| 1. |
- Dietrich, Paul M., et al.
(author)
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Near ambient pressure-x-ray photoelectron spectroscopy spectra of lithium bis (trifluoromethane-sulfonyl) imide in propylene carbonate
- 2023
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In: Surface Science Spectra. - : American Vacuum Society. - 1055-5269 .- 1520-8575. ; 30:1
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Journal article (peer-reviewed)abstract
- Near ambient pressure-x-ray photoelectron spectroscopy (NAP-XPS) is a less traditional form of XPS that allows samples to be analyzed at relatively high pressures, i.e., at greater than 5000 Pa. NAP-XPS can probe moderately volatile liquids, biological samples, porous materials, and/or polymeric materials that outgas significantly. In this submission, we show the survey, Li 1s, S 2p, C 1s, N 1s, O 1s, and F 1s NAP-XPS spectra of a Li-based electrolyte solution, which is a material that would be difficult to analyze by conventional XPS. The measurements were performed at 200 Pa in ambient gas atmosphere to compensate for surface charging. Peak fits of the C 1s, O 1s, and F 1s narrow scans are presented.
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| 2. |
- Maibach, Julia, 1984, et al.
(author)
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Toward Operando Characterization of Interphases in Batteries
- 2023
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In: ACS Materials Letters. - 2639-4979. ; 5:9, s. 2431-2444
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Research review (peer-reviewed)abstract
- Electrode/electrolyte interfaces are the most importantand leastunderstood components of Li-ion and next-generation batteries. Animproved understanding of interphases in batteries will undoubtedlylead to breakthroughs in the field. Traditionally, evaluating thoseinterphases involves using ex situ surface sensitiveand/or imaging techniques. Due to their very dynamic and reactivenature, ex situ sample manipulation is undesirable.From this point of view, operando surface sensitivetechniques represent a major opportunity to push boundaries in batterydevelopment. While numerous bulk spectroscopic, scattering, and imagingtechniques are well established and widely used, surface sensitive operando techniques remain challenging and, to a largerextent, restricted to the model systems. Here, we give a perspectiveon techniques with the potential to characterize solid/liquid interfacesin both model and realistic battery configurations. The focus is ontechniques that provide chemical and structural information at lengthand time scales relevant for the solid electrolyte interphase (SEI)formation and evolution, while also probing representative electrodeareas. We highlight the following techniques: vibrational spectroscopy,X-ray photoelectron spectroscopy (XPS), neutron and X-ray reflectometry,and grazing incidence scattering techniques. Comprehensive overviews,as well as promises and challenges, of these techniques when used operando on battery interphases are discussed in detail.
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| 3. |
- Schäfer, David, et al.
(author)
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Multiscale Investigation of Sodium-Ion Battery Anodes: Analytical Techniques and Applications
- 2024
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In: Advanced Energy Materials. - 1614-6840 .- 1614-6832. ; 14:15
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Journal article (peer-reviewed)abstract
- The anode/electrolyte interface behavior, and by extension, the overall cell performance of sodium-ion batteries is determined by a complex interaction of processes that occur at all components of the electrochemical cell across a wide range of size- and timescales. Single-scale studies may provide incomplete insights, as they cannot capture the full picture of this complex and intertwined behavior. Broad, multiscale studies are essential to elucidate these processes. Within this perspectives article, several analytical and theoretical techniques are introduced, and described how they can be combined to provide a more complete and comprehensive understanding of sodium-ion battery (SIB) performance throughout its lifetime, with a special focus on the interfaces of hard carbon anodes. These methods target various length- and time scales, ranging from micro to nano, from cell level to atomistic structures, and account for a broad spectrum of physical and (electro)chemical characteristics. Specifically, how mass spectrometric, microscopic, spectroscopic, electrochemical, thermodynamic, and physical methods can be employed to obtain the various types of information required to understand battery behavior will be explored. Ways are then discussed how these methods can be coupled together in order to elucidate the multiscale phenomena at the anode interface and develop a holistic understanding of their relationship to overall sodium-ion battery function.
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| 4. |
- Stottmeister, Daniel, et al.
(author)
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Unraveling Propylene Oxide Formation in Alkali Metal Batteries
- 2024
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In: ChemSusChem. - 1864-5631 .- 1864-564X. ; 17:3
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Journal article (peer-reviewed)abstract
- The increasing need for electrochemical energy storage drives the development of post-lithium battery systems. Among the most promising new battery types are sodium-based battery systems. However, like its lithium predecessor, sodium batteries suffer from various issues like parasitic side reactions, which lead to a loss of active sodium inventory, thus reducing the capacity over time. Some problems in sodium batteries arise from an unstable solid electrolyte interphase (SEI) reducing its protective power e. g., due to increased solubility of SEI components in sodium battery systems. While it is known that the electrolyte affects the SEI structure, the exact formation mechanism of the SEI is not yet fully understood. In this study, we follow the initial SEI formation on a piece of sodium metal submerged in propylene carbonate with and without the electrolyte salt sodium perchlorate. We combine X-ray photoelectron spectroscopy, gas chromatography, and density functional theory to unravel the sudden emergence of propylene oxide after adding sodium perchlorate to the electrolyte solvent. We identify the formation of a sodium chloride layer as a crucial step in forming propylene oxide by enabling precursors formed from propylene carbonate on the sodium metal surface to undergo a ring-closing reaction. Based on our combined theoretical and experimental approach, we identify changes in the electrolyte decomposition process, propose a reaction mechanism to form propylene oxide and discuss alternatives based on known synthesis routes.
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