Browsing by Author "Wissel, Kerstin"

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    Direct recycling of all‐solid‐state batteries with a halide solid electrolyte via water‐based separation : interactions of electrode materials in aqueous Li3InCl6 solutions
    (2025) Jacob, Martine; Moreno Fernández, Harol; Haben, Aaron; Waidha, Aamir Iqbal; Özel, Simay; Hofmann, Jan P.; Kautenburger, Ralf; Clemens, Oliver; Wissel, Kerstin
    Despite extensive research in the field of all‐solid‐state batteries, there has been limited attention to their recycling, which is crucial for achieving long‐term sustainability. Different electrolyte and electrode combinations must be considered for the recycling of these batteries, each requiring a detailed investigation of potential recycling approaches. The halide‐based solid electrolyte, Li3InCl6, has attracted significant attention due to its high‐room‐temperature lithium‐ion conductivity and its ability to recover its initial crystal structure after dissolution in water without significant electrochemical deterioration. This structural reversibility could potentially enable a direct recycling approach, allowing for the separation of the electrolyte from active electrode materials when dissolved in H2O. To assess the recycling compatibility, the interactions of Li3InCl6 with different electrode materials (Li4Ti5O12, LiCoO2, LiMn2O4, carbon‐coated LiFePO4, LiNi0.8Mn0.1Co0.1O2, and LiNi0.8Co0.15Al0.05O2) are studied during dissolution. Interactions arising from Lewis‐acid and Lewis‐base reactions can be identified using a combination of X‐ray diffraction, X‐ray photoelectron spectroscopy, and inductively coupled plasma mass spectrometry. Depending on the material combination, these interactions significantly impact the electrochemical properties of both recycled Li3InCl6 and the electrode materials compared to the pristine samples.
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    Recycling of all‐solid‐state Li‐ion batteries : a case study of the separation of individual components within a system composed of LTO, LLZTO and NMC
    (2023) Waidha, Aamir Iqbal; Salihovic, Amila; Jacob, Martine; Vanita, Vanita; Aktekin, Burak; Brix, Kristina; Wissel, Kerstin; Kautenburger, Ralf; Janek, Jürgen; Ensinger, Wolfgang; Clemens, Oliver
    With the current global projection of over 130 million electric vehicles (EVs), there soon will be a need for battery waste management. Especially for all‐solid‐state lithium‐ion batteries (lithium ASSBs), aspects of waste management and circular economy have not been addressed so far. Within such ASSBs, the use of solid‐electrolytes like garnet‐type Li6.5La3Zr1.5Ta0.5O12 (LLZTO) may shift focus on strategies to recover not only the transition metal elements but also elements like La/Zr/Ta. In this work, we present a two‐step recycling approach using citric acid as the leaching agent to separate and recover the individual components of a model cell comprising of Li4Ti5O12 (LTO) anode, Li6.5La3Zr1.5Ta0.5O12 (LLZTO) garnet electrolyte and LiNi1/3Mn1/3Co1/3O2 (NMC) cathode. We observe that by adjusting the concentration of citric acid, it was possible to separate the materials from each other without strong mixing of individual phases and also to maintain their principle performance characteristics. Thus, the process developed has a potential for upscaling and can guide towards considering separation capability of battery components in the development of lithium ASSBs.
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    Revealing an intercalation nature of high‐capacity conversion cathode materials for fluoride‐ion batteries by operando studies
    (2025) Chen, Hong; Schoch, Roland; Chotard, Jean‐Noel; Thiebes, Yannick M.; Wissel, Kerstin; Niewa, Rainer; Bauer, Matthias; Clemens, Oliver
    To improve the performance of high‐energy‐density electrode materials for all‐solid‐state fluoride‐ion batteries (ASSFIBs), it is important to understand the structure and phase evolution during operation, which is closely correlated to capacity fading. In this study, an operando cell is designed compatible with laboratory X‐ray diffraction (XRD) to monitor real‐time structural changes of bismuth trifluoride (BiF3) cathodes and degradation of the ionic conductor BaSnF4 under negative potentials at 100 °C. Supported by ex‐situ XRD, our results reveal a multi‐step defluorination of BiF3: from orthorhombic (o‐BiF3) to cubic (c‐BiF3), then to distorted orthorhombic (o’‐BiF3), and finally to metallic bismuth (Bi), indicating partial intercalation‐type character. Formation of bismuth oxidefluoride (BiOF) beyond 200 mAh g-1 is attributed to oxygen impurities introduced via solid‐state synthesis. operando X‐ray absorption spectroscopy (XAS) confirms a continuous reduction of Bi3+ to Bi0 with intermediate phases. Rietveld refinement quantifies the phase fractions and structural transitions, enabling a model for BiF3 defluorination. Comparison of operando XRD and XAS reveals that BaSnF4 contributes transport of both fluoride and oxygen impurities, leading to BiOF formation. BaSnF4 also exhibits a broad stability window, with degradation occurring below -200 mV, rather than the expected -50 mV vs. Sn/SnF2.
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    Towards recycling of all‐solid‐state batteries with argyrodite sulfide electrolytes : insights into electrolyte and electrode degradation in dissolution‐based separation processes
    (2025) Wissel, Kerstin; Hu, Zian; Wu, Xuebin; Jacob, Martine; Küster, Kathrin; Starke, Ulrich; Clemens, Oliver
    All‐solid‐state Li‐ion batteries (ASSBs) represent a promising leap forward in battery technology, rapidly advancing in development. Among the various solid electrolytes, argyrodite thiophosphates Li6PS5X (X=Cl, Br, I) stand out due to their high ionic conductivity, structural flexibility, and compatibility with a range of electrode materials, making them ideal candidates for efficient and scalable battery applications. However, despite significant performance advancements, the sustainability and recycling of ASSBs remain underexplored, posing a critical challenge for achieving efficient circular processes. This study investigates the dissolution‐based separation and recovery of argyrodite thiophosphate electrolytes and transition metal oxide electrode materials as a potential recycling strategy for ASSBs. A focus is set on the impact of solvent treatments on the recrystallization behavior of these electrolytes. Furthermore, the interactions between dissolved argyrodite thiophosphates and various transition metal oxide electrode materials (LiCoO2, LiMn2O4, LiNi0.8Mn0.1Co0.1O2, LiFePO4 and Li4Ti5O12) is examined to assess their influence on the functional properties of both the electrolytes and electrode materials. Structural, compositional and morphological changes are analyzed using X‐ray diffraction, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, inductively coupled plasma mass spectrometry and X‐ray photoelectron spectroscopy. Our findings provide insights into the complexities of recycling ASSBs, but also highlight the potential for developing efficient, sustainable recycling processes.