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Metal Chalcogenides Syntheses Using Reactions of Ionic Liquids

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Metal Chalcogenides Syntheses Using Reactions of Ionic Liquids Metal chalcogenides syntheses using reactions of ionic liquids Dissertation zur Erlangung des akademischen Grades Doctor rerum naturaluim (Dr. rer. nat.) vorgelegt dem Bereich Mathematik und Naturwissenschaften der Technischen Universität Dresden von M.Eng. Tao Zhang geboren am 12. April 1989 in Shandong (China) Eingereicht am 29. März 2018 Die Dissertation wurde in der Zeit von Oktober 2014 bis März 2018 an der Professur für Anorganische Chemie II angefertigt. Gutachter: Prof. Dr. Michael Ruck (TU Dresden) Prof. Dr. Claus Feldmann (KIT) Tag der Verteidigung: 30. Mai 2018 Contents 1. Background and motivation ................................................................ 1 1.1. Properties of ILs and DESs ................................................................. 3 1.2. Reactions of ionic liquids and deep eutectic solvents ............................ 5 1.2.1 Reactions of metal-containing ionic liquids ...................................... 5 1.2.2. Reactions of fluorine-containing ionic liquids ................................... 6 1.2.3. Reactions of hydroxide-based ionic liquids ...................................... 7 1.2.4. Reactions of chalcogen-containing ionic liquids ............................... 8 1.2.5. Reactions of deep eutectic solvents ............................................. 10 1.3. Motivation ...................................................................................... 12 1.4. References ..................................................................................... 13 2. Solvothermal synthesis and enhanced photoelectrochemical perfor- mance of hierarchically structured strontium titanate particles ........ 21 2.1. Background .................................................................................... 23 2.2. Experimental section ....................................................................... 24 2.2.1. Chemicals ................................................................................ 24 2.2.2. Preparation of SrTiO3 ................................................................. 24 2.2.3. Characterization of SrTiO3 .......................................................... 25 2.2.4. Photo-electrochemical measurement ........................................... 25 2.3. Results and discussion ..................................................................... 26 2.3.1. Structural characterization of SrTiO3 particles ............................... 26 2.3.2. Growth mechanism of SrTiO3 particles ......................................... 27 2.3.3. Nitrogen physisorption of SrTiO3 particles ..................................... 34 2.3.4. Optical and photoelectrochemical properties of SrTiO3 particles ....... 35 2.4. Conclusions .................................................................................... 37 2.5. References ..................................................................................... 37 3. Synthesis of metal sulfides from a deep eutectic solvent precursor .. 43 3.1. Background .................................................................................... 45 3.2. Experimental section ....................................................................... 45 3.2.1. Chemicals ................................................................................ 45 Metal chalcogenides syntheses using reactions of ionic liquids 3.2.2. Synthesis of the DESs ................................................................ 46 3.2.3. Synthesis of metal sulfides ......................................................... 46 3.2.4. Materials’ characterization .......................................................... 46 3.3. Results and discussion ..................................................................... 47 3.3.1. Structural and morphological analysis of metal sulfides .................. 47 3.3.2. Influence of the DESP composition .............................................. 55 3.3.3. Comparison with DES synthesis at ambient pressure ..................... 56 3.3.4. Mechanism of formation of final products ..................................... 58 3.4. Conclusions .................................................................................... 60 3.5. References ..................................................................................... 60 4. Dissolution behavior and activation of selenium in phosphonium based ionic liquids ............................................................................. 65 4.1. Background .................................................................................... 67 4.2. Experimental section ....................................................................... 68 4.2.1. Chemicals ................................................................................ 68 4.2.2. Dissolution of Se in [P6 6 6 14]Cl .................................................... 68 4.2.3. Dissolution of Se in [P6 6 6 14][decanoate] ...................................... 69 4.2.4. Dissolution of Se in [P4 4 4 4]Cl ..................................................... 69 4.2.5. Preparation of trioctylphosphane selenide solution......................... 69 4.2.6. Synthesis of nickel diselenides .................................................... 69 4.2.7. Synthesis of zinc diselenides ....................................................... 70 4.3. Results and discussion ..................................................................... 70 4.3.1. Dissolution tests of selenium in phosphonium ionic liquids .............. 70 4.3.2. Synthesis of metal selenides in phosphonium ionic liquids .............. 74 4.4. Conclusions .................................................................................... 77 4.5. References ..................................................................................... 77 5. Dissolution behavior of tellurium in phosphonium based ionic liquids for syntheses of tellurium and tellurides nanostructures .................. 81 5.1. Background .................................................................................... 83 5.2. Experimental section ....................................................................... 84 5.2.1. Chemicals ................................................................................ 84 5.2.2. Dissolution of tellurium in [P6 6 6 14]Cl ........................................... 84 5.2.3. Dissolution of tellurium in [P6 6 6 14][N(CN)2] .................................. 85 5.2.4. Dissolution of tellurium in [P6 6 6 14][decanoate] ............................. 85 5.2.5. Dissolution of tellurium in [P4 4 4 4][decanoate] .............................. 85 5.2.6. Synthesis of Bi2Te3 in [P6 6 6 14]Cl ................................................. 86 Contents 5.2.7. Synthesis of Bi-decanoate and Bi2Te3 in [P6 6 6 14][decanoate] .......... 86 5.2.8. Synthesis of Ag2Te in [P6 6 6 14][N(CN)2] ........................................ 87 5.2.9. Materials characterization........................................................... 87 5.3. Results and discussion ..................................................................... 87 5.3.1. Dissolution tests in phosphonium based ionic liquids ...................... 88 5.3.2. Synthesis of Bi2Te3 and Ag2Te from phosphonium ionic liquids ........ 99 5.4. Conclusions .................................................................................. 102 5.5. References ................................................................................... 103 6. Conclusions and perspectives ......................................................... 107 Abbreviations ...................................................................................... 111 List of Publications .............................................................................. 113 Acknowledgements ............................................................................. 115 Collaborations ..................................................................................... 117 Versicherung ....................................................................................... 119 Erklärung ............................................................................................ 119 Metal chalcogenides syntheses using reactions of ionic liquids Chapter 1 Background and motivation 1 Metal chalcogenides syntheses using reactions of ionic liquids 2 Background and motivation Conventional inorganic materials synthesis following the high temperature solid- state reaction route is quite time- and energy-consuming. The low temperature synthesis relies heavily on water and traditional organic solvents. Alternatively, the fabrication of inorganic materials using, or in presence of, ionic liquids or deep eutectic solvents provides a promising direction in materials chemistry. Ionic liquids and deep eutectic solvents offer many unique properties and therefore provide great opportunities to discover new compounds or new phases which are not accessible in conventional organic or aqueous solvents or with a solid-state method.[1-3] 1.1. Properties of ionic liquids and deep eutectic solvents Figure 1.1. Popular cations and anions of ionic liquids. Ionic liquids (ILs), first reported by Walden in 1914,[4] are nowadays a large and widely explored class of ionic compounds that melt below 100 °C.[5] Figure 1.1 presents a few popularly used cations and anions of ILs. Although the use of ILs for organic chemistry has widely and extensively studied since the 1980s, their application in inorganic materials synthesis just began in the early
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