TY - JOUR A1 - Hilger, A. A1 - Kardjilov, N. A1 - Lange, A. A1 - Kupsch, Andreas A1 - Hentschel, M. P. A1 - Manke, I. T1 - Neutron darkfield imaging of fiber composites N2 - While X-ray based darkfield imaging with grating interferometers is already widely used, darkfield imaging with neutrons has still a relatively small user community focused mostly on magnetic materials. Here, we demonstrate the application of neutron darkfield imaging byTalbot-Lau type grating interferometry to fiber reinforced plastics. Common carbon and glass fiber composites have been investigated including characteristic damage structures. The darkfield images show a strong signal response caused by fiber delamination, suitable fiber direction, particles, pores and cracks. The basic principles of neutron darkfield imaging applied to fiber composites are highlighted. KW - Neutron radiography KW - Darkfield imaging KW - Talbot-Lau interferometer KW - Fiber composites KW - Non-destructive testing PY - 2021 DO - https://doi.org/10.1515/mt-2020-0103 SN - 2195-8572 SN - 0025-5300 VL - 63 IS - 7 SP - 623 EP - 629 PB - De Gruyter CY - Berlin AN - OPUS4-53077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lu, J. A1 - Zhang, S. A1 - Yao, J. A1 - Guo, Z. A1 - Osenberg, M. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Manke, I. A1 - Zhang, X. A1 - Sun, F. A1 - Cui, G. T1 - Synergistic Effect of CO2 in Accelerating the Galvanic Corrosion of Lithium/Sodium Anodes in Alkali Metal−Carbon Dioxide Batteries N2 - Rechargeable alkali metal−CO2 batteries, which combine high theoretical energy density and environmentally friendly CO2 fixation ability, have attracted worldwide attention. Unfortunately, their electrochemical performances are usually inferior for practical applications. Aiming to reveal the underlying causes, a combinatorial usage of advanced nondestructive and postmortem characterization tools is used to intensively study the failure mechanisms of Li/Na−CO2 batteries. It is found that a porous interphase layer is formed between the separator and the Li/Na anode during the overvoltage rising and battery performance decaying process. A series of control experiments are designed to identify the underlying mechanisms dictating the observed morphological evolution of Li/Na anodes, and it is found that the CO2 synergist facilitates Li/Na chemical corrosion, the process of which is further promoted by the unwanted galvanic corrosion and the electrochemical cycling conditions. A detailed compositional analysis reveals that the as-formed interphase layers under different conditions are similar in species, with the main differences being their inconsistent quantity. Theoretical calculation results not only suggest an inherent intermolecular affinity between the CO2 and the electrolyte solvent but also provide the most thermodynamically favored CO2 reaction pathways. Based on these results, important implications for the further development of rechargeable alkali metal−CO2 batteries are discussed. The current discoveries not only fundamentally enrich our knowledge of the failure mechanisms of rechargeable alkali metal−CO2 batteries but also provide mechanistic directions for protecting metal anodes to build high-reversible alkali metal−CO2 batteries. KW - Alkali metal batteries KW - Synchrotron X-ray computed tomography KW - Lithium/sodium−carbon dioxide batteries KW - Battery failure mechanisms KW - Alkali metal anodes PY - 2024 DO - https://doi.org/10.1021/acsnano.4c02329 SP - 1 EP - 16 AN - OPUS4-59922 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zhang, X. A1 - Zhang, S. A1 - Lu, J. A1 - Tang, F. A1 - Dong, K. A1 - Yu, Z. A1 - Hilger, A. A1 - Osenberg, M. A1 - Markötter, Henning A1 - Wilde, F. A1 - Zhang, S. A1 - Zhao, J. A1 - Xu, G. A1 - Manke, I. A1 - Sun, F. A1 - Cui, G. T1 - Unveiling the Electro-Chemo-Mechanical Failure Mechanism of Sodium Metal Anodes in Sodium–Oxygen Batteries by Synchrotron X-Ray Computed Tomography N2 - Rechargeable sodium–oxygen batteries (NaOBs) are receiving extensive research interests because of their advantages such as ultrahigh energy density and cost efficiency. However, the severe failure of Na metal anodes has impeded the commercial development of NaOBs. Herein, combining in situ synchrotron X-ray computed tomography (SXCT) and other complementary characterizations, a novel electro-chemo-mechanical failure mechanism of sodium metal anode in NaOBs is elucidated. It is visually showcased that the Na metal anodes involve a three-stage decay evolution of a porous Na reactive interphase layer (NRIL): from the initially dot-shaped voids evolved into the spindle-shaped voids and the eventually-developed ruptured cracks. The initiation of this three-stage evolution begins with chemical-resting and is exacerbated by further electrochemical cycling. From corrosion science and fracture mechanics, theoretical simulations suggest that the evolution of porous NRIL is driven by the concentrated stress at crack tips. The findings illustrate the importance of preventing electro-chemo-mechanical degradation of Na anodes in practically rechargeable NaOBs. KW - Synchrotron radiation KW - X-ray imaging KW - NaO-battery PY - 2024 DO - https://doi.org/10.1002/adfm.202402253 SN - 1616-301X SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-59820 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, R. A1 - Boenke, T. A1 - Dörfler, S. A1 - Abendroth, T. A1 - Härtel, P. A1 - Althues, H. A1 - Kaskel, S. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Sintschuk, Michael A1 - Hilger, A. A1 - Manke, I. A1 - Risse, S. T1 - Multimodal Operando Analysis of Lithium Sulfur Multilayer Pouch Cells: An In-Depth Investigation on Cell Component Design and Performance N2 - This study presents an innovative operando analysis of lithium-sulfur (Li/S) multilayer pouch cells, employing a combination of lab-source and synchrotron x-ray imaging to investigate sulfur crystallite dissolution and lithium dendrite formation. By integrating advanced X-ray imaging, impedance spectroscopy, and simultaneous monitoring of temperature and pressure, the research uncovers critical insights into the behavior of active and inactive cell components. The analysis reveals significant degradation increments, primarily driven by side product accumulation and the deterioration of lithium microstructures, which contribute to performance loss over cycling. Additionally, temperature distribution analysis shows a strong correlation between joule heating, polarization resistance, and the observed endothermic processes during crystallization. These findings provide a comprehensive understanding of the mechanistic processes within industrially relevant pouch cells, highlighting opportunities for optimizing Li/S cell designs and advancing high-energy-density battery systems for commercial applications. KW - Current collector perforation KW - Impedance spectroscopy KW - Lthium sulfur batteries KW - Multilayer pouch cells KW - X-ray imaging PY - 2025 DO - https://doi.org/10.1002/aenm.202404256 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-62436 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sun, F. A1 - Wang, C. A1 - Osenberg, M. A1 - Dong, K. A1 - Zhang, S. A1 - Yang, C. A1 - Wang, Y. A1 - Hilger, A. A1 - Zhang, J. A1 - Dong, S. A1 - Markötter, Henning A1 - Manke, I. A1 - Cui, G. T1 - Clarifying the Electro-Chemo-Mechanical Coupling in Li10SnP2S12 based All-Solid-State Batteries N2 - A fundamental clarification of the electro-chemo-mechanical coupling at the solid–solid electrode|electrolyte interface in all-solid-state batteries (ASSBs) is of crucial significance but has proven challenging. Herein, (synchrotron) X-ray tomography, electrochemical impedance spectroscopy (EIS), time-of-flight secondary-ion mass spectrometry (TOF-SIMS), and finite element analysis (FEA) modeling are jointly used to decouple the electro-chemo-mechanical coupling in Li10SnP2S12-based ASSBs. Non-destructive (synchrotron) X-ray tomography results visually disclose unexpected mechanical deformation of the solid electrolyte and electrode as well as an unanticipated evolving behavior of the (electro)chemically generated interphase. The EIS and TOFSIMS probing results provide additional information that links the interphase/electrode properties to the overall battery performance. The modeling results complete the picture by providing the detailed distribution of the mechanical stress/strain and the potential/ionic flux within the electrolyte. Collectively, these results suggest that 1) the interfacial volume changes induced by the (electro)chemical reactions can trigger the mechanical deformation of the solid electrode and electrolyte; 2) the overall electrochemical process can accelerate the interfacial chemical reactions; 3) the reconfigured interfaces in turn influence the electric potential distribution as well as charge transportation within the SE. These fundamental discoveries that remain unreported until now significantly improve the understanding of the complicated electro-chemo-mechanical couplings in ASSBs. KW - All-solid-state batteries KW - Lithium metal batteries KW - Solid electrolytes KW - Sulfide solid electrolytes KW - Synchrotron X-ray tomography PY - 2022 DO - https://doi.org/10.1002/aenm.202103714 SN - 1614-6832 SP - 2103714 PB - Wiley VHC-Verlag AN - OPUS4-54431 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziesche, R.F. A1 - Hack, J. A1 - Rasha, L. A1 - Maier, M. A1 - Tan, C. A1 - Heenan, T.M.M. A1 - Markötter, Henning A1 - Kardjilov, N. A1 - Manke, I. A1 - Kockelmann, W. A1 - Brett, D.J.L. A1 - Shearing, P.R. T1 - High-speed 4D neutron computed tomography for quantifying water dynamics in polymer electrolyte fuel cells N2 - In recent years, low-temperature polymer electrolyte fuel cells have become an increasingly important pillar in a zero-carbon strategy for curbing climate change, with their potential to power multiscale stationary and mobile applications. The performance improvement is a particular focus of research and engineering roadmaps, with water management being one of the major areas of interest for development. Appropriate characterisation tools for mapping the evolution, motion and removal of water are of high importance to tackle shortcomings. This article demonstrates the development of a 4D high-speed neutron imaging technique, which enables a quantitative analysis of the local water evolution. 4D visualisation allows the time-resolved studies of droplet formation in the flow fields and water quantification in various cell parts. Performance parameters for water management are identified that offer a method of cell classification, which will, in turn, support computer modelling and the engineering of next-generation flow field designs. KW - Neutron imaging KW - Tomography KW - Polymer electrolyte membrane fuel cell PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-545978 DO - https://doi.org/10.1038/s41467-022-29313-5 VL - 13 IS - 1 SP - 1616 PB - Nature Publishing Group UK CY - London AN - OPUS4-54597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tang, F A1 - Wu, Z A1 - Yang, C A1 - Osenberg, M A1 - Hilger, A A1 - Dong, K A1 - Markötter, Henning A1 - Manke, I A1 - Sun, F A1 - Chen, L A1 - Cui, G T1 - Synchrotron X-ray tomography for rechargeable battery research: Fundamentals, setups and applications N2 - Understanding the complicated interplay of the continuously evolving electrode materials in their inherent 3D states during the battery operating condition is of great importance for advancing rechargeable battery research. In this regard, the synchrotron X-ray tomography technique, which enables non-destructive, multi-scale, and 3D imaging of a variety of electrode components before/during/after battery operation, becomes an essential tool to deepen this understanding. The past few years have witnessed an increasingly growing interest in applying this technique in battery research. Hence, it is time to not only summarize the already obtained battery-related Knowledge by using this technique, but also to present a fundamental elucidation of this technique to boost future studies in battery research. To this end, this review firstly introduces the fundamental principles and experimental Setups of the synchrotron X-ray tomography technique. After that, a user guide to ist application in battery research and examples of its applications in Research of various types of batteries are presented. The current review ends with a discussion of the future opportunities of this technique for next-generation rechargeable batteries research. It is expected that this review can enhance the reader’s understanding of the synchrotron X-ray tomography technique and stimulate new ideas and opportunities in battery research. KW - 3D imaging KW - Batteries KW - Synchrotron X-Ray KW - Tomography PY - 2021 DO - https://doi.org/10.1002/smtd.202100557 VL - 5 IS - 9 SP - 2100557 PB - Wiley-VCH AN - OPUS4-53394 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jamro, R. A1 - Mente, Tobias A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Al-Falahat, Ala'A. M. A1 - Woracek, R. A1 - Manke, I. A1 - Griesche, Axel T1 - Temperature distribution during welding measured by neutron imaging N2 - This study was carried out to investigate the neutron transmission signal as a function of sample temperature during a welding process. A theoretical description that includes the Debye-Waller factor was used to describe the temperature influence on the neutron crosssections. Neutron imaging using a monochromatic beam helps to observe transmission variations related to the material temperature. In-situ neutron imaging of welding experiments show the distribution of the temperature in bulk steel samples. The performed finite element modelling of expected temperature distributions shows good agreement with the obtained experimental data. KW - Neutron imaging KW - Debye-Waller-Faktor PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-586268 DO - https://doi.org/10.1088/1742-6596/2605/1/012026 VL - 2605 SP - 1 EP - 10 PB - IOP Publishing Ltd. AN - OPUS4-58626 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Falahat, A. A1 - Kardjilov, N. A1 - Markötter, Henning A1 - Kupsch, Andreas A1 - Woracek, R. A1 - Alrwashdeh, S. A1 - Manke, I. T1 - Investigation of detector backlighting and other effects in neutron darkfield images N2 - Neutron imaging can provide unique contrast mechanisms. In order to yield reliable and reproducible attenuation coefficients for quantification, one needs to fully understand and characterize the experimental set-up. One effect that has been largely overlooked in scintillator-camera based neutron imaging systems is the backlight scattering or back illumination in the detection system which can significantly affect the quantification of attenuation coefficients and lead to severe errors and image artifacts. Herein, backlighting is investigated by varying the illuminated detector area and the magnitude of the attenuation. The attenuation coefficient of multiple metal plates was determined by polychromatic neutrons bu the CONRAD V7 instrument. The strength of the back illumination strongly depends upon the sample absorption. While it is relatively moderate (a few percent) for weak absorbing samples, it can be severe when the sample is a strong absorber or thick. KW - Attenuation coefficient KW - Neutron imaging KW - Neutron scattering KW - Polycromatic neutrons KW - Scintillator PY - 2024 SN - 1073-9149 DO - https://doi.org/10.1080/10739149.2024.2380772 SP - 1 EP - 11 PB - Taylor & Francis AN - OPUS4-60752 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziesche, R. A1 - Robinson, J. A1 - Kok, M. A1 - Markötter, Henning A1 - Kockelmann, W. A1 - Kardjilov, N. A1 - Manke, I. A1 - Brett, D. A1 - Shearing, P. T1 - Editors’ Choice—4D Neutron and X-ray Tomography Studies of High Energy Density Primary Batteries: Part I. Dynamic Studies of LiSOCl2 during Discharge N2 - The understanding of dynamic processes in Li-metal batteries is an important consideration to enable the full capacity of cells to be utilised. These processes, however, are generally not directly observable using X-ray techniques due to the low attenuation of Li; and are challenging to visualise using neutron imaging due to the low temporal resolution of the technique. In this work, complementary X-ray and neutron imaging are combined to track the dynamics of Li within a primary Li/SOCl2 cell. The temporal challenges posed by neutron imaging are overcome using the golden ratio imaging method which enables the identification of Li diffusion in operando. This combination of techniques has enabled an improved understanding of the processes which limit rate performance in Li/SOCl2 cells and may be applied beyond this chemistry to other Li-metal cells. KW - Nneutron imaging KW - X-ray imaging KW - Tomography KW - Primary Battery PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515802 DO - https://doi.org/10.1149/1945-7111/abbbbc SN - 1945-7111 VL - 13 IS - 167 SP - 130545 PB - IOP Publishing AN - OPUS4-51580 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -