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 U6 - 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 - 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 U6 - 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 - 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 U6 - 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 - Müller, Bernd R. A1 - Cabeza, S. A1 - Pereyra, R. A1 - Fernández, R. A1 - González-Doncelc, G. A1 - Kupsch, Andreas A1 - Bruno, Giovanni T1 - Nachweis der Schädigungsentwicklung mittels Synchrotron-Röntgenrefraktionstechnik während des Kriechversuchs einer Al-Mg-Legierung N2 - Um die Gültigkeit der Vorhersagen des aktuellen Solid-State-Transformation-Creep (SSTC)-Modells zu verifizieren, wurde die Schadensakkumulation während eines Kriecheversuchs an einer Al-3,85Mg Legierung mittels Synchrotron Röntgenrefraktionstechnik untersucht. Das Röntgenrefraktionsverfahren erfasst die innere spezifische Oberfläche (d.h. Oberfläche pro Volumeneinheit) im durchstrahlten Volumen. Dabei liegt die Detektierbarkeit von Rissen und Poren in der Größenordnung von wenigen Nano- bis Mikrometern. Im Vergleich zu CT-Messungen mit vergleichbarer Sensitivität ist das untersuchte Probenvolumen jedoch um den Faktor 10 größer. Ein signifikanter Anstieg der inneren spezifischen Oberfläche mit zunehmender Kriechzeit wurde beobachtet, was den Nachweis für die Entstehung einer feinkörnigen Substruktur liefert, wie sie im SSTC-Modell vorhergesagt wird. Diese feinkörnige Substruktur wurde auch mittels Rasterelektronenmikroskopie beobachtet. T2 - DACH-Tagung 2019 CY - Friedrichshafen, Germany DA - 26.05.2019 KW - Aluminiumlegierungen KW - Kriechverhalten KW - Schädigungsverhalten KW - Synchrotron Röntgen Refraktion PY - 2019 AN - OPUS4-48492 LA - deu 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 U6 - http://nbn-resolving.de/urn/resolver.pl?urn:nbn:de:kobv:b43-515060 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 - 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 U6 - 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 - CONF A1 - Müller, Bernd R. A1 - Mack, D.E. A1 - Laquai, René A1 - Helle, O. A1 - Sebold, D. A1 - Vaßen, R. A1 - Bruno, Giovanni T1 - Evolution of porosity, crack density, and CMAS penetration in thermal barrier coatings subjected to burner rig testing N2 - Degradation of thermal barrier coatings (TBCs) in gas‐turbine engines due to calcium–magnesium–aluminosilicate (CMAS) glassy deposits from various sources has been a persistent issue since many years. In this study, state of the art electron microscopy was correlated with X‐ray refraction techniques to elucidate the intrusion of CMAS into the porous structure of atmospheric plasma sprayed (APS) TBCs and the formation and growth of cracks under thermal cycling in a burner rig. Results indicate that the sparse nature of the infiltration as well as kinetics in the burner rig are majorly influenced by the wetting behavior of the CMAS. Despite the obvious attack of CMAS on grain boundaries, the interaction of yttria‐stabilized zirconia (YSZ) with intruded CMAS has no immediate impact on structure and density of internal surfaces. At a later stage the formation of horizontal cracks is observed in a wider zone of the TBC layer. T2 - Eleventh Joint BER II and BESSY II User Meeting CY - Wilhelm-Conrad-Roentgen-Campus, Berlin-Adlershof, Germany DA - 04.12.2019 KW - Characterization KW - CMAS KW - Synchrotron X-ray refraction radiography KW - Thermal arrier coatings PY - 2019 AN - OPUS4-49857 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Liens, A. A1 - Reveron, H. A1 - Douillard, T. A1 - Blanchard, N. A1 - Lughi, V. A1 - Sergo, V. A1 - Laquai, René A1 - Müller, Bernd R. A1 - Bruno, Giovanni A1 - Schomer, S. A1 - Fürderer, T. A1 - Adolfsson, E. A1 - Courtois, N. A1 - Swain, M. A1 - Chevalier, J. T1 - Phase transformation induces plasticity with negligible damage in ceria-stabilized zirconia-based ceramics N2 - Ceramics and their composites are in general brittle materials because they are predominantly made up of ionic and covalent bonds that avoid dislocation motion at room temperature. However, a remarkable ductile behavior has been observed on newly developed 11 mol.% ceria-stabilized zirconia (11Ce-TZP) composite containing fine alumina (8 vol.% Al2O3) and elongated strontium hexa-aluminate (8 vol.% SrAl12O19) grains. The as-synthesized composite also has shown full resistance to Low Temperature Degradation (LTD), relatively high strength and exceptionally high Weibull modulus, allowing its use in a broader range of biomedical applications. In this study, to deepen the understanding of plastic deformation in Ce-TZP based composites that could soon be used for manufacturing dental implants, different mechanical tests were applied on the material, followed by complete microstructural characterization. Distinct from pure Ce-TZP material or other zirconia-based ceramics developed in the past, the material here studied can be permanently strained without affecting the Young modulus, indicating that the ductile response of tested samples cannot be associated to damage occurrence. This ductility is related to the stress-induced tetragonal to monoclinic (t-m) zirconia phase transformation, analogue to Transformation-Induced Plasticity (TRIP) steels, where retained austenite is transformed to martensite. The aim of this study is to corroborate if the observed plasticity can be associated exclusively to the zirconia t-m phase transformation, or also to microcraking induced by the transformation. The t-m transformed-zones produced after bending and biaxial tests were examined by X-ray refraction and SEM/TEM coupled with Raman. The results revealed that the observed elastic-plastic behavior occurs without extensive microcracking, confirming a purely elastic-plastic behavior driven by the phase transformation (absence of damage). KW - Zirconia KW - Ceria KW - Ceramic matrix composite KW - Plasticity KW - Phase transformation KW - X-Ray Refraction PY - 2020 UR - http://www.sciencedirect.com/science/article/pii/S1359645419307177 U6 - https://doi.org/10.1016/j.actamat.2019.10.046 SN - 1359-6454 VL - 183 SP - 261 EP - 273 PB - Elsevier Ltd. AN - OPUS4-49740 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 U6 - 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 - Ulbricht, Alexander A1 - Gollwitzer, Christian A1 - Kupsch, Andreas A1 - Léonard, Fabien A1 - Müller, Bernd R. A1 - Oesch, Tyler A1 - Onel, Yener A1 - Thiede, Tobias A1 - Zscherpel, Uwe ED - Puente León, F. ED - Zagar, B. T1 - Moderne Methoden der CT-gestützten Strukturanalyse T1 - Modern techniques of CT based structure analysis N2 - Durch den großflächigen Einsatz der Computertomographie (CT) in unterschiedlichen Industriebereichen steigen auch die Anforderungen an die quantitative Bildanalyse. Subjektive Bildwahrnehmung muss durch objektive Algorithmen ersetzt werden. In diesem Artikel stellt die Bundesanstalt für Materialforschung und -prüfung (BAM), die seit den 1980er Jahren an der Entwicklung der industriellen CT beteiligt ist, anhand ausgewählter Beispiele den aktuellen Stand ihrer Analysemethoden an verschiedenen Anwendungsbeispielen der CT vor. N2 - The increasing use of computed tomography (CT) in various industrial sectors requires more sophisticated techniques of quantitative image analysis. Subjective image perception needs to be replaced by objective algorithms. The German Federal Institute for Materials Research and Testing (BAM) has been involved in the development of industrial CT since the 1980s. This paper summarizes the current status of quantitative 3D image analysis techniques based on selected examples. KW - Computed tomography KW - Computertomographie KW - Röntgen-Refraktion KW - X-Ray refraction KW - Schadensanalyse KW - Damage analysis KW - Normung KW - standardization PY - 2020 U6 - https://doi.org/10.1515/teme-2019-0125 SN - 0171-8096 SN - 2196-7113 VL - 87 IS - 2 SP - 81 EP - 91 PB - de Gruyter CY - Berlin AN - OPUS4-50337 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -