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Nitrido-, Oxonitrido-, and Oxonitridocarbidosilicates for Solid

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Nitrido-, Oxonitrido-, and Oxonitridocarbidosilicates for Solid Dissertation zur Erlangung des Doktorgrades der Fakultät für Chemie und Pharmazie der Ludwig-Maximilians-Universität München Nitrido-, Oxonitrido-, and Oxonitridocarbidosilicates for Solid-State Lighting by a Multiple Cation and Anion Approach Christian Andreas Maak aus Bad Aibling, Deutschland 2019 Erklärung Diese Dissertation wurde im Sinne von § 7 der Promotionsordnung vom 28. November 2011 von Herrn Prof. Dr. Wolfgang Schnick betreut. Eidesstattliche Versicherung Diese Dissertation wurde eigenständig und ohne unerlaubte Hilfe erarbeitet. München, den 20.05.2019 ....................................... (Christian Andreas Maak) Dissertation eingereicht am 02.04.2019 1. Gutachter Prof. Dr. Wolfgang Schnick 2. Gutachter Prof. Dr. Oliver Oeckler Mündliche Prüfung am 17.05.2019 Danksagung Ganz besonderer Dank gilt Herrn Prof. Dr. Wolfgang Schnick für die Möglichkeit, meine Dissertation über dieses sehr spannende Thema in seinem Arbeitskreis anfertigen zu können. Die hervorragenden Arbeitsbedingungen und die Freiheiten bei der Themengestaltung und Umsetzung neuer Ideen waren perfekte Voraussetzungen für den Erfolg meiner Promotion. Auch für die zahlreichen konstruktiven Gespräche und positiven Anregungen, die Möglichkeit meine Ergebnisse in wissenschaftlichen Fachzeitschriften zu publizieren, sowie zahlreiche Tagungen besuchen zu können, möchte ich mich herzlich bedanken. Insbesondere der Besuch des Phosphor Global Summit in Kalifornien zusammen mit dem LED-Team war für meine weitere Promotion sehr inspirierend. Ich möchte mich ganz herzlich bei Herrn Prof. Dr. Oliver Oeckler für die Übernahme des Koreferats meiner Dissertation sowie die große Hilfe bei diversen kristallographischen Fragestellungen von der Bachelorarbeit bis zur Promotion bedanken. Weiterhin bedanke ich mich für die große Unterstützung durch TEM und Synchrotronmessungen sowie die sehr gute Zusammenarbeit bei allen gemeinsamen Projekten. Herrn Prof. Dr. Hubert Huppertz, Herrn Prof. Dr. Achim Hartschuh, Herrn Prof. Dr. Hans- Christian Böttcher und Herrn Prof. em. Dr. Wolfgang Beck danke ich herzlich für ihre Bereitschaft, als Teil der Prüfungskommission meiner Doktorarbeit zur Verfügung zu stehen. Großer Dank gilt allen Beteiligten der Kooperation mit Lumileds für die tolle Zusammenarbeit. Insbesondere Herrn Dr. Peter J. Schmidt, Herrn Dr. Christoph Martiny, Herrn Volker Weiler, Frau Petra Huppertz sowie Frau Cora Hecht danke ich für die Unterstützung bei der detaillierten Charakterisierung und Interpretation von Lumineszenzeigenschaften. Die Diskussionen bei unseren Meetings sowie die großartige Unterstützung von Herrn Dr. Peter J. Schmidt bei unseren gemeinsamen Manuskripten haben sehr zu meinem Verständnis beigetragen und die Qualität unserer Publikationen gesteigert. Darüber hinaus bedanke ich mich bei all meinen weiteren Co-Autoren, PD Dr. Constantin Hoch, Dr. Philipp Strobel, Dr. Dajana Durach, Robin Niklaus, Lucien Eisenburger, Markus Nentwig, Mathias Mallmann, Franziska Friedrich, Andre Mähringer und Dr. Jonathan P. Wright für die sehr gute Zusammenarbeit und Ihren Beitrag zu meiner Dissertation. Herzlichst bedanken möchte ich mich bei Dr. Markus Seibald, der schon während meiner Bachelorarbeit meine Begeisterung für Festkörperchemie und Leuchtstoffe geweckt hat und mir zudem in zahlreichen Gesprächen sehr viel von seinem Wissen übertragen hat. Hierdurch konnten wir perfekte Voraussetzungen für meine Promotion schaffen. Großer Dank für viele inspirierende Diskussionen und Gespräche über Lumineszenz sowie kristallographische und sonstige Problemchen geht auch an meine Kollegen und Freunde aus der Schreibstube, Dr. Philipp Strobel, Dr. Simon Kloß und Philipp Bielec. Beim gesamten LED-Team möchte ich mich für die super Stimmung und den guten Austausch bedanken. Insbesondere unseren Ausflug zum PGS 2016 in Newport Beach und die anschließende Tour werde ich nie vergessen. Besonderer Dank gilt meinen Laborkollegen aus D2.100, Dr. Christine Pösl, Dr. Lukas Neudert, Dr. Philipp Strobel, Robin Niklaus, Lucien Eisenburger und Eugenia Elzer für die tolle gemeinsame Zeit. Auch für die coole Zeit und die lustigen Abende mit dem „Pressenteam und friends“ möchte ich mich bedanken. Weiterhin danke ich natürlich auch allen anderen Mitgliedern der Arbeitskreise Schnick, Oeckler, Hoch, Johrendt und Lotsch für die super Arbeitsatmosphäre und die tolle Zeit im 2. Stock. Vielen Dank auch an meine Praktikanten Franziska Friedrich, Andre Mähringer, Mara Egenhöfer und Dominik Gelsheimer, die alle einen hervorragenden Beitrag zu meiner Arbeit geleistet haben. Ich danke Dr. Steffen Schmidt, Dr. Markus Döblinger und Christian Minke für das Einlernen und die tolle Unterstützung am REM. Bei Dr. Peter Mayer möchte ich mich für die Messung von Einkristallbeugungsdaten herzlich bedanken. Besonderer Dank gilt auch Wolfgang Wünschheim, Thomas Miller und Olga Lorenz für die Hilfe bei allen technischen und organisatorischen Fragestellungen. Durch Euch war es möglich, sich ganz auf die eigene Forschung zu konzentrieren. Größter Dank gilt meinen Eltern, ohne deren großartige Unterstützung all dies nicht möglich gewesen wäre. Allergrößter Dank gilt meiner Ehefrau Moni und unseren Söhnen Lukas und Simon. Ihr macht jeden Tag in meinem Leben zu etwas ganz Besonderem. „ “ Table of Contents Table of Contents 1 Introduction ............................................................................................................... 1 2 Nitridolithosilicates Li38.7RE3.3AE5.7[Li2Si30N59]O2F as Promising Host Materials 3+ for Ce Doping ........................................................................................................15 3+ 2.1 Unprecedented Deep-Red Ce Luminescence of the Nitridolithosilicates Li38.7RE3.3Ca5.7[Li2Si30N59]O2F (RE = La, Ce, Y) ..................................................15 2.1.1 Introduction .................................................................................................16 2.1.2 Experimental Section ..................................................................................17 2.1.2.1 Synthesis ................................................................................................17 2.1.2.2 Electron Microscopy ................................................................................18 2.1.2.3 Single-Crystal X-ray Diffraction ...............................................................18 2.1.2.4 Powder X-ray Diffraction .........................................................................18 2.1.2.5 Crystallographic Data ..............................................................................18 2.1.2.6 UV/Vis Spectroscopy ..............................................................................19 2.1.2.7 Luminescence .........................................................................................19 2.1.3 Results and Discussion ..............................................................................19 2.1.3.1 Synthesis and Chemical Analysis ............................................................19 2.1.3.2 Crystal Structure Refinement and Description .........................................20 2.1.3.3 UV/Vis Spectroscopy ..............................................................................25 2.1.3.4 Luminescence .........................................................................................26 2.1.4 Conclusion ..................................................................................................28 2.1.5 References .................................................................................................29 2.2 Unpublished Results in the System Li38.7RE3.3AE5.7[Li2Si30N59]O2F .....................33 2+ 3 Narrow-Band Yellow-Orange Emitting La3−xCa1.5xSi6N11:Eu (x ≈ 0.77): A Promising Phosphor for Next-Generation Amber pcLEDs ........................................35 3.1 Introduction ........................................................................................................36 3.2 Experimental Section .........................................................................................37 3.2.1 Synthesis ....................................................................................................37 3.2.2 Electron Microscopy ...................................................................................38 I Table of Contents 3.2.3 Fourier Transform Infrared Spectroscopy ................................................... 38 3.2.4 Single-Crystal X-ray Diffraction .................................................................. 38 3.2.5 Powder X-ray Diffraction ............................................................................ 38 3.2.6 UV/Vis Spectroscopy.................................................................................. 39 3.2.7 Luminescence ............................................................................................ 39 3.3 Results and Discussion ..................................................................................... 39 3.3.1 Synthesis and Chemical Analysis ............................................................... 39 3.3.2 Crystal Structure ........................................................................................ 40 3.3.3 UV/Vis Spectroscopy.................................................................................. 43 3.3.4 Luminescence ............................................................................................ 44 3.4 Conclusion ........................................................................................................
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