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, Itziar A1 - Müller, Bernd A1 - Kupsch, Andreas A1 - Bruno, Giovanni A1 - Laquai, Rene' T1 - X-ray refractio techniques non-destructively quantify and classify defects in am materials 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). 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, they can detect objects with size above a few wavelengths of the radiation. 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. The use of X-ray refraction analysis yields quantitative information, which can be directly input in kinetics, mechanical and damage models. We hereby show the application of non-destructive X-ray refraction radiography (SXRR, 2D mapping also called topography) to problems in additive manufacturing: 1) Porosity analysis in PBF-LM-Ti64. Through the use of SXRR, we could not only map the (very sparse) porosity distribution between the layers and quantify it, but also classify, and thereby separate, the filled porosity (unmolten powder) from the keyhole and gas pores (Figure 1). 2) In-situ heat treatment of laser powder bed fusion PBF-LM-AlSi10Mg to monitor microstructure and porosity evolution as a function of temperature (Figure 2). By means of SXRR we indirectly observed the initial eutectic Si network break down into larger particles as a function of increasing temperature. We also could detect the thermally induced porosity (TIP). Such changes in the Si-phase morphology upon heating is currently only possible using scanning electron microscopy, but with a much smaller field-of-view. SXRR also allows observing the growth of some individual pores, usually studied via X-ray computed tomography, but again 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 defect distribution and the susceptibility of any material to thermally induced damage and/or microstructure evolution over statistically relevant volumes. T2 - AAMS 2023 CY - Madrid, Spain DA - 27.09.2023 KW - X-ray Refaction radiography KW - Defects KW - Large Scale Facilities KW - Computed tomography PY - 2023 AN - OPUS4-58508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Piault, Pierre A1 - King, Andrew A1 - Henry, Laura A1 - Bruno, Giovanni T1 - Understanding the hot isostatic pressing efectiveness of laser powder bed fusion Ti‑6Al‑4V by in‑situ X‑ray imaging and difraction experiments JF - Scientific reports N2 - In the present study, in-situ observation of Hot Isostatic Pressure (HIP) procedure of laser powder bed fusion manufactured Ti-6Al-4V parts was performed to quantitatively estimate the densifcation rate of the material and the infuence of the defect initial size and shape on such rate. The observations were performed in-situ using the Ultrafast Tomography Paris-Edinburgh Cell and the combination of fast phase-contrast synchrotron X-ray tomography and energy dispersive difraction. With this strategy, we could quantify how the efectiveness of HIP depends on the characteristics of a defect. Smaller defects showed a higher densifcation rate, while the defect shape did not have signifcant efect on such rate. KW - Additive manufacturing KW - Laser powder bed fusion KW - X-ray computed tomography KW - Hot isostatic pressing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-587702 DO - https://doi.org/10.1038/s41598-023-45258-1 SN - 2045-2322 VL - 13 IS - 1 SP - 1 EP - 11 AN - OPUS4-58770 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Khrapov, D. A1 - Paveleva, A. A1 - Kozadayeva, M. A1 - Evsevleev, Sergei A1 - Mishurova, Tatiana A1 - Bruno, Giovanni A1 - Surmenev, R. A1 - Koptyug, A. A1 - Surmeneva, M. T1 - Trapped powder removal from sheet-based porous structures based on triply periodic minimal surfaces fabricated by electron beam powder bed fusion JF - Materials Science & Engineering A N2 - Electron Beam Powder Bed Fusion-manufactured (E-PBF) porous components with narrow pores or channels and rough walls or struts can be filled with trapped powder after the manufacturing process. Adequate powder removal procedures are required, especially for high-density porous structures. In the present research, sheetbased porous structures with different thicknesses based on triply periodic minimal surfaces fabricated by EPBF were subjected to different post-processing methods, including a traditional powder recovery system for EPBF, chemical etching and ultrasound vibration-assisted powder removal. Wall thickness, internal defects, microstructure and morphology features, powder distribution inside the specimens, mechanical properties and deformation modes were investigated. A powder recovery system could not remove all residual powder from dense structures. In turn, chemical etching was effective for surface morphology changes and subsurface layers elimination but not for powder removal, as it affected the wall thickness, considerably influencing the mechanical properties of the whole structure. The ultrasound vibration method was quite effective for the removal of residual powder from sheet-based TMPS structures and without a severe degradation of mechanical properties. 10.1016/j.msea.2022.144479 Ultrasound vibration also caused grain refinement. KW - Additive manufacturing KW - Residual powder removal KW - Ti6Al4V alloy KW - Electron beam powder bed fusion KW - TPMS structures PY - 2023 DO - https://doi.org/10.1016/j.msea.2022.144479 VL - 862 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-56564 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - De la Hoz Alford, L. A1 - Pecanha de Souza, C. G. A1 - Paciornik, S. A1 - d` Almeida, J. R. M. A1 - Santos Leite, B. A1 - Avila, H. C. A1 - Léonard, F. A1 - Bruno, Giovanni T1 - Three-Dimensional Characterization of Polyurethane Foams Based on Biopolyols JF - Three-Dimensional Characterization of Polyurethane Foams Based on Biopolyols N2 - Two biopolyol-based foams derived from banana leaves (BL) or stems (BS) were produced, and their compression mechanical behavior and 3D microstructure were characterized. Traditional compression and in situ tests were performed during 3D image acquisition using X-ray microtomography. A methodology of image acquisition, processing, and analysis was developed to discriminate the foam cells and measure their numbers, volumes, and shapes along with the compression steps. The two foams had similar compression behaviors, but the average cell volume was five times larger for the BS foam than the BL foam. It was also shown that the number of cells increased with increasing compression while the average cell volume decreased. Cell shapes were elongated and did not change with compression. A possible explanation for these characteristics was proposed based on the possibility of cell collapse. The developed methodology will facilitate a broader study of biopolyol-based foams intending to verify the possibility of using these foams as green alternatives to the typical petrol-based foams. KW - Compression mechanical KW - Biopolyol KW - Banana KW - 3D microstructure KW - X-ray microtomography PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571982 DO - https://doi.org/10.3390/ma16052118 SN - 1996-1944 VL - 16 IS - 5 SP - 1 EP - 12 PB - MDPI CY - Basel AN - OPUS4-57198 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 JF - Journal of the American Ceramic Society 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 - JOUR A1 - Schröder, Jakob A1 - Evans, Alexander A1 - Luzin, V. A1 - Abreu Faria, G. A1 - Degener, Sebastian A1 - Polatidis, E. A1 - Čapek, J. A1 - Kromm, Arne A1 - Dovzhenko, G. A1 - Bruno, Giovanni T1 - Texture-based residual stress analysis of laser powder bed fused Inconel 718 parts JF - Journal of Applied Crystallography N2 - Although layer-based additive manufacturing methods such as laser powder bed fusion (PBF-LB) offer an immense geometrical freedom in design, they are typically subject to a build-up of internal stress (i.e. thermal stress) during manufacturing. As a consequence, significant residual stress (RS) is retained in the final part as a footprint of these internal stresses. Furthermore, localized melting and solidification inherently induce columnar-type grain growth accompanied by crystallographic texture. Although diffraction-based methods are commonly used to determine the RS distribution in PBF-LB parts, such features pose metrological challenges in their application. In theory, preferred grain orientation invalidates the hypothesis of isotropic material behavior underlying the common methods to determine RS. In this work, more refined methods are employed to determine RS in PBF-LB/M/IN718 prisms, based on crystallographic texture data. In fact, the employment of direction-dependent elastic constants (i.e. stress factors) for the calculation of RS results in insignificant differences from conventional approaches based on the hypothesis of isotropic mechanical properties. It can be concluded that this result is directly linked to the fact that the {311} lattice planes typically used for RS analysis in nickel-based alloys have high multiplicity and less strong texture intensities compared with other lattice planes. It is also found that the length of the laser scan vectors determines the surface RS distribution in prisms prior to their removal from the baseplate. On removal from the baseplate the surface RS considerably relaxes and/or redistributes; a combination of the geometry and the scanning strategy dictates the sub-surface RS distribution. KW - Additive manufacturing KW - Electron backscattered diffraction KW - Principal stress KW - Residual stress PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-578331 DO - https://doi.org/10.1107/S1600576723004855 SN - 1600-5767 VL - 56 IS - Pt 4 SP - 1076 EP - 1090 AN - OPUS4-57833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Fioresi, R. A1 - Faglioni, F. A1 - Bruno, Giovanni T1 - Synthetic Data Generation for Automatic Segmentation of X-ray Computed Tomography Reconstructions of Complex Microstructures JF - Journal of Imaging N2 - The greatest challenge when using deep convolutional neural networks (DCNNs) for automatic segmentation of microstructural X-ray computed tomography (XCT) data is the acquisition of sufficient and relevant data to train the working network. Traditionally, these have been attained by manually annotating a few slices for 2D DCNNs. However, complex multiphase microstructures would presumably be better segmented with 3D networks. However, manual segmentation labeling for 3D problems is prohibitive. In this work, we introduce a method for generating synthetic XCT data for a challenging six-phase Al–Si alloy composite reinforced with ceramic fibers and particles. Moreover, we propose certain data augmentations (brightness, contrast, noise, and blur), a special in-house designed deep convolutional neural network (Triple UNet), and a multi-view forwarding strategy to promote generalized learning from synthetic data and therefore achieve successful segmentations. We obtain an overall Dice score of 0.77. Lastly, we prove the detrimental effects of artifacts in the XCT data on achieving accurate segmentations when synthetic data are employed for training the DCNNs. The methods presented in this work are applicable to other materials and imaging techniques as well. Successful segmentation coupled with neural networks trained with synthetic data will accelerate scientific output. KW - Automatic segmentation KW - 3D deep convolutional neural network (3D DCNN) KW - Dice score KW - Metal matrix composite (MMC) KW - Modified U-Net architectures KW - Multi-phase materials PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-571243 DO - https://doi.org/10.3390/jimaging9020022 VL - 9 IS - 2 SP - 1 EP - 23 PB - MDPI AN - OPUS4-57124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bruno, Giovanni T1 - Strategies to use neutrons as an industrial problem-solving tool N2 - For how trivial or provocative it can sound, the best neutron spectrometer in the world does not produce science and technology by itself. By definition of “Materials Science”, neutron scattering data on engineering materials must be used as a tool to understand, and even tailor, materials performance. In order for this to happen, neutron data need to be 1. Acquired under the most relevant condition possible 2. Coupled to other experimental techniques 3. Capitalized by means of proper simulations and data analysis Point 1- calls for an intense use and the development of top-notch of in-situ techniques; Point 2- means that the sole use of neutron data will not lead to any solution of a global problem; All points above hint to the fact that access to neutron sources is not routine, and therefore it is imperative to search ways to make neutron data rentable and sustainable for the material science and industrial research community. In this presentation, and based on two examples, we will show a couple of strategies to combine neutron data with other experiments, and with theoretical models to raise the validity of experiments to the level of problem-solving. As one might imagine, these are only a few among the almost infinite combinations possible to help improving material properties, performance, and safety, i.e., ripe for everyday use. T2 - MORIS Workshop CY - Garching, Germany DA - 26.04.2023 KW - Neutron Diffraction KW - Residual Stress KW - Large Scale Facilities KW - X-ray Computed Tomography PY - 2023 AN - OPUS4-57361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rieder, Philipp A1 - Petrich, Lukas A1 - Serrano Munoz, Itziar A1 - Fernández, Ricardo A1 - Bruno, Giovanni A1 - Schmidt, Volker T1 - Statistical Comparison of Substructures in Pure Aluminum Before and After Creep Deformation, Based on EBSD Image Data JF - Microscopy and Microanalysis N2 - Electron backscatter diffraction (EBSD) images of extruded pure aluminum were statistically analyzed to investigate creep-induced subgrain structures after applying two different levels of creep stress, corresponding to the power law (PL) and power-law breakdown (PLB) regimes. Kernel average misorientation analysis of EBSD measurements revealed 2D morphologies, which were subdivided by a multi-step segmentation procedure into subgranular arrangements. Various descriptors were employed to characterize the “subgrains” quantitatively, including their size, shape, spatial arrangement, and crystallographic orientation. In particular, the analysis of the orientations of subgrains was conducted by neglecting rotations around the loading axis. This approach facilitated the individual investigation of the {001} and {111} subgrain families with respect to the loading axis for two investigated stress levels plus a reference specimen. For the PL regime, the statistical analysis of subgrain descriptors computed from segmented image data revealed a similar degree of strain accumulation for {111} and {001} subgrains. In contrast, for the PLB regime, the analyzed descriptors indicate that {111} subgrains tend to accumulate significantly more strain than {001} ones. These observations suggest that the mechanisms leading to PLB may be associated with strain localization dependent on intergranular stress, hindering the recovery process within {111} grains. KW - Crystallographic descriptor KW - Dislocation-climb-controlled creep KW - Electron backscatter diffraction (EBSD) KW - Geometric descriptor KW - Ernel average misorientation (KAM) KW - pure aluminum KW - Qquantification and segmentation KW - Statistical image analysis KW - subgrain PY - 2023 DO - https://doi.org/10.1093/micmic/ozad121 SN - 1431-9276 SP - 1 EP - 12 PB - Oxford University Press AN - OPUS4-58730 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zurcher, Theo A1 - Serrano-Munoz, Itziar A1 - Mishurova, Tatiana A1 - Abreu Faria, Guilherme A1 - Degener, Sebastian A1 - Fridrici, Vincent A1 - Charkaluk, Eric A1 - Bruno, Giovanni T1 - Sliding wear resistance and residual stresses of parts repaired by laser metal deposition JF - Journal of Material Science N2 - Large temperature gradients inherent to additive manufacturing (AM) processes induce large residual stress (RS) in the final part. Because RS can influence the tribological properties, this study focuses on the relationship between wear sliding properties and RS in IN718 coatings. Such coatings were deposited with a Laser metal deposition (LMD) machine using two different scanning strategies. The wear resistance and RS state were investigated after surface milling. RS were measured before and after wear tests on a reciprocating sliding test apparatus. Two different X-ray diffraction techniques were employed to measure the surface and subsurface state RS: Laboratory Energy Dispersive X-ray Diffraction (LEDXD) and Synchrotron X-ray Energy Dispersive Diffraction (SXEDD). Due to the milling process, the coatings show similar depth distributions of RS from 22 to 92 μm depth, but exhibit different magnitudes depending on the scanning strategy used. Reciprocating sliding wear tests induced high compressive residual stresses that erased the initial RS state, and a similar wear behavior was observed in the two samples. These samples possess similar texture and grain morphology. This demonstrates that the influence of RS on wear resistance is a second-order effect. Nevertheless, it was observed that RS can still impact the wear performance at the early testing stages of the repaired parts. KW - Additive manufacturing KW - Wear resistance KW - Residual stress PY - 2023 DO - https://doi.org/10.1007/s10853-023-09129-4 SN - 0022-2461 SP - 1 EP - 18 PB - Springer AN - OPUS4-59084 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kupsch, Andreas A1 - Trappe, Volker A1 - Müller, Bernd R. A1 - Bruno, Giovanni T1 - Rissentwicklung in CFK-Laminaten nachgewiesen durch in situ Röntgen-Refraktion T2 - DGZfP-Berichtsband BB 180 N2 - In Leichtbauanwendungen sind Materialien mit geringen Dichten und hohen Festigkeiten gefragt. Insbesondere Faser-Kunststoff-Verbunde (FKV) erfüllen diese Anforderungen und werden zunehmend für Strukturbauteile eingesetzt. Die Oberflächen moderner Rotorblätter von Windkraftanlagen werden aus FKV gefertigt. Das Versagen dieser Materialien hat massiven Einfluss auf die Einsatzfähigkeit der gesamten Windkraftanlage. Daher ist die Kenntnis des Versagensverhaltens dieser Komponenten unter statischer und zyklischer Belastung von großem Interesse, um die Betriebsbeanspruchung abzuschätzen. Im Idealfall wird die Schadensentwicklung unter Betriebslast mit zerstörungsfreien in-situ-Prüfverfahren ermittelt. Hier berichten wir über die Beobachtung der Rissentwicklung in Carbon-Faserverstärkten Kunststoffen (CFK) unter kontinuierlicher Zugbelastung durch in-situ Synchrotron-Röntgenrefraktionsradiographie. Eine selbst entwickelte elektromechanische Zugprüfmaschine mit einem Kraftbereich bis zu 15 kN wurde in den Strahlengang an der BAMline (BESSY II) integriert. Da in herkömmlichen (Absorptions-) Radiographien Defekte wie Zwischenfaserbrüche oder Faser-Matrix-Enthaftung keinen ausreichenden Kontrast verursachen, wird zur Kontrastanhebung die Röntgenrefraktion benutzt. Hier wird das sogenannte Diffraction Enhanced Imaging (DEI) angewandt, um Primär- und gebrochene Strahlung mit Hilfe eines Analysatorkristalls zu trennen. Diese Technik ermöglicht schnelle Messungen mit einem Gesichtsfeld von einigen Quadratmillimetern (hier: 14 mm × 7.2 mm) und ist ideal für in-situ Untersuchungen. Die Bildgebung und der Zugversuch erfolgen mit einer Bildfrequenz von 0.7 / s und einer Dehnrate von 0.00055 / s . Bei 0°/90° Fasergelegen treten die ersten Zwischenfaserrisse bei 380 MPa (Dehnung 0.8 %) auf. Vor dem Versagen bei ca. 760 MPa (Dehnung 2.0 %) beobachten wir die Ausbildung eines nahezu äquidistanten Rissmusters (Risse in ca. 1 mm Abstand), das sich im geschädigten Zustand über die gesamte Probe erstreckt. T2 - DACH-Jahrestagung 2023 CY - Friedrichshafen, Germany DA - 15.05.2023 KW - Röntgen-Refraktion KW - Synchrotronstrahlung KW - CFK KW - Rissentwicklung PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-576230 SN - 978-3-947971-29-9 VL - BB 180 SP - 1 EP - 8 AN - OPUS4-57623 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dayani, Shahabeddin A1 - Markötter, Henning A1 - Krug von Nidda, Jonas A1 - Schmidt, Anita A1 - Bruno, Giovanni T1 - Quantification of the Deep Discharge Induced Asymmetric Copper Deposition in Lithium‐Ion Cells by Operando Synchrotron X‐Ray Tomography JF - Advanced Materials Technologies N2 - AbstractLithium‐ion cells connected in series are prone to an electrical safety risk called overdischarge. This paper presents a comprehensive investigation of the overdischarge phenomenon in lithium‐ion cells using operando nondestructive imaging. The study focuses on understanding the behavior of copper dissolution and deposition during overdischarge, which can lead to irreversible capacity loss and internal short‐circuits. By utilizing synchrotron X‐ray computed tomography (SXCT), the concentration of dissolved and deposited copper per surface area is quantified as a function of depth of discharge, confirming previous findings. The results also highlight for the first time a nonuniform distribution pattern for copper deposition on the cathode. This research provides insights for safer battery cell design. KW - Lithium Ion Batteries KW - Deep Discharge KW - Computer Tomography KW - Copper Deposition KW - Litium Ion Cells PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-592717 DO - https://doi.org/10.1002/admt.202301246 SP - 1 EP - 7 PB - Wiley AN - OPUS4-59271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fernández, R. A1 - Bokuchava, G. A1 - Bruno, Giovanni A1 - Serrano Munoz, Itziar A1 - González Doncel, G. T1 - On the dependence of creep-induced dislocation configurations on crystallographic orientation in pure Al and Al-Mg JF - Journal of Applied Crystallography N2 - The peak broadening in neutron diffraction experiments on tensile specimens of pure Al (99.8%) and an Al-Mg alloy pre-deformed at different creep strains is analysed. These results are combined with the kernel angular misorientation of electron backscatter diffraction data from the creep-deformed microstructures. It is found that differently oriented grains possess different microstrains. These microstrains vary with creep strain in pure Al, but not in the Al-Mg alloy. It is proposed that this behaviour can explain the power-law breakdown in pure Al and the large creep strain observed in Al-Mg. The present findings further corroborate a description of the creep-induced dislocation structure as a fractal, predicated on previous work. KW - Creep KW - Aluminium alloys KW - Dislocations KW - Fractals KW - Diffraction peak width PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-575527 DO - https://doi.org/10.1107/S1600576723003771 SN - 0021-8898 VL - 56 IS - Pt 3 SP - 764 EP - 775 AN - OPUS4-57552 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tsamos, Athanasios A1 - Evsevleev, Sergei A1 - Bruno, Giovanni T1 - Noise and blur removal from corrupted X-ray computed tomography scans: A multilevel and multiscale deep convolutional framework approach with synthetic training data (BAM SynthCOND) JF - Tomography of Materials and Structures N2 - Regardless of the experimental care practiced in acquiring X-ray computed tomography (XCT) data, artifacts might still exist, such as noise and blur. This is typical for fast XCT data acquisitions (e.g., in-situ investigations), or low-dose XCT. Such artifacts can complicate subsequent analysis of the data. Digital filters can moderately cure extensive artifacts. The selection of filter type, intensity, and order of application is not always straight forward. To tackle these problems, a complete sequential multilevel, multi-scale framework: BAM SynthCOND, employing newly designed deep convolutional neural networks (DCNNs), was formulated. Although data conditioning with neural networks is not uncommon, the main complication is that completely artifact-free XCT data for training do not exist. Thus, training data were acquired from an in-house developed library (BAM SynthMAT) capable of generating synthetic XCT material microstructures. Some novel DCNN architectures were introduced (2D/3D ACEnet_Denoise, 2D/3D ACEnet_Deblur) along with the concept of Assertive Contrast Enhancement (ACE) training, which boosts the performance of neural networks trained with continuous loss functions. The proposed methodology accomplished very good generalization from low resemblance synthetic training data. Indeed, denoising, sharpening (deblurring), and even ring artifact removal performance were achieved on experimental post-CT scans of challenging multiphase Al-Si Metal Matrix Composite (MMC) microstructures. The conditioning efficiencies were: 92% for combined denoising/sharpening, 99% for standalone denoising, and 95% for standalone sharpening. The results proved to be independent of the artifact intensity. We believe that the novel concepts and methodology developed in this work can be directly applied on the CT projections prior to reconstruction, or easily be extended to other imaging techniques such as: Microscopy, Neutron Tomography, Ultrasonics, etc. KW - XCT Data Conditioning KW - Denoising Deblurring Sharpening KW - Deep Convolutional Neural Network (DCNN) KW - Synthetic Training Data KW - ACEnet KW - Metal Matrix Composite (MMC) PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-579129 DO - https://doi.org/10.1016/j.tmater.2023.100011 VL - 2 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-57912 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dayani, Shahabeddin A1 - Markötter, Henning A1 - Schmidt, Anita A1 - Widjaja, Martinus Putra A1 - Bruno, Giovanni T1 - Multi-level X-ray computed tomography (XCT) investigations of commercial lithium-ion batteries from cell to particle level JF - Journal of Energy Storage N2 - Adopting X-ray computed tomography (XCT) for ex-situ characterization of battery materials has gained interest in the past decade. The main goal of this paper is to demonstrate the effectiveness of several X-ray computer tomography techniques to study commercial batteries. General guidelines are provided to select the most suitable imaging equipment and parameters for investigations of lithium-ion batteries, spanning the length scales from cell to electrode, down to particle level. Relevantly, such parameters would also be suitable for operando experiments. Safety mechanisms and manufacturing inconsistencies at cell level as well as defects and inhomogeneity in cathode and anode is illustrated and quantified. Furthermore, relation of beam energy and sample-detector-distance on contrast retrieved from attenuation and phase shift is inspected using Synchrotron XCT. KW - Non-destructive testing KW - X-ray computed tomography KW - Synchrotron X-ray computed tomography KW - Lithium-ion battery PY - 2023 DO - https://doi.org/10.1016/j.est.2023.107453 SN - 2352-152X VL - 66 SP - 107453 PB - Elsevier Ltd. AN - OPUS4-57512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mehta, B. A1 - Mishurova, Tatiana A1 - Evsevleev, Sergei A1 - Markötter, Henning A1 - Bruno, Giovanni A1 - Hryha, E. A1 - Nyborg, L. A1 - Virtanen, E. T1 - Microstructure, mechanical properties and fracture mechanisms in a 7017 aluminium alloy tailored for powder bed fusion – laser beam JF - Materials and Design N2 - This study addressed a 7017 Al-alloy tailored for powder bed fusion – laser beam (PBF-LB) process. The alloy was prepared by mixing 3 wt% Zr and 0.5 wt% TiC powder to standard pre-alloyed 7017 grade aluminium powder. This made printing of the alloys possible avoiding solidification cracking in the bulk and achieving high relative density (99.8 %). Such advanced alloys have significantly higher Young’s modulus (>80 GPa) than conventional Al-alloys (70–75 GPa), thus making them attractive for applications requiring high stiffness. The resulting microstructure in as-printed condition was rich in particles originating from admixed powders and primary precipitates/inclusions originating from the PBF-LB process. After performing a T6-like heat treatment designed for the PBF-LB process, the microstructure changed: Zr-nanoparticles and Fe- or Mg/Zn- containing precipitates formed thus providing 75 % increase in yield strength (from 254 MPa to 444 MPa) at the cost of decreasing ductility (∼20 % to ∼9 %). In-situ tensile testing combined with SXCT, and ex-situ tensile testing combined with fracture analysis confirmed that the fracture initiation in both conditions is highly dependent on defects originated during printing. However, cracks are deflected from decohesion around Zr-containing inclusions/precipitates embedded in the Al-matrix. This deflection is seen to improve the ductility of the material. KW - Additive manufacturing KW - Powder bed fusion Laser beam KW - X-ray computed tomography KW - Strengthening mechanisms KW - Crack propagation KW - Zirconium PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568243 DO - https://doi.org/10.1016/j.matdes.2023.111602 SN - 0264-1275 VL - 226 SP - 1 EP - 14 PB - Elsevier Science CY - Amsterdam [u.a.] AN - OPUS4-56824 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zocca, Andrea A1 - Müller, Bernd R. A1 - Laquai, René A1 - Kupsch, Andreas A1 - Wieder, Frank A1 - Benemann, Sigrid A1 - Wilbig, Janka A1 - Günster, Jens A1 - Bruno, Giovanni T1 - Microstructural characterization of AP40 apatite-wollastonite glass-ceramic JF - Ceramics international N2 - The microstructure of an apatite-wollastonite (code name AP40) glass-ceramic is analyzed in this study by combining 2D microscopy, phase analysis, X-ray absorption and synchrotron X-ray refraction computed tomography (XCT and SXRCT, respectively). It is shown that this combination provides a useful toolbox to characterize the global microstructure in a wide scale range, from sub-micrometer to millimeter. The material displays a complex microstructure comprising a glassy matrix with embedded fluorapatite and wollastonite small crystals. In this matrix, large (up to 200 μm) spike-shaped structures are distributed. Such microstructural features are oriented around a central sphere, thereby forming a structure resembling a sea urchin. A unique feature of SXRCT, in contrast to XCT, is that internal interfaces are visualized; this allows one to show the 3D distribution of these urchins with exceptionally good contrast. Furthermore, it is revealed that the spike-shaped structures are not single crystals, but rather composed of sub-micrometric crystals, which are identified as fluorapatite and diopside phases by SEM-EDX analysis. KW - Glass-ceramic KW - X-ray refraction KW - Computed tomography KW - Microstructure PY - 2023 DO - https://doi.org/10.1016/j.ceramint.2022.12.130 SN - 0272-8842 VL - 49 IS - 8 SP - 12672 EP - 12679 PB - Elsevier Science CY - Amsterdam AN - OPUS4-57452 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Bruno, Giovanni A1 - Kachanov, M. A1 - Sevostianov, I. ED - Bruno, Giovanni ED - Altenbach, H. ED - Eremeyev, V. ED - Müller, W. ED - Gutkin, M. T1 - Micromechanical Modeling of Non-linear Stress–Strain Behavior of Polycrystalline Microcracked Ceramics T2 - Mechanics of Heterogeneous Materials N2 - We discuss the non-linear stress–strain behavior of microcracked polycrystalline ceramics under uniaxial tension and compression (displacement control). Micromechanics explanation and modeling of its basic features, such as non-linearity and hysteresis in stress–strain curves, are developed, with stable microcrack propagation and “roughness” of intergranular cracks playing critical roles in tension and crack sliding playing a critical role in compression. Experiments involving complex loading histories are explained, and themodel is shown to reproduce the basic features of the observed stress–strain curves. KW - Neutron Diffraction KW - X-ray diffraction KW - Mechanical Properties KW - X-ray refraction radiography KW - Microcracking KW - Aluminum Titanate PY - 2023 SN - 978-3-031-28743-5 DO - https://doi.org/10.1007/978-3-031-28744-2 SN - 1869-8433 SP - 1 EP - 22 PB - Springer CY - Heidelberg AN - OPUS4-57938 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ulbricht, Alexander A1 - Avila Calderon, Luis A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Evans, Alexander A1 - Skrotzki, Birgit A1 - Bruno, Giovanni T1 - Evolution of Creep Damage of 316L Produced by Laser Powder Bed Fusion JF - Advanced Engineering Materials N2 - The damage mechanisms of metallic components produced by process laser powder bed fusion differ significantly from those typically observed in conventionally manufactured variants of the same alloy. This is due to the unique microstructures of additively manufactured materials. Herein, the focus is on the study of the evolution of creep damage in stainless steel 316L specimens produced by laser powder bed fusion. X-ray computed tomography is used to unravel the influence of the process-specific microstructure from the influence of the initial void distribution on creep damage mechanisms. The void distribution of two specimens tested at 600 °C and 650 °C is analyzed before a creep test, after an interruption, and after fracture. The results indicate that the formation of damage is not connected to the initial void distribution. Instead, damage accumulation at grain boundaries resulting from intergranular cracking is observed. KW - Creep KW - Computed Tomography KW - PBF-LB/M/316L KW - Laser Powder Bed Fusion KW - Microstructure KW - AISI 316L KW - Additive Manufacturing PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-574127 DO - https://doi.org/10.1002/adem.202201581 SP - 1 EP - 9 PB - Wiley-VCH GmbH CY - Weinheim AN - OPUS4-57412 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -