TY - CONF A1 - Bruno, Giovanni A1 - Ehrig, Karsten A1 - Haarring, Holger A1 - Harwardt, Michael A1 - Hentschel, Manfred P. A1 - Illerhaus, Bernhard A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Meinel, Dietmar A1 - Müller, Bernd R. A1 - Onel, Yener A1 - Staude, Andreas A1 - Wolk, Thomas T1 - Industrial and synchrotron X-ray CT applications for materials characterisation T2 - Conference on Industrial Computed Tomography (ICT) 2014 - Proceedings N2 - The combination of tomographic, microstructural data with other experimental techniques and with modeling is paramount, if we want to extract the maximum amount of information on material and component properties. In particular, quantitative image analysis, statistical approaches, direct discretization of tomographic reconstructions represent concrete possibilities to extend the power of the tomographic 3D representation to insights into the material and component performance. This logic thread holds equally for industrial and academic research, and valorizes expensive experiments such as those carried out at synchrotron sources, which cannot be daily repeated. We shall show a few examples of possible use of X-ray tomographic data for quantitative assessment of damage evolution and microstructural properties, as well as for non-destructive testing. We will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces. T2 - iCT Conference 2014 - Conference on industrial computed tomography CY - Wels, Austria DA - 25.02.2014 KW - X-ray absorption and refraction CT KW - Quantitative image analysis KW - Statistical analysis KW - Complex microstructure PY - 2014 SN - 978-3-8440-2557-6 SP - 15 EP - 31 PB - Shaker CY - Aachen AN - OPUS4-30484 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 T2 - ECNDT 2014 - 11th European conference on non-destructive testing (Proceedings) 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 - 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 (Proceedings) 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 - 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 JF - Journal of ceramic science and technology 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 - 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: advanced X-ray techniques and new statistical analysis methods JF - Advances in science and technology N2 - Bi-continuous porous ceramics for filtration applications possess a particularly complicated microstructure, whereby porosity and solid matter are 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 3D computed tomography (CT) at different resolutions, and several X-ray refraction-based techniques, we quantitatively evaluated porosity and pore orientation in cordierite diesel particulate filter ceramics.Moreover, applying both Fast Fourier Transform (FFT) and a newly developed image analysis algorithm (directional interface variance analysis, DIVA), we quantitatively evaluated porosity and pore orientation. Both the experimental techniques and the statistical approach allow extraction of spatially resolved or average values.Porosity values from synchrotron computed tomography used turn out to agree with mercury intrusion measurements, while pore orientation factors agree with published crystallographic texture data. This latter point also implies that the study of the pore/matter interface is sufficient to describe the morphological properties of these materials. KW - Diesel particulate filters KW - DIVA Algorithm KW - Pore Orientation KW - Porous Ceramics KW - X-Ray Computed Tomography KW - X-Ray Refraction PY - 2014 DO - https://doi.org/10.4028/www.scientific.net/AST.91.64 SN - 1662-0356 VL - 91 SP - 64 EP - 69 PB - Techna CY - Faenza AN - OPUS4-32069 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 JF - Journal of the European Ceramic Society 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 - 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 T2 - Proceeedings of the 19th World Conference on Non-Destructive Testing 2016 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 - 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 JF - Acta Materialia 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 - JOUR A1 - Müller, Bernd R. A1 - Léonard, Fabien A1 - Lange, Axel A1 - Kupsch, Andreas A1 - Bruno, Giovanni T1 - X-ray refraction techniques for fast, high-resolution microstructure characterization and non-destructive testing of lightweight composites JF - Materials science forum N2 - X-ray refraction is based on optical deflection of X-rays, similar to the well-known small angle X-ray scattering, but hundreds of times more intense, thus enabling shorter measurement time. We show that X-ray refraction techniques are suitable for the detection of pores, cracks, and in general defects. Indeed, the deflected X-ray intensity is directly proportional to the internal specific surface (i.e., surface per unit volume) of the objects. Although single defects cannot be imaged, the presence of populations of those defects can be detected even if the defects have sizes in the nanometer range.We present several applications of X-ray refraction techniques to composite materials:- To visualize macro and microcracks in Ti-SiC metal matrix composites (MMC);- To correlate fatigue damage (fibre de-bonding) of carbon fibre reinforced plastics (CFRP) to X-ray refraction intensity;- To quantify the impact damage by spatially resolved single fibre de-bonding fraction as a function of impact energy in CFRP laminates.An example of classic high-resolution computer tomography of an impact-damaged CFRP will also be presented, as a benchmark to the present state-of-the-art imaging capabilities. It will be shown that while (absorption) tomography can well visualize and quantify delamination, X-ray refraction techniques directly yield (spatially resolved) quantitative information about fibre de-bonding, inaccessible to absorption tomography. KW - X-ray KW - Synchrotron radiation KW - Refraction KW - Metal matrix composites KW - Delamination KW - Fiber de-bonding PY - 2015 DO - https://doi.org/10.4028/www.scientific.net/MSF.825-826.814 SN - 0255-5476 VL - 825-826 SP - 814 EP - 821 PB - Trans Tech Publications CY - Aedermannsdorf, Switzerland AN - OPUS4-33265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Onel, Yener A1 - Lange, Axel A1 - Staude, Andreas A1 - Ehrig, Karsten A1 - Kupsch, Andreas A1 - Hentschel, Manfred P. A1 - Wolk, Thomas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Evaluating porosity in cordierite Diesel particulate filter materials, Part 2 statistical analysis of computed tomography data JF - Journal of ceramic science and technology N2 - Complementary to Part 1 of this work, the bi-continuous microstructure of porous synthetic cordierite ceramics for filtration applications was investigated using 3D x-ray computed tomography at different resolutions. Applying both Fast Fourier Transform and a newly developed image analysis algorithm, we quantitatively evaluated porosity and pore orientation. The statistical approach allows extraction of spatially resolved or average values. Porosity values based on x-ray absorption agree with mercury intrusion measurements, while pore orientation factors agree with x-ray refraction data (Part 1 of this work), and with published crystallographic texture data. KW - Pore orientation KW - Porous ceramics KW - Computed tomography KW - 3D microstructure PY - 2013 DO - https://doi.org/10.4416/JCST2013-00022 SN - 2190-9385 VL - 05 IS - 01 SP - 13 EP - 22 PB - Göller CY - Baden-Baden AN - OPUS4-30379 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -