TY - JOUR A1 - Amano, K. A1 - Hahn, S. A1 - Tschirschwitz, Rico A1 - Rappsilber, Tim A1 - Krause, U. T1 - An Experimental Investigation of Thermal Runaway and Gas Release of NMC Lithium-Ion Pouch Batteries Depending on the State of Charge Level N2 - In this study, 19 experiments were conducted with 25 pouch cells of NMC cathode to investigate thermal runaway and the release of gases from lithium-ion batteries (LIBs). Single cells, double cells, and a four-cell battery stack were forced to undergo thermal runaway inside an air-tight reactor vessel with a volume of 100 dm3 . The study involved two series of tests with two types of ignition sources. In the Series 1 tests, a heating plug was used to initiate thermal runaway in LIBs in the ranges of 80–89% and 90–100% SOC. In the Series 2 tests, a heating plate was used to trigger thermal runaway in LIBs in the ranges of 30–50%, 80–89%, and 90–100% SOC. Thermal runaway started at an onset temperature of 344 ± 5 K and 345 K for the Series 1 tests and from 393 ± 36 K to 487 ± 10 K for the Series 2 tests. Peak reaction temperatures ranged between 642 K and 1184 K, while the maximum pressures observed were between 1.2 bar and 7.28 bar. Thermal runaway induced explosion of the cells and lead to a rate of temperature increase greater than 10 K/s. The amounts of gases released from the LIBs were calculated from pressures and temperatures measured in the reactor. Then, the gas composition was analyzed using a Fourier transform infrared (FTIR) spectrometer. The highest gaseous production was achieved at a range of 90–100% SOC and higher battery capacities 72 L, 1.8 L/Ah (Series 1, battery stack) and 103 L, 3.2 L/Ah (Series 2, 32 Ah cell)). Among the gases analyzed, the concentration of gaseous emissions such as C2H4 , CH4 , and C2H6 increased at a higher cell capacity in both series of tests. The study results revealed characteristic variations of thermal behavior with respect to the type of ignition source used. KW - Lithium-ion batteries KW - Battery KW - Pouch cell KW - NMC Cathode KW - Thermal runaways PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-548601 DO - https://doi.org/10.3390/batteries8050041 VL - 8 IS - 5 SP - 1 EP - 16 PB - MDPI CY - Basel, Switzerland AN - OPUS4-54860 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - How does solid microanalysis profit from innovations in EUV research N2 - Research into new sources for EUV lithography is driving advancements in experimental methods tailored for this short wavelength range. This progress enables the exploration of spectroscopic techniques aimed at monitoring electronic transitions within this energy spectrum. Laser-induced breakdown spectroscopy (LIBS) serves as a rapid tool for elemental analysis, primarily established in the UV-vis range. However, LIBS encounters challenges such as limited repeatability precision and elevated background noise resulting from continuum radiation. In parallel, laser-induced extreme UV spectroscopy (LIXS) delves into the initial stages of plasma evolution, characterized by the emergence of soft X-ray and extreme UV radiation. The method benefits from a fast timeframe and constrained plasma confinement, leading to better precision. Nevertheless, LIXS encounters convoluted spectra arising from unresolved transition arrays (UTA), particularly pronounced for heavier elements. This complexity renders conventional univariate data analysis impractical, demanding the adoption of a multivariate data analysis approach. Multiple cathode samples, each coated with varying stoichiometries of lithium nickel manganese cobalt oxide (NMC), were prepared and used for calibration purposes. Through the application of Partial Least Squares (PLS) regression, a robust correlation with an R2 value exceeding 0.97 was achieved. The LIXS technique underwent a comparative evaluation against UV-vis LIBS. Furthermore, a comparison between univariate and multivariate analysis approaches was conducted, incorporating validation through y-randomization to mitigate overfitting risks. The viability of this approach was confirmed through the testing of an NMC reference material. The results showed metrological compatibility with reference values, underscoring the potential capability of the proposed methodology. T2 - 322. PTB Seminar 2023 - VUV and EUV Metrology CY - Berlin, Germany DA - 14.11.2023 KW - Laser induced XUV spectroscopy KW - Lithium-ion batteries KW - Solid microanalysis PY - 2023 UR - https://www.euv2023.ptb.de/ AN - OPUS4-58834 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böttcher, Nils T1 - Lithium-Ionen-Batterien: Aktuelles aus der Forschung Optimierungsmöglichkeiten beim Transport kritisch-defekter Batterien N2 - Durch den gekühlte Transport von kritisch defekten Lithium-Batterien können Zellen unterhalb ihrer initialen Reaktionstemperatur inert und ohne thermisches Durchgehen sicher transportiert werden. Allerdings kann das Auftauen von kritischen Zellen je nach Beständigkeit der Kurzschlusses dennoch zum thermischen Durchgehen führen. Zusätzlich sollte ein direkter Kontakt mit dem Kühlmedium sollte unterbunden werden, da dieses sonst in die Zellen eindringen kann. Anhand der vorgestellten Ergebnisse zeigt sich zudem keine allgemeingültige sichere Transporttemperatur. T2 - IAA Transportation CY - Hannover, Germany DA - 19.09.2024 KW - Thermal runaway KW - Low temperature KW - Lithium-ion batteries KW - Abuse testing PY - 2024 AN - OPUS4-62320 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Morcillo, Dalia T1 - High-resolution optical isotopic spectrometry as a tool for aging studies of Li-ion batteries N2 - Current activities on Department Analytical Chemistry, Reference Materials about optical isotopic spectrometry as a tool for aging studies of Li-ion batteries. T2 - Adlershofer Kolloquium - FB 1.6 CY - Online meeting DA - 18.05.2021 KW - High-resolution KW - Battery aging KW - Storage Technologies KW - Optical isotopic spectrometry KW - Lithium-ion batteries KW - Inorganic Reference Materials KW - Pouch cell KW - Anode KW - Cathode KW - Electrochemistry KW - Isotope PY - 2021 AN - OPUS4-53712 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schmidt, Anita T1 - Safety in transport of Li-ion batteries N2 - Safety in transport is the pre-requisite for bringing Lithium-ion batteries on the market. In order to consider the different types and degree of hazards, UN has set out to define a new classification system based on testing. BAM has participated in the test rounds and presents here the results. T2 - Technical Workshop on Advanced Materials Challenges and Standardisation Needs for Net Zero Technologies (AMCSNZT-2023) CY - New Delhi, India DA - 09.10.2023 KW - Lithium-ion batteries KW - Propagation testing KW - Safety PY - 2023 AN - OPUS4-59274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Böttcher, Nils A1 - Dayani, Shahabeddin A1 - Markötter, Henning A1 - Bau, Alexander A1 - Setzchen, Max A1 - Schmidt, Anita A1 - Kowal, Julia A1 - Krug von Nidda, Jonas T1 - High Precision Nail‐Penetration Setup for the Controlled Thermal Runaway Initiation of Lithium‐Ion Cells at Very Low Temperatures N2 - A high precision nail‐penetration (NP) tool for characterizing the mechanically induced thermal‐runaway (TR) of lithium‐ion battery (LIB) cells in a defined range of temperatures down to −140 °C was developed. To understand the cell specific behavior at low temperatures aiming at the determination of safe handling conditions, different scenarios are analyzed. First, accuracy tests of the NP‐tool regarding motion and penetration depth are conducted with cylindrical cells at different temperatures. Thus, postmortem computer tomographic (CT) images are compared to the data measured with the newly integrated 3‐axis force sensor which is further combined with a high‐resolution position sensor. The herein developed setup allows evaluation of the NP‐metrics at an accuracy of ±1 pierced electrode layer without CT‐scans. Further NP examinations at 20 °C of fully charged cylindrical lithium nickel manganese cobalt oxide cells reveal a reproducible minimum damage as a reliable TR‐trigger. Moreover, NP‐tests at low temperature disclose a relation of the short circuit conductivity and TR‐reactions during subsequent rethermalization to room temperature. Finally, the implementation of a novel fixture for a controlled very fast cooling of LIB‐cells during critical damage opens the way to investigate the individual steps during a TR and, thus, to gain important information of the specific TR‐mechanism of different LIB‐cells. KW - Battery Safety KW - High-precision nail penetration KW - Lithium-ion batteries KW - Abuse testing KW - Thermal runaway PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-598127 DO - https://doi.org/10.1002/ente.202301379 SN - 2194-4288 SP - 1 EP - 13 PB - Wiley VHC-Verlag AN - OPUS4-59812 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane T1 - Transformation of fluorinated electrolytes from lithium-ion batteries N2 - Lithium-ion battery (LiB) operation remains challenging, particularly in terms of safety, cycling stability, capacity rates and high-voltage applications. Although the electrolytes of LiBs account for 10-15% of the total battery weight, they are still an underestimated part. Data suggest that the composition of electrolytes offers great potential to deal with all these issues. In particular, fluorinated electrolyte solvents or even fluorinated additives offer several advantages due to the strength of the C-F bond, providing chemical and oxidative stability and increased electronegativity, exhibiting flame retardant properties and facilitating anode-mediated degradation, resulting in a LiF-rich and more stable solid electrolyte interphase (SEI), enabling more efficient surface passivation. Therefore, studies suggest that fluorinated equivalents, as well as entirely new compounds, are promising for solving battery-related problems. But what happens to fluorinated organic compounds (FOCs) during usage? And what are the new potential risks associated with their release into the environment? The environmental and application-specific fate of FOCs is investigated by a selection of different fluorinated electrolytes, the application of various simulation methods, including the TOP (Total Oxidizable Precursor) Assay, electrochemistry, photo-induced degradation, and cycling of FOC-prepared self-assembled coin cells. Gas chromatography and liquid chromatography coupled with high resolution mass spectrometry (GC/LC-HRMS) are used to identify transformation products (TP). T2 - Tag der Chemie 2023 CY - Berlin, Germany DA - 05.07.2023 KW - Transformation products KW - Lithium-ion batteries KW - PFAS KW - TP KW - Batteries PY - 2023 AN - OPUS4-58265 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane T1 - Fluorinated Additives used in LiBs: Forever Chemicals of Tomorrow? N2 - Fluorinated organic compounds (FOCs) are a type of man-made chemicals characterized by their robust carbon-fluorine bonds, which contribute to their chemical stability and resistance to degradation. This durability makes them valuable in various applications, such as lithium-ion batteries (LiBs) [1-3], could have a significant impact on the environment, but this potential has not yet been fully considered. This study examines the environmental impact of two fluorinated aromatics, tris(pentafluorophenyl)borane (TPFPB) and tris(pentafluorophenyl)phosphine (TPFPP), given their role in enhancing the performance of LiBs[4, 5]. In order to achieve this, a number of laboratory simulation methods were employed, including total oxidizable precursor assay, electrochemistry (EC), Fenton reaction, UV-C irradiation, and hydrolysis. Liquid chromatography and gas chromatography coupled with high-resolution mass spectrometry were employed for the identification of transformation products (TPs) and the prediction of their molecular formulae. Notwithstanding their structural similarities, TPFPB and TPFPP exhibited distinct differences in their electrochemical behavior and degradation pathways. TPFPB was readily transformed via hydroxylation and hydrolysis, resulting in a diverse range of 49 TPs. In total, 28 TPs were newly identified, including oligomers and highly toxic dioxins. In contrast, TPFPP degraded only under extreme conditions, highlighting the need to develop new conditioning protocols for EC. Overall, the simulation experiments produced 9 structurally unique compounds, including 7 previously unidentified partially defluorinated byproducts. This study emphasizes the potential hazards linked to the use of FOCs in lithium-ion batteries and enhances our understanding of the complex environmental interactions of these compounds. T2 - Adlershofer Forschungsforum 2024 CY - Berlin, Germany DA - 11.11.2024 KW - PFAS KW - Lithium-ion batteries KW - Fluorinated Compounds KW - Simulation methods KW - Liquid chromatography/ QTOF-MS KW - Gas chromatography/ QTOF-MS KW - Electrochemistry KW - Photochemistry KW - Top-Assay PY - 2024 AN - OPUS4-61681 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane T1 - Fate of fluorinated electrolytes used in lithium-ion batteries N2 - The use of per- and polyfluorinated alkyl substances (PFAS), which are very persistent and cannot be completely degraded in the environment, is a well-known problem worldwide. In contrast, fluorinated organic compounds used as electrolytes in lithium-based batteries (LiBs) have been less studied. Despite their increasing use in LiBs due to beneficial properties, such as improving safety, cycling performance, or even enabling high-voltage applications, there is little data on their distribution, transformation, and fate in the environment. To fill this gap, fluorine-containing electrolyte components are studied in oxidative and reductive transformation processes. The identified transformation products (TP) will be determined in relevant environmental matrices and LiBs. T2 - ANAKON 2023 CY - Vienna, Austria DA - 11.04.2023 KW - Transformation products KW - Lithium-ion batteries KW - PFAS KW - TP KW - Batteries PY - 2023 AN - OPUS4-57502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane T1 - Degradation and Impact of Fluorinated electrolytes from Lithium-Ion Batteries N2 - Lithium-based batteries (LiBs) have become increasingly important in modern society, as cutting-edge portable energy storage systems and as a crucial component in the energy revolution. However, they still face challenges such as safety concerns, capacity degradation, and the ever-growing demand for higher energy density. To address these issues, researchers have turned their attention to fluorinated organic compounds (FOCs) as part of LiBs electrolytes. These substances, closely related to per- and polyfluorinated alkyl substances (PFAS), have shown great potential in optimizing LiBs. Specifically, their strong fluorine-carbon bond offers enhanced oxidative and chemical resistance. Nevertheless, their environmental impact is a cause for concern. Fluorinated organics can persist in the environment or can lead to the formation of persistent end-products, which accumulate and contribute to global health problems. To study the fate of fluorinated organic electrolytes in different environmental and application scenarios, a range of simulation methods are employed, including the TOP (Total Oxidizable Precursor) Assay, electrochemistry, photo-induced degradation, and cycling of self-assembled coin cells prepared with FOCs. Transformation products (TP) are identified using gas chromatography and liquid chromatography coupled with high resolution mass spectrometry (GC/LC-HRMS). T2 - 23. Norddeutsches Doktorandenkolloquium CY - Berlin, Germany DA - 05.10.2023 KW - Transformation products KW - Lithium-ion batteries KW - PFAS KW - TP KW - Batteries KW - Electrolytes PY - 2023 AN - OPUS4-58511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Scholl, Juliane T1 - Fluorinated Additives used in LiBs - Forever Chemicals of Tomorrow? N2 - Lithium-ion batteries (LiBs) are increasingly crucial in modern society, serving as advanced portable energy storage systems and playing a vital role in the energy revolution. Despite their importance, challenges such as safety risks, capacity decline, and the need for higher energy density persist. Researchers are exploring the use of fluorinated organic compounds (FOCs) in LiBs electrolytes as a potential solution [1-3]. These compounds, similar to per- and polyfluorinated alkyl substances (PFAS), offer improved oxidative and chemical resistance due to their strong fluorine-carbon bond. However, concerns over their environmental impact remain, as FOCs could persist in the environment or create harmful degradation products, which accumulate and contribute to global health problems. To investigate the environmental fate of two structurally similar and prominent FOCs found in electrolytes, various methods are used to simulate transformation products (TPs). These methods include the TOP (total oxidizable precursor) assay, the Fenton reaction, electrochemistry, photoinduced degradation, and hydrolysis. TPs are identified using gas chromatography and liquid chromatography coupled with high resolution mass spectrometry (GC- and LC-HRMS). First results of this TP screening will be presented. T2 - ISC 2024 CY - Liverpool, GB DA - 06.10.2024 KW - Transformation products KW - Lithium-ion batteries KW - Fluorinated Compounds KW - Gas chromatography/ QTOF-MS KW - Liquid chromatography/ QTOF-MS KW - PFAS PY - 2024 AN - OPUS4-61341 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Winckelmann, Alexander T1 - Investigation of degradation of the aluminum current collector in lithium-ion batteries by glow-discharge optical emission spectroscopy N2 - Lithium-ion batteries (LIBs) are one technology to overcome the challenges of climate and energy crisis. They are widely used in electric vehicles, consumer electronics, or as storage for renewable energy sources. However, despite innovations in batteries' components like cathode and anode materials, separators, and electrolytes, the aging mechanism related to metallic aluminum current collector degradation causes a significant drop in their performance and prevents the durable use of LIBs.[1] Glow-discharge optical emission spectroscopy (GD-OES) is a powerful method for depth-profiling of batteries' electrode materials. This work investigates aging-induced aluminum deposition on commercial lithium cobalt oxide (LCO) batteries' cathodes. The results illustrate the depth-resolved elemental distribution from the cathode surface to the current collector. An accumulation of aluminum is found on the cathode surface by GD-OES, consistent with results from energy-dispersive X-ray spectroscopy (EDX) combined with focused ion beam (FIB) cutting. In comparison to FIB-EDX, GD-OES allows a fast and manageable depth-profiling. Results from different positions on an aged cathode indicate an inhomogeneous aluminum film growth on the surface. The conclusions from these experiments can lead to a better understanding of the degradation of the aluminum current collector, thus leading to higher lifetimes of LIBs. T2 - European Winter Conference on Plasma Spectrochemistry (EWCPS 2023) CY - Ljubljana, Slovenia DA - 29.01.2023 KW - Lithium-ion batteries KW - Aging mechanisms KW - Depth-profiling PY - 2023 AN - OPUS4-56992 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Böttcher, Nils T1 - Nominal and Off-Nominal Battery / High Energy Storage Testing Off-Nominal cell and battery testing at BAM N2 - The abuse testing of electrochemical energy storage systems poses a major safety challenge. Thanks to its core competence in ensuring safety in technology and chemistry, BAM has the capabilities to carry out safety tests from small to large scale. Tests up to approx. 200Wh (lithium-ion batteries) can be carried out in the cell test center and abuse tests up to 20kWh are possible in the open field test on the TTS. T2 - Europe Energy Storage Safety Summit CY - Petten, Netherlands DA - 08.10.2024 KW - Battery Safety KW - Abuse testing KW - Lithium-ion batteries KW - Safety critical tests PY - 2024 AN - OPUS4-62321 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Morcillo, Dalia A1 - Oelze, Marcus A1 - Seena Prem, Pranav A1 - de Oliveira Guilherme Buzanich, Ana A1 - Emmerling, Franziska A1 - Recknagel, Sebastian A1 - Panne, Ulrich A1 - Abad Andrade, Carlos Enrique T1 - Lithium isotope fractionation as an early indicator of degradation mechanisms in lithium-ion batteries N2 - Aging in lithium-ion batteries (LIBs) degrades performance and hinders sustainability, demanding advanced diagnostics for early failure prediction. We investigate lithium isotope fractionation (LIF) as an innovative probe of degradation in lithium cobalt oxide (LCO) coin cells aged over 0−700 cycles. High-precision multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) quantified δ7Li variations across cell stages: non-cycled (0 cycles), newly formed (5 cycles), semi-aged (250 cycles), and fully aged (700 cycles). During early cycling (≤ 45 cycles), chemical processes drive 7Li enrichment at the anode (δ7Li vs LSVEC = +12 ‰) through solid electrolyte interphase (SEI) formation, while the cathode depletes in 7Li (δ7Li vs LSVEC = −0.7 ‰). Beyond 45 cycles, electric field-induced migration predominates, promoting 6Li intercalation into the anode and increasing the δ7Li of the cathode by 8.1 ‰. Mass balance verifies isotope conservation, attributing shifts to redistribution and trapping. Complementary electrochemical impedance spectroscopy (EIS) and X-ray absorption spectroscopy and diffraction confirm SEI expansion, cobalt oxidation, lattice shrinkage, and changes in electrode structure, corroborating LIF trends. Notably, a δ7Li inflection at approximately 270 cycles anticipates end-of-life by 70 cycles, surpassing traditional methods in sensitivity. LIF emerges as a predictive indicator of aging mechanisms, informing optimized designs for durable LIBs. KW - Lithium isotope fractionation KW - Lithium-ion batteries KW - Degradation mechanisms KW - LiCoO2 cathodes KW - LCO KW - Isotopic tracing KW - Lithium isotopes PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-650945 DO - https://doi.org/10.26434/chemrxiv-2025-16lvq SP - 1 EP - 19 AN - OPUS4-65094 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholl, Juliane A1 - Scharpmann, Philippa A1 - Bagheri, Abbas A1 - Lisec, Jan A1 - Meiers, Emelie A1 - Jaeger, Carsten A1 - Leonhardt, Robert A1 - Haase, Hajo A1 - Koch, Matthias T1 - Beyond the lab: Real-world composition of commercial Li-ion battery electrolytes N2 - This study presents a systematic, characterization of electrolytes from commercial lithium-ion batteries (LIB), encompassing 90 batteries from leading global manufacturers across diverse formats and application sectors. An integrated, complementary mass spectrometric workflow combining LC–MS/MS, GC–MS, and high-resolution MS was employed. To ensure robust structural annotation, molecular identifications were assigned confidence levels following Schymanski et al. (2014). Across all formats, PF6− was confirmed as the dominant Li+ counterion, frequently coexisting with BF4−, PO2F2−, and bis(fluorosulfonyl)imide (FSI−), forming binary and ternary salt systems optimized for both conductivity and safety. Solvent systems revealed the widespread use of propylene carbonate (PC) combined with diverse carbonate mixtures, demonstrating trends in performance optimization specific to cell format. A variety of additives were identified, reflecting a clear shift towards multifunctional, synergistic additive packages and the gradual replacement of fluorinated species with environmentally safer alternatives. Cycling studies demonstrated that electrolyte degradation mechanisms are strongly influenced by electrode composition and additive chemistry, with oxidative degradation pathways dominating. Together, these findings provide rare empirical insight into the evolving formulation strategies of electrolytes in commercial LIB, still employing classic carbonates and LiPF6, but highlighting a trend toward safer, more robust, and sustainable electrolyte architectures by using synergistic multifunctional systems. KW - Mass Spectrometry KW - Lithium-ion batteries KW - Electrolyte degradation PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656254 DO - https://doi.org/10.1016/j.jpowsour.2026.239739 SN - 0378-7753 VL - 673 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-65625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -