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Iron-Based Superconductors Via Soft Chemistry

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Iron-Based Superconductors Via Soft Chemistry Dissertation zur Erlangung des Doktorgrades der Fakultät für Chemie und Pharmazie der Ludwig‐Maximilians‐Universität München Iron‐based Superconductors via Soft Chemistry Gina Maya Friederichs aus Dachau, Deutschland 2015 Erklärung: Diese Dissertation wurde im Sinne von §7 der Promotionsordnung vom 28. November 2011 von Herrn Prof. Dr. Dirk Johrendt betreut. Eidesstattliche Versicherung: Diese Dissertation wurde eigenständig und ohne erlaubte Hilfe erarbeitet. München, den 27.05.2015 _________________________________ Gina Maya Friederichs Dissertation eingereicht am: 09.06.2015 1. Gutachter: Prof. Dr. Dirk Johrendt 2. Gutachter: Prof. Dr. Hubert Huppertz Mündliche Prüfung am: 30.06.2015 Danksagung An dieser Stelle möchte ich mich bei allen Menschen bedanken, die mich bei dieser Arbeit unterstützt haben. Mein besonderer Dank gilt hierbei Prof. Dr. Dirk Johrendt für die Aufnahme in seinen Arbeitskreis und die Möglichkeit dieses interessante Thema unter hervorragenden Bedingungen und großem Freiraum bearbeiten zu dürfen. Prof. Dr. Hubert Huppertz danke ich sehr herzlich für die Übernahme des Zweitgutachtens. Prof. Dr. Konstantin Karaghiosoff, Prof. Dr. Hendrik Zipse, Prof. Dr. Hans‐Christian Böttcher und Prof. Dr. Andreas Kornath danke ich sehr herzlich, dass sie sich bereit erklärt haben an meinem Rigorosum teilzunehmen. Ausserdem möchte ich mich bei den folgenden Personen bedanken: Für die superherzliche Aufnahme in den AK und eine wirklich lustige und unvergessliche Zeit in vielerlei Hinsicht danke ich im Besonderen Rainer Frankovsky, Franziska Hummel, Marcus Tegel und Erwin Wiesenmayer. Allen ehemaligen und aktuellen AK‐Kollegen für das tolle, freundschaftliche Miteinander und die schöne Zeit: Daniel Bichler, Katharina Förg, Marianne Martin (geb. Rotter), Veronika Zinth, Constantin von Schirnding, Lola Lilensten, Andreas Binek, Fabian Nitsche, Tina Markovic, Anne Schulz, Juliane Stahl, Lars Bulthaupt, Tobias Stürzer, Christine Stürzer (geb. Hieke), Roman Pobel, Simon Peschke, Ursula Pachmayr und Catrin Löhnert. Allen Mitgliedern der Arbeitskreise Schnick, Lotsch, Oeckler, Schmedt auf der Günne und Fässler (TU) für die gute Zusammenarbeit. Meinen Bacheloranden und Praktikanten Christian Wagner, Yury Vilk, Matthias Wörsching und Katharina Iwan, für ihre tolle, engagierte Arbeit. Prof. Dr. Rainer Pöttgen, Inga Schellenberg und Sirko Kamusella für Mößbauer Messungen; Prof. Dr. Lorenz Kienle und Viola Duppel für TEM Messungen; Prof. Dr. Jörn Schmedt auf der Günne und Christian Minke für NMR Messungen. Ohne euch wäre mein Studium nicht mal halb so schön gewesen: Tanja Prommnitz, Johanna Haidt, Annette Frischmuth, Veronika Werner, Tobias Blümke, Ramona Pichl (geb. Branzan), Stefan Pichl und Florian Achrainer. Vielen Dank für die vielen unvergesslichen Momente! Meiner Familie, im Besonderen meinen Eltern, Großeltern und meiner Schwester, danke ich von Herzen für die stetige Unterstützung und Ermutigung. Mama und Schirin ich danke euch für das starke Band, das uns verbindet. Danke Floh, für deine Geduld, dein Verständnis und die wunderschöne gemeinsame Zeit. Wege entstehen dadurch, dass man sie geht. Kafka Table of Contents 1 Introduction .............................................................................................................. 1 2 Preparative and analytical methods ................................................................ 5 2.1 Starting materials .................................................................................................................. 5 2.2 Vacuum and inert gas line .................................................................................................. 6 2.3 Solid state reactions .............................................................................................................. 6 2.4 Synthesis under mild conditions ..................................................................................... 6 2.5 X‐ray powder diffraction .................................................................................................... 7 2.6 Energy dispersive X‐ray analysis (EDX) ...................................................................... 7 2.7 Magnetic measurements ..................................................................................................... 7 2.8 Electrical resistivity .............................................................................................................. 8 2.9 Mössbauer spectroscopy .................................................................................................... 9 2.10 Solid‐state NMR ...................................................................................................................... 9 2.11 High resolution transmission electron microscopy (HRTEM) ........................... 9 3 FeSe via metathesis ............................................................................................. 11 3.1 Introduction .......................................................................................................................... 11 3.2 Synthesis ................................................................................................................................. 12 3.3 Crystal structure .................................................................................................................. 13 3.4 Magnetic measurements .................................................................................................. 16 3.5 Electrical resistivity ........................................................................................................... 19 3.6 57Fe‐Mössbauer spectroscopy ....................................................................................... 20 3.7 Conclusion .............................................................................................................................. 23 4 Annealing effects in Fe1+xTe1‐ySey (x = 0‐0.1, y = 0.1‐0.4) ........................ 25 4.1 Introduction .......................................................................................................................... 25 4.2 Synthesis ................................................................................................................................. 26 4.3 Crystal structure .................................................................................................................. 27 4.4 Magnetic measurements .................................................................................................. 30 4.5 Electrical resistivity ........................................................................................................... 34 4.6 Conclusion .............................................................................................................................. 35 4.7 Appendix ................................................................................................................................. 37 5 K1‐xFe2‐ySe2 via reductive intercalation ......................................................... 43 5.1 Introduction ........................................................................................................................... 43 5.2 Synthesis.................................................................................................................................. 45 5.3 Crystal structure .................................................................................................................. 46 5.4 Magnetic measurements .................................................................................................. 50 5.5 Electrical resistivity ............................................................................................................ 52 5.6 Conclusion .............................................................................................................................. 53 6 NaFe1‐yCoyAs ........................................................................................................... 55 6.1 Introduction ........................................................................................................................... 55 6.2 Synthesis.................................................................................................................................. 56 6.3 Crystal structure .................................................................................................................. 56 6.4 Magnetic measurements .................................................................................................. 58 6.5 Conclusion .............................................................................................................................. 59 7 Na1‐xFe2‐yAs2 via oxidative deintercalation .................................................. 61 7.1 Introduction ........................................................................................................................... 61 7.2 Synthesis.................................................................................................................................. 62 7.3 Crystal structure .................................................................................................................. 63 7.4 Magnetic measurements .................................................................................................. 67 7.5 57Fe‐Mößbauer spectroscopy ......................................................................................... 68 7.6 Solid state NMR spectroscopy .......................................................................................
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