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Ion Insertion into Electrode Materials Studied with X-Ray and Electron Spectroscopic Methods
Uppsala University, Teknisk-naturvetenskapliga vetenskapsområdet, Physics, Department of Physics.
2002 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Ion insertion into electrode materials can be used to store energy in battery applications. In this thesis, photoelectron spectroscopic and x-ray absorption spectroscopic methods have been used to study the change of the electronic structure of host materials during electrochemical ion insertion.

Specifically, the properties of ion insertion into nanoporous TiO2 were studied. It is demonstrated that the insertion of Li ions results in a reduction of the Ti4+ sites in TiO2 to Ti3+ sites close to the inserted Li ion. The intensity of the Ti3+ is directly correlated to the number of inserted electrons. It is also shown that the two phases resulting from moderate insertion can be detected by studying the electronic structure of inserted Li ions and the behavior observed can be correlated with electrochemical measurements.

Insertion of ions into tungsten oxides is a potential candidate for smart window and display applications. Ion insertion into these materials was, also studied with electron spectroscopic methods. The insertion of H+ reduces W6+ to W5+ and further insertion results in a reduction to W4+. Cyclic voltammerty shows two reduction peaks where the first peak implies reduction of W6+ to W5+ and the second peak can be associated with further reduction to W4+.

During the first charge/discharge cycles of a battery based on graphite anodes a solid electrolyte interface layer is formed on the electrode surface. This layer consumes some of the charge carrying Li ions, hence decreases the capacity of the battery. A careful characterization of this layer has been performed to aid in the further development of this type of battery.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis , 2002. , p. 60
Series
Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1104-232X ; 698
Keywords [en]
Physics
Keywords [sv]
Fysik
National Category
Physical Sciences
Research subject
Physics
Identifiers
URN: urn:nbn:se:uu:diva-1885ISBN: 91-554-5268-X (print)OAI: oai:DiVA.org:uu-1885DiVA, id: diva2:161460
Public defence
2002-04-12, Häggsalen, Ångström Laboratory, Uppsala, 10:15
Opponent
Available from: 2002-03-21 Created: 2002-03-21Bibliographically approved
List of papers
1. TiO2 (anatase) and electrochemically Li-inserted TiO2 studied with photoelectron (PES, RPES)- and x-ray absorption (XAS) spectroscopy
Open this publication in new window or tab >>TiO2 (anatase) and electrochemically Li-inserted TiO2 studied with photoelectron (PES, RPES)- and x-ray absorption (XAS) spectroscopy
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In: Article in journal (Refereed) Submitted
Identifiers
urn:nbn:se:uu:diva-89728 (URN)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2016-04-20
2. Li insertion in thin film anatase TiO2: Identification of a two-phase regime with photoelectron spectroscopy
Open this publication in new window or tab >>Li insertion in thin film anatase TiO2: Identification of a two-phase regime with photoelectron spectroscopy
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Article in journal (Refereed) Submitted
Identifiers
urn:nbn:se:uu:diva-89729 (URN)
Available from: 2002-03-21 Created: 2002-03-21Bibliographically approved
3. Initial and final state effects in x-ray absorption spectra of transition metal oxides
Open this publication in new window or tab >>Initial and final state effects in x-ray absorption spectra of transition metal oxides
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(English)Article in journal (Refereed) Submitted
National Category
Natural Sciences
Identifiers
urn:nbn:se:uu:diva-89730 (URN)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2017-01-25Bibliographically approved
4. Electronic structure and x-ray absorption spectroscopy of TiO2 and Li0.5TiO2
Open this publication in new window or tab >>Electronic structure and x-ray absorption spectroscopy of TiO2 and Li0.5TiO2
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(English)Manuscript (Other academic)
National Category
Physical Sciences
Identifiers
urn:nbn:se:uu:diva-89731 (URN)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2017-01-25Bibliographically approved
5. Lithium ion insertion in nanoporous anatase TiO2 studied with RIXS
Open this publication in new window or tab >>Lithium ion insertion in nanoporous anatase TiO2 studied with RIXS
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Article in journal (Refereed) Submitted
Identifiers
urn:nbn:se:uu:diva-89732 (URN)
Available from: 2002-03-21 Created: 2002-03-21Bibliographically approved
6. Electrochemical insertion of Na and Li ions into nanoporous TiO2 studied by means of electron- and x-ray spectroscopic methods
Open this publication in new window or tab >>Electrochemical insertion of Na and Li ions into nanoporous TiO2 studied by means of electron- and x-ray spectroscopic methods
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In: Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-89733 (URN)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2016-04-20
7. Determination of the electronic density of states at a nanostructured TiO2/Ru-dye/electrolyte interface by means of photoelectron spectroscopy
Open this publication in new window or tab >>Determination of the electronic density of states at a nanostructured TiO2/Ru-dye/electrolyte interface by means of photoelectron spectroscopy
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2002 (English)In: Chemical Physics, ISSN 0301-0104, E-ISSN 1873-4421, Vol. 285, no 1, p. 157-165Article in journal (Refereed) Published
Abstract [en]

In this work, photoelectron spectroscopy is used to measure the electronic density of states in the band gap region of a nanostructured TiO2 film. Such nanostructured films are used in dye-sensitized solar cells, and in this study a plain TiO2 film as well as a dye-sensitized film were examined. Further, to simulate the electrolyte effect on the energy levels at the oxide/dye/electrolyte interface in a solar cell, the density of states in the band gap region for an electrochemically prepared TiO2 film inserted with Li+ ions was measured. From the experimental findings we discuss the distribution and chemical nature of electron trap states in the band gap and the energy matching between the LUMO level of the adsorbed dye, cis-bis(4,4-dicarboxy-2,2-bipyridine)-bis(isothiocyanato)ruthenium(II), and the TiO2 conduction band edge.

National Category
Natural Sciences
Identifiers
urn:nbn:se:uu:diva-89734 (URN)10.1016/S0301-0104(02)00699-7 (DOI)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2017-12-14Bibliographically approved
8. Proton insertion in polycrystalline WO3 studied with electron spectroscopy and semiempirical calculations
Open this publication in new window or tab >>Proton insertion in polycrystalline WO3 studied with electron spectroscopy and semiempirical calculations
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In: Article in journal (Refereed) Submitted
Identifiers
urn:nbn:se:uu:diva-89735 (URN)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2016-04-20
9. Redox properties of nanoporous TiO2 (anatase) surface modified with phosphotungstic acid
Open this publication in new window or tab >>Redox properties of nanoporous TiO2 (anatase) surface modified with phosphotungstic acid
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1998 In: Thin Solid Films, Vol. 323, p. 141-145Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-89736 (URN)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2016-04-20
10. Insertion of H+, Li+, Na+ and K+ into thin films of silicotungstic acid studied by means of photoelectron spectroscopy
Open this publication in new window or tab >>Insertion of H+, Li+, Na+ and K+ into thin films of silicotungstic acid studied by means of photoelectron spectroscopy
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Manuscript (Other academic)
Identifiers
urn:nbn:se:uu:diva-89737 (URN)
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2016-04-20Bibliographically approved
11. Electrochemically lithiated graphite characterised by photoelectron spectroscopy
Open this publication in new window or tab >>Electrochemically lithiated graphite characterised by photoelectron spectroscopy
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2003 (English)In: Journal of Power Sources, ISSN 0378-7753, E-ISSN 1873-2755, Vol. 119-121, p. 522-527Article in journal, Meeting abstract (Refereed) Published
Abstract [en]

X-ray photoelectron spectroscopy (XPS) has been used to study the depth profile of the solid–electrolyte interphase (SEI) formed on a graphite powder electrode in a Li-ion battery. The morphology of the SEI-layer, formed in a 1 M LiBF4 EC/DMC 2:1 solution, consists of a 900 Å porous layer of polymers (polyethylene oxide) and a 15–20 Å thin layer of Li2CO3 and LiBF4 reduction–decomposition products. Embedded LiF crystals as large as 0.2 μm were found in the polymer matrix. LiOH and Li2O are not major components on the surface but rather found as a consequence of sputter-related reactions. Monochromatised Al Kα XPS-analysis based on the calibration of Ar+ ion sputtering of model compounds combined with a depth profile analysis based on energy tuning of synchrotron XPS can describe the highly complex composition and morphology of the SEI-layer.

National Category
Inorganic Chemistry
Identifiers
urn:nbn:se:uu:diva-89738 (URN)10.1016/S0378-7753(03)00277-5 (DOI)
Conference
11th International Meeting on Lithium Batteries, June 23 - 28, 2002, Monterey, California
Available from: 2002-03-21 Created: 2002-03-21 Last updated: 2017-12-30

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