@article{ErdmannKupschMuelleretal.2019, author = {Erdmann, Maren and Kupsch, Andreas and M{\"u}ller, Bernd Randolf and Hentschel, Manfred P. and Niebergall, Ute and B{\"o}hning, Martin and Bruno, Giovanni}, title = {Diesel-induced transparency of plastically deformed high-density polyethylene}, series = {Journal of materials science}, volume = {54}, journal = {Journal of materials science}, number = {17}, publisher = {Springer}, address = {New York}, issn = {0022-2461}, doi = {10.1007/s10853-019-03700-8}, pages = {11739 -- 11755}, year = {2019}, abstract = {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.}, language = {en} } @article{KupschMuellerLangeetal.2017, author = {Kupsch, Andreas and Mueller, Bernd R. and Lange, Axel and Bruno, Giovanni}, title = {Microstructure characterisation of ceramics via 2D and 3D X-ray refraction techniques}, series = {Journal of the European Ceramic Society}, volume = {37}, journal = {Journal of the European Ceramic Society}, publisher = {Elsevier}, address = {Oxford}, issn = {0955-2219}, doi = {10.1016/j.jeurceramsoc.2016.12.031}, pages = {1879 -- 1889}, year = {2017}, abstract = {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. (C) 2016 Elsevier Ltd. All rights reserved.}, language = {en} } @article{LaquaiMuellerSchneideretal.2020, author = {Laquai, Rene and M{\"u}ller, Bernd R. and Schneider, Judith Ann and Kupsch, Andreas and Bruno, Giovanni}, title = {Using SXRR to probe the nature of discontinuities in SLM additive manufactured inconel 718 specimens}, series = {Metallurgical and Materials Transactions A}, volume = {51}, journal = {Metallurgical and Materials Transactions A}, number = {8}, publisher = {Springer}, address = {New York}, issn = {1073-5623}, doi = {10.1007/s11661-020-05847-5}, pages = {4146 -- 4157}, year = {2020}, abstract = {The utilization of additive manufacturing (AM) to fabricate robust structural components relies on understanding the nature of internal anomalies or discontinuities, which can compromise the structural integrity. While some discontinuities in AM microstructures stem from similar mechanisms as observed in more traditional processes such as casting, others are unique to the AM process. Discontinuities in AM are challenging to detect, due to their submicron size and orientation dependency. Toward the goal of improving structural integrity, minimizing discontinuities in an AM build requires an understanding of the mechanisms of formation to mitigate their occurrence. This study utilizes various techniques to evaluate the shape, size, nature and distribution of discontinuities in AM Inconel 718, in a non-hot isostatic pressed (HIPed) as-built, non-HIPed and direct age, and HIPed with two step age samples. Non-destructive synchrotron radiation refraction and transmission radiography (SXRR) provides additional information beyond that obtained with destructive optical microscopy. SXRR was able to distinguish between voids, cracks and lack of melt in, due to its sensitivity to the orientation of the discontinuity.}, language = {en} } @article{LaquaiSchauppGriescheetal.2022, author = {Laquai, Ren{\´e} and Schaupp, Thomas and Griesche, Axel and M{\"u}ller, Bernd R. and Kupsch, Andreas and Hannemann, Andreas and Kannengiesser, Thomas and Bruno, Giovanni}, title = {Quantitative analysis of hydrogen-assisted microcracking in duplex stainless steel through X-ray refraction 3D imaging}, series = {Advanced engineering materials}, volume = {24}, journal = {Advanced engineering materials}, number = {6}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1527-2648}, doi = {10.1002/adem.202101287}, pages = {10}, year = {2022}, abstract = {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. Herein, it is shown 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 the literature, but this time using a nondestructive technique, it is shown that the hydrogen charge does not penetrate to the center of tensile specimens. By the comparison between virgin and hydrogen-charged specimens, it is deduced that cracks in the specimen bulk are due to the rolling process rather than hydrogen-assisted. It is shown that (micro)cracks propagate from the surface of tensile specimens to the interior with increasing applied strain, and it is deduced that a significant crack propagation can only be observed short before rupture.}, language = {en} } @article{MagkosKupschBruno2020, author = {Magkos, Sotirios and Kupsch, Andreas and Bruno, Giovanni}, title = {Direct iterative reconstruction of computed tomography trajectories reconstruction from limited number of projections with DIRECTT}, series = {Review of scientific instruments : a monthly journal devoted to scientific instruments, apparatus, and techniques}, volume = {91}, journal = {Review of scientific instruments : a monthly journal devoted to scientific instruments, apparatus, and techniques}, number = {10}, publisher = {American Institute of Physics}, address = {Melville}, issn = {0034-6748}, doi = {10.1063/5.0013111}, pages = {8}, year = {2020}, abstract = {X-ray computed tomography has many applications in materials science and non-destructive testing. While the standard filtered back-projection reconstruction of the radiographic datasets is fast and simple, it typically fails in returning accurate results from missing or inconsistent projections. Among the alternative techniques that have been proposed to handle such data is the Direct Iterative REconstruction of Computed Tomography Trajectories (DIRECTT) algorithm. We describe a new approach to the algorithm, which significantly decreases the computational time while achieving a better reconstruction quality than that of other established algorithms.}, language = {en} } @article{MagkosKupschBruno2021, author = {Magkos, Sotirios and Kupsch, Andreas and Bruno, Giovanni}, title = {Suppression of cone-beam artefacts with Direct Iterative Reconstruction Computed Tomography Trajectories (DIRECTT)}, series = {Journal of imaging : open access journal}, volume = {7}, journal = {Journal of imaging : open access journal}, number = {8}, publisher = {MDPI}, address = {Basel}, issn = {2313-433X}, doi = {10.3390/jimaging7080147}, pages = {9}, year = {2021}, abstract = {The reconstruction of cone-beam computed tomography data using filtered back-projection algorithms unavoidably results in severe artefacts. We describe how the Direct Iterative Reconstruction of Computed Tomography Trajectories (DIRECTT) algorithm can be combined with a model of the artefacts for the reconstruction of such data. The implementation of DIRECTT results in reconstructed volumes of superior quality compared to the conventional algorithms.}, language = {en} } @article{ManiKupschMuelleretal.2022, author = {Mani, Deepak and Kupsch, Andreas and M{\"u}ller, Bernd R. and Bruno, Giovanni}, title = {Diffraction Enhanced Imaging Analysis with Pseudo-Voigt Fit Function}, series = {Journal of imaging : open access journal}, volume = {8}, journal = {Journal of imaging : open access journal}, number = {8}, publisher = {MDPI}, address = {Basel}, issn = {2313-433X}, doi = {10.3390/jimaging8080206}, pages = {13}, year = {2022}, abstract = {Diffraction enhanced imaging (DEI) is an advanced digital radiographic imaging technique employing the refraction of X-rays to contrast internal interfaces. This study aims to qualitatively and quantitatively evaluate images acquired using this technique and to assess how different fitting functions to the typical rocking curves (RCs) influence the quality of the 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.}, language = {en} } @article{MuellerCooperLangeetal.2017, author = {M{\"u}ller, B. R. and Cooper, R. C. and Lange, A. and Kupsch, Andreas and Wheeler, M. and Hentschel, M. P. and Staude, A. and Pandey, A. and Shyam, A. and Bruno, Giovanni}, title = {Stress-induced microcrack density evolution in beta-eucryptite ceramics}, series = {Acta materialia}, volume = {144}, journal = {Acta materialia}, publisher = {Elsevier}, address = {Oxford}, issn = {1359-6454}, doi = {10.1016/j.actamat.2017.10.030}, pages = {627 -- 641}, year = {2017}, abstract = {In order to investigate their microcracking behaviour, the microstructures of several beta-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.}, language = {en} } @misc{MuellerKupschLaquaietal.2018, author = {M{\"u}ller, Bernd Randolf and Kupsch, Andreas and Laquai, Rene and Nellesen, Jens and Tillmann, Wolfgang and Kasperovich, Galina and Bruno, Giovanni}, title = {Microstructure Characterisation of Advanced Materials via 2D and 3D X-Ray Refraction Techniques}, series = {Materials Science Forum}, volume = {941}, journal = {Materials Science Forum}, publisher = {Trans Tech Publications Ltd}, address = {Zurich}, isbn = {978-3-0357-1208-7}, issn = {0255-5476}, doi = {10.4028/www.scientific.net/MSF.941.2401}, pages = {2401 -- 2406}, year = {2018}, abstract = {3D imaging techniques have an enormous potential to understand the microstructure, its evolution, and its link to mechanical, thermal, and transport properties. In this conference paper 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. 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 in an Al/Al2O3 metal matrix composite during tensile load and the identification of void formation (different kinds of defects, particularly unsintered powder hidden in pores, and small inhomogeneity's like cracks) in Ti64 parts produced by selective laser melting using synchrotron X-ray refraction radiography and tomography.}, language = {en} } @article{NellesenLaquaiMuelleretal.2018, author = {Nellesen, Jens and Laquai, R. and M{\"u}ller, B. R. and Kupsch, Andreas and Hentschel, M. P. and Anar, N. B. and Soppa, E. and Tillmann, W. and Bruno, Giovanni}, title = {In situ analysis of damage evolution in an Al/ Al2O3 MMC under tensile load by synchrotron X-ray refraction imaging}, series = {Journal of materials science}, volume = {53}, journal = {Journal of materials science}, number = {8}, publisher = {Springer}, address = {New York}, issn = {0022-2461}, doi = {10.1007/s10853-017-1957-x}, pages = {6021 -- 6032}, year = {2018}, abstract = {The in situ analysis of the damage evolution in a metal matrix composite (MMC) using synchrotron X-ray refraction radiography (SXRR) is presented. The investigated material is an Al alloy (6061)/10 vol MMC after T6 heat treatment. In an interrupted tensile test the gauge section of dog bone-shaped specimens is imaged in different states of tensile loading. On the basis of the SXRR images, the relative change of the specific surface (proportional to the amount of damage) in the course of tensile loading was analyzed. It could be shown that the damage can be detected by SXRR already at a stage of tensile loading, in which no observation of damage is possible with radiographic absorption-based imaging methods. Moreover, the quantitative analysis of the SXRR images reveals that the amount of damage increases homogeneously by an average of 25\% with respect to the initial state. To corroborate the experimental findings, the damage distribution was imaged in 3D after the final tensile loading by synchrotron X-ray refraction computed tomography (SXRCT) and absorption-based synchrotron X-ray computed tomography (SXCT). It could be evidenced that defects and damages cause pronounced indications in the SXRCT images.}, language = {en} }