Analytische Chemie
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Im Rahmen der von der BAM und anderen Partnern ins Leben gerufenen Initiative „Digitale Qualitätsinfrastruktur“ liegt der Fokus u.a. auf der Entwicklung von neuen Zertifizierungsworkflows. Dabei ist eine besondere Bedeutung dem Zusammenführen von Operational Technology (OT) und Informationstechnik (IT) beizumessen. Zur Datenintegration aus der Sensor-Feldebene einer Versuchs-wasserstofftankstelle wurde eine solche Infrastruktur zunächst in einer Laborumgebung aufgebaut.
Introduction
Lithium-ion batteries (LIBs) are one key technology to overcome the climate crisis and energy transition challenges. Demands of electric vehicles on higher capacity and power drives research on innovative cathode and anode materials. These high energy-density LIBs are operated at higher voltages, leading to increased electrolyte decay and the current collectors' degradation. Even though this fundamental corrosion process significantly affects battery performance, insufficient research is being done on the aluminum current collector. Fast and convenient analytical methods are needed for monitoring the aging processes in LIBs.
Methods
In this work glow-discharge optical emission spectrometry (GD-OES) was used for depth profile analysis of aged cathode material. The measurements were performed in pulsed radio frequency mode. Under soft and controlled plasma conditions, high-resolution local determination (in depth) of the elemental composition is possible. Scanning electron microscopy (SEM) combined with a focused ion beam (FIB) cutting and energy dispersive X-ray spectroscopy (EDX) was used to confirm GD-OES results and obtain additional information on elemental distribution.
Results
The aging of coin cells manufactured with different cathode materials (LCO, LMO, NMC111, NMC424, NMC532, NMC622, and NMC811) was studied. GD-OES depth profiling of new and aged cathode materials was performed. Quantitative analysis was possible through calibration with synthetic standards and correction by sputter rate. Different amounts of aluminum deposit on the cathode surface were found for different materials. The deposit has its origin in the corrosion of the aluminum current collector. The results are compatible with results from FIB-EDX. However, GD-OES is a faster and less laborious analytical method. Therefore, it will accelerate research on corrosion processes in high energy-density batteries.
Innovative aspects
- Quantitative depth profiling of cathode material
-Monitoring of corrosion processes in high energy-density lithium-ion batteries
- Systematic investigation of the influence of different cathode materials
Um die internationale Spitzenposition deutscher Unternehmen der Prozessindustrie auch in Zukunft sicher zu stellen, müssen die Unternehmen ihre Prozesse und Geschäftsabläufe digitalisieren und gemeinsam mit der Forschung innovative neue Methoden, Apparate, Anlagen, Sensoren und Automatisierungstechnik sowie Datenkonzepte entwickeln. All dies erfordert den Aufbau neuer Fähigkeiten, Investition in Talente, interdisziplinäre Kommunikation zwischen verschiedenen Personen und Abteilungen und eine Bereitschaft zur Veränderung.
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
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.
Der Beitrag beinhaltet Themen vom H2Safety@BAM-Kompetenzfeld Sensorik, Analytik und zertifizierte Referenzmaterialien (SensRef) mit Fokus auf Mess- und Prüfverfahren mit verschiedenen Sensortechnologien und Ultraschallwellen:
Metrologie zur Wasserstoffspeicherung - Euramet-Vorhaben "MefHySto",
Erkennung von freigesetztem Wasserstoff sowie die Bestimmung des Wasserstoff-Luftverhälntisses mit Gassensoren, zerstörungsfreie Fehlstellenerkennung mit integriertem Zustandsüberwachungssystem basierend auf geführten Ultraschallwellen zur Lebensdauerüberwachung von Composite-Behältern (Wasserstoffspeicher) sowie faseroptische Sensorik zur Schadenfrüherkennung von Wasserstoffspeichern aufgrund erkennbarer Dehnungsänderungen an Druckbehältern.
Investigation of degradation of the aluminum current collector in lithium-ion batteries by GD-OES
(2022)
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. 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.
High-resolution absorption isotopic spectrometry as a tool for aging studies of Li-ion batteries
(2022)
Lithium (Li) is the key element in the manufacturing of batteries. Isotopic study of Li may help to identify the causes of battery aging due to isotopic fractionation during charge/discharge cycles.
Isotopic ratio determination is based on monitoring the isotopic components of lithium by their spin-orbit coupling and its isotopic shift of about 15 pm for the 22P←22S electronic transition around 670.788 nm. In this work, we propose improvements to our previous work [1] by using a higher-resolution double echelle modular spectrometer (HR-DEMON II) coupled to a continuum source graphite furnace atomic absorption spectrometer (HR-CS-GF-AAS) for the isotopic analysis of Li.
The data analysis was carried out by using a decision-tree-based ensemble machine learning (ML) algorithm (XGBoost). A set of samples with 6Li isotope amount fractions ranging from 0.0004 to 0.99 mol mol-1 was used for the algorithm's training. Subsequently, the procedure was validated by a set of stock chemicals (Li2CO3, LiNO3, LiCl, and LiOH) and a BAM candidate reference material, a cathode material (NMC111). Finally, the ML model was applied to determine the isotope ratio of geological samples, including anorthosite, granite, soil, rhyolite, nepheline syenite, and basalt and battery samples. These samples were measured as digested without any further purification step.
Improvements in the optical resolution resolve the lithium isotopic components of the atomic spectra. In the studied geological samples, were found δ7Li values between -0.5 and 4.5 ‰ with a precision range of 1 to 2 ‰. In addition, the proposed method was validated with multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS), and these results are comparable and compatible.
Im Rahmen von der BAM und anderen Partnern ins Leben gerufene Initiative „Digitale Qualitätsinfrastruktur“ ist der Fokus auf die Entwicklung von neuen Regelwerken und Zertifizierungsworkflows ausgerichtet. Dabei ist eine besondere Bedeutung dem Zusammenführen von Operational Technology (OT) und Informationstechnik (IT) beizumessen, wenn aktuelle Prozess- und Parameterdaten
zuverlässig zur Verfügung gestellt werden sollen. In dem Use Case Wasserstofftankstelle werden digitale Abbilder erprobt, die u.a. der Kalibrierung von Sensoren, dem Nachweis über die Wasserstoffreinheit und der vorausschauenden Wartung dienen sollen.
Großenteils der verfahrenstechnischen Bestandsanlagen, die sogenannten Brownfield-Anlagen, sind nach einem konservativen und hierarchischen Automatisierungskonzept ausgelegt. Hierbei können sämtliche Prozessdaten,
besonders aus der Feldebene, einer oberen informationstechnische Ebene
unzugänglich bleiben. Eine Brückentechnologie nach der NAMUR Open Architecture (NOA) soll möglichst viele Informationen und Daten aus der vorgegebenen Brownfield-Automatisierung sicher und rückwirkungsfrei zur
Verfügung stellen. Zusätzliche Sensorik soll ebenso zu der Datenerweiterung beitragen und letztendlich den digitalen Zwilling, bzw. das digitale Abbild des verfahrenstechnischen Prozesses, ergänzen.
Die Herausforderungen einer solchen Infrastruktur gelten vor allem einer universellen
Kommunikationsschnittstelle und der Sicherheit. Darüber hinaus werden vorgeschlagene Normen und Empfehlungen untersucht und erprobt.