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Consequences of Air Exposure on the Lithiated Graphite SEI
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Molecular and condensed matter physics.
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Molecular and condensed matter physics.
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2013 (English)In: Electrochimica Acta, ISSN 0013-4686, E-ISSN 1873-3859, Vol. 105, 83-91 p.Article in journal (Refereed) Published
Abstract [en]

In the present work, consequences of air exposure on the surface composition of one of the most reactive lithium-ion battery components, the lithiated graphite, was investigated using 280–835 eV soft X-ray photoelectron spectroscopy (SOXPES) as well as 1486.7 eV X-ray photoelectron spectroscopy (XPS) (∼2 and ∼10 nm probing depth, respectively). Different depth regions of the solid electrolyte interphase (SEI) of graphite cycled vs. LiFePO4 were thereby examined. Furthermore, the air sensitivity of samples subject to four different combinations of pre-treatments (washed/unwashed and exposed to air before or after vacuum treatment) was explored. The samples showed important changes after exposure to air, which were found to be largely dependent on sample pre-treatment. Changes after exposure of unwashed samples exposed before vacuum treatment were attributed to reactions involving volatile species. On washed, air exposed samples, as well as unwashed samples exposed after vacuum treatment, effects attributed to lithium hydroxide formation in the innermost SEI were observed and suggested to be associated with partial delithiation of the surface region of the lithiated graphite electrode. Moreover, effects that can be attributed to LiPF6 decomposition were observed. However, these effects were less pronounced than those attributed to reactions involving solvent species and the lithiated graphite.

Place, publisher, year, edition, pages
Elsevier, 2013. Vol. 105, 83-91 p.
National Category
Materials Chemistry
Research subject
Chemistry with specialization in Materials Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-196470DOI: 10.1016/j.electacta.2013.04.118OAI: oai:DiVA.org:uu-196470DiVA: diva2:610202
Available from: 2013-03-08 Created: 2013-03-08 Last updated: 2017-12-06
In thesis
1. Insights into Li-ion Battery and Stainless Steel Interfaces Using Refined Photoelectron Spectroscopy Methodology
Open this publication in new window or tab >>Insights into Li-ion Battery and Stainless Steel Interfaces Using Refined Photoelectron Spectroscopy Methodology
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

If sacrificing some of its material to form a passivating layer at the surface, materials may expand the range of environments where they can be used and further material degradation can decrease. This thesis aims to contribute with insights into passivating layers on especially Li-ion battery anodes (solid electrolyte interphase, SEI) but also on stainless steels, as well as the non-passivating Li-ion battery cathode/electrolyte interface layers (solid permeable interface, SPI). The studies have been performed using new possibilities offered by photoelectron spectroscopy techniques.

Depth gradients in the SEI and SPI layers were studied by combining synchrotron-based hard and soft X-ray photoelectron spectroscopy (HAXPES and SOXPES), which was further developed for Li-ion battery investigations. Stainless steel depth profiles were acquired combining HAXPES with angle resolved X-ray photoelectron spectroscopy (ARXPS).

In the Li-ion battery, organic species were more common in the outermost SEI, while some inorganic compounds were only detected in the more bulk sensitive measurements. No depth gradients were observed in the SPI. The interface between the graphite and the SEI was studied for the first time indicating lithium enrichment at the graphite surface. Furthermore, the influence of the film-forming additive propargyl methanesulphonate (PMS) on the electrode/electrolyte interfaces was studies, and cells cycled to end of life at 22°C and 55°C were compared.

For stainless steels, the thicknesses of the oxide film as well as the nickel enriched metal layer underneath the oxide were determined. A similar methodology was applied to estimate the Li-ion battery SEI thickness.

Finally, experiences from PES methodology work on the Li-ion battery systems are discussed aiming to facilitate further studies of the experimentally challenging electrochemically modified samples.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2013. 69 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1031
National Category
Materials Chemistry
Identifiers
urn:nbn:se:uu:diva-197153 (URN)978-91-554-8624-2 (ISBN)
Public defence
2013-05-03, Häggsalen, Ångströmslaboratoriet, Lägerhyddsvägen 1, Uppsala, 10:15 (English)
Opponent
Supervisors
Available from: 2013-04-12 Created: 2013-03-18 Last updated: 2013-08-30Bibliographically approved

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Malmgren, SaraCiosek, KatarzynaLindblad, RebeckaPlogmaker, StefanRensmo, HåkanEdström, KristinaHahlin, Maria

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