Concept for the Analysis of the Electrolyte Composition within the Cell Manufacturing Process: From Sealing to Sample Preparation

Horsthemke, Fabian; Winkler, Volker; Diehl, Marcel; Winter, Martin; Nowak, Sascha

doi:10.1002/ente.201801081

Cited by 12 publications

(8 citation statements)

References 21 publications

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“…The cells were filled with 700 μL of the respective electrolyte formulation (Table 1) and vacuum‐sealed at 165 °C and a relative pressure of −90 kPa for 5 s. After wetting for 24 h, two constant current/constant voltage (CC/CV) charge (0.2 C; <0.05 C) and CC discharge (0.2 C) cycles were performed in a voltage window between 3.0 and 4.2 V. After formation, cells were opened in a glovebox (O 2 <0.1 ppm, H 2 O<5 ppm) and the electrolyte was regained via centrifugation. For validation and detailed description of the sample preparation the reader is kindly referred to previous studies [44] …”

Section: Methodsmentioning

confidence: 99%

Analysis of Carbonate Decomposition During Solid Electrolyte Interphase Formation in Isotope‐Labeled Lithium Ion Battery Electrolytes: Extending the Knowledge about Electrolyte Soluble Species

Peschel

Horsthemke

Leißing

et al. 2020

Batteries & Supercaps

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Sufficient interphase formation during the first cycles is crucial for the long‐term performance of lithium ion batteries. During the first cycles, electrolyte salt and solvent molecule decomposition caused by electrochemical instabilities leads to a wide range of decomposition species contributing to the formation of performance‐beneficial interphases at the electrodes as well as performance‐impairing side reactions. Due to structural similarities of carbonate educts, elucidation of underlying reaction pathways is complex. In this work, isotope‐labeled ethylene carbonate (13C3−EC) is applied to differentiate contributions of cyclic and linear carbonates to occurring interphase and decomposition reactions. Thereby, carbon atom tracing of electrolyte soluble species is performed by means of gas chromatography‐mass spectrometry (GC−MS). Reaction pathways are postulated based on identified molecular origins. Among others, a new DMC‐EC cross reactivity via lithium ethylene monocarbonate is considered. Moreover, radical reactions resulting in C−C bond formation are investigated and radical polymerizations of stoichiometric equivalents of ethene formed in situ during EC reduction are proposed. Finally, alkyl carbonates with C>4 alkyl chains are identified considering underlying reactivities. Discussed electrolyte decomposition reactions extend the understanding of EC‐based solid electrolyte interphase (SEI) formation emphasizing possible radical reactivities and solvent molecule contributions.

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Section: Methodsmentioning

confidence: 99%

Analysis of Carbonate Decomposition During Solid Electrolyte Interphase Formation in Isotope‐Labeled Lithium Ion Battery Electrolytes: Extending the Knowledge about Electrolyte Soluble Species

Peschel

Horsthemke

Leißing

et al. 2020

Batteries & Supercaps

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“…The identified proportion of sodium indicated the use of carboxymethyl cellulose (CMC) as a binder material, which is commonly applied as sodium salt. [44,45] Binder polymers were further analyzed by Pyr-GC-MS. Sulfur could originate from additionally applied sulfur containing conducting salt anions like bis((trifluoromethyl)sulfonyl)imide (TFSI À ) or bis(fluorosulfonyl)imide (FSI À ) which was further investigated by IC-CD-IT-TOF-MS, and from application of sulfur containing electrolyte additives, as further investigated by Pyr-GC-MS and GC-HRMS.…”

Section: Chemistry-a European Journalmentioning

confidence: 99%

Comprehensive Characterization of Shredded Lithium‐Ion Battery Recycling Material

Peschel

Wickeren

Preibisch

et al. 2022

Chemistry A European J

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Herein we report on an analytical study of dry‐shredded lithium‐ion battery (LIB) materials with unknown composition. Samples from an industrial recycling process were analyzed concerning the elemental composition and (organic) compound speciation. Deep understanding of the base material for LIB recycling was obtained by identification and analysis of transition metal stoichiometry, current collector metals, base electrolyte and electrolyte additive residues, aging marker molecules and polymer binder fingerprints. For reversed engineering purposes, the main electrode and electrolyte chemistries were traced back to pristine materials. Furthermore, possible lifetime application and accompanied aging was evaluated based on target analysis on characteristic molecules described in literature. With this, the reported analytics provided precious information for value estimation of the undefined spent batteries and enabled tailored recycling process deliberations. The comprehensive feedstock characterization shown in this work paves the way for targeted process control in LIB recycling processes.

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“…Within the development of sample preparation methods, Horsthemke et al investigated the influence of reduced pressure protocols applied during the manufacturing of 18650-type cells [206]. The used protocol was found to be non-destructive with respect to the ratio between the linear and cyclic carbonates.…”

Section: Gc Investigations On Electrolyte Componentsmentioning

confidence: 99%

Chromatographic Techniques in the Research Area of Lithium Ion Batteries: Current State-of-the-Art

et al. 2019

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Lithium ion batteries (LIBs) are widely used in numerous application areas, including portable consumer electronics, medicine, grid storage, electric vehicles and hybrid electric vehicles. One major challenge during operation and storage is the degradation of the cell constituents, which is called aging. This phenomenon drastically reduces both storage lifetime and cycle lifetime. Due to numerous aging effects, originating from both the individual LIB cell constituents as well as their interactions, a wide variety of instruments and methods are necessary for aging investigations. In particular, chromatographic methods are frequently applied for the analysis of the typically used liquid non-aqueous battery electrolytes based on organic solvents or ionic liquids. Moreover, chromatographic methods have also been recently used to investigate the composition of electrode materials. In this review, we will give an overview of the current state of chromatographic methods in the context of LIB cell research.

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Concept for the Analysis of the Electrolyte Composition within the Cell Manufacturing Process: From Sealing to Sample Preparation

Cited by 12 publications

References 21 publications

Analysis of Carbonate Decomposition During Solid Electrolyte Interphase Formation in Isotope‐Labeled Lithium Ion Battery Electrolytes: Extending the Knowledge about Electrolyte Soluble Species

Analysis of Carbonate Decomposition During Solid Electrolyte Interphase Formation in Isotope‐Labeled Lithium Ion Battery Electrolytes: Extending the Knowledge about Electrolyte Soluble Species

Comprehensive Characterization of Shredded Lithium‐Ion Battery Recycling Material

Chromatographic Techniques in the Research Area of Lithium Ion Batteries: Current State-of-the-Art

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