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MOCVD of Tungsten and Molybdenum Nitrides MOCVD of Tungsten and Molybdenum Nitrides Daniel Rische; Doktorarbeit 2007 MOCVD of Tungsten and Molybdenum Nitrides Dissertation zur Erlangung der Doktorwürde der Fakultät für Chemie der Ruhr-Universität Bochum vorgelegt von Diplom-Chemiker Daniel Rische aus Bochum Referenten: Prof. Dr. Roland A. Fischer Prof. Dr. Christof Wöll Die vorliegende Arbeit entstand in der Zeit von Juli 2004 bis November 2007 am Lehrstuhl für Anorganische Chemie II der Ruhr-Universität Bochum Mein besonderer Dank gilt an Prof. Dr. Roland A Fischer, für die interessante Aufgabenstellung, das in mich gesetzte Vertrauen bei der Bearbeitung eines interessanten und herausfordernden Forschungsthemas, und den Rat mit dem er mir zur Seite stand. Danksagung Juniorprof. Dr. Anjana Devi Anjana und Harish danke ich für die Unterstützung in Form & Dr. Harish Parala von konstruktiver Kritik in vielen Bereichen und der Unterstützung bei XRD und TG/DTA Andrian Milanov Danke für die Unterstützung bei TG/DTA Messungen , sowie häufigen Gedankenaustausch Daniela Bekermann Danke für die tatkräftige Unterstützung bei Syntheseproblemen Sabine Masukowitz Vielen Dank für die Unterstützung in allen organisatorischen Fragen und bei dem Umgang mit dem RUB’schen Büroapparat. Stephan Spöllmann Stephan danke ich für die tatkräftige Unterstützung bei den Experimenten am Aixtron-Reaktor Manuela Winter Dank an Manuela für die Messungen der Einkristallstrukturen und Hilfe bei der Lösung derselben Dr. Rolf Neuser Herrn Neuser danke ich für die SEM- und EDX Messungen. H.C. Starck GmbH Danke an die H.C. Starck GmbH für die großzügige Chemikalienspende. Andreas Kempter Für den gemeinsamen Weg durch das Studium, von Vordiplom über Diplom bis jetzt. Desweiteren möchte ich mich bei meinem gesamten Lehrstuhl für die schöne Zeit in der Gruppe bedanken. Dazu gehören Saeed Amirjalayer, Dr. Raghunandan Bhakta, Thomas Cadenbach, Mirza Cokoja, Rolf Deibert, Daniel Esken, Lina Freitag, Dr. Eliza Gemel, Malte Hellwig, Stephan Hermes, Ursula Herrmann, Todor Hikov, Heike Kampschulte, Andreas Kempter, Dr. Jayaprakash Khanderi, Dr. Emmanuel Lamouroux, Dr. Eva Maile, Mikhail Meilikhov, Andrian Milanov, Maike Müller, Dr. Rochus Schmid, Felicitas Schröder, Dr. Jelena Sekulic, Stephan Spöllmann, Tobias Thiede, Dr. Maxim Tafipolsky, Tim Wilmsen, Manuela Winter, Dr. Wenhua Zhang und Xiaoning Zhang Zudem danke ich allen die meinen Dank verdienen, die ich aber in meiner Liste vergessen habe. “Science is like sex: Something useful comes out, but that’s not the reason we are doing it.” Richard P. Feynman Für Jenny Abbreviations ALD: Atomic Layer Deposition tBu: tert- Butyl CVD: Chemical Vapor Deposition Cy: Cyclohexyl DME: 1,2-Dimethoxyethane DTA: Differential Thermal Analysis EI-MS: Electron Ionization Mass Spectroscopy Et: Ethyl FT-IR Fourier-Transform-Infrared Spectroscopy GC: Gas Chromatography MBE: Molecular Beam Epitaxy Me: Methyl Mes: Mesityl MOCVD: Metal Organic Chemical Vapor Deposition MS: Mass Spectroscopy NMR: Nuclear Magnetic Resonance Ph: Phenyl iPr: iso-Propyl PVD: Physical Vapor Deposition py: Pyridine SEM: Scanning Electron Microscopy SIMS: Secondary Ion Mass Spectroscopy S/N-ratio Signal to Noise ratio SNMS: Secondary Neutral Mass Spectroscopy THF: Tetrahydrofurane TMEDA: N,N,N’,N’-Tetramethylethylenediamine TG: Thermogravimetric Analysis XRD: X-Ray Diffraction Table of Contents Table of Contents 1. Introduction .......................................................................................................................... 1 1.1. Motivation and Goals...................................................................................................... 1 1.2. Tungsten Nitride Materials.............................................................................................. 2 1.3. Molybdenum Nitride Materials....................................................................................... 3 1.4. Applications of Tungsten and Molybdenum Nitrides..................................................... 4 1.4.1. Schottky Diodes ....................................................................................................... 4 1.4.2. Conductive Diffusion Barriers ................................................................................. 5 1.4.3. Hard Coatings........................................................................................................... 7 1.4.4. Catalysis ................................................................................................................... 7 1.5. Thin Film Deposition Techniques via gas Phase ............................................................ 7 1.5.1. Physical Vapour Deposition (PVD) ......................................................................... 7 1.5.2. Chemical Vapour Deposition (CVD)....................................................................... 9 1.5.3. Atomic Layer Deposition (ALD) ........................................................................... 13 2. State of the Art.................................................................................................................... 15 2.1. Precursors for MOCVD and ALD ................................................................................ 15 2.1.1. Tungsten nitride...................................................................................................... 15 2.1.2. Molybdenum nitride............................................................................................... 20 2.2. Guanidinato ligands....................................................................................................... 22 3. Synthesis of the Tungsten Compounds............................................................................. 25 3.1. [WCl2(Nt-Bu)2py2] (1) .................................................................................................. 25 3.2. [W(Nt-Bu)2Cl{(Ni-Pr)2CNi-Pr2] (3) ............................................................................. 27 3.3. [W(Nt-Bu)2Cl{(Ni-Pr)2CNMe2}] (4) ............................................................................ 31 3.4. [W(Nt-Bu)2Cl{(Ni-Pr)2CNEt2}] (5).............................................................................. 33 3.5. [W(Nt-Bu)2Cl{(NCy)2CNEt2}] (6) ............................................................................... 35 3.6. [W(Nt-Bu)2NMe2{(Ni-Pr)2CNi-Pr2}] (7)...................................................................... 37 3.7. [W(Nt-Bu)2(NMe2){(Ni-Pr)2CNMe2}] (8).................................................................... 39 3.8. [W(Nt-Bu)2(N3){(Ni-Pr)2CNi-Pr2}] (9) ........................................................................ 39 3.9. [W(Nt-Bu)2H{(Ni-Pr)2CNMe2}] (10)........................................................................... 40 3.10. [W(Nt-Bu)2Cl{NC(NMe2)2}]2 (11) ............................................................................. 42 3.11. [W(Nt-Bu)2(N3){NC(NMe2)2}]2 (12).......................................................................... 45 2 3.12. [(W(Nt-Bu)2(N3)(µ -N3)py)]2 (13) .............................................................................. 47 3.13. Conclusions for Chapter 3........................................................................................... 50 Table of Contents 4. Synthesis of the Molybdenum Compounds...................................................................... 52 4.1. Starting Compound for the Molybdenum synthesis...................................................... 52 4.2. [Mo(Nt-Bu)2Cl{(Ni-Pr)2CNMe2}] (15) ........................................................................ 55 4.3. [Mo(Nt-Bu)2I{(Ni-Pr)2CNMe2}] (16)........................................................................... 55 4.4. [Mo(Nt-Bu)2(N3){(Ni-Pr)2CNMe2}] (17) ..................................................................... 57 4.5. Conclusions for Chapter 4............................................................................................. 59 5. MOCVD-Experiments of Tungsten Nitride..................................................................... 60 5.1. Thermal Characterization of the precursors.................................................................. 60 5.2. Depositions on the home-built MOCVD reactor .......................................................... 61 5.2.1. XRD analysis and surface morphology.................................................................. 62 5.2.2 Composition of the films (SNMS analysis) ............................................................ 68 5.2.3 Growth rates & resistivities..................................................................................... 73 5.3. Characterization of the Exhaust gases........................................................................... 74 5.4. Experiments on the Aixtron 200 RF reactor ................................................................. 77 5.4.1 The Reactor ............................................................................................................. 77 5.4.2 The Bubbler Design ................................................................................................ 79 5.4.3 The Experiments ..................................................................................................... 79 5.5. Comparison of the Guanidinato Precursors to Imido/Amido Precursors...................... 84 5.6. Conclusions for Chapter 5............................................................................................. 85 6. MOCVD-Experiments of Molybdenum Nitride.............................................................
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