TY - CONF A1 - Mehmood, Asad T1 - Ionothermal Template Transformation as a Sustainable Route Towards Carbon Electrodes in Energy Storage and Conversion N2 - Porous carbons with tuneable functionalities and morphologies have extensively been employed as electrode materials in a variety of electrochemical energy conversion and storage systems for instance in fuel cells and electrolysers as active catalysts and catalyst supports, and in secondary batteries as anode materials. Amorphous carbons with well-developed pore structures are of particular interest due to their superior mass-transport characteristics and remarkable charge storage capacities. The salt-templating method with its advantage of combined soft and hard templating effects provides a sustainable way to synthesize nano- and mesoporous carbons with tailored porosities via in-situ ionothermal template transformation [1]. In this work, we utilized a MgCl2-based salt melt to prepare nitrogen doped carbons (N-C) with different morphologies and porosities, which were evaluated as anode materials in sodium ion batteries. Simultaneously, use of MgCl2 salt leads to the formation of Mg-N4 moieties in those carbons by means of a pyrolytic template-ion effect (active site imprinting) [2]. Porous carbon frameworks with imprinted Mg-N4 sites are interesting particularly for electrocatalysis applications as they offer an ideal platform to prepare M-N-C catalysts (where M= Co, Fe, Ni etc.) by ion-exchange reactions at low temperatures. The resultant M-N-C catalysts consist purely of M-N4 active sites and high porosity of carbon framework facilitates efficient mass-transport of reacting species. We utilized Mg-N4 imprinted carbons to synthesize morphologically equivalent Ni-N-Cs and Co-N-Cs, containing phase pure Ni-N4 and Co-N4 sites, for electrochemical reduction of carbon dioxide (CO2RR). In electrochemical tests, Ni-N-Cs exhibited an excellent CO2 reduction activity with considerably higher CO selectivity and mass activity as compared to Co-N-C. The faradic efficiency value of Ni-N-C for CO formation was 95% at U= -0.5 to -0.8 VRHE (vs reversible hydrogen electrode) and a mass activity of 23 A g-1. The performance stability test carried out at -0.65 VRHE demonstrated above 90 % retention of the current density and CO selectivity after 100 h of continuous operation, reflecting the structural robustness of the Ni-N-C catalyst. Finally, these ionothermal carbons with two different morphologies (but without any Ni or Co incorporation) were employed as the anode materials in sodium-ion batteries to evaluate the effects of carbon morphology and functionalization on sodium storage capacities. Compared to the reference carbon material, substantially higher reversible sodium storage capacities were reached with these high porosity carbons that were in the range of 300-500 mAh g-1 [3]. Although the reversible capacity was obtained only after extensive SEI formation, our results reveal the potential for much higher reversible capacities than usually observed using carbons with a tailored porosity in sodium-ion batteries. The talk will include greater details of the structural analysis and sodium storage and CO2 reduction results of these ionothermal carbons. T2 - Materials for Sustainable Development Conference (MAT-SUS) CY - Barcelona, Spain DA - 24.10.2022 KW - Porous carbons KW - Sodium ion batteries KW - Anode materials KW - Single atom catalysts KW - Electrochemical CO2 reduction PY - 2022 AN - OPUS4-61985 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Bioinspired atomically dispersed M-N-C catalysts via active-site imprinting into nitrogen doped carbons N2 - Proton-exchange membrane fuel cells are amongst the most promising energy conversion technologies today. Herein non-precious iron-coordinated nitrogen doped carbons (Fe-N-Cs) are very promising alternatives for Pt-based cathode catalysts.[1-3] The early reports on the application of such materials date back to the 1960´s when Jasinski demonstrated that - similar to natural porphyrins - N-coordinated transition metal complexes can be active sites for the ORR.[3] The preparation of these catalysts was strongly optimized over the years; still they typically remain with harsh reaction conditions that complicate the selective formation of active FeN4 sites. The employment of pyrolytic temperatures has been a dogma for the synthesis of MN4 sites, however coming with unfavorable side reactions. We recently introduced a mild procedure, which is conservative toward the carbon support and leads to active-site formation at low temperatures in a wet-chemical step, essentially decoupling the preparation of nitrogen doped carbons (NCs) from the preparation of the active sites.[4, 5] The key concept therein is the so-called active site imprinting into the NC using the less reactive template ions Mg2+ [4] or Zn2+.[5] The presentation will introduce the concept of active site imprinting with a focus on Fe-N-C electrocatalyst development and testing. The broad potential of the synthetic approach will be exemplified by recent results, including the selective synthesis of tetrapyrrolic single site catalysts, the assignment of the role of the transition metal compared to the carbon scaffold and a facile method to evaluate specific activity. T2 - GDCh Electrochemistry 2022 CY - Berlin, Germany DA - 27.09.2022 KW - Bioinspired carbon catalysts PY - 2022 AN - OPUS4-61960 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krug von Nidda, Jonas T1 - Separating Initial Loss from Storage Capacity: Core-Shell Materials as Advanced Anode Materials for Sodium Ion Batteries N2 - The current imperative to shift towards an energy grid equipped with sustainable energy storage solutions has caused a renewed interest in sodium-ion batteries (SIBs). Hard carbons (HCs) are a promising option high-capacity anode materials in SIBs. Nevertheless, their elevated capacities frequently come at the cost of experiencing substantial non-reversible initial capacity losses Commonly, significant losses are associated with irreversible reactions, such as the creation of the solid electrolyte interphase (SEI), that occur during the initial sodium insertion in HC-materials. Intriguingly, high values of irreversible capacity are often found for samples with experimentally determined low specific surface area.[1] A more comprehensive understanding of the structure-property relations is essential for quantifying and grasping the potential of hard carbon materials in sodium-ion batteries (SIBs). Thus, the objective is to employ analytical methods to establish a link between the structure and the electrochemical attributes of HC materials. This has been a challenge, partly due to the non-stoichiometric nature of the sodium storage mechanism and the disordered structure of HCs. To address the challenges mentioned above, our approach is to explore whether a core-shell structure can separate sodium storage and SEI-formation. This way, we can investigate and fine-tune storage capacity and irreversible losses, independently. The strategy involves the synthesis of various porous carbon structures to serve as the core material and their combination with sodium-conductive structures to core-shell materials. Herein, we will present different synthesis routes towards tailor-made carbon core materials. Moreover, different coatings concepts will be introduced, and the electrochemical performance of the core and core-shell materials compared. To elucidate the storage mechanism, the results of advanced analytical methods such as operando NMR and -SAXS will be presented. Generally, these core-shell anodes promise to enable high capacities accompanied with low irreversible losses due to optimized SEI-formation. T2 - Advanced Battery Power Conference 2024 CY - Münster, Germany DA - 10.04.2024 KW - Battery KW - Anode KW - Hard Carbon PY - 2024 AN - OPUS4-61968 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Effects of Acid Activation via Sol-Gel Chemistry towards Nitrogen-Doped Carbon Structure N2 - Porous carbon materials are known for their applicability in important areas such as sorption, catalysis and electrochemistry (e.g. fuel cell catalysts, supercapacitor or battery electrodes). It was shown that nitrogen doped carbons (NDCs) act as an inexpensive and highly active non-metal catalyst in the oxygen reduction reaction (ORR), with the potential to reach performances of practical need one day. A key strategy towards improvement for this aim comprises the generation of advantageous porosity, which typically means high surface area and mass transport pores as well as the control over the chemistry of catalytically active sites. My group is developing novel sol-gel type strategies that are using molten salts or molten acids as unconventional reaction medium for the porogenesis in doped carbons, thereby revisiting classic activation techniques.[1,2] Carbon materials with extra high surface area of ~2800 m2 g- 1 and pore volumes, up to four times as high as in commercial activated carbons, are obtained.[3] It turns out that the meso- and macrostructure is generated by means of phase separation rather than leaching reactions. However, chemical reactions between the carbon precursor and the melt are also involved. The salt cations Mg2+ and Zn2+ act as template ions, which results in metal coordination sites, embedded into the carbon structure.[4,5] The imprinted structure may be utilized as catalytically active site by performing ion-exchange reactions. The novel preparation strategy towards highly active electrocatalysts will be presented for Mg and Zn and further discussed for lighter elements. T2 - International Sol-Gel Conference 2022 CY - Lyon, France DA - 24.06.2022 KW - Sol-Gel-Carbonization KW - Boron-Nitrogen-Doped Carbon PY - 2022 AN - OPUS4-61958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wutthiprom, Juthaporn T1 - Sol-Gel Carbonization towards Tailor-Made Boron- and Nitrogen-doped Carbon N2 - The activation of carbon is normally proceeded in top-down or bottom-up strategies. Therein pore formation (porogenesis) occurs by reaction with steam, CO2 , KOH, or the use of acidic agents, in which chemical leaching of carbon atoms occurs. The sol-gel type synthesis of N-doped carbon in excess amounts of molten acids was presented recently, questioning the general validity of a leaching activation mechanism.[1] The protocol using inorganic salt melts (MgCl2 or ZnCl2 ) and organic precursors additionally generated N functionalities. Interestingly, it can be noticed that the imprinting cations play a crucial role towards the chemical structure of N-doped carbon framework. The coordinated geometry is wellknown from phthalocyanine, a macrocyclic Ncomplexes (MN4 -sites, where M is metal cation) which are desirable surface complexes, e.g. in electrocatalysis. The analogous phenomenon may be observed when using H3BO3 agent via sol-gel chemistry. T2 - International Sol-Gel Conference 2022 CY - Lyon, France DA - 24.06.2022 KW - Boron-Nitrogen-Doped-Carbon KW - Sol-Gel-Carbonization PY - 2022 AN - OPUS4-61959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mehmood, Asad A1 - Fellinger, Tim-Patrick T1 - Porous Carbon Supported Ni and Co Single Atom Catalysts for Electrochemical Reduction of Carbon Dioxide N2 - Non-precious metal single atom catalysts (generally labelled as M/NCs where M= Co, Fe, Ni etc.) consist of active metal centres dispersed on nitrogen doped porous carbon (NC) matrix at atomic level and exhibit promising activities e. g. for electrochemical reduction of CO2, selectively forming CO. We herein use identical Mg/NCs as platform for ion-exchange reactions towards morphologically equivalent Ni/NCs and Co/NCs. The Ni/NC catalyst shows almost double the specific activity and a Faraday efficiency of >80% at a very low overpotential of U= -0.43 V (even 95% at U= -0.5 to -0.8 V) with high stability. T2 - GDCh Electrochemistry 2022 CY - Berlin, Germany DA - 27.09.2022 KW - Electrochemical CO2 conversion KW - Single atom catalysts KW - Porous Carbons PY - 2022 AN - OPUS4-61980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon T1 - Synthesis of Atomically Dispersed Electrocatalyst by Imprinting with Different Template Ions throughout Carbonization N2 - Atomically dispersed metal-nitrogen doped carbons (M-N-C) are promising catalysts for the activation of small molecules such as O2 and CO2. These single atom catalysts (SAC) operate at the interface between homogenous and heterogenous catalysts. Currently, many examples of M-N-C are known with good oxygen reduction reaction activity but lacking a controlled synthesis of the specific active sites of the precatalyst. T2 - GDCh Electrochemistry 2022 CY - Berlin, Germany DA - 27.09.2022 KW - Elechtrochemistry KW - Oxygen reduction reaction KW - Porous carbons PY - 2022 AN - OPUS4-61982 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Appel, Paul Alexander T1 - Developing Tailor-Made Core-Shell Carbon Anode Materials for Sodium Ion Batteries N2 - The current strong interest in electromotive mobility and the need to transition to an energy grid with sustainable energy storage has led to a renewed interest in sodium ion batteries (SIBs). Hard carbons are promising candidates for high-capacity negative electrode materials in SIBs. Their high capacities, however, are often accompanied with high irreversible capacity losses during the initial cycles.[1] The goal of this project is to use analytical techniques to establish a correlation between the structure and the capacities of hard carbons. This has previously been difficult, in part because the sodium storage mechanism is not stoichiometric and due to the disordered structure of hard carbons. Large irreversible capacities associated with hard carbons are often in contradiction to the experimentally determined low surface area of the sample material.[1] A better understanding of the structure-property relationship should enable quantification and understanding of the potential of hard carbon materials for SIBs. Our approach is to explore whether a core-shell structure can separate sodium storage and solid electrolyte interphase formation so that storage capacity and irreversible losses can be investigated separately. The synthesis of a selection of porous carbon structures serving as the core material, will be attempted. Simultaneously, sodium-conducting shell structures will be developed to allow for separation of sodium ions and electrolyte molecules. Subsequently the combination of core and shell materials will be undertaken. These anodes should enable high capacities accompanied with low irreversible capacity due to optimized solid electrolyte interphase formation. T2 - ECS Gothenburg CY - Gothenburg, Sweden DA - 08.10.2023 KW - Energy Materials PY - 2023 AN - OPUS4-62003 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Appel, Paul Alexander T1 - Development of tailormade core-shell hard carbon materials as anode materials in sodium ion batteries N2 - The current strong interest in electromotive mobility and the need to transition to an energy grid with sustainable energy storage has led to a renewed interest in sodium ion batteries (SIBs). Hard carbons are promising candidates for high-capacity negative electrode materials in SIBs. Their high capacities, however, are often accompanied with high irreversible capacity losses, during the initial cycles.[1] The goal of this project is to synthesize carbon materials using different zeolite templates to obtain electrode materials that feature a defined and adjustable pore structure. A better understanding of the structure-property relationship by investigating porosity-tailored anode materials, should enable quantification and understanding of the potential of hard carbon materials for SIBs. Furthermore, a goal is to explore whether a core-shell structure can separate sodium storage and solid electrolyte interphase formation allowing the independent investigation of storage capacity and irreversible losses. T T2 - 34. Deutsche Zeolith-Tagung CY - Vienna, Austria DA - 21.02.2023 KW - Energy Materials PY - 2023 AN - OPUS4-62002 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Shu-Han T1 - Synthetic Carbon Anodes for SIBs N2 - Hard carbon (HC) is currently one of the most promising anode materials for sodium-ion batteries (SIBs). However, the Na storage mechanism remains controversial, leaving the theoretical limits carbon anodes unclear. To deconvolute the specific capacity from irreversible capacity losses resulting from the formation of solid electrolyte interphase (SEI), core-shell carbon materials with tailored pore structure and defined surface functionalities are synthesized. Meanwhile, these synthetic designer carbons could achieve more competitive capacities for use as better anodes for SIBs. T2 - Adlershofer Forschungsforum (AFF) CY - Berlin, Germany DA - 11.11.2024 KW - Na-ion Battery PY - 2024 AN - OPUS4-61998 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wu, Shu-Han T1 - Mole sieving, artificial cathode electrolyte interphase enables stable cycling of room temperature sodium sulfur cells N2 - Porous carbon particles derived from zeolitic imidazolate framework (ZIF-8) were used as a matrix to improve the electrode conductivity and buffer the volume change of sulfur (S). In addition, the porous carbon particles were coated with an additional ion-sieving tailor-made covalent organic framework (COF) shell, which can be regarded as an artificial cathode electrolyte interphase (CEI). The introduced shell can avoid polysulfides from dissolving in the ether-based electrolyte, thus, preventing the shuttling of polysulfides. The as-synthesized sulfur-infiltrated core-shell cathode delivers a reversible capacity of 975 mAh gS–1 (@C/33) and a reasonable rate capability. T2 - 5th International Sodium Battery Symposium, SBS-5 CY - Berlin, Germany DA - 23.09.2024 KW - NaS Battery PY - 2024 AN - OPUS4-61992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Appel, Paul Alexander T1 - Investigation and Development of Tailor-Made Core-Shell Hard Carbon Materials to be used as Negative Electrodes in Sodium Ion Batteries N2 - The current strong interest in electromotive mobility and the need to transition to an energy grid with sustainable energy storage has led to a renewed interest in sodium ion batteries (SIBs). Hard carbons are promising candidates for high-capacity negative electrode materials in SIBs. Their high capacities, however, are often accompanied with high irreversible capacity losses during the initial cycles.[1] The goal of this project is to use analytical techniques to establish a correlation between the structure and the capacities of hard carbons. This has previously been difficult, in part because the sodium storage mechanism is not stoichiometric and due to the disordered structure of hard carbons. Large irreversible capacities associated with hard carbons are often in contradiction to the experimentally determined low surface area of the sample material.[1] A better understanding of the structure-property relationship should enable quantification and understanding of the potential of hard carbon materials for SIBs. Our approach is to explore whether a core-shell structure can separate sodium storage and solid electrolyte interphase formation so that storage capacity and irreversible losses can be investigated separately. The synthesis of a selection of porous carbon structures serving as the core material, will be attempted. Simultaneously, sodium-conducting shell structures will be developed to allow for separation of sodium ions and electrolyte molecules. Subsequently the combination of core and shell materials will be undertaken. These anodes should enable high capacities accompanied with low irreversible capacity due to optimized solid electrolyte interphase formation. T2 - GDCH Electrochemistry 2022 CY - Berlin, Germany DA - 27.09.2022 KW - Energy Materials PY - 2022 AN - OPUS4-62001 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dietzmann, Simon T1 - X-Ray Absorption Spectroscopy to Reveal the „Molecular“ Structure of Metal and Nitrogen doped Carbon Electrocatalysts N2 - High-performance electrocatalysts and sodium-ion (Na+) storage materials for Na-ion batteries anodes are required for energy conversion and storage systems. Metal and nitrogen enriched carbons (M-N-Cs) are promising candidates as they are conductive and can be tuned to the desired properties by appropriate modification. Structural characterization is essential to understand and optimize the active sites at the pseudo-molecular level and the storage of Na+ in the anode T2 - Bessy User Meeting CY - Berlin, Germany DA - 11.12.2024 KW - Single-atom-catalyst KW - Electrochemistry KW - Porous carbons PY - 2024 AN - OPUS4-62074 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Appel, Paul Alexander A1 - Prinz, Carsten A1 - Low, Jian Liang A1 - Asres, Nahom Enkubahri A1 - Wu, Shu-Han A1 - Freytag, Annica A1 - Krug von Nidda, Jonas A1 - de Sousa Amadeu, Nader A1 - Fellinger, Tim-Patrick T1 - Kern–Schale: Versiegelung nanoporöser Partikel mit semipermeablen Kohlenstoffschichten befreit Hartkohlenstoffanoden von ihrem Dilemma N2 - In der vorliegenden Arbeit wird eine Kern-Schale-Strategie vorgestellt, die das grundlegende Problem gängiger nichtgraphitischer Hartkohlenstoff-Anoden adressiert: Hohe reversible Kapazitäten gehen bislang typischerweise mit erheblichen irreversiblen Verlusten in den ersten Zyklen einher. Analog zu Graphit, das sowohl Lithiumspeicherung als auch die Abtrennung von Elektrolytlösungsmitteln in einer homogenen Struktur vereint, zeigen wir, dass sich diese beiden Funktionen auch in nichtgraphitischen Kohlenstoffen gezielt in einer heterogenen Architektur kombinieren lassen. Hochporöse Aktivkohlen werden durch kinetisch kontrollierte Gasphasenabscheidung mit einer dünnen Schicht nichtgraphitischen Kohlenstoffs überzogen, sodass eine funktionale Kern-Schale-Struktur entsteht. Gasadsorptionsmessungen an Kern-, Schalen-, Kern-Schale- und mechanisch beschädigte Kern-Schale-Partikeln, bestätigen, dass die Porosität des Kerns erhalten bleibt und die Schale semipermeabel ist. Die Sorption von Diethylcarbonat wird als geeignetere Methode im Vergleich zu N2- oder CO2-Sorptionsmessungen eingeführt, um die irreversiblen Verluste des ersten Zyklus mit der tatsächlichen Flüssig-Fest-Grenzfläche von Kohlenstoffanoden zu verknüpfen. Die funktionalen Kern-Schale-Partikel zeigen eine stark reduzierte Aufnahme von Diethylcarbonat, was hohe reversible Kapazitäten bei deutlich geringeren Erstzyklusverlusten ermöglicht. Bei einer reversiblen Kapazität von 400 ± 24 mAh g−1 und einer initialen Coulombeffizienz von 82 ± 2% zeigt sich, dass die dreistufige Natriumspeicherung in der gezielt entwickelten Kern-Schale-Architektur den größeren Ionenradius von Natrium gegenüber Lithium (372 mAh g−1 in Graphit) kompensieren kann. Die entwickelten Kern-Schale-Anoden erreichen damit ein Leistungsniveau, das für eine kommerzielle Anwendung vielversprechend ist. KW - Kern-Schale-Struktur KW - Natriumionenbatterie KW - Hartkohlenstoffanode KW - Diethylcarbonatdampfsorption KW - Aktivkohle PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655354 DO - https://doi.org/10.1002/ange.202519457 SN - 1521-3757 N1 - Es gibt eine parallele Sprachausgabe (englisch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (English), a link is in the field related identifier SP - 1 EP - 10 PB - Wiley-VCH CY - Weinheim AN - OPUS4-65535 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Appel, Paul Alexander A1 - Prinz, Carsten A1 - Low, Jian Liang A1 - Asres, Nahom Enkubahri A1 - Wu, Shu-Han A1 - Freytag, Annica A1 - Krug von Nidda, Jonas A1 - de Sousa Amadeu, Nader A1 - Fellinger, Tim-Patrick T1 - Core‐Shell: Resolving the Dilemma of Hard Carbon Anodes by Sealing Nanoporous Particles With Semi‐Permeable Coatings N2 - A core-shell strategy is introduced to overcome the dilemma of common non-graphitic hard carbon anodes, linking high reversible storage capacity to practically unacceptable irreversible losses in the first cycle(s). Just as Graphite homogeneously combines effective lithium storage with an electrolyte solvent-sieving function, we show that both of these functions could be strategically integrated into non-graphitic carbons in a heterogeneous structure. Highly porous activated carbons are sealed by kinetically tuned gas-phase deposition of non-graphitic carbon to form a functional core-shell structure. Gas sorption porosimetry on core, shell, core–shell, and cracked core-shell particles confirms preserved core porosity and a semi-permeable shell. Diethyl carbonate sorption analysis is introduced as a more suitable probe than N2 or CO2 sorption, linking first-cycle losses to the liquid–solid interface of carbon anodes. The functional core-shell particles with much reduced diethyl carbonate uptake allow for high storage capacity and reduced first cycle losses. Delivering 400 ± 24 mAh g−1 with 82 ± 2% first-cycle reversibility, it is shown that three-stage Na storage in designed core-shell anodes can compensate for the larger size of sodium compared to lithium stored in graphite anodes (372 mAh g−1). The designed core-shell anodes show state-of-the-art performance with commercial promise. KW - Sodium-ion battery KW - Activated carbon KW - Core-shell KW - Hard carbon anode KW - Diethyl carbonate vapor sorption PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-655346 DO - https://doi.org/10.1002/anie.202519457 SN - 1433-7851 N1 - Es gibt eine parallele Sprachausgabe (deutsch), ein Link befindet sich im Feld zugehöriger Identifikator - There is a parallel language edition (German), a link is in the field related identifier SP - 1 EP - 9 PB - Wiley-VCH CY - Weinheim AN - OPUS4-65534 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pedersen, Angus T1 - Coupling Single Atom Electrocatalysts with a Bioreactor for CO2 to C2+ Conversion N2 - To alleviate CO2 emissions impact on climate change, and close the carbon cycle, converting carbon dioxide into valuable products such as multi-carbon organic chemicals is of great importance. Each approach offers distinct merits but also certain challenges in terms of process efficiency, product selectivity and implementation at scale. Developing coupled CO2 conversion systems, for instance bio-electrochemical reactors, can address some of the challenges.[1] Precious-metal free biocompatible single atoms in N-doped C (M-N-C, where M = Fe, Ni, Co) electrocatalysts, based on Mg active site imprinting of bioinspired MN4 sites,[2][3] have shown state-of-the-art activity and selectivity for conversion of CO2 to CO.[4] Pyrolysis of Mg-N-C is carried out in a salt-melt at high temperatures (≥ 800 oC) and followed by an exchange with stoichiometric amounts of Ni or Co at low temperatures. N2-sorption of the materials reveal a micro-mesoporous structure with high surface areas (> 1000 m2 g-1) and a mass-transport enabling pore system. Extended X-ray absorption fine structure reveal the existence of atomically dispersed single atom active sites with defined active site structure. These catalysts were implemented in a home-made bio-electrocatalytic system (BES) consisting of a bioreactor coupled to a CO2 electrolysis cell.[5] Here, CO2 is first electrochemically converted to CO in the electrolysis cell which is then directly fed to bacteria (Clostridium ragsdalei) in the bioreactor which further metabolize it to valuable carbon compounds, such as acetate. An acetate formation rate of 1.8 mg L-1 h-1 was achieved and an acetate concentration of 0.103 g L-1, corresponding to acetate formation rate of 0.73 mmol d-1. We have successfully demonstrated the validity of a coupled bio-electrocatalytic system operating with resource efficient single atom Co- and Ni-N-C electrocatalysts for CO2 conversion. T2 - Electrifying Organic Synthesis CY - Mülheim an der Ruhr, Germany DA - 03.09.2025 KW - Single atom KW - Electrochemical CO2 conversion KW - Bioelectrolysis PY - 2025 AN - OPUS4-64037 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mehmood, Asad T1 - ZIF-derived Atomically Dispersed Non-precious Metal Catalysts (M-N-C) for Electrochemical Energy Applications N2 - Zeolitic imidazolate frameworks (ZIFs) which are a subtype of metal organic frameworks (MOFs) have been extensively used to prepare catalyst materials for a variety of electrochemical reactions for energy conversion and storage applications. Most notable examples of ZIFs used for that purpose include ZIF-8 and ZIF-67 etc. Particularly ZIF-8 with its high surface area, defined pore structure and tunable particle size is widely utilized as a platform material to prepare so-called metal- and nitrogen-doped carbon (M-N-C) catalysts with M= Co, Fe, Ni, Zn etc., which are an emerging class of catalyst materials and consist of nitrogen-doped porous carbon matrix hosting atomically distributed active metal sites.[1, 2] The active sites in M-N-Cs ideally have M-N4 coordination resembling to metal centres in macromolecules such as porphyrins and phthalocyanines.[3] Most representative examples of M-N-Cs include Fe-N-Cs, Co-N-Cs and Ni-N-Cs etc. which are showing promising activities for a variety of electrochemical reactions e.g. oxygen reduction reaction (ORR), carbon dioxide reduction reaction (CO2RR) and hydrogen evolution reaction (HER). The structures of M-N-C catalysts are quite complex and require a fine balance between morphological, electronic, and chemical properties to reach optimal electrocatalytic activities. In this talk, I will present our activities on (i) preparation of phase-pure M-N-C catalysts derived from ZIF-8 via active-site imprinting [4, 5] and highlight the benefits of our strategy to achieve high density of active sites and enhanced electrochemical performance levels [6] and (ii) feasibility of using gas physisorption techniques as a new approach to quantify active sites in M-N-Cs. The challenges of maximizing active site utilization and eliminating unfavourable mass-transport characteristics faced by ZIF-8 derived M-N-Cs in electrochemical energy devices e.g. fuel cells will also be briefly discussed. T2 - Materials for Sustainable Development Conference (MAT-SUS) CY - Sevilla, Spain DA - 03.03.20225 KW - Electrochemical energy conversion KW - Single atom catalysts KW - Electrochemical CO2 reduction KW - Fuel cells KW - Electrolyzers PY - 2025 DO - https://doi.org/https://doi.org/10.29363/nanoge.matsusspring.2025.251 AN - OPUS4-62927 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Batteries: Basics, Challenges and Trends N2 - In this lecture the fundamental principles of batteries are briefly introduced aligned by the historical development of the technology. The introduction is continued with an overview on current challenges regarding performance, durability, sustainability, cost and safety. Lastly, research trend on approaches to tackle the challenges are discussed by selected examples. T2 - 2025 Scientific and Technological Training Course "Design and Evaluation Methods of Fire Safety Engineered Materials" CY - Hefei, China DA - 20.10.2025 KW - Fundamentals of Batteries KW - Safety KW - Active Materials KW - Research Topics PY - 2025 AN - OPUS4-64917 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Appel, Paul Alexander T1 - Connecting Porosity to Storage Capacity: Core-Shell Carbon Material As High-Capacity Negative Electrodes for Sodium Ion Batteries N2 - Due to abundant raw materials, low costs and promising high reversible specific capacities, hard carbons (HCs) are a common choice for commercially manufactured anodes in sodium-ion batteries (SIBs). Despite their potential and extensive use, the storage mechanism is still under debate. The non-stoichiometric adsorption mechanism also means that the search for an upper limit for the reversible capacity is ongoing. There is a strong requirement for synthetic anodes that enable a better understanding of the theoretical capacity associated with HC-anodes. We have developed core-shell carbon anodes consisting of a highly porous carbon core and (almost) non-porous shell. Thus, the reversible capacity can be deconvoluted from irreversible capacity losses, arising from the formation of the solid electrolyte interphase (SEI). Moreover, the porosity of the carbon-core can be linked to the reversible capacities gained. A range of microporous activated carbons were coated via an optimized chemical vapour deposition technique.[1][2] These materials were characterised using a range of techniques including powder x-ray diffraction, small angle x-ray diffraction (SAXS), gas physisorption (N2, CO2) measurements and electrochemical characterisation at coin cell level. After coating, the material showed a significant reduction in detectable surface area (up to a factor of 192x) by N2-physisorption. The tailor-made shell allows the stable cycling of a carbon anode vs metallic Na-electrode in coin cells at room temperature. For the best performing material, the reversible capacity increased from 139 ± 2 mAhg-1 to 396 ± 2 mAhg-1 while irreversible capacity is decreased from 636 ± 3 mAhg-1 to 89 ± 3 mAhg-1 (see Figure 1). After initial stabilization, a CE of 99% was achieved. The coating technique was usefully applied to a range of materials. [3] The successful formation of core-shell structures with high capacities enables separation of the storage mechanism from SEI-formation. In turn a proposed calculation to rank the contributions of surface adsorption and pore filling capacity can be confirmed. The materials also create the opportunity to conduct a range of operando experiments (e.g., SAXS) that can shed further light on the sodium storage mechanism. T2 - ECS Montreal 2025 CY - Montreal, Canada DA - 18.05.2025 KW - Electrochemical Energy Materials KW - Negative Electrodes KW - Sodium Ion Batteries PY - 2025 AN - OPUS4-65115 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fellinger, Tim-Patrick T1 - Sicherheit von NIB und das Potenzial synthetischer Kohlenstoff-Anoden N2 - Nach einer kurzen Einleitung zu kommerziellen Natrium-Ionen-Batterien, deren Zusammensetzung und Sicherheitstest die auch an der BAM untersucht wurden, folgt eine Vorstellung der Forschungsarbeiten des Fachbereich 3.6 im Rahmen des Verbundprojekts Dialysorb. Die Forschungsergebnisse stellen u.a. das Potenzial von synthetischen Anodenmaterialien dar. T2 - Deutsches Batterieforum 2025 CY - Berlin, Germany DA - 21.01.2025 KW - Natrium-Ionen-Batterien KW - Zusammensetzung KW - Potenzial KW - Sicherheit KW - Synthetische Anoden PY - 2025 AN - OPUS4-64904 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pauw, Paul T1 - Designing Core-Shell Carbon Structures as High- Capacity Negative Electrodes for Sodium Ion Batteries N2 - Due to abundant raw materials, low costs and promising high reversible specific capacities, hard carbons (HCs) are a common choice for commercially manufactured anodes in sodium-ion batteries (SIBs). Despite their potential and extensive use, the storage mechanism is still under debate. The non-stoichiometric adsorption mechanism also means that the search for an upper limit for the reversible capacity is ongoing. There is a strong requirement for synthetic anodes that enable a better understanding of the theoretical capacity associated with HC-anodes. We have developed core-shell carbon anodes consisting of a highly porous carbon core and (almost) non-porous shell. Thus, the reversible capacity can be deconvoluted from irreversible capacity losses, arising from the formation of the solid electrolyte interphase (SEI). Moreover, the porosity of the carbon-core can be linked to the reversible capacities gained. A range of microporous activated carbons were coated via an optimized chemical vapour deposition technique.[1][2] These materials were characterised using a range of techniques including powder x-ray diffraction, small angle x-ray diffraction (SAXS), gas physisorption (N2, CO2) measurements and electrochemical characterisation at coin cell level. After coating, the material showed a significant reduction in detectable surface area (up to a factor of 192x) by N2-physisorption. The tailor-made shell allows the stable cycling of a carbon anode vs metallic Na-electrode in coin cells at room temperature. For the best performing material, the reversible capacity increased from 139 ± 2 mAhg-1 to 396 ± 2 mAhg-1 while irreversible capacity is decreased from 636 ± 3 mAhg-1 to 89 ± 3 mAhg-1 (see Figure 1). After initial stabilization, a CE of 99% was achieved. The coating technique was usefully applied to a range of materials. [3] The successful formation of core-shell structures with high capacities enables separation of the storage mechanism from SEI-formation. In turn a proposed calculation to rank the contributions of surface adsorption and pore filling capacity can be confirmed. The materials also create the opportunity to conduct a range of operando experiments (e.g., SAXS) that can shed further light on the sodium storage mechanism. T2 - MatSUS Conference Sevilla CY - Sevilla, Spain DA - 03.03.2025 KW - Electrochemical Energy Materials KW - Negative Electrodes KW - Sodium Ion Batteries PY - 2025 AN - OPUS4-65113 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Low, Jian Liang T1 - Elucidating the Intrinsic CO2RR performance at MN4 sites using Morphologically Comparable M-N-Cs N2 - Metal- and nitrogen-doped carbons (M-N-Cs) are a promising class of low-cost electrocatalysts derived from earth-abundant elements for various electrochemical applications including ORR and CO2RR [1,2]. Traditionally, M-N-Cs containing active metals (M = Fe, Co, and Ni) are synthesized through direct pyrolysis of inorganic and organic precursors. However, this process often leads to the undesired formation of inorganic side phases via carbothermal reduction, hindering both the efficient incorporation of active metal and the intrinsic activity comparison among active sites. To overcome these challenges, we developed an active-site imprinting strategy where active metals are introduced post-pyrolysis through ion-exchange [3-5]. In this work, we applied a Mg imprinting strategy to synthesize Co-N-Cs and Ni-N-Cs with comparable morphology and metal dopant concentrations, enabling a more direct comparison of their intrinsic activities. Notably, Ni-N-Cs produced via this method consistently demonstrated superior activity and selectivity compared to isomorphic Co-N-Cs, achieving CO Faraday efficiencies of up to 95% at relatively low overpotentials. Furthermore, the Ni-N-C catalyst exhibited excellent stability at -0.65 VRHE, retaining 92.5% of its current density and 97.6% of its CO selectivity after 100 hours of continuous operation. A distinct advantage of the imprinting strategy lies in the suppression of inorganic side phases, enabling an accurate local structure characterization of the porphyrin-like tetrapyrrolic MN4 coordination structure using Extended X-ray Absorption Fine Structure (EXAFS). The characterization of the tetrapyrrolic NiN4 site is especially puzzling, as density functional theory (DFT) simulations often predict these sites to be inert to both CO2RR and HER. Drawing on recent studies which highlight the crucial role of cations for CO2RR on noble metal catalysts like Cu, Ag and Au [6-7], we performed mechanistic investigations using DFT to extend the relevance of cations to the CO2RR/HER performance at the MN4 sites, and further illustrate the advantage of the pyrrolic N atoms in anchoring them near the active metals. T2 - 4th Conference of the GDCh Division of Chemistry and Energy CY - Duisburg, Germany DA - 09.04.2025 KW - Electrochemical CO2 reduction KW - Active-site imprinting KW - Metal- and Nitrogen-doped Carbon (M-N-C) KW - Single Atom Catalyst PY - 2025 AN - OPUS4-65145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Low, Jian Liang T1 - Mg-based Imprinting for Assessing Intrinsic Behavior of Co/Ni-N4 sites towards CO2RR N2 - Metal-and nitrogen-doped carbons (MN-Cs) represent a promising class of low cost electrocatalysts derived from nature-abundant elements for various electrochemical processes including CO 2 RR [1, 2]. Traditionally, MN-Cs containing active metals (M= Fe, Co, Ni) are synthesized by direct pyrolysis of inorganic and organic precursors, a process that often results in the undesired formation of inorganic side phases through carbothermal reduction, impeding the effective integration of active metals like Fe, Co and Ni. Furthermore, comparing the intrinsic activities of different MN-Cs can be complicated due to variations in catalyst morphology and active site concentration that arise during the pyrolysis. To address these challenges, we developed an active-site imprinting strategy in which active metals are introduced post-pyrolysis via ion-exchange [3-5]. In this work, we employed the Mg imprinting strategy to produce Co-N-Cs and Ni-N-Cs with comparable morphology and metal dopant concentration. Our approach allows for a more direct comparison of the intrinsic activities that arise from the metal dopant. The Ni-N-Cs derived this way are consistently higher in activity and selectivity than the corresponding Co-N-Cs, exhibiting a CO Faraday efficiency of up to 95% at potentials between-0.5 to-0.8 V RHE. The Ni-NC catalyst maintains high stability at-0.65 V RHE, with 92.5% retention of current density and 97.6% retention of CO selectivity after 100 hours of continuous operation. T2 - The Materials for Sustainable Development Conference (MATSUS) Spring Meeting 2025 CY - Seville, Spain DA - 03.03.2025 KW - Electrochemical CO2 reduction KW - Active-site imprinting KW - Metal- and Nitrogen-doped Carbon (M-N-C) KW - Single Atom Catalyst PY - 2025 AN - OPUS4-65144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Appel, Paul Alexander T1 - Developing Tailor-Made Core-Shell Carbon Negative Electrode Materials for Sodium Ion Batteries N2 - Hard carbons (HCs) are currently one of the most promising anode materials for sodium-ion batteries (SIBs). However, the Na storage mechanism remains controversial, leaving the theoretical limits of carbon anodes unclear. To deconvolute the specific capacity from irreversible capacity losses, resulting from the formation of solid electrolyte interphase (SEI), core-shell carbon materials were synthesized. Based on these core-shell materials, an investigation of the storage mechanism of sodium is possible. T2 - Batterieforum 2025 CY - Berlin, Germany DA - 21.01.2025 KW - Electrochemical Energy Materials KW - Negative Electrodes KW - Sodium Ion Batteries PY - 2025 AN - OPUS4-65110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nitz, Phillip D. H. A1 - Rosaz, Paul A1 - Kreysina, Daniela A1 - Kasprzak, Dawid A1 - Qi, Naiyu A1 - Baller, Johannes A1 - Graeber, Gustav T1 - Water-in-Salt Electrolytes Embedded in Polyacrylamide Hydrogels: A First Step toward Deformable Sodium-Ion Batteries N2 - The development of flexible, safe, and sustainable Energy storage systems is critical for next-generation technologies, including wearable electronics, biomedical devices, and soft robotics. In this work, we provide a systematic investigation of sodium perchlorate-based water-in-salt (WIS) electrolytes embedded in polyacrylamide (PAM) hydrogels as a potential platform for deformable sodium-ion batteries or aqueous supercapacitors. Using Raman spectroscopy, we track the transition from free to intermediate water states with increasing salt concentration, identifying the onset of the WIS regime around 10 mol kg−1. Electrochemical measurements reveal that both the aqueous and hydrogel-based electrolytes exhibit a broadened electrochemical stability window (ESW) at higher salt concentrations, reaching up to 2.75 V. Impedance spectroscopy shows that while aqueous electrolytes achieve higher peak conductivity (156 mS cm−1), hydrogel-based electrolytes offer greater stability across a range of concentrations. This observation was supported by cyclic voltammetry, as it showed enhanced electrochemical stability of the PAM hydrogel compared to the aqueous electrolyte. This comprehensive and systematic study demonstrates that highly concentrated WIS electrolytes can be successfullyembedded into PAM hydrogels, while preserving good electrochemical stability and ionic conductivity. This could make them a promising foundation for all-hydrogel, sodium-based energy storage devices that are safe, sustainable, and mechanically compliant. KW - Battery PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-653156 DO - https://doi.org/10.1021/acsapm.5c03031 SN - 2637-6105 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-65315 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 - CONF A1 - Markötter, Henning T1 - Tomographic Imaging Capabilities with hard X-Rays at BAMline (Bessy II) N2 - The BAMline at the synchrotron X-ray source BESSY II (Berlin, Germany) is supporting researchers especially in materials science. 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 imaging capabilities allow for in-situ and operando experiments. In this presentation the equipment, data handling pipeline as well as various examples from material science are presented. T2 - Correlative Materials Characterization Workshop 2023 CY - Brno, Czech Republic DA - 09.11.2023 KW - Tomography KW - X-ray imaging KW - Li-ion battery PY - 2023 AN - OPUS4-58958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Okeke, Joseph T1 - In situ and operando imaging, spectroscopy and tomography of batteries N2 - The development of more powerful and more efficient lithium-ion batteries (LIBs) is a key area in battery research, aiming to support the ever-increasing demand for energy storage systems. To better understand the causes and mechanisms of degradation, and thus the diminishing cycling performance and lifetime often observed in LIBs, in operando techniques are essential, because battery chemistry can be monitored non-invasively, in real time. Moreover, there is increasing interest in developing new battery chemistries. Beyond LIBs, sodium ion batteries (NIBs) have gained increasing interest in recent years, as they are a promising candidate to complement LIBs, owing to their improved sustainability and lower cost, while still maintaining high energy density.[1] Initial phases of NIB commercialisation have occurred in the past year. However, for the widespread commercialisation of NIBs, there are still challenges that need to be overcome in developing optimized electrode materials and electrolytes. For the development of such materials and greater understanding of sodium storage mechanisms, solid electrolyte interface (SEI) formation and stability, and degradation processes, in operando methodologies are crucial. Among the techniques available for in operando analysis, nuclear magnetic resonance spectroscopy (NMR) and imaging (MRI) are becoming increasingly used to characterize the chemical composition of battery materials, study the growth and distribution of dendrites, and investigate battery storage and degradation mechanisms. In situ and in operando 1H, 7Li and 23Na NMR and MRI have recently been used to study LIBs and NIBs, identifying chemical changes in Li and Na species respectively, in metallic, quasimetallic and electrolytic environment as well as directly and indirectly studying dendrite formation in both systems.[2-4] The ability of NMR and MRI to probe battery systems across multiple environments can further be complemented by the enhanced spatial resolution of micro-computed X-ray tomography (μ-CT) which can provide insight into battery material microstructure and defect distribution. Here, we report in operando 1H and 7Li NMR and MRI experiments that investigate LIB performance, and the identification of changes in the Li signal during charge cycling, as well as the observation of signals in both 1H and 7Li NMR spectra that we attribute to diminishing battery performance, capacity loss and degradation. Additionally, recent operando methodology are adapted and implemented to study Sn based anodes in NIBs. 23Na spectroscopy is performed to monitor the formation and evolution of peaks assigned to stages of Na insertion into Sn, while 1H MRI is used to indirectly visualize the volume expansion of Sn anodes during charge cycling. Battery operation and degradation is further explored in these NIBs, using μ-CT, where the anode is directly visualized to a higher resolution and the loss of electrolyte in the cell, during cycling is observed T2 - 17th International Conference on Magnetic Resonance Microscopy CY - Singapore DA - 27.08.2023 KW - Sodium ion battery KW - Lithium ion battery KW - NMR KW - MRI KW - Tomography PY - 2023 AN - OPUS4-58421 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 - 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 - CONF A1 - Radnik, Jörg T1 - The role of Critical Raw Materials in Advanced Materials for the Energy Transition N2 - The energy transition needs advanced materials, especially for batteries, solar cells, and fuel cells. Therefore, critical raw materials are necessary. In this presentation the use of critcal raw materials and strategies for the optimisation of their use are discussed. T2 - Critical Raw Material Workshop during VAMAS Annual Meeting CY - Teddington, United Kingdom DA - 17.09.2025 KW - Advanced solar cells KW - Iridium oxide KW - Aerogels KW - Advanced carbon materials PY - 2025 AN - OPUS4-64290 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 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 - 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 - TY - JOUR A1 - Habibimarkani, Heydar A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan A1 - John, Elisabeth T1 - Probing Surface Changes in Fe–Ni Oxide Nanocatalysts with a ToF-SIMS-Coupled Electrochemistry Setup and Principal Component Analysis N2 - Understanding catalyst surface dynamics under operating conditions is essential for improving electrocatalytic performance. Here, we present a novel approach combining electrochemical treatment with contamination-free transfer to Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), followed by principal component analysis (PCA), to probe surface and interfacial changes in Ni–Fe oxide nanoparticles stabilized by polyvinylpyrrolidone (PVP) during the oxygen evolution reaction (OER). The surface analysis at three distinct treatment stages revealed distinct chemical fingerprints across pristine nanoparticles, after exposure to 1 M KOH electrolyte, and after cyclic voltammetry treatment. The results highlight a progressive transition from ligand-rich to ligand-depleted interfaces, with PVP-related fragments dominant in the early stages and metal- and electrolyte-derived species emerging after activation. Complementary ToF-SIMS analysis of electrolyte deposited on Si wafers after each treatment step confirms the concurrent leaching of PVP and Fe–Ni-based fragments during OER. These findings underscore the dynamic nature of catalyst–electrolyte interfaces and demonstrate a robust strategy for monitoring surface-sensitive chemical changes associated with the nanoparticles, especially during the initial cycles of the OER. KW - Fe-Ni oxide KW - Nanocatalysts KW - ToF-SIMS KW - Electrochemistry KW - PCA (principal component analysis) KW - OER PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-652667 DO - https://doi.org/10.1021/acs.analchem.5c03894 SN - 0003-2700 SP - 1 EP - 8 PB - American Chemical Society (ACS) AN - OPUS4-65266 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paulus, Daniel A1 - Bresch, Sophie A1 - Moos, Ralf A1 - Schönauer-Kamin, Daniela T1 - Powder aerosol deposited calcium cobaltite as textured P-type thermoelectric material with power factors approaching single crystal values N2 - In this work, the thermoelectric material calcium cobaltite Ca3Co4O9 (CCO), a promising p-type conducting thermoelectric oxide with anisotropic properties, was processed by the powder aerosol deposition method (PAD) to form a dense ceramic CCO film with a thickness in the µm range. The prepared films were characterized regarding their microstructure and thermoelectric properties between room temperature and 900 °C. After heat treatment at 900 °C, the CCO PAD film in-plane shows excellent properties in terms of electrical conductivity (280 S/cm at 900 °C) and Seebeck coefficient (220 µV/K at 900 °C). The calculated power factor in-plane (ab) reaches with 1125 µW/(m K2) 40 % of the single crystal value, surpassing the known-properties of CCO bulk ceramics. Examination of the microstructure shows a strong fiber texture of the film as well as a strong coarsening of the grains during the first heat treatment up to 900 °C. KW - thermoelectrics KW - calcium cobaltite KW - thermoelectric oxide KW - aerosol deposition method (ADM) PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-606246 DO - https://doi.org/10.1016/j.jeurceramsoc.2024.116717 SN - 0955-2219 VL - 44 IS - 15 SP - 1 EP - 8 PB - Elsevier BV AN - OPUS4-60624 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Risse, S. A1 - Juhl, A. A1 - Mascotto, S. A1 - Arlt, T. A1 - Markötter, Henning A1 - Hilger, A. A1 - Manke, I. A1 - Fröba, M. T1 - Detailed and Direct Observation of Sulfur Crystal Evolution During Operando Analysis of a Li-S Cell with Synchrotron Imaging N2 - Herein, we present a detailed investigation of the electrochemically triggered formation and dissolution processes of α- and β-sulfur crystals on a monolithic carbon cathode using operando high-resolution synchrotron radiography (438 nm/pixel). The combination of visual monitoring with the electrical current response during cyclic voltammetry provides valuable insights into the sulfur formation and dissolution mechanism. Our observations show that the crystal growth process is mainly dictated by a rapid equilibrium between long-chain polysulfides on one side and solid sulfur/short-chain polysulfides on the other side, which is consistent with previous studies in this field. The high temporal and spatial resolution of synchrotron imaging enables the observation of different regimes during the sulfur formation and dissolution process. The appearance of short-chain polysulfides after the first anodic CV peak initiates a rapid dissolution process of α-sulfur crystals on the cathode. The increase in the long-chain lithium polysulfide concentration at the cathode surface during charge results in an increased crystal growth rate, which in turn produces imperfections in α- and β-sulfur crystals. There are strong indications that these defects are fluid inclusions, which may trap dissolved polysulfides and therefore reduce the electrochemical cell capacity. KW - LiS battery KW - Radiography KW - Synchrotron Imaging PY - 2020 DO - https://doi.org/10.1021/acs.jpclett.0c01284 VL - 11 IS - 14 SP - 5674 EP - 5679 AN - OPUS4-51100 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - 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 - 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 - 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 - 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 - 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 - TY - CONF A1 - Ulbricht, Alexander T1 - Skalenübergreifende Materialcharakterisierung basierend auf Computertomographiedaten N2 - Die BAM präsentiert anhand ausgewählter Beispiele wie mithilfe von Computertomographiedaten dringende technische Fragestellungen zum Verständnis von Schädigungsmechanismen in verschiedensten Materialien und Komponenten, zum Beispiel in additiv gefertigten Metallen oder Batterien, beantwortet werden können. T2 - VisiConsult Röntgen-Technologietag 2024 -- Transformation in der ZfP CY - Stockelsdorf, Germany DA - 10.10.2024 KW - Computertomographie KW - Batterie KW - Additive Fertigung KW - Synchrotron KW - BAMline PY - 2024 AN - OPUS4-61431 LA - mul AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Stargardt, Patrick A1 - Moos, Ralf A1 - Mieller, Björn T1 - Co‐Fired Multilayer Thermoelectric Generators Based on Textured Calcium Cobaltite N2 - Thermoelectric generators are very attractive devices for waste heat energy harvesting as they transform a temperature difference into electrical power. However, commercially available generators show poor power density and limited operation temperatures. Research focuses on high‐temperature materials and innovative generator designs. Finding the optimal design for a given material system is challenging. Here, a theoretical framework is provided that allows appropriate generator design selection based on the particular material properties. For high‐temperature thermoelectric oxides, it can be clearly deduced that unileg multilayer generators have the highest potential for effective energy harvesting. Based on these considerations, prototype unileg multilayer generators from the currently best thermoelectric oxide Ca3Co4O9 are manufactured for the first time by industrially established ceramic multilayer technology. These generators exhibit a power density of 2.2 mW/cm² at a temperature difference of 260 K, matching simulated values and confirming the suitability of the technology. Further design improvements increase the power density by a factor of 22 to facilitate practicable power output at temperature differences as low as 7 K. This work demonstrates that reasonable energy harvesting at elevated temperatures is possible with oxide materials and appropriate multilayer design. KW - Optical and Magnetic Materials KW - Electronic PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-596306 DO - https://doi.org/10.1002/aelm.202300636 SN - 2199-160X VL - 10 IS - 3 SP - 1 EP - 12 PB - Wiley VHC-Verlag AN - OPUS4-59630 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tang, F. A1 - Li, D. A1 - Liu, X. A1 - Huang, H. A1 - Wu, C. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Manke, I. A1 - Sun, F. A1 - Chen, L. T1 - Exploring optimal Li composite electrode anodes for lithium metal batteries through in situ X-ray computed tomography N2 - The uncontrolled Li dissolution/deposition dynamics and rapid Li pulverizations hinder the widespread deployment of Li metal batteries (LMB). Designing a Li composite electrode possessing a mechanically robust and lithiophilic three-dimensional (3D) framework represents a promising strategy to address these challenges. This study involves the preparation of three uniquely tailored Li-B-Mg composites using a combined metallurgical process of melting, casting, and rolling, along with the synergistic application of in situ X-ray computed tomography (CT) and post-mortem failure analysis to explore the most promising composite electrode candidate for LMBs. During the in-depth investigation, the optimal 70Li-B-Mg composite electrode stands out due to its robust skeleton fiber structure, uniform Li dissolution/deposition characteristics and high capacity of free-Li. Its promising prospects for enabling high-performance LMBs are showcased by the superior performance of the built Li||O2, Li||LiFePO4, Li||NCM622 and Li||NCM811 battery systems. This work offers a novel approach for exploring universally applicable and robust Li composite electrodes to realize high-performance LMBs using in situ CT analysis. KW - Li metal batteries KW - Li composite electrode KW - X-ray computed tomography KW - Li-B-Mg PY - 2024 DO - https://doi.org/10.1016/j.ensm.2024.103746 VL - 72 SP - 12 PB - Elsevier B.V. AN - OPUS4-61039 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mieller, Björn T1 - Synthesis and testing of beta aluminate sodium electrolyte (BASE) for sodium ion battery development N2 - Sodium beta aluminate, or beta aluminate solid electrolyte (BASE), is an established material for tubular electrolytes in NaNiCl2 and NaS batteries, and a promising candidate for planar electrolytes in safe all solid-state batteries. The synthesis of BASE with high ionic conductivity is still challenging due to process dependent formation of different phases in the sintered material. However, to drive forward the development of active materials for all solid-state sodium ion batteries, the fabrication of solid electrolyte specimens with reproducible performance is required. With respect to the various testing scenarios in the field, for example cell assembly for cycling, electrolyte parts are needed in various shapes, sizes, and thicknesses in the lab. Different ceramic shaping technologies can be applied to produce such geometries, including pressing combined with green or hard machining, or tape casting combined with punching. Typically, different shaping technologies require adapted pre-treatment of the powder which might affect the resulting properties and thus need to be investigated. In this contribution, starting from the raw materials mixture, aspects of milling, drying, aqueous slurry preparation for tape casting, and firing are discussed with respect to particle size distribution, stability, energy consumption and resulting material properties. Finally, the fabrication and cyclic testing of Na/electrolyte/Na coin cells is presented. T2 - XIXth Conference of the European Ceramic Society / SBS6 International Sodium Battery Symposium CY - Dresden, Germany DA - 01.09.2025 KW - Ceramics KW - Beta aluminate solid electrolyte KW - Sodium ion battery PY - 2025 AN - OPUS4-64054 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zheng, Y. A1 - Zhang, S. A1 - Ma, J. A1 - Sun, F. A1 - Osenberg, M. A1 - Hilger, A. A1 - Markötter, Henning A1 - Wilde, F. A1 - Manke, I. A1 - Hu, Z. A1 - Cui, G. T1 - Codependent failure mechanisms between cathode and anode in solid state lithium metal batteries: mediated by uneven ion flux N2 - An in-depth understanding of the degradation mechanisms is a prerequisite for developing the nextgeneration all solid-state lithium metal battery (ASSLMB) technology. Herein, synchrotron X-ray computed tomography (SXCT) together with other probing tools and simulation method were employed to rediscover the decaying mechanisms of LiNi0.8Co0.1Mn0.1O2 (NCM)|Li6PS5Cl (LPSCl)|Li ASSLMB. It reveals that the detachment and isolation of NCM particles cause the current focusing on the remaining active regions of cathode. The extent of Li stripping and the likelihood of Li+ plating into LPSCl facing the active NCM particles becomes higher. Besides, the homogeneity of Li stripping/plating is improved by homogenizing the electrochemical reactions at the cathode side by LiZr2(PO4)3 (LZP) coating. These results suggest a codependent failure mechanism between cathode and anode that is mediated by uneven Li ion flux. This work contributes to establish a holistic understanding of the degradation mechanisms in ASSLMBs and opens new opportunities for their further optimization and evelopment. KW - Current density distribution KW - Lithium ion flux KW - Solid-state lithium metal batteries KW - Codependent failure mechanism KW - Cathode deactivation PY - 2023 DO - https://doi.org/10.1016/j.scib.2023.03.021 SN - 2095-9273 VL - 68 IS - 8 SP - 813 EP - 825 PB - Elsevier B.V. AN - OPUS4-57309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martínez, E. A1 - Lejeune, N. A1 - Frechilla, J. A1 - Porta-Velilla, L. A1 - Forneau, E. A1 - Angurel, L. A. A1 - de la Fuente, G. F. A1 - Bonse, Jörn A1 - Silhanek, A. V. A1 - Badía-Majós, A. T1 - Laser engineered architectures for magnetic flux manipulation on superconducting Nb thin films N2 - Custom shaped magnetic flux guiding channels have been fabricated on superconducting Nb thin films by laser nanopatterning of their surface. Preferential pathways are defined by suitable combination of imprinted anisotropic pinning domains through laser-induced periodic surface structures (LIPSS). Generated by the selective energy deposition of femtosecond UV laser pulses, quasi-parallel ripple structures are formed under optimized irradiation conditions. On average, each domain is formed by grooves with a lateral period of 260–270 nm and a depth about 80 nm. By combination of scanning and transmission electron microscopy, magneto-optical imaging, and conductive atomic force microscopy techniques, we conclude that the boundaries of the LIPSS-covered domains play a prominent role in the magnetic flux diversion process within the film. This is confirmed by dedicated modeling of the flux dynamics, combined with the inversion of the magneto-optical signal. The created metasurfaces enable control of the flux penetration process at the microscale. KW - Laser-induced periodic surface structures (LIPSS) KW - Magnetic flux KW - Magneto-optical imaging (MOI) KW - Critical current density PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-611243 UR - https://www.sciencedirect.com/science/article/pii/S0169433224019287 DO - https://doi.org/10.1016/j.apsusc.2024.161214 SN - 1873-5584 (Online) SN - 0169-4332 (Print) VL - 679 SP - 1 EP - 12 PB - Elsevier AN - OPUS4-61124 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lucaßen, J. T1 - Bottom-up grown CISe micro absorber arrays: microstructure analysis and solar cell integration N2 - A reduction of critical raw materials like indium and gallium in chalcopyrite thin-film solar cells is aimed for the micro-concentrator concept. Bottom-up grown micro absorbers for operation under light concentration on the micrometer scale allow improved heat dissipation. T2 - 41st European Photovoltaic Solar Energy Conference and Exhibition (EU PVSEC 2024) CY - Vienna, Austria DA - 23.09.2024 KW - Laser-assisted MO-CVD KW - CISe micro-absorber KW - Micro solar cell arrays KW - Solar cell efficiency PY - 2024 AN - OPUS4-62075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -