In Situ Characterization of Electrode Materials for Lithium-Ion Batteries by Raman and IR Microscopy Author(s): Publication Date: Permanent Link:
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1 Research Collection Doctoral Thesis In Situ Characterization of Electrode Materials for Lithium-Ion Batteries by Raman and IR Microscopy Author(s): Lanz, Patrick Publication Date: 2014 Permanent Link: Rights / License: In Copyright - Non-Commercial Use Permitted This page was generated automatically upon download from the ETH Zurich Research Collection. For more information please consult the Terms of use. ETH Library
2 DISS. ETH NO IN SITU CHARACTERIZATION OF ELECTRODE MATERIALS FOR LITHIUM-ION BATTERIES BY RAMAN AND IR MICROSCOPY A thesis submitted to attain the degree of DOCTOR OF SCIENCES of ETH ZURICH (Dr. sc. ETH Zurich) presented by PATRICK LANZ MSc ETH Chemistry, ETH Zurich born on 23 November 1985 citizen of Walterswil BE accepted on the recommendation of Prof. Dr. P. Novák Prof. Dr. M. Kovalenko 2014
3 IX Abstract Although lithium-ion batteries currently dominate the market for rechargeable batteries, improvements in terms of energy density, cycling stability and safety are required. Many improvements may result from a deeper understanding of the surface reactions in lithium-ion batteries. In situ methods are particularly attractive since they allow the direct characterization of such processes during electrochemical cycling. Furthermore, the investigation of vibrational modes by Raman and IR microscopy provides information about structural and chemical changes, respectively, on a chosen spot of the working electrode. In a novel combined in situ approach, the complementary nature of Raman and IR microscopy is exploited in order to simultaneously investigate structural changes in the electrode materials and chemical reactions at the interfaces of the electrodes with the organic electrolyte. In preliminary experiments it was demonstrated that stainless steel mesh is an excellent current collector for spectroscopic experiments under oxidative and reductive conditions, that manganese dissolves from high-energy nickel cobalt manganese oxide (HE-NCM) and deposits onto the graphite counter electrode during electrochemical cycling (X-ray photoelectron spectroscopy, XPS), that lithium intercalation and graphite exfoliation can be detected by the selected in situ Raman method and that the IR reflectivity of polished single graphite particles is comparable to glassy carbon (GC) discs. At the positive electrode, ageing of HE-NCM in a humid atmosphere was demonstrated to lead to the formation of a Li 2 CO 3 surface film responsible for a deterioration in electrochemical performance. Ex situ Raman investigations of nickel cobalt manganese oxides (NCM) showed that the Raman spectrum of HE-NCM is a superposition of stoichiometric NCM and Li 2 MnO 3, and that the Li 2 MnO 3 disappears after the first cycle, demonstrating its irreversible electrochemical activation and confirming the domain model. A new band at ~545 cm -1 observed during in situ Raman experiments, which was stable over a wider potential window in HE-NCM than in stoichiometric NCM, was explained by the formation of Li 2 O during electrochemical activation. Finally, in situ Raman investigations of Li 2 MnO 3 at 50 C provided evidence of electrochemical activation positive to 4.4 V vs. Li + /Li, in excellent agreement with the potential plateau typically observed during initial charging of Li 2 MnO 3 and HE-NCM. At the negative electrode, combined in situ Raman and IR microscopy was applied to the same spot on a GC electrode. Raman microscopy showed no significant lithium intercalation while IR microscopy demonstrated an increase in the concentration of free solvents and a decrease in the concentration of solvent molecules coordinated to lithium ions. Subsequently, the combined method was also applied to the same spot on a graphite electrode. Raman microscopy showed clear evidence of lithium intercalation negative to 0.4 V vs. Li + /Li and allowed the determination of the true local degree of lithium intercalation at the investigated spot despite the slow kinetics of the large, polished single graphite particle. IR microscopy demonstrated a decrease in the concentration of free solvents and solvent molecules coordinated to lithium ions during charge and an increase in both species during discharge. The decrease in the concentration of solvents and new IR signals at 1.0/0.7 V vs. Li + /Li during charge were explained by solid electrolyte interphase (SEI) formation. Finally, a jump in absorbance at 0.7/0.4 V vs. Li + /Li was attributed to lithium intercalation.
4 XI Zusammenfassung Obwohl Lithiumionen-Batterien zurzeit den Markt für wiederaufladbare Batterien dominieren, sind Verbesserungen hinsichtlich der Energiedichte, Zyklenfestigkeit und Sicherheit nötig. Viele Verbesserungen können aus einem vertieften Verständnis der Oberflächenreaktionen in Lithiumionen-Batterien resultieren. In situ Methoden sind besonders geeignet, da sie die direkte Charakterisierung solcher Prozesse während des elektrochemischen Zyklisierens erlauben. Desweitern liefert die Untersuchung von Schwingungsmoden mittels Raman- und IR-Mikroskopie Informationen über die strukturellen beziehungsweise chemischen Veränderungen an einem ausgewählten Punkt der Arbeitselektrode. In einem neuen kombinierten in situ Ansatz wird die Komplementarität von Raman- und IR-Mikroskopie genutzt um gleichzeitig die strukturellen Veränderungen in den Elektrodenmaterialien und die chemischen Reaktionen an den Grenzflächen der Elektroden mit dem organischen Elektrolyten zu untersuchen. In Vorversuchen wurde demonstriert, dass Edelstahlnetz ein hervorragender Stromsammler für spektroskopische Experimente unter oxidativen und reduktiven Bedingungen ist, dass sich Mangan während des elektrochemischen Zyklisierens aus Hoch-Energie-Nickel-Cobalt-Mangan-Oxid (HE-NCM) herauslöst und auf der Graphitgegenelektrode ablagert (Röntgenphotoelektronenspektroskopie, XPS), dass Lithiuminterkalation und Graphitexfoliation mittels der gewählten in situ Raman-Methode detektiert werden können und dass die IR-Reflektivität polierter einzelner Graphitpartikel vergleichbar mit Glaskohlenstoffscheiben (GC) ist. An der positiven Elektrode wurde demonstriert, dass die Alterung von HE-NCM in feuchter Atmosphäre zur Bildung eines Oberflächenfilms aus Li 2 CO 3 führt, der verantwortlich für eine verschlechterte elektrochemische Leistungsfähigkeit ist. Ex situ Raman-Untersuchungen von Nickel-Cobalt- Mangan-Oxid (NCM) zeigten, dass das Raman-Spektrum von HE-NCM eine Überlagerung von stöchiometrischem NCM und Li 2 MnO 3 ist, und dass das Li 2 MnO 3 nach dem ersten Zyklus verschwindet, was dessen irreversible elektrochemische Aktivierung demonstriert und das Domänenmodell bestätigt. Eine während der in situ Raman-Experimente beobachtete neue Bande bei ~545 cm -1, die in HE-NCM über ein breiteres Potentialfenster stabil war als in stöchiometrischem NCM, wurde durch die Bildung von Li 2 O während der elektrochemischen Aktivierung erklärt. Schließlich wiesen in situ Raman-Untersuchungen von Li 2 MnO 3 bei 50 C elektrochemische Aktivierung positiv zu 4.4 V vs. Li + /Li nach, im Einklang mit dem typischerweise beobachteten Potentialplateau während des ursprünglichen Ladens von Li 2 MnO 3 und HE-NCM. An der negativen Elektrode wurde kombinierte in situ Raman- und IR-Mikroskopie auf den gleichen Punkt einer GC-Elektrode angewandt. Raman-Mikroskopie zeigte keine signifikante Lithiuminterkalation, während IR-Mikroskopie eine Zunahme der Konzentration freier Lösungsmittel und eine Abnahme der Konzentration an Lithiumionen koordinierter Lösungsmittelmoleküle demonstrierte. Nachfolgend wurde die kombinierte Methode ebenfalls auf den gleichen Punkt einer Graphitelektrode angewandt. Raman-Mikroskopie wies klare Lithiuminterkalation negativ zu 0.4 V vs. Li + /Li nach und erlaubte die Bestimmung des tatsächlichen lokalen Grades der Lithiuminterkalation am untersuchten Punkt, trotz der langsamen Kinetik des großen, polierten einzelnen Graphitpartikels. IR-Mikroskopie demonstrierte eine Abnahme der Konzentration freier und an Lithium koordinierter Lösungsmittelmoleküle während des Ladens und eine Zunahme beider Spezies während des Entladens. Die Abnahme der Konzentration der Lösungsmittel und neue IR-Signale bei 1.0/0.7 V vs. Li + /Li während des Ladens wurden durch die Bildung von Solid Electrolyte Interphase
5 XII (SEI) erklärt. Schließlich wurde ein Sprung in der Absorbanz bei 0.7/0.4 V vs. Li + /Li der Lithiuminterkalation zugeordnet.
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