TY - JOUR A1 - Serrano-Munoz, Itziar A1 - Roveda, Ilaria A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Synchrotron X-ray refraction detects microstructure and porosity evolution during in-situ heat treatments N2 - For the first time, synchrotron X-ray refraction radiography (SXRR) has been paired with in-situ heat treatment to monitor microstructure and porosity evolution as a function of temperature. The investigated material was a laser powder bed fusion (LPBF) manufactured AlSi10Mg, where the initial eutectic Si network is known to disintegrate and spherodize into larger particles with increasing temperature. Such alloy is also prone to thermally induced porosity (TIP). We show that SXRR allows detecting the changes in the Si-phase morphology upon heating, while this is currently possible only using scanning electron microscopy. SXRR also allows observing the growth of pores, usually studied via X-ray computed tomography, but on much smaller fields-of-view. Our results show the great potential of in-situ SXRR as a tool to gain in-depth knowledge of the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes. KW - Synchrotron X-ray refraction radiography KW - Si network disintegration KW - Thermally induced porosity (TIP) KW - Laser powder bed fusion (LPBF) KW - Statistically relevant volumes KW - AlSi10Mg alloy PY - 2022 DO - https://doi.org/10.1016/j.msea.2022.142732 SN - 0921-5093 VL - 838 SP - 1 EP - 11 PB - Elsevier CY - Amsterdam AN - OPUS4-54297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni A1 - Kupsch, Andreas A1 - Serrano-Munoz, Itziar T1 - Absorption and refraction tomography: Characterization and Non-destructive Testing of Micro-structured Materials 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. I will 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. I will also show how X-ray refraction computed tomography (CT) can be highly complementary to classic absorption CT, being sensitive to internal interfaces. T2 - MPA Seminar 2024 CY - Stuttgart, Germany DA - 08.10.2024 KW - X-ray Refaction radiography KW - X-ray computed tomography KW - Damage KW - Composites KW - Large Scale facilites KW - Synchrotron PY - 2024 AN - OPUS4-61347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Reveron, H. A1 - Serrano-Munoz, Itziar A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Chevalier, J. A1 - Bruno, Giovanni T1 - Transformation-induced plasticity in zirconia during tensile loading: A combined microscopy and synchrotron X-ray refraction study N2 - The stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation can provide a certain degree of plasticity to Ceria-stabilized (Ce-TZP) zirconia-based composites. Characterizing and monitoring this phase transition on a millimeter-size range, within the bulk and in-situ remains a challenge. In this work, the mechanical behavior of Ce-TZP based composite was studied in tension, combining microscopy and synchrotron Xray refraction techniques. In contrast with microscopy methods, which only provide surface information, X-ray refraction radiography (SXRR) allowed the visualization of all the transformation bands, over the entire length and thickness of tested specimens, opening up new avenues for in-situ stress-induced t-m transformation studies. KW - Zirconia KW - Ceria KW - Composite KW - Phase transformation KW - Plasticity KW - Synchrotron X-ray refraction PY - 2024 DO - https://doi.org/10.1016/j.matlet.2024.136445 SN - 0167-577X SN - 1873-4979 VL - 366 SP - 1 EP - 4 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-59977 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 - CONF A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Serrano-Munoz, Itziar A1 - Laquai, René A1 - Bruno, Giovanni T1 - Anwendungen der Röntgenrefraktionstechnik zur zerstörungsfreien Charakterisierung von Keramiken und Verbundwerkstoffen N2 - Die Brechung von Röntgenstrahlen (Röntgenrefraktion) an Grenzflächen zwischen Materialien unterschiedlicher Dichte ist analog zur Ablenk-ung von sichtbarem Licht an z.B. Glasoberflächen. Es gibt jedoch zwei wesentliche Unterschiede: a) konvexe Grenzflächen verursachen Divergenz (d.h. der Brechungsindex n ist kleiner als 1), und b) die Ablenkungswinkel sind sehr klein, und reichen von einigen Bogensekunden bis zu einigen Bogenminuten (d.h. n ist nahe bei 1); Wie auch bei sichtbarem Licht ist die Ablenkungsrichtung der Röntgenstrahlen abhängig von der Orientierung der durchstrahlten Grenzfläche. Aufgrund dieser Eigenschaften eignen sich Röntgenrefraktionsmethoden hervorragend für: a) die Erkennung und Quantifizierung von Defekten wie Poren und Mikrorissen und b) die Bewertung von Porosität und Partikeleigenschaften wie Orientierung, Größe und räumliche Verteilung. Wir zeigen die Anwendung der Röntgenrefraktionsradiographie (2,5D Technik) und der -tomographie (3D Technik) für die Untersuchung verschiedener Probleme in der Werkstoffwissenschaft und -technologie: a) Sintern von SiC-Grünkörpern b) Porositätsanalyse in Dieselpartikelfiltersilikaten c) Faser-Matrix-Haftung in Metall- und Polymermatrixverbundwerkstoffen d) Mikrorissbildung in Glaskeramik. Wir zeigen, dass der Einsatz von Röntgenrefraktionsmethoden quantitative Ergebnisse liefert, die direkt als Parameter in Werkstoffmodellen verwendet werden können. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Verbundwerkstoffe KW - Keramik PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576171 UR - https://jahrestagung.dgzfp.de/Portals/jt2023/BB180/Inhalt/p9.pdf UR - https://jahrestagung.dgzfp.de/Portals/jt2023/BB180/Inhalt/default.htm SN - 978-3-947971-29-9 SP - 1 EP - 16 PB - Deutsche Gesellschaft für Zerstörungsfreie Prüfung (DGZfP) CY - Berlin AN - OPUS4-57617 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Buljak, Vladimir A1 - Serrano-Munoz, Itziar A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Prasek, Marko A1 - Contillo, Adriano A1 - Mouiya, Mossaab A1 - Huger, Marc A1 - Bruno, Giovanni T1 - On the closure of thermally induced micro-cracks in aluminum titanate ceramics N2 - Aluminum Titanate (AT) refractory ceramics (as some other ceramic composites) are prone to microcracking, due to the thermal expansion anisotropy of AT and to the mismatch with the thermal expansion of the constituents. Such microcracks cause the room temperature Young's modulus to be only a fraction of that of the non-microcracked material. As a function of temperature, the Young's modulus increases non-linearly. Such increase suggests that microcracks close or even heal at high temperatures. Upon cooling, thermal stress accumulates again, and microcracks re-open. This cycle is fully reversible. While confirming the hysteretic behavior of the Young's modulus, we observe that the amount of microcracks (as determined by in-situ Synchrotron X-ray refraction radiography) decreases linearly upon heating. The apparent mismatch between the Young's modulus and the microcrack content dependence on temperature is explained by a simple FEM model. Such model employs cohesive elements upon cooling, in order to estimate the amount of initial microcracks. On purpose, the model does not include healing upon heating and only allows crack closure. It predicts that crack closure continuously occurs upon heating, thereby qualitatively reproducing the nearly linear dependence of the X-ray refraction signal. It is therefore concluded that the sudden and non-linear increase of Young's modulus with temperature is mainly caused by crack healing. Such finding agrees with previous work and paves the road to a more systematic separation of crack closure and healing in flexible ceramics. KW - X-ray computed tomography KW - X-ray refraction radiography KW - In-situ imaging KW - BAMline KW - Micromechanics KW - BESSY II PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645082 DO - https://doi.org/10.1016/j.ceramint.2025.09.237 SN - 0272-8842 VL - 51 IS - 27 SP - 55141 EP - 55152 PB - Elsevier CY - Amsterdam AN - OPUS4-64508 LA - eng 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 - CONF A1 - Serrano-Munoz, Itziar A1 - Mouiya, Mossaab A1 - Prasek, Marco A1 - Kupsch, Andreas A1 - Bruno, Giovanni T1 - High temperature in-situ heat treatment of a refractory material by means of synchrotron refraction radiography N2 - The stress–strain behavior of certain ceramics, such as aluminum titanate (AT, Al2TiO5), has features that are unusual for brittle material. In particular, a substantial nonlinearity under uniaxial tension, and load–unload hysteresis caused by the increase of the incremental stiffness at the beginning of unloading. These features are observed experimentally and attributed to microcracking. In this study, we investigate the mechanical response of an AT material at room and high temperature. Microstructure and microcracking are analyzed by means of electron microscopy, and both synchrotron micro computed tomography (µCT) and refraction radiography (SXRR). Synchrotron refraction radiography is combined with in-situ heating at high-temperatures (up to 1400°C) to be able to monitor the relative closure of microcracks as a function of increasing/decreasing temperatures. T2 - ECCM21 CY - Nantes, France DA - 02.07.2024 KW - Refractory materials KW - Microcracking KW - Synchrotron µCT and refraction radiography KW - In-situ heating up to 1400°C PY - 2024 UR - https://gem.ec-nantes.fr/en/eccm21-proceedings/ SN - 978-2-912985-01-9 DO - https://doi.org/10.60691/yj56-np80 SP - 47 EP - 53 PB - The European Society for Composite Materials (ESCM) and the Ecole Centrale de Nantes. CY - Nantes AN - OPUS4-60581 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -