@article{ChenMuellerPrinzetal.2020, author = {Chen, Cong and M{\"u}ller, Bernd R. and Prinz, Carsten and Stroh, Julia and Feldmann, Ines and Bruno, Giovanni}, title = {The correlation between porosity characteristics and the crystallographic texture in extruded stabilized aluminium titanate for diesel particulate filter applications}, series = {Journal of the European Ceramic Society}, volume = {40}, journal = {Journal of the European Ceramic Society}, number = {4}, publisher = {Elsevier}, address = {Oxford}, issn = {0955-2219}, doi = {10.1016/j.jeurceramsoc.2019.11.076}, pages = {1592 -- 1601}, year = {2020}, abstract = {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.}, language = {en} } @article{ChenMuellerLebedevetal.2019, author = {Chen, Cong and M{\"u}ller, Bernd Randolf and Lebedev, Oleg I. and Giovannelli, Fabien and Bruno, Giovanni and Delorme, Fabian}, title = {Effects of impurities on the stability of the low thermal conductivity in Fe2TiO5 ceramics}, series = {Materials characterization}, volume = {149}, journal = {Materials characterization}, publisher = {Elsevier}, address = {New York}, issn = {1044-5803}, doi = {10.1016/j.matchar.2019.01.021}, pages = {111 -- 117}, year = {2019}, abstract = {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 Xray 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.}, 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{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{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} } @article{ShashevKupschLangeetal.2017, author = {Shashev, Yury and Kupsch, Andreas and Lange, Axel and Evsevleev, Sergei and M{\"u}ller, Bernd R. and Osenberg, Markus and Manke, Ingo and Hentschel, Manfred P. and Bruno, Giovanni}, title = {Optimizing the visibility of X-ray phase grating interferometry}, series = {Materials testing : Materialpr{\"u}fung ; materials and components, technology and application}, volume = {59}, journal = {Materials testing : Materialpr{\"u}fung ; materials and components, technology and application}, publisher = {Hanser}, address = {M{\"u}nchen}, issn = {0025-5300}, doi = {10.3139/120.111097}, pages = {974 -- 980}, year = {2017}, abstract = {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.}, language = {en} } @article{ShashevKupschLangeetal.2016, author = {Shashev, Yury and Kupsch, Andreas and Lange, Axel and M{\"u}ller, Bernd R. and Bruno, Giovanni}, title = {Improving the visibility of phase gratings for Talbot-Lau X-ray imaging}, series = {Materials testing : Materialpr{\~A}¼fung ; materials and components, technology and application}, volume = {58}, journal = {Materials testing : Materialpr{\~A}¼fung ; materials and components, technology and application}, publisher = {Hanser}, address = {M{\"u}nchen}, issn = {0025-5300}, doi = {10.3139/120.110948}, pages = {970 -- 974}, year = {2016}, abstract = {Talbot-Lau interferometry provides X-ray imaging techniques with significant enhancement of the radiographic contrast of weakly absorbing objects. The grating based technique allows separation of absorption, refraction and small angle scattering effects. The different efficiency of rectangular and triangular shaped phase gratings at varying detector distances is investigated. The interference patterns (Talbot carpets) are modeled for parallel monochromatic radiation and measured by synchrotron radiation. In comparison to rectangular shapes of phase gratings much higher visibility is obtained for triangular shapes which yield enhanced contrast of a glass capillary test specimen.}, language = {en} }