TY - JOUR A1 - Ziesche, R. F. A1 - Robinson, J. B. A1 - Markötter, Henning A1 - Bradbury, R. A1 - Tengattini, A. A1 - Lenoir, N. A1 - Helfen, L. A1 - Kockelmann, W. A1 - Kardjilov, N. A1 - Manke, I. A1 - Brett, D. J. L. A1 - Shearing, P. R. T1 - Editors’ Choice—4D Neutron and X-ray Tomography Studies of High Energy Density Primary Batteries: Part II. Multi-Modal Microscopy of LiSOCl2 Cells N2 - The ability to track electrode degradation, both spatially and temporally, is fundamental to understand performance loss during operation of lithium batteries. X-ray computed tomography can be used to follow structural and morphological changes in electrodes; however, the direct detection of electrochemical processes related to metallic lithium is difficult due to the low sensitivity to the element. In this work, 4-dimensional neutron computed tomography, which shows high contrast for lithium, is used to directly quantify the lithium diffusion process in spirally wound Li/SOCl2 primary cells. The neutron dataset enables the quantification of the lithium transport from the anode and the accumulation inside the SOCl2 cathode to be locally resolved. Complementarity between the collected neutron and X-ray computed tomographies is shown and by applying both methods in concert we have observed lithium diffusion blocking by the LiCl protection layer and identified all cell components which are difficult to distinguish using one of the methods alone. KW - Lithium-ion battery KW - Room-temperature KW - Thermal runaway KW - Gas evolution KW - Cells PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-520890 DO - https://doi.org/10.1149/1945-7111/abbfd9 VL - 167 SP - 140509 PB - IOP Science AN - OPUS4-52089 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Yao, J. A1 - Zhu, G. A1 - Dong, K. A1 - Osenberg, M. A1 - Hilger, A. A1 - Markötter, Henning A1 - Ju, J. A1 - Sun, F. A1 - Manke, I. A1 - Cui, G. T1 - Progress and Perspective of Controlling Li Dendrites Growth in All-Solid-State Li Metal Batteries via External Physical Fields N2 - Li dendrites penetration through solid electrolytes (SEs) challenges the development of solid-state Li batteries (SSLBs). To date, significant efforts are devoted to understand the mechanistic dynamics of Li dendrites nucleation, growth, and propagation in SEs, and various strategies that aim to alleviate and even inhibit Li dendrite formation have been proposed. Nevertheless, most of these conventional strategies require either additional material processing steps or new materials/layers that eventually increase battery cost and complexity. In contrast, using external fields, such as mechanical force, temperature physical field, electric field, pulse current, and even magnetic field to regulate Li dendrites penetration through SEs, seems to be one of the most cost-effective strategies. This review focuses on the current research progress of utilizing external physical fields in regulating Li dendrites growth in SSLBs. For this purpose, the mechanical properties of Li and SEs, as well as the experimental results that visually track Li penetration dynamics, are reviewed. Finally, the review ends with remaining open questions in future studies of Li dendrites growth and penetration in SEs. It is hoped this review can shed some light on understanding the complex Li dendrite issues in SSLBs and potentially guide their rational design for further development. KW - Li dendrites KW - Li dendrites penetration mechanisms KW - Solid electrolytes KW - Solid-state batteries PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-588331 DO - https://doi.org/10.1002/aesr.202300165 SN - 2699-9412 SP - 1 EP - 44 PB - Wiley-VCH CY - Weinheim AN - OPUS4-58833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Müller, Bernd R. A1 - Kupsch, Andreas A1 - Evsevleev, Sergei A1 - Arlt, T. A1 - Ulbricht, Alexander A1 - Dayani, Shahabeddin A1 - Bruno, Giovanni T1 - A Review of X-Ray Imaging at the BAMline (BESSY II) N2 - The hard X-ray beamline BAMline at BESSY II (Berlin, Germany) has now been in service for 20 years. Several improvements have been implemented in this time, and this review provides an overview of the imaging methods available at the BAMline. Besides classic full-field synchrotron X-ray computed tomography (SXCT), also absorption edge CT, synchrotron X-ray refraction radiography (SXRR), and synchrotron X-ray refraction tomography (SXRCT) are used for imaging. Moreover, virtually any of those techniques are currently coupled in situ or operando with ancillary equipment such as load rigs, furnaces, or potentiostats. Each of the available techniques is explained and both the current and the potential usage are described with corresponding examples. The potential use is manifold, the examples cover organic materials, composite materials, energy-related materials, biological samples, and materials related to additive manufacturing. The article includes published examples as well as some unpublished applications. KW - Material science KW - Radiography KW - Refraction KW - Tomography KW - X-ray imaging PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-572417 DO - https://doi.org/10.1002/adem.202201034 SN - 1438-1656 SP - 1 EP - 22 PB - Wiley VHC-Verlag AN - OPUS4-57241 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Campos de Oliveira, Paula A1 - Markötter, Henning A1 - Zhang, Wen A1 - Eddah, Mustapha A1 - Widjaja, Martinus Putra A1 - Remacha, Clément A1 - Bruno, Giovanni T1 - Enhanced image segmentation of refractories using synchrotron X-ray computed tomography and machine learning techniques N2 - The microstructure of refractory materials is complex, featuring a variety of mineral phases, agglomerates, defects, and controlled porosity. The behavior of refractories at high temperatures adds another layer of complexity, as phase transitions and particle rearrangements can strongly affect their properties. To analyze such intricate microstructure, advanced imaging techniques such as Synchrotron X-ray Computed Tomography (SXCT) allow detailed 3D visualization and quantification of features up to 1 μm. However, the intricacy of these microstructures makes phase identification (known as image segmentation) in digital images a challenging process. X-ray images often contain noise and image artifacts, making the analysis more difficult. Therefore, this work describes image segmentation and artifact reduction methods to characterize refractories using X-ray imaging. We studied refractory ceramics used in the aerospace industry, primarily composed of fused silica. For image segmentation, the traditional approach of greyscale thresholding was compared with machine learning. Greyscale thresholding relies on predefined algorithms to assign phases based on intensity values. In contrast, machine learning extracts patterns from large datasets, enabling more adaptive and accurate segmentation. By combining high-resolution SXCT and machine learning analysis algorithms, we successfully segmented previously uncharacterized 3D microstructural key features of refractories, including agglomerates, grain boundaries, pore size distribution and interconnectivity. Compared to traditional methods, the machine learning-enhanced segmentation presented a more accurate quantification of porosity and defects. The integration of advanced imaging techniques with machine learning segmentation significantly improves the characterization of refractory materials, providing a more precise understanding of the relationship between microstructure and material performance, supporting the development of innovative industrial solutions. T2 - The 19th Biennial International Technical Conference on Refractories (UNITECR 2025) CY - Cancún, Mexiko DA - 27.10.2025 KW - Synchrotron X-ray Tomography KW - Machine learning KW - Image segmentation KW - Ceramics KW - Refractories PY - 2025 SP - 478 EP - 481 AN - OPUS4-64803 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pohl, P. A1 - Kümmel, F. A1 - Schunk, C. A1 - Serrano-Munoz, Itziar A1 - Markötter, Henning A1 - Göken, M. A1 - Höppel, H. W. T1 - About the Role of Interfaces on the Fatigue Crack Propagation in Laminated Metallic Composites N2 - The influence of gradients in hardness and elastic properties at interfaces of dissimilar materials in laminated metallic composites (LMCs) on fatigue crack propagation is investigated experimentally for three different LMC systems: Al/Al-LMCs with dissimilar yield stress and Al/Steel-LMCs as well as Al/Ti/Steel-LMCs with dissimilar yield stress and Young’s modulus, respectively. The damage tolerant fatigue behavior in Al/Al-LMCs with an alternating layer structure is enhanced significantly compared to constituent monolithic materials. The prevalent toughening mechanisms at the interfaces are identified by microscopical methods and synchrotron X-ray computed tomography. For the soft/hard transition, crack deflection mechanisms at the vicinity of the interface are observed, whereas crack bifurcation mechanisms can be seen for the hard/soft transition. The crack propagation in Al/Steel-LMCs was studied conducting in-situ scanning electron microscope (SEM) experiments in the respective low cycle fatigue (LCF) and high cycle fatigue (HCF) regimes of the laminate. The enhanced resistance against crack propagation in the LCF regime is attributed to the prevalent stress redistribution, crack deflection, and crack bridging mechanisms. The fatigue properties of different Al/Ti/Steel-LMC systems show the potential of LMCs in terms of an appropriate selection of constituents in combination with an optimized architecture. The results are also discussed under the aspect of tailored lightweight applications subjected to cyclic loading. KW - Laminated metallic composites KW - Toughening mechanisms KW - Interfaces KW - Fatigue crack propagation KW - Fatigue crack growth PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-526531 DO - https://doi.org/10.3390/ma14102564 VL - 14 IS - 10 SP - 2564 PB - MDPI AN - OPUS4-52653 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Silveira, A. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Longo, E. A1 - Greving, I. A1 - Lasch, P. A1 - Shahar, R A1 - Zaslansky, P. T1 - Water flow through bone: Neutron tomography reveals differences in water permeability between osteocytic and anosteocytic bone material N2 - Vertebrate bones are made of a nanocomposite consisting of water, mineral and organics. Water helps bone material withstand mechanical stress and participates in sensation of external loads. Water diffusion across vertebrae of medaka (bone material lacking osteocytes) and zebrafish (bone material containing osteocytes) was compared using neutron tomography. Samples were measured both wet and following immersion in deuterated-water (D2O). By quantifying H+ exchange and mutual alignment with X-ray lCT scans, the amount of water expelled from complete vertebra was determined. The findings revealed that anosteocytic bone material is almost twice as amenable to D2O diffusion and H2O exchange, and that unexpectedly, far more water is retained in osteocytic zebrafish bone. Diffusion in osteocytic bones (only 33 % – 39 % water expelled) is therefore restricted as compared to anosteocytic bone (~ 60 % of water expelled), presumably because water flow is confined to the lacunar-canalicular network (LCN) open-pore system. Histology and Raman spectroscopy showed that anosteocytic bone contains less proteoglycans than osteocytic bone. These findings identify a previously unknown functional difference between the two bone materials. Therefore, this study proposes that osteocytic bone retains water, aided by non-collagenous proteins, which contribute to its poroelastic mechano-transduction of water flow confined inside the LCN porosity. KW - Bone porosity KW - Anosteocytic bone KW - Water permeability KW - Neutron tomography KW - Proteoglycans PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564563 DO - https://doi.org/10.1016/j.matdes.2022.111275 VL - 224 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-56456 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, Z. A1 - Dong, K. A1 - Mazzio, K. A. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Heinemann, T. A1 - Manke, I. A1 - Adelhelm, P. T1 - Phase transformation and microstructural evolution of CuS electrodes in solid-state batteries probed by in situ 3D X-ray tomography N2 - Copper sulfide shows some unique physico-chemical properties that make it appealing as a cathode active material (CAM) for solid-state batteries (SSBs). The most peculiar feature of the electrode reaction is the reversible formation of μm-sized Cu crystals during cycling, despite its large theoretical volume change (75%). Here, the dynamic microstructural evolution of CuS cathodes in SSBs is studied using in situ synchrotron X-ray tomography. The formation of μm-sized Cu within the CAM particles can be clearly followed. This process is accompanied by crack formation that can be prevented by increasing the stack pressure from 26 to 40 MPa. Both the Cu inclusions and cracks show a preferential orientation perpendicular to the cell stack pressure, which can be a result of a z-oriented expansion of the CAM particles during lithiation. In addition, cycling leads to a z-oriented reversible displacement of the cathode pellet, which is linked to the plating/stripping of the Li counter electrode. The pronounced structural changes cause pressure changes of up to 6 MPa within the cell, as determined by operando stack pressure measurements. Reasons for the reversibility of the electrode reaction are discussed and are attributed to the favorable combination of soft materials. KW - Copper sulfide KW - Crack evolution KW - Digital volume correlation KW - Phase transformation KW - Solid-state batteries PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-564577 DO - https://doi.org/10.1002/aenm.202203143 IS - 2203143 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-56457 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Van Tran, K. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Abou-Ras, D. A1 - Puplampu, S. A1 - Förster, C. A1 - Penumadu, D. A1 - Dahlberg, C. F. O. A1 - Banhart, J. A1 - Manke, I. T1 - Torsion of a rectangular bar: Complex phase distribution in 304L steel revealed by neutron tomography N2 - Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale. KW - Neutron tomography KW - Phase distribution KW - Rectangular cross-section KW - Torsion KW - Geometrical effect PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-561649 DO - https://doi.org/10.1016/j.matdes.2022.111037 SN - 0264-1275 VL - 222 SP - 111037 PB - Elsevier Ltd. AN - OPUS4-56164 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tran, K. V. A1 - Woracek, R. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Abou-Ras, D. A1 - Puplampu, S. A1 - Förster, C. A1 - Penumadu, D. A1 - Dahlberg, C. F. O. A1 - Banhart, J. A1 - Manke, I. T1 - Torsion of a rectangular bar: Complex phase distribution in 304L steel revealed by neutron tomography N2 - Metastable austenitic stainless steel (304L) samples with a rectangular cross-section were plastically deformed in torsion during which they experienced multiaxial stresses that led to a complex martensitic phase distribution owing to the transformation induced plasticity effect. A three-dimensional characterization of the phase distributions in these cm-sized samples was carried out by wavelength-selective neutron tomography. It was found that quantitatively correct results are obtained as long as the samples do not exhibit any considerable preferential grain orientation. Optical microscopy, electron backscatter diffraction, and finite element modeling were used to verify and explain the results obtained by neutron tomography. Altogether, neutron tomography was shown to extend the range of microstructure characterization methods towards the meso- and macroscale. KW - Neutron tomography KW - Phase distribution KW - Rectangular cross-section KW - Torsion KW - Geometrical effect PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-569101 DO - https://doi.org/10.1016/j.matdes.2022.111037 VL - 222 SP - 1 EP - 13 PB - Elsevier Ltd. AN - OPUS4-56910 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pacheco, V. A1 - Marattukalam, J. J. A1 - Karlsson, D. A1 - Dessieux, L. A1 - Tran, K. V. A1 - Beran, P. A1 - Manke, I. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Sahlberg, M. A1 - Woracek, R. T1 - On the relationship between laser scan strategy, texture variations and hidden nucleation sites for failure in laser powder-bed fusion N2 - While laser powder-bed fusion has overcome some of the design constraints of conventional manufacturing methods, it requires careful selection of process parameters and scan strategies to obtain favorable properties. Here we show that even simple scan strategies, complex ones being inevitable when printing intricate designs, can inadvertently produce local alterations of the microstructure and preferential grain orientation over small areas – which easily remain unnoticed across the macroscale. We describe how a combined usage of neutron imaging and electron backscatter diffraction can reveal these localized variations and explain their origin within cm-sized parts. We explain the observed contrast variations by linking the neutron images to simulated data, pole figures and EBSD, providing an invaluable reference for future studies and showing that presumably minor changes of the scan strategy can have detrimental effects on the mechanical properties. In-situ tensile tests reveal that fracture occurs in a region that was re-melted during the building process. KW - Laser powder-bed fusion KW - Texture KW - Preferential orientation KW - Diffraction contrast neutron imaging KW - Bragg-edge PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-568054 DO - https://doi.org/10.1016/j.mtla.2022.101614 VL - 26 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-56805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bouabadi, Bouchra A1 - Hilger, André A1 - Kamm, Paul H. A1 - Neu, Tillmann R. A1 - Kardjilov, Nikolay A1 - Sintschuk, Michael A1 - Markötter, Henning A1 - Schedel‐Niedrig, Thomas A1 - Abou‐Ras, Daniel A1 - García‐Moreno, Francisco A1 - Risse, Sebastian T1 - Morphological Evolution of Sn‐Metal‐Based Anodes for Lithium‐Ion Batteries Using Operando X‐Ray Imaging N2 - Sn‐based electrodes are promising candidates for next‐generation lithium‐ion batteries. However, it suffers from deleterious micro‐structural deformation as it undergoes drastic volume changes upon lithium insertion and extraction. Progress in designing these materials is limited to complex structures. There is a significant need to develop an alloy‐based anode that can be industrially manufactured and offers high reversible capacity. This necessitates a profound understanding of the interplay between structural changes and electrochemical performance. Here, operando X‐ray imaging is used to correlate the morphological evolution to electrochemical performance in foil and foam systems. The 3D Sn‐foam‐like structure electrode is fabricated in‐house as a practical approach to accommodate the volume expansion and alleviate the mechanical stress experienced upon alloying/dealloying. Results show that generating pores in Sn electrodes can help manage the volume expansion and mitigate the severe mechanical stress in thick electrodes during alloying/dealloying processes. The foam electrode demonstrates superior electrochemical performance compared to non‐porous Sn foil with an equivalent absolute capacity. This work advances the understanding of the real‐time morphological evolution of Sn bulky electrodes. KW - Synchrotron radiation KW - X-ray imaging KW - Lithium-ion battery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-640112 DO - https://doi.org/10.1002/advs.202414892 SN - 2198-3844 VL - 12 IS - 10 SP - 1 EP - 10 PB - Wiley AN - OPUS4-64011 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 - Mouiya, Mossaab A1 - Markötter, Henning A1 - Huger, Marc A1 - Bruno, Giovanni A1 - Schmidt, Volker T1 - Statistical analysis of grains and pores within polycrystalline Al2TiO5 ceramics, based on X-ray computed tomography N2 - Advanced statistical image analysis workflows were developed to segment and quantitatively evaluate 2D electron-backscatter diffraction (EBSD) maps and 3D synchrotron X-ray computed tomography (SXCT) volumes of a polycrystalline Al2TiO5 refractory composite that contains microcracks and pores. Several size, shape, and further geometric descriptors were determined for both the solid phase (Al2TiO5 grains) and the pore space. The resulting pore-size distribution is distinctly bimodal: coarse pores (tens to hundreds of micrometers), traced to incomplete powder compaction, coexist with fine pores generated during sintering. The two pore populations appear to be correlated with grain growth and crystallographic orientation in different ways. Finally, the descriptors obtained from the 2D EBSD and 3D SXCT data sets are internally consistent but complementary, highlighting the value of characterizations based on EBSD and SXCT in the microstructural study of refractory ceramics. KW - Synchrotron X-ray computed tomography KW - Electron-backscatter diffraction KW - Aluminum titanate KW - Morphological reconstruction KW - Image Segmentation KW - Statistical image analysis PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-643918 DO - https://doi.org/10.1016/j.matchar.2025.115602 SN - 1044-5803 VL - 229 SP - 1 EP - 13 PB - Elsevier Inc. AN - OPUS4-64391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bruson, Danilo A1 - Serrano-Munoz, Itziar A1 - Fritsch, Tobias A1 - Markötter, Henning A1 - Galati, Manuela T1 - Revealing the (positive) role of porosity within polymeric additively manufactured lattices via X-ray computed tomography N2 - The mechanical properties of lattice geometries are known to be significantly influenced by a variety of manufacturing defects. This study investigates the influence of porosity on the mechanical behaviour of strut-based body-centred cubic (BCC) lattice structures produced with powder bed fusion with laser beam PBF-LB/P using PA2200 nylon powder. The study combines advanced techniques, including in-situ laboratory X-ray computed tomography (XCT), synchrotron XCT to visualise pores and roughness in high resolution at a single-cell level and image-based finite element analysis (FEA). The findings show that failure in thin-walled AM lattices is governed by the combined effects of porosity morphology, location, surface roughness, and cross-section reduction. The presence of internal porosity is found to attenuate both the amplitude of elastic modulus fluctuations and the severity of stress concentrations induced by surface irregularities. KW - Nylon Pa2200 KW - Laser powder bed fusion (PBF-LB) KW - Processing defects KW - Synchrotron X-ray computed tomography (XCT) KW - Digital volume correlation (DVC) KW - Image-based finite element simulations PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-633245 DO - https://doi.org/10.1016/j.ijsolstr.2025.113488 SN - 0020-7683 VL - 320 SP - 1 EP - 16 PB - Elsevier B.V. AN - OPUS4-63324 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pfaff, Jonas A1 - Schopferer, Sebastian A1 - Markötter, Henning A1 - Rack, Alexander A1 - Bruno, Giovanni A1 - Schmidt, Anita A1 - Tichter, Tim A1 - Böttcher, Nils T1 - High-speed synchrotron radiography of nail penetration-induced thermal runaway: Understanding the explosive behavior of commercial sodium-ion batteries with NFM cathode N2 - The dynamics of mechanically initiated thermal runaway (TR) events in cylindrical 18650 cells with NFM (Na(Ni1/3Fe1/3Mn1/3)O2), LFP (LiFePO4), and NMC532 (LiNi1/2Mn1/3Co1/5O2) cathode chemistries were investigated using high-speed synchrotron X-ray imaging. Structural similarity index measures (SSIM) were employed to identify and track rapid structural changes. In this manner, thermal decompositions and internal propagation dynamics, influencing the safety mechanisms of the cells, were studied. This lead to two major findings: (I) Among NFM, LFP, and NMC532 cells, the TR-characteristics differ significantly in temperature and internal propagation speed. Internal safety mechanisms appear, however, visually similar. Among all samples, LFP cells exhibit higher safety performance concerning the initiation of TR by nail penetration and the progression of TR. (II) The NFM cells used in this study displayed an almost explosive TR. This finding appears counterintuitive on a first glance, since sodium-ion batteries are usually considered safe. High-speed imaging revealed that the explosive TR is not necessarily caused by the thermochemical decomposition reactions, but rather by a failure of the venting mechanism. This results in a significant pressure buildup within the cell upon TR initiation and eventually a severely violent TR. These results underline that battery safety depends on many factors and not solely on optimized cell chemistries or materials. KW - High-speed X-ray radiography KW - Synchrotron X-rays KW - 18650 KW - SIB KW - Na-NFM KW - Structure similarity index measure PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-642649 DO - https://doi.org/10.1016/j.powera.2025.100188 SN - 2666-2485 VL - 36 SP - 1 EP - 7 PB - Elsevier Ltd. AN - OPUS4-64264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Markötter, Henning A1 - Dayani, Shahabeddin T1 - Tomographic Imaging of Battery Materials at BAMline (Bessy II) N2 - Different scientific questions in battery research can be addressed by synchrotron X-Ray imaging. The BAMline at the 3rd generation synchrotron X-ray source BESSY II has been supporting researchers in a wide range of research areas for over 20 years. Being a non-destructive characterization method, synchrotron X-ray imaging, in particular tomography (SXCT), plays a particularly important role in structural characterization. This poster gives few examples from battery research conducted at BAMline. As a non-destructive characterization method, synchrotron X-ray imaging, especially tomography with hard X-Rays, plays an important role in structural 3D characterization. The upgraded dual multilayer monochromator offers flexibility by providing different energy spectra to optimize flux and energy resolution as desired. The upgraded detector (in white beam configuration, equipped with an sCMOS camera) allows the higher flux to be exploited with reduced readout times. Shorter tomographic acquisition times in the range of seconds are now possible. Hence, in-situ and operando examinations are routinely available. An integrated slip ring allows continuous rotation of the sample stage for ease of wiring. The pink beam option allows tomographic observation of processes occurring in the time domain of a few seconds with a resolution down to ~ 1 µm. The in-situ capabilities include electrochemical cycling, mechanical load (tension and compression) and heating up to 1100°C. Ergebnisse The method, equipment, data handling pipeline as well as various examples from battery research conducted at BAMline are presented and discussed. In particular, the 3D morphology and distribution of deposited Li within the widely used Celgard® 2325 polyolefin separator are visualized in situ, thus promoting the understanding of the short-circuiting process of Li metal batteries. In addition, we also visualized and quantified the spatial distribution of Li depositions inside a porous carbon host to unravel the deposition behavior that can hardly be probed by surface imaging techniques. The Li electrodeposition behavior found here could help to promote the understanding and development of surface modifications related to Li anodes, separators as well as novel 3D geometry electrode designs for accommodation of Li depositions and alleviation of volumetric changes. T2 - Batterieforum Deutschland CY - Berlin, Germany DA - 18.01.2023 KW - BAMline KW - X-ray tomography KW - Li-ion battery PY - 2023 AN - OPUS4-56909 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Jaenisch, Gerd-Rüdiger A1 - Kardjilov, N. A1 - Tötzke, C. A1 - Markötter, Henning A1 - Hilger, A. A1 - Manke, I. T1 - X-ray compton line scan tomography N2 - The potentials of incoherent X-ray scattering (Compton) computed tomography (CT) are investigated. The imaging of materials of very different atomic number or density at once is generally a perpetual challenge for X-ray tomography or radiography. In a basic laboratory set-up for simultaneous perpendicular Compton scattering and direct beam attenuation tomography are conducted by single channel photon counting line scans. This results in asymmetric distortions of the projection profiles of the scattering CT data set. In a first approach, corrections of Compton scattering data by taking advantage of rotational symmetry yield tomograms without major geometric artefacts. A cylindrical sample composed of PE, PA, PVC, glass and wood demonstrates similar Compton contrast for all the substances, while the conventional absorption tomogram only reveals the two high order materials. Comparison to neutron tomography reveals astonishing similarities except for the glass component (without hydrogen). Therefore, Compton CT offers the potential to replace neutron tomography, which requires much more efforts. KW - X-ray compton scattering KW - Computed tomography KW - Neutron tomography PY - 2015 DO - https://doi.org/10.3139/120.110799 SN - 0025-5300 VL - 57 IS - 11-12 SP - 985 EP - 991 PB - Hanser CY - München AN - OPUS4-34963 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markötter, Henning A1 - Manke, I. A1 - Krüger, P. A1 - Arlt, Tobias A1 - Huassmann, J. A1 - Klages, M. A1 - Riesemeier, Heinrich A1 - Hartnig, C. A1 - Scholta, J. A1 - Banhart, J. T1 - Investigation of 3D water transport paths in gas diffusion layers by combined in-situ synchrotron X-ray radiography and tomography N2 - The three-dimensional water distribution and water transport paths in the gas diffusion layer (GDL) and the adjacent micro-porous layer (MPL) of a polymer electrolyte membrane fuel cell (PEMFC) were analyzed during cell operation. The technique of quasi in-situ X-ray tomography was used for a 3D visualization of the water distribution and the structure of the GDL at different operating conditions. Based on findings from in-situ radiographic measurements water transport paths were detected and subsequently examined by tomography. The combination of these 2D and 3D techniques allows for a fully three-dimensionally resolved visualization of transport paths through the GDL. KW - Polymer electrolyte membrane fuel cell (PEMFC) KW - Radiography KW - Tomography KW - Synchrotron X-ray imaging KW - Gas diffusion layer (GDL) KW - Water transport paths PY - 2011 DO - https://doi.org/10.1016/j.elecom.2011.06.023 SN - 1388-2481 VL - 13 IS - 9 SP - 1001 EP - 1004 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-25244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Arlt, Tobias A1 - Manke, I. A1 - Wippermann, K. A1 - Tötzke, C. A1 - Markötter, Henning A1 - Riesemeier, Heinrich A1 - Mergel, J. A1 - Banhart, J. T1 - Investigation of the three-dimensional ruthenium distribution in fresh and aged membrane electrode assemblies with synchrotron X-ray absorption edge tomography N2 - Synchrotron X-ray absorption edge imaging was used to investigate the ruthenium distribution in both fresh and aged Pt/Ru-based membrane electrode assemblies (MEA) of direct methanol fuel cells. MEAs aged in different ways were analyzed: artificially aged by MeOH depletion and aged for 1700 h in an operating fuel cell stack. An element sensitive tomographic technique – differential X-ray absorption edge tomography – was applied allowing for a 3D-visualization of the ruthenium distribution within the MEA. We found a markedly changed Ru distribution after aging which is correlated to the GDL structure, the flow field geometry, and CO2 transport in the methanol solution. KW - Edge tomography KW - Ruthenium distribution KW - Direct methanol fuel cells KW - Synchrotron X-ray KW - PtRu corrosion PY - 2011 DO - https://doi.org/10.1016/j.elecom.2011.05.013 SN - 1388-2481 VL - 13 IS - 8 SP - 826 EP - 829 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-25243 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tötzke, C. A1 - Gaiselmann, G. A1 - Osenberg, M. A1 - Bohner, J. A1 - Arlt, Tobias A1 - Markötter, Henning A1 - Hilger, A. A1 - Wieder, F. A1 - Kupsch, Andreas A1 - Müller, Bernd R. A1 - Hentschel, Manfred P. A1 - Banhart, J. A1 - Schmidt, V. A1 - Lehnert, W. A1 - Manke, I. T1 - Three-dimensional study of compressed gas diffusion layers using synchrotron X-ray imaging N2 - We present a synchrotron X-ray tomographic study on the morphology of carbon fiber-based gas diffusion layer (GDL) material under compression. A dedicated compression device is used to provide well-defined compression conditions. A flat compression punch is employed to study the fiber geometry at different degrees of compression. Transport relevant geometrical parameters such as porosity, pore size and tortuosity distributions are calculated. The geometric properties notably change upon compression which has direct impact on transport conditions for gas and fluid flow. The availability of broad 3D paths, which are most important for the transport of liquid water from the catalyst layer through the GDL, is markedly reduced after compression. In a second experiment, we study the influence of the channel-land-pattern of the flow-field on shape and microstructure of the GDL. A flow-field compression punch is employed to reproduce the inhomogeneous compression conditions found during fuel cell assembly. While homogenously compressed underneath the land the GDL is much less and inhomogeneously compressed under the channel. The GDL material extends far into the channel volume where it can considerably influence gas and fluid flow. Loose fiber endings penetrate deeply into the channel and form obstacles for the discharge of liquid water droplets. KW - Synchrotron X-ray tomography KW - Gas diffusion layer (GDL) KW - Microstructure KW - Water transport path KW - Pore size analysis KW - Geometrical tortuosity PY - 2014 DO - https://doi.org/10.1016/j.jpowsour.2013.12.062 SN - 0378-7753 VL - 253 SP - 123 EP - 131 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-29979 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eddah, Mustapha A1 - Markötter, Henning A1 - Mieller, Björn A1 - Sintschuk, Michael A1 - Beckmann, Jörg A1 - Bruno, Giovanni T1 - Mitigation of DMM-induced stripe patterns in synchrotron X-ray radiography through dynamic tilting N2 - In synchrotron X-ray radiography, achieving high image resolution and an optimal signal-to-noise ratio (SNR) is crucial for the subsequent accurate image analysis. Traditional methods often struggle to balance these two parameters, especially in situ applications where rapid data acquisition is essential to capture specific dynamic processes. For quantitative image data analysis, using monochromatic X-rays is essential. A double multilayer monochromator (DMM) is successfully used for this aim at the BAMline, BESSY II (Helmholtz Zentrum Berlin, Germany). However, such DMMs are prone to producing an unstable horizontal stripe pattern. Such an unstable pattern renders proper signal normalization difficult and thereby causes a reduction of the SNR. We introduce a novel approach to enhance SNR while preserving resolution: dynamic tilting of the DMM. By adjusting the orientation of the DMM during the acquisition of radiographic projections, we optimize the X-ray imaging quality, thereby enhancing the SNR. The corresponding shift of the projection during this movement is corrected in post-processing. The latter correction allows a good resolution to be preserved. This dynamic tilting technique enables the homogenization of the beam profile and thereby effectively reduces noise while maintaining high resolution. We demonstrate that data captured using this proposed technique can be seamlessly integrated into the existing radiographic data workflow, as it does not need hardware modifications to classical X-ray imaging beamline setups. This facilitates further image analysis and processing using established methods. KW - Double multilayer monochromators KW - Synchrotron X-ray imaging KW - Signal normalization KW - BAMline KW - Dynamic tilting PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-615049 DO - https://doi.org/10.1107/S1600577524008646 SN - 1600-5775 VL - 31 SP - 1551 EP - 1560 PB - International Union of Crystallography (IUCr) AN - OPUS4-61504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -