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Li-insertion into V6O13 battery cathodes studied by soft X-ray spectroscopies
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics, Physics II.
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics.
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics.
Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics, Physics II.
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2004 (English)In: Journal of Applied Physics, ISSN 0021-8979, E-ISSN 1089-7550, Vol. 95, 6444- p.Article in journal (Refereed) Published
Abstract [en]

Changes in the electronic structure of V6O13 on lithium-ion insertion into battery cathodes were studied by soft x-ray absorption (SXA) spectroscopy and resonant soft x-ray emission (SXE) spectroscopy. SXA and resonant SXE spectra were recorded ex situ for cycled battery cathodes discharged to different potentials corresponding closely to distinct lithiated stages (LixV6O13,x=0,1,…,6). Large systematic changes were observed in the vanadium and oxygen x-ray spectra, reflecting the effects of electrochemical reduction associated with the Li-ion insertion. Spectral shape analysis indicates that a large fraction of the vanadium ions have been reduced to V3+ ions for the highest degree of lithiation,x=6. Nevertheless, further lithiation may be possible, in view of the linear development of the vanadium and oxygen bands on charge uptake. 

Place, publisher, year, edition, pages
2004. Vol. 95, 6444- p.
National Category
Physical Sciences
Identifiers
URN: urn:nbn:se:uu:diva-91457DOI: 10.1063/1.1713041OAI: oai:DiVA.org:uu-91457DiVA: diva2:164192
Available from: 2004-03-05 Created: 2004-03-05 Last updated: 2017-12-14Bibliographically approved
In thesis
1. The Challenge of Probing Lithium Insertion Mechanisms in Cathode Materials
Open this publication in new window or tab >>The Challenge of Probing Lithium Insertion Mechanisms in Cathode Materials
2004 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The Li-ion battery has, from its commercialisation in the early 1990's, now become the most widely used power source for portable low-power electronics: laptops, cellular phones and MP3-players are a few examples. To further develop existing and find new electrode materials for these batteries, it is vital to understand the lithium insertion/extraction mechanisms taking place during battery operation. In this thesis, single-crystal X-ray diffraction has been used to investigate lithium insertion/extraction mechanisms in the cathode materials V6O13 and LiFePO4. A novel single-crystal electrochemical cell for in situ single-crystal X-ray diffraction studies has also been developed.

The phases Li3V6O13 and Li3+xV6O13, 0<x<1, both contain a disordered lithium ion. A low-temperature study of Li3.24V6O13 (at 95 K) shows that this disorder is static rather than dynamic; the lithium ion is equally distributed above and below an inversion centre in the centrosymmetric V6O13 host structure. Short-range-ordering between this disordered lithium ion and the lithium ion inserted into Li3V6O13 gives rise to solid-solution behaviour not observed earlier in the LixV6O13 system. A model is proposed for the lithium insertion mechanism up to the end-member composition Li6V6O13.

Lithium has also been electrochemically extracted from LiFePO4 single crystals. On the basis of the shapes of the LiFePO4 and FePO4 reflections, it is concluded that FePO4 is formed at the crystal surface and that the LiFePO4/FePO4 interface propagates into the crystal. This is in agreement with an earlier proposed model for lithium extraction from LiFePO4 particles.

Initial experiments with the newly developed single-crystal electrochemical cell for in situ single-crystal X-ray diffraction demonstrate that it is possible to insert lithium into a single crystal of V6O13 and then collect single-crystal X-ray diffraction data. The method needs further development but promises to become a powerful tool for studying lithium insertion/extraction mechanisms.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2004. 58 p.
Series
Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1104-232X ; 949
Keyword
Inorganic chemistry, Li-ion battery, cathode materials, insertion mechanism, single-crystal X-ray diffraction, vanadium oxide, lithium iron phosphate, Oorganisk kemi
National Category
Inorganic Chemistry
Identifiers
urn:nbn:se:uu:diva-4055 (URN)91-554-5895-5 (ISBN)
Public defence
2004-03-26, Häggsalen, Ångström Laboratory, Lägerhyddsvägen 1, Uppsala, 10:15
Opponent
Supervisors
Available from: 2004-03-05 Created: 2004-03-05Bibliographically approved

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