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Defect Chemistry in Alkali Peroxides and Superoxides

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Defect Chemistry in Alkali Peroxides and Superoxides Defect Chemistry in Alkali Peroxides and Superoxides Von der Fakultät Chemie der Universität Stuttgart zur Erlangung der Würde eines Doktors der Naturwissenschaften (Dr. rer. nat.) genehmigte Abhandlung Vorgelegt von Oliver Gerbig aus Darmstadt Hauptberichter: Prof. Dr. J. Maier Mitberichter: Prof. Dr. J. Bill Prüfungsvorsitzender: Prof. Dr. J. van Slageren Tag der Einreichung: 28. Februar 2014 Tag der mündlichen Prüfung: 7. Mai 2014 Max-Planck-Institut für Festkörperforschung Stuttgart 2014 Erklärung Die vorliegende Doktorarbeit wurde vom Autor selbst in der Abteilung von Prof. J. Maier am Max- Planck-Institut für Festkörperforschung im Zeitraum von Januar 2010 bis März 2014 angefertigt. Der Inhalt ist die eigene Arbeit des Autors, Ausnahmen sind gekennzeichnet und wurden noch nicht zur Erlangung einer Qualifizierung oder eines Titels an der einer akademischen Institution eingereicht. Stuttgart, den 28. Februar 2014 Oliver Gerbig Declaration The work described in this thesis was carried out by the author in the Department of Prof. J. Maier at the Max Planck Institute for Solid State Research from January 2010 to March 2014. The content is the original work of the author except where indicated otherwise and has not been previously submitted to obtain any other degree or qualification at any academic institution. Stuttgart, 28th February 2014 Oliver Gerbig Table of Contents 1 Introduction and Motivation ........................................................................................................... 1 1.1 Inorganic Peroxides and Superoxides ..................................................................................... 1 1.2 Solid State Defect Chemistry .................................................................................................. 4 2 Experimental ................................................................................................................................... 6 2.1 Powder Preparation ................................................................................................................. 6 2.1.1 Lithium Peroxide............................................................................................................. 6 2.1.2 Sodium Peroxide ............................................................................................................. 7 2.1.3 Potassium Peroxide ......................................................................................................... 7 2.1.4 Potassium, Rubidium and Cesium Superoxide ............................................................... 8 2.2 Electrochemical Techniques ................................................................................................... 8 2.2.1 Pellet Preparation for Electrochemical Measurements ................................................... 8 2.2.2 Direct Current Polarization Measurement .................................................................... 10 2.2.3 Electrochemical Impedance Spectroscopy .................................................................... 11 2.2.4 Conductivity Relaxation Measurement ......................................................................... 12 2.2.5 Electromotive Force Measurement ............................................................................... 13 2.3 Chemical, Thermal, Thermochemical, Microstructural and Magnetic Characterization Techniques ........................................................................................................................................ 15 2.3.1 Scanning Electron Microscopy ..................................................................................... 15 2.3.2 Differential Scanning Calometry .................................................................................. 16 2.3.3 Thermogravimetric Measurement ................................................................................. 16 2.3.4 X-ray diffraction ........................................................................................................... 16 2.3.5 Inductive Coupled Plasma – Optical Emission Spectroscopy ...................................... 16 2.3.6 Raman Spectroscopy ..................................................................................................... 16 2.3.7 Infrared Spectroscopy ................................................................................................... 16 2.3.8 Electron Paramagnetic Resonance Spectroscopy .......................................................... 17 2.4 Oxygen Isotope Exchange and Gas Phase Analysis ............................................................. 17 3 Results and Discussion ................................................................................................................. 19 3.1 Lithium Peroxide .................................................................................................................. 19 3.1.1 Chemical Characterization and Thermal Stability of Li2O2 .......................................... 19 3.1.2 Electrochemical characterization .................................................................................. 23 3.1.3 Defect Chemistry .......................................................................................................... 30 3.1.4 Chemical oxygen exchange kinetics in Li2O2 ............................................................... 41 3.1.5 Li2O2-Au composite ...................................................................................................... 42 3.2 Sodium Peroxide ................................................................................................................... 44 3.2.1 Chemical characterization and Crystallographic Structure ........................................... 44 3.2.2 Electrochemical characterization .................................................................................. 45 3.2.3 Defect Chemistry .......................................................................................................... 49 3.3 Potassium Peroxide ............................................................................................................... 52 3.3.1 Chemical characterization ............................................................................................. 52 3.3.2 Thermodynamic Stability of K2O2 ................................................................................ 53 3.3.3 Electrochemical characterization .................................................................................. 54 3.4 Potassium Superoxide ........................................................................................................... 58 3.4.1 Chemical characterization and Crystallographic Structure ........................................... 58 3.4.2 Electrochemical characterization .................................................................................. 59 3.5 Rubidium and Cesium Superoxide ....................................................................................... 68 3.5.1 Chemical Characterization, Thermodynamic Stability and Crystallographic Structure 68 3.5.2 Electrochemical Characterization ................................................................................. 71 3.6 Electromotive Force Measurements of Alkali Superoxides .................................................. 74 3.7 Oxygen Isotope Exchange .................................................................................................... 78 3.8 Concluding Discussion ......................................................................................................... 85 4 Summary ....................................................................................................................................... 90 Zusammenfassung Während Bildung und Transport von Punktdefekten in Oxiden an vielen Beispielen untersucht wurde, ist die Defektchemie der Metall-Peroxide und Superoxide praktisch unbekannt. Diese Thematik ist sowohl von grundlegendem Interesse (was sind die relevanten Ladungsträger, ergeben sich durch die Peroxid- und Superoxidionen Unterschiede zu Oxiden etc.) als auch von technologischer Bedeutung für neuartige elektrochemische Energiespeicher. Bei der elektrischen Entladung von Alkalimetall-Sauerstoff-Batterien mit nicht-wässrigen Elektrolyten reagieren Sauerstoff und Alkalimetall-Ionen unter Aufnahme der Elektronen aus dem elektrischen Stromkreis zu Alkalimetallperoxiden oder –superoxiden. Im Vergleich zu herkömmlichen Alkalimetall-Ionen-Batterien, bei denen die Alkalimetall-Ionen von einem Wirtsmaterial aus üblicherweise schweren Übergangsmetalloxiden- oder phosphaten aufgenommen werden (durch Interkalation oder Phasenumwandlung), könnten deutlich höhere spezifische Energiedichten erreicht werden, die insbesondere für Elektroantriebe von Kraftfahrzeugen erforderlich sind. Da die Alkalimetallperoxide und –superoxide bei jedem Entlade- und Ladezyklus neu gebildet und wieder zersetzt werden, kommt der Transport- und Reaktionskinetik dieser Materialien eine erhebliche Bedeutung für die Leistungsfähigkeit der Batterien zu. In der vorliegenden Arbeit werden die elektrischen Transporteigenschaften, die Sauerstoffaustauschkinetik sowie die Defektchemie der Peroxide von Lithium, Natrium und Kalium sowie der Superoxide von Kalium, Rubidium und Cäsium untersucht. Aufgrund der hohen Empfindlichkeit der Substanzen gegenüber Kohlenstoffdioxid und Wasser sowie der elektrischen Transporteigenschaften gegenüber Verunreinigungen wurde besonderes Augenmerk auf die Herstellung,
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