germany DA - 2010-11-22 KW - Aircraft KW - Wind turbine blades KW - Automotive KW - X-ray refraction KW - Fibre orientation KW - WAXS technique KW - X-ray computed tomography PY - 2010 SN - 978-3-940283-28-3 IS - DGZfP-BB 124 (Tu.2.B.1) SP - 1 EP - 6 AN - OPUS4-22724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Bruno, Giovanni A1 - Onel, Yener A1 - Wolk, Thomas A1 - Staude, Andreas A1 - Ehrig, Karsten A1 - Müller, Bernd R. T1 - Evaluating porosity in cordierite diesel particulate filter materials: advanced X-ray techniques and new statistical analysis methods T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 2014-10-06 KW - Porous ceramics KW - Diesel particulate filters KW - Pore orientation KW - X-ray computed tomography KW - X-ray refraction KW - DIVA algorithm KW - Phase contrast KW - Edge artefact KW - Soft matter radiography KW - Wavelet transform KW - Huygens elementary waves PY - 2014 SN - 978-80-214-5018-9 SP - 1 EP - 8(?) AN - OPUS4-31973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Cong A1 - Müller, Bernd R. A1 - Lebedev, O. A1 - Giovannelli, F. A1 - Bruno, Giovanni A1 - Delorme, F. T1 - Effects of impurities on the stability of the low thermal conductivity in Fe2TiO5 ceramics N2 - The stability of the low thermal conductivity in Fe2TiO5 pseudobrookite ceramics has been studied. An increase in thermal diffusivity is observed after only three cycles of measurement. X-ray refraction shows an increase in the mean value of specific surface after the thermal diffusivity measurements. By using scanning electron microscopy and high‐angle annular dark‐field scanning transmission electron microscope equipped with energy dispersive X-ray spectroscopy, we observe a segregation of Ca- and F-rich nanocrystals at grain boundaries after three cycles of thermal diffusivity measurement. Therefore, impurities seem to be more efficient to scatter phonons as point defects in the pseudobrookite lattice rather than as nanocrystals at pseudobrookite grain boundaries. This emphasizes the importance of precursor purity and the influence of redistribution of impurities on thermoelectric properties: stability of micro-/nano-structures is a key point, and repeated thermoelectric measurements may allow detecting such metastable micro- /nano-structures and producing stable and reliable data. KW - Fe2TiO5 KW - Impurity segregation KW - Thermoelectrics KW - X-ray refraction KW - Scanning transmission electron microscopy PY - 2019 UR - http://www.sciencedirect.com/science/article/pii/S1044580318329309 DO - https://doi.org/10.1016/j.matchar.2019.01.021 SN - 1044-5803 SN - 1873-4189 VL - 149 SP - 111 EP - 117 PB - Elsevier Inc. AN - OPUS4-47255 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Müller, Bernd R. A1 - Laquai, René A1 - Kupsch, Andreas A1 - Wieder, Frank A1 - Benemann, Sigrid A1 - Wilbig, Janka A1 - Günster, Jens A1 - Bruno, Giovanni T1 - Microstructural characterization of AP40 apatite-wollastonite glass-ceramic N2 - The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis. KW - Glass-ceramic KW - X-ray refraction KW - Computed tomography KW - Microstructure PY - 2023 DO - https://doi.org/10.1016/j.ceramint.2022.12.130 SN - 0272-8842 VL - 49 IS - 8 SP - 12672 EP - 12679 PB - Elsevier Science CY - Amsterdam AN - OPUS4-57452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chen, Cong A1 - Müller, Bernd R. A1 - Prinz, Carsten A1 - Stroh, Julia A1 - Feldmann, Ines A1 - Bruno, Giovanni T1 - The correlation between porosity characteristics and the crystallographic texture in extruded stabilized aluminium titanate for diesel particulate filter applications N2 - Porous ceramic diesel particulate filters (DPFs) are extruded products that possess macroscopic anisotropic mechanical and thermal properties. This anisotropy is caused by both morphological features (mostly the orientation of porosity) and crystallographic texture. We systematically studied those two aspects in two aluminum titanate ceramic materials of different porosity using mercury porosimetry, gas adsorption, electron microscopy, X-ray diffraction, and X-ray refraction radiography. We found that a lower porosity content implies a larger isotropy of both the crystal texture and the porosity orientation. We also found that, analogous to cordierite, crystallites do align with their axis of negative thermal expansion along the extrusion direction. However, unlike what found for cordierite, the aluminium titanate crystallite form is such that a more pronounced (0 0 2) texture along the extrusion direction implies porosity aligned perpendicular to it. KW - Preferred orientation KW - X-ray refraction KW - Pore orientation KW - Crystal structure KW - Extrusion KW - Microstructure-property relations PY - 2020 DO - https://doi.org/10.1016/j.jeurceramsoc.2019.11.076 SN - 0955-2219 VL - 40 IS - 4 SP - 1592 EP - 1601 PB - Elsevier Ltd. AN - OPUS4-50325 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Müller, Bernd R. A1 - Kasperovich, G. A1 - Requena, G. A1 - Haubrich, J. A1 - Bruno, Giovanni T1 - Classification of defect types in SLM Ti-6Al-V4 by X-ray refraction topography N2 - Porosity in additively manufactured materials, such as laser powder bed fusion Ti-Al6-V4, can play an important role in their mechanical performance. Not only the total porosity but also the shape/morphology of the individual pores need to be considered. Therefore, it is necessary to determine the distributions of different defect types (especially fusing defects and keyhole pores) and their dependence on process parameters. We show that synchrotron X-ray refraction radiography allows analysis of large samples (up to several millimeters) without compromising the detectability of submicrometer defects. Correspondingly, a classification tool is introduced that is able to quantitatively distinguish defects such as keyhole pores and binding defects with a confidence level of 94 %, even when the shape cannot be discerned because of limited spatial resolution. KW - Additive manufacturing KW - Selective laser melting KW - X-ray refraction KW - Microscopy KW - Porosity KW - X-ray computed tomography KW - BAMline KW - Synchrotron Radiation PY - 2020 DO - https://doi.org/10.1520/MPC20190080 SN - 2379-1365 VL - 9 IS - 1 SP - 82 EP - 93 PB - ASTM International CY - West Conshohocken, PA AN - OPUS4-50470 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - 3D Crack analysis in hydrogen charged lean duplex stainless steel with synchrotron refraction CT N2 - Hydrogen in metals can cause a degradation of the mechanical properties, the so-called hydrogen embrittlement. In combination with internal stresses, hydrogen assisted cracking (HAC) can occur. This phenomenon is not completely understood yet. To better characterise the cracking behaviour, it is important to gain information about the evolution of the 3D crack network. For this purpose samples of lean duplex stainless steel were loaded with hydrogen by means of electrochemical charging and investigated by means of synchrotron refraction CT and SEM fractography after uniaxial tensile loading. Synchrotron refraction CT is an analyser-based imaging (ABI) technique. It uses a Si (111) single crystal as analyser, which is placed into the beam path between sample and detector. According to Bragg’s law only incident x-rays within a narrow range around the Bragg-angle are diffracted from the analyser into the detector. Hence, the analyser acts as an angular filter for the transmitted beam. This filtering allows to turn the refraction and scattering of x-rays into image contrast. Refraction occurs at all interfaces, where the density of the material changes and is more sensitive to density changes than the attenuation. Therefore, it is possible to detect smaller cracks than with classical x-ray imaging techniques, like CT, with comparable spacial resolution. It also visualises the 3D structure of the cracks and gains quantitative information about their morphology and distribution. Since cracks introduced by HAC are usually very small and have a small opening displacement, synchrotron refraction CT is expected to be well suited for imaging this cracking mechanism and can be a valuable tool to characterise the formation and the evolution of a 3D crack network. T2 - WCNDT 2016 CY - München, Germany DA - 13.06.2016 KW - X-ray refraction KW - Computed tomography KW - Hydrogen assisted cracking KW - Duplex stainless steel PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-366481 SN - 978-3-940283-78-8 VL - BB 158 SP - Tu.4.B.3, 1 EP - 9 AN - OPUS4-36648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Müller, Bernd R. A1 - Kasperovich, G. A1 - Haubrich, J. A1 - Requena, G. A1 - Bruno, Giovanni T1 - X-ray refraction distinguishes unprocessed powder from empty pores in selective laser melting Ti-6Al-4V N2 - For the first time, X-ray refraction techniques are proven for the identification of void formation in Ti-6Al-4V parts produced by selective laser melting. The topology and volume fraction of pores are measured in samples produced with different laser energy density. Unique X-ray refraction methods identify different kinds of defects, characteristic to the regions below and above the Optimum laser energy density, namely unprocessed powder (unmolten powder particles, balling effect, and Fusion defects) from empty keyhole pores. Furthermore, it is possible to detect small inhomogeneities (voids or cracks) with sizes below the spatial resolution of optical microscopy and X-ray computed tomography. KW - Additive manufacturing KW - X-ray refraction KW - Microscopy KW - X-ray computed tomography KW - Porosity PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-434041 DO - https://doi.org/10.1080/21663831.2017.1409288 SN - 2166-3831 VL - 6 IS - 2 SP - 130 EP - 135 PB - Taylor & Francis Group CY - London, UK AN - OPUS4-43404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Laquai, René A1 - Schaupp, Thomas A1 - Griesche, Axel A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Hannemann, Andreas A1 - Kannengießer, Thomas A1 - Bruno, Giovanni T1 - Quantitative analysis of hydrogen-assisted microcracking in duplex stainless steel through X-ray refraction 3D imaging N2 - While the problem of the identification of mechanisms of hydrogen assisted damage has and is being thoroughly studied, the quantitative analysis of such damage still lacks suitable tools. In fact, while, for instance, electron microscopy yields excellent characterization, the quantitative analysis of damage requires at the same time large field-of-views and high spatial resolution. Synchrotron X-ray refraction techniques do possess both features. In this work, we show how synchrotron X-ray refraction computed tomography (SXRCT) can quantify damage induced by hydrogen embrittlement in a lean duplex steel, yielding results that overperform even those achievable by synchrotron X-ray absorption computed tomography. As already reported in literature, but this time using a non-destructive technique, we show that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, we deduce that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. We show that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and we deduce that a significant crack propagation can only be observed short before rupture. KW - 2101 duplex stainless steel KW - Hydrogen embrittlement KW - Synchrotron radiation KW - X-ray refraction KW - Computed tomography KW - Microcracking PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-542811 DO - https://doi.org/10.1002/adem.202101287 SN - 1438-1656 SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-54281 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evolution of CFRP stress cracks observed by in situ X-ray refractive imaging N2 - Modern air-liners and wind turbine rotor blades are made up primarily of fiber reinforced plastics. Failure of these materials heavily impairs the serviceability and the operational safety. Consequently, knowledge of the failure behavior under static and cyclic loads is of great interest to estimate the operational strength and to compare the performance of different materials. Ideally, the damage evolution under operational load is determined with in situ non-destructive testing techniques. Here, we report in-situ synchrotron X-ray imaging of tensile stress induced cracks in carbon fiber reinforced plastics due to inter-fiber failure. An inhouse designed compact tensile testing machine with a load range up to 15 kN was integrated into the beamline. Since conventional radiographs do not reveal sufficient contrast to distinguish cracks due to inter-fiber failure and micro cracking from fiber bundles, the Diffraction Enhanced Imaging (DEI) technique is applied in order to separate primary and scattered (refracted) radiation by means of an analyzer crystal. This technique allows fast measurements over large fields-of-view and is ideal for in-situ investigations. Imaging and the tensile test are run at the highest possible frame rate (0.7 s-1 ) and the lowest possible strain rate (5.5∙10-4 s -1 ). For 0°/90° non-crimp fabrics, the first inter-fiber cracks occur at 380 MPa (strain 0.8 %). Prior to failure at about 760 MPa (strain 2.0 %), we observe the evolution of nearly equidistant (1 mm distance) cracks running across the entire sample in the fully damaged state. KW - X-ray refraction KW - Diffraction Enhanced Imaging KW - Carbon Fiber Reinforced Plastics KW - In situ tensile test KW - Crack evolution PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515060 DO - https://doi.org/10.1088/1757-899X/942/1/012035 SN - 1757-8981 SN - 1757-899X VL - 942 SP - 012035-1 EP - 012035-9 PB - IOP publishing CY - Bristol, UK AN - OPUS4-51506 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Absorption and refraction techniques: Characterization and Non-Destructivetesting of materials N2 - X-ray techniques developed and used in BAM FB 8.5 (Micro NDE) for characterization of ceramic materials. T2 - Sitzung der Technischen Kommission des Verbands der Keramischen Industrie CY - Berlin, Gremany DA - 10.3.2017 KW - X-ray KW - X-ray refraction KW - Computed Tomography PY - 2017 AN - OPUS4-39322 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Erdmann, Maren A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. A1 - Niebergall, Ute A1 - Böhning, Martin A1 - Bruno, Giovanni ED - Erdmann, Maren T1 - Diesel-induced transparency of plastically deformed high-density polyethylene N2 - High-density polyethylene becomes optically transparent during tensile drawing when previously saturated with diesel fuel. This unusual phenomenon is investigated as it might allow conclusions with respect to the material behavior. Microscopy, differential scanning calorimetry, density measurements are applied together with two scanning X-ray scattering techniques: wide angle X-ray scattering (WAXS) and X-ray refraction, able to extract the spatially resolved crystal orientation and internal surface, respectively. The sorbed diesel softens the material and significantly alters the yielding characteristics. Although the crystallinity among stretched regions is similar, a virgin reference sample exhibits strain whitening during stretching, while the diesel-saturated sample becomes transparent. The WAXS results reveal a pronounced fiber texture in the tensile direction in the stretched region and an isotropic orientation in the unstretched region. This texture implies the formation of fibrils in the stretched region, while spherulites remain intact in the unstretched parts of the specimens. X-ray refraction reveals a preferred orientation of internal surfaces along the tensile direction in the stretched region of virgin samples, while the sample stretched in the diesel-saturated state shows no internal surfaces at all. Besides from stretching saturated samples, optical transparency is also obtained from sorbing samples in diesel after stretching. KW - PE-HD Sorption KW - Cavitation KW - Diesel Fuel KW - X-ray refraction KW - WAXS KW - Internal Surfaces KW - Crystal Texture PY - 2019 DO - https://doi.org/10.1007/s10853-019-03700-8 SN - 1573-4803 SN - 0022-2461 VL - 54 IS - 17 SP - 11739 EP - 11755 PB - Springer US CY - US AN - OPUS4-48226 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Onel, Yener A1 - Wolk, Thomas A1 - Staude, Andreas A1 - Ehrig, Karsten A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evaluating porosity in cordierite diesel particulate filter materials, part 1 X-ray refraction N2 - Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, with porosity and solid matter being intermingled. Mechanical, thermal, and filtration properties can only be precisely estimated if the morphology of both solid matter and porosity can be quantitatively determined. Using x-ray absorption and refraction, we quantitatively evaluate porosity and pore orientation in cordierite diesel particulate filter ceramics. Porosity values turn out to agree with mercury intrusion measurements, while pore orientation factors agree with published crystallographic texture data. KW - Porous ceramics KW - Pore orientation KW - X-ray refraction KW - Synchrotron KW - Interface PY - 2013 DO - https://doi.org/10.4416/JCST2013-00021 SN - 2190-9385 VL - 4 IS - 4 SP - 169 EP - 176 PB - Göller CY - Baden-Baden AN - OPUS4-29939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Hentschel, Manfred P. A1 - Lange, Axel A1 - Bruno, Giovanni A1 - Müller, Bernd R. T1 - Direct X-ray refraction of micro structures N2 - For the first time we present direct 2D imaging of refracted X-rays without any discrimination of the Primary radiation. X-refraction works in analogy to visible light optics: X-rays are entirely deflected at interfaces where discontinuities of (electron) density occur. This is demonstrated at the example of inner and outer surfaces of model samples of well-defined geometry (fibres, capillaries, and monodisperse micro particles). The samples are scanned through a 50 μm monochromatic (20 keV) pencil beam. In order to warrant a sufficient angular resolution a 2D detector (pixel size 7 μm) is placed 3 m downstream of the sample. Scanning the sample in micron steps allows for detecting local changes of interface / surface orientation directly in two dimensions. At the actual angular resolution of about 3 seconds of arc (scattering vector increments Δk = 10-3 nm-1) and 50 μm spatial resolution (scanning) the material’s inner surfaces (with nanometer separation) can be characterized even at sampling rates below 1 second per frame. Moreover, our technique is suited to directly determine particle diameters of up to 250 nm by means of diffraction fringes. Some potential applications to technical submicron structures are discussed. T2 - ECNDT 2014 - 11th European conference on non-destructive testing CY - Prague, Czech Republic DA - 06.10.2014 KW - X-ray refraction KW - Phase contrast KW - Edge artefact KW - Soft matter radiography KW - Wavelet transformation KW - Huygens elementary waves PY - 2014 SN - 978-80-214-5018-9 SP - 1 EP - 9 AN - OPUS4-31970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Staude, Andreas A1 - Meinel, Dietmar A1 - Hentschel, Manfred P. A1 - Müller, Bernd R. ED - Grellmann, W. ED - Frenz, H. T1 - Moderne bildgebende hochauflösende Röntgenverfahren für die Materialcharakterisierung N2 - Die Computertomographie (CT) ist in der Medizin als Standardtechnik etabliert, in der zerstörungsfreien Prüfung wird sie zunehmend angewendet, in einzelnen Fällen sogar als Referenzverfahren eingesetzt. Gegenwärtig ist eine starke Zunahme von Anwendungen der CT in der Materialcharakterisierung zu verzeichnen. Zudem werden weitere moderne 3D-Techniken für werkstoffwissenschaftliche Fragestellungen genutzt, um die Mikrostruktur - auch in situ (z.B. Druck, Temperatur) - aufzuklären. Hier werden neben der konventionellen Absorptions-CT auch die Potenziale der Refraktions-CT zur Beantwortung prozesstechnischer sowie werkstofflicher Fragestellungen aufgezeigt, die ein „ganzheitliches Bild“ des jeweiligen Werkstoffs zum Ziel haben. T2 - Tagung Werkstoffprüfung 2014 - Fortschritte in der Werkstoffprüfung für Forschung und Praxis - Werkstoffeinsatz, Qualitätssicherung und Schadensanalyse CY - Berlin, Germany DA - 04.12.2014 KW - Computer tomography KW - X-ray refraction KW - Ceramics KW - Concrete KW - Inhomogeneous materials KW - Computertomographie KW - Röntgenrefraktion KW - Keramik KW - Beton KW - Mehrphasige Materialien PY - 2014 SN - 978-3-9814516-8-9 SN - 1861-8154 SP - 1 EP - 12 AN - OPUS4-32565 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Serrano-Munoz, Itziar A1 - Kupsch, Andreas A1 - Müller, Bernd R. T1 - X-Ray-Refraction-Imaging-Techniques high-resolution microstructural characterization N2 - X-ray refraction is analogous to visible light deflection by matter; it occurs at boundaries between different media. The main difference between visible light and X-rays is that in the latter case deflection angles are very small, from a few seconds to a few minutes of arc (i.e., the refraction index n is near to 1). Trivially but importantly, deflection of X-rays is also sensitive to the orientation of the object boundaries. These features make X-ray refraction techniques extremely suitable to a) detect defects such as pores and microcracks and quantify their densities in bulk (not too heavy) materials, and b) evaluate porosity and particle properties such as orientation, size, and spatial distribution (by mapping). While X-ray refraction techniques cannot in general image single defects, their detectability is simply limited by the wavelength of the radiation. We thereby show the application of X-ray refraction 2D mapping (topography) and tomography to different sorts of problems in materials science and technology: 1) Sintering of SiC green bodies; 2) Porosity analysis in additively manufactured alloys; 3) Fiber de-bonding in metal and polymer matrix composites. Such techniques, especially at the Synchrotron BESSY II, Berlin, Germany, can be used in-situ, i.e. when the specimen is subjected to temperatures or external loads. Applications of in-situ X-ray refraction radiography on aluminum alloys and composites are also shown. The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models. T2 - ICT 2023 CY - Fürth, Germany DA - 27.02.2023 KW - X-ray refraction KW - Composites KW - In-situ KW - Additive Manufacturing KW - Sintering KW - Ceramics PY - 2023 AN - OPUS4-57200 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Evsevleev, Sergei A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Kupsch, Andreas T1 - Refraction driven X-ray caustics at curved interfaces N2 - X-ray refraction related interaction has received rising interest since about two decades in the field of imaging, beam shaping and analysis although being discovered a century ago. Due to refraction at interfaces in inhomogeneous media X-rays undergo natural focusing (or defocusing) of waves, revealing caustics. Such Kind of intensity patterns are well-known for visible light, but have been sparsely discussed for X-rays. The Variation of irradiation density may be predicted in case of known shapes. Analogously to light optics, the intensity distributions cover several orders of magnitude including complete extinction. The partly convergent (and divergent) caustic stripes originate from narrow zones of typical size of some 10−6 of the boundary curvature radius. For the deflection of plane wave synchrotron radiation (energy in the range of some keV to some ten keV) at rods and tubes of several μm diameter, we find good Agreement between experiments and modeling by ray tracing according to Snell’s law without additional diffraction contributions. Apart from Basic Research implications, caustics may influence the performance of irradiation technologies such as sterilization or molecular cross-linking. KW - X-ray caustics KW - X-ray refraction KW - Irradiation KW - Radiation shielding KW - Synchrotron Radiation PY - 2019 UR - http://www.sciencedirect.com/science/article/pii/S0168900218314591 DO - https://doi.org/10.1016/j.nima.2018.10.152 SN - 0168-9002 SN - 1872-9576 VL - 916 SP - 275 EP - 282 PB - Elsevier AN - OPUS4-46924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mani, Deepak A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Diffraction Enhanced Imaging Analysis with Pseudo-Voigt Fit Function N2 - Diffraction enhanced imaging (DEI) is an advanced digital radiographic imaging technique employing the refraction of X-rays to contrast internal interfaces. This study aims at qualitatively and quantitatively evaluating images acquired using this technique and to assess how different fitting functions to the typical rocking curves (RCs) influence the quality of images. RCs are obtained for every image pixel. This allows the separate determination of the absorption and the refraction properties of the material in a position-sensitive manner. Comparison of various types of fitting functions reveals that the Pseudo-Voigt (PsdV) function is best suited to fit typical RCs. A robust algorithm was developed in the Python programming language, which reliably extracts the physically meaningful information from each pixel of the image. We demonstrate the potential of the algorithm with two specimens: a silicone gel specimen that has well-defined interfaces, and an additively manufactured polycarbonate specimen. KW - Diffraction Enhanced Imaging KW - Analyzer-Based Imaging KW - X-ray refraction KW - Non-Destructive Evaluation KW - Pseudo-Voigt fit function KW - Python PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-553791 DO - https://doi.org/10.3390/jimaging8080206 SN - 2313-433X VL - 8 IS - 8 SP - 1 EP - 13 PB - MDPI CY - Basel, Switzerland AN - OPUS4-55379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - 3D imaging of hydrogen assisted cracking in metals using refraction enhanced synchrotron CT N2 - Hydrogen in metals can cause a degradation of the mechanical properties with possible subsequent hydrogen assisted cracking (HAC). Though, the mechanism of HAC is not completely understood yet and thus suitable methods for in situ investigations to characterise the crack formation are needed. X-ray computed tomography (CT) is a well-known tool for analysing these properties. However, the effective resolution of the detector system limits the detection of small defects by CT. Analyser based imaging (ABI) takes advantage of x-ray refraction at interfaces between volumes of different density, i.e. of cracks, pores, inclusions, etc., within the sample to detect defects smaller than the resolution of the detector system. In this study, measurements on an aluminium alloy weld showed that ABI allows us to resolve the 3D structure of cracks undetected by absorption based CT. Prospective investigations will analyse HAC in steels. T2 - NDT-CE 2015 - International symposium non-destructive testing in civil engineering CY - Berlin, Germany DA - 2015-09-15 KW - Wasserstoffversprödung KW - Wasserstoffunterstützte Rissbildung KW - Röntgenrefraktion KW - CT KW - Hydrogen embrittlement (HE) KW - Hydrogen assisted cracking (HAC) KW - Aluminium alloy KW - X-ray refraction KW - Analyser based imaging KW - Computed tomography (CT) KW - Synchrotron radiation PY - 2015 SN - 1435-4934 SP - 1217 EP - 1224 AN - OPUS4-34287 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Laquai, René A1 - Schaupp, Thomas A1 - Müller, Bernd R. A1 - Griesche, Axel A1 - Bruno, Giovanni A1 - Kannengießer, Thomas T1 - 3D imaging of hydrogen assisted cracking using analyser-based imaging N2 - To better understand the mechanism of hydrogen assisted cracking (HAC), it is important to investigate the 3D structure of the cracks non-destructively. Since, cracks introduced by HAC are usually very small, conventional x-ray imaging methods often lack the required spatial resolution. However, the detection of those cracks can be enhanced by taking advantage of refraction at interfaces within the sample. To image this refractive deflection we employ analyser based imaging (ABI). In this work we aim at proving the enhanced crack detection of ABI by investigating an alluminum alloy weld. T2 - BESSY User Meeting 2015 CY - Berlin, Germany DA - 09.12.2015 KW - X-ray refraction KW - Synchrotron KW - Analyser-based imaging KW - Hydrogen assisted cracking KW - Welding PY - 2015 AN - OPUS4-38278 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Microstructure characterization of materials using X-ray refraction techniques N2 - X-ray refraction is an excellent tool for the characterization of the microstructure of materials. However, there are only a few (synchrotron) laboratories in the world that use this technique for material characterisation. Therefore, the seminar will first explain the basic principles of X-ray refraction and the measurement techniques installed at the hard X-ray beamline BAMline at BESSY II (Berlin, Germany). This is followed by examples of investigations on fibre-reinforced plastic composites (CFRP) as well as ceramic (Cordierite, ZrO2-SiO2) and metallic materials (Ti-6Al-4V, Inconel). Some of the investigations were carried out both ex-situ and in-situ under mechanical and thermal load. The results are correlated with the mechanical properties of the materials. T2 - LNLS Users Group Seminar Series CY - Campinas, Brasil DA - 25.10.2022 KW - X-ray refraction KW - Analyzer-Based Imaging KW - BAMline PY - 2022 AN - OPUS4-56117 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Shashev, Yury A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Evsevleev, Sergei A1 - Müller, Bernd R. A1 - Osenberg, Markus A1 - Manke, Ingo A1 - Hentschel, Manfred P. A1 - Bruno, Giovanni T1 - Optimizing the visibility of X-ray phase grating interferometry N2 - The performance of grating interferometers coming up now for Imaging interfaces within materials depends on the efficiency (visibility) of their main component, namely the phase grating. Therefore, experiments with monochromatic synchrotron radiation and corresponding simulations are carried out. The visibility of a Phase grating is optimized by different photon energies, varying detector to grating distances and continuous rotation of the phase grating about the grid lines. Such kind of rotation changes the projected grating shapes, and thereby the distribution profiles of phase shifts. This yields higher visibilities than derived from ideal rectangular shapes. By continuous grating rotation and variation of the propagation distance, we achieve 2D visibility maps. Such maps provide the visibility for a certain combination of grating orientation and detector position. Optimum visibilities occur at considerably smaller distances than in the standard setup. KW - Synchrotron, BAMline KW - Talbot-Lau interferometer KW - X-ray imaging KW - X-ray refraction KW - Grating interferometry KW - X-ray phase contrast PY - 2017 DO - https://doi.org/10.3139/120.111097 SN - 0025-5300 VL - 59 IS - 11-12 SP - 974 EP - 980 PB - Hanser Verlag AN - OPUS4-42955 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Lange, Axel A1 - Bruno, Giovanni T1 - Microstructure Characterization of Ceramics via 2D and 3D X-Ray Refraction Techniques N2 - 3D imaging techniques are very fashionable nowadays, and allow enormous progress in understanding ceramic microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this feature article, we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining internal specific surface (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. While the techniques are limited by the X-ray absorption of the material under investigation, we demonstrate showcases of ceramics and composite materials, where understanding of process parameter influence or simply of microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. KW - X-ray refraction KW - Porosity KW - Specific surface KW - Crack detection KW - Composites PY - 2017 DO - https://doi.org/10.1016/j.jeurceramsoc.2016.12.031 SN - 0955-2219 SN - 1873-619X VL - 37 IS - 5 SP - 1879 EP - 1889 PB - Elsevier CY - Amsterdam AN - OPUS4-39094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Müller, Bernd R. T1 - Microstructure characterization of materials using X-ray refraction techniques N2 - X-ray imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this lecture we report the use of a powerful, yet not so wide-spread, set of X-ray techniques based on refraction effects. X-ray refraction allows determining the internal specific surface of materials (surface per unit volume) in a non-destructive fashion, position and orientation sensitive, and with a nanometric detectability. We demonstrate showcases of ceramics and composite materials, where microstructural parameters could be achieved in a way unrivalled even by high-resolution techniques such as electron microscopy or computed tomography. We present in situ analysis of the damage evolution during tensile load and the identification of void formation in parts produced by selective laser melting. T2 - MIMENIMA Summerschool CY - TU-Bremen, Germany DA - 22.8.2018 KW - X-ray refraction KW - Cracks KW - Pores PY - 2018 AN - OPUS4-45790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. T1 - Edge artefacts of radiographic images by X-ray refraction N2 - The relevance of nano sized structures and interfaces in upcoming technologies requires new non-destructive Xray techniques exploiting attenuation as well as scattering. In the course of driving the resolution and the contrast of modern radiography into micro and nano metre dimension the inevitable scattering effects require increased attention. Several radiologists interpret the observed edge artefacts simply by 'phase contrast' due to different X-ray path lengths within the sample and others refer to Fresnel scattering. The ultra small angle scattering is of high intensity and may reach the level of the primary beam. We present monochromatic synchrotron measurements on rather simply shaped objects (such as plates and cylinders) which prove clearly the dominance of refraction intensity over total reflection and coherent small angle scattering. The refraction conditions hold for angles of incidence of several degrees to the surface, but typical deflection angles range from several seconds to minutes of arc. Additionally to the concept of 'phase contrast' of the primary beam its deflection becomes the essential issue. The appropriate removal of the attenuation contribution enables the imaging of inner surfaces and interfaces by refraction scanning topography. The presented measurements of reference particles demonstrate the reliability of laboratory refraction scanners applying X-ray tubes. T2 - 18th WCNDT - World conference on nondestructive testing CY - Durban, South Africa DA - 16.04.2012 KW - X-ray refraction KW - Small angle scattering KW - Phase contrast radiography KW - Refraction topography KW - Nanostructures KW - Nanocracks PY - 2012 UR - http://www.ndt.net/article/wcndt2012/papers/274_wcndtfinal00274.pdf SN - 978-0-620-52872-6 SP - 1 EP - 11 AN - OPUS4-25836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -