Hydrophobic Nanoreactor Templating
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1 - Mathematik Hydrophobic Nanoreactor Templating for Nanostructured Metal - Tin-rich ITO Materials vorgelegt von M.Sc. Amandine Guiet Geb. in Angers, Frankreich Von der Fakultat II und Naturwissenschaften dertechnischen Universitat Berlin zur Erlangung des akademischen Grades Doktor der Naturwissenschaften Dr. rer. nat. genehmigte Dissertation Promotionsausschuss: Vorsitzender: Prof. Dr. rer. nat. Marga Lensen Gutachter: Prof. Dr. rer. nat. Arne Thomas Prof. Dr. rer. nat. Christina Roth Dr. rer. nat. Anna Fischer Tag der wissenschaftlichen Aussprache: 12. Juni 2014 Berlin 2014 D83
2 TABLE OF CONTENT 1 INTRODUCTION Motivation/Aim of the work Transparent conducting oxides (TCO) Theoretical background of TCO materials Electrical and optical properties of TCO materials Immobilization of NPs into nanostructured metal oxides Immobilization of NPs into mesoporous metal oxides Encapsulation of NPs into yolk-shell structure Single source precursor approach for a new alternative to ITO Indium(l) tin(ll) tris-te/t-butoxide (ITBO) as single-source precursor Single-source molecular approach for synthesis of ITOTR thin film Experimental section Synthesis of indium(l) tin(ll) tris-rerr-butoxide (ITBO) Preparation of planar ITOTR thin films 37 2 CHARACTERIZATION METHODS Electron microscopy Fundamentals Electron-matter interactions Transmission electron microscopy (TEM) Scanning electron microscopy (SEM) Energy dispersive X-ray spectroscopy (EDX) X-rays scattering Fundamentals Small Angle X-ray Scattering (SAXS) Anomalous Small Angle X-ray Scattering (ASAXS) Wide Angle X-ray Scattering (WAXS) X-ray absorption (XAS) 51 8
3 2.4 Gas physisorption Gas sorption isotherms Specific surface area determination Characterization of electrical conductivity Dynamic light scattering (DLS) Instrumental details NMR spectroscopy UV-vis spectroscopy Thermogravimetric analysis (TGA) Dynamic Light Scattering (DLS) X-Ray Diffraction (XRD) Small-Angle X-ray Scattering (SAXS) X-ray absorption near edge spectroscopy (XANES) Electron microscopy Conductivity measurements X-ray photoelectron spectroscopy (XPS) 61 3 PS-B-P4VP INVERSE MICELLES AS HYDROPHOBIC TEMPLATE Introduction Nanostructuration of ITOTR with traditional block copolymer as template Nanostructuration of ITOTR with preformed PSm-b-P4VP micelles as hydrophobic template Synthesis and characterization of PSm-b-P4VPn block copolymer Formation of PS111-i-P4VP96 inverse micelles PS-fe-P4VP inverse micelles as versatile template for ITOTRoxide Conclusion Experimental section Materials Preparation of mesoporous ITOTR thin films with F127 block copolymer as template Synthesis of mesoporous ITOTR thin films via hydrophobic templating strategy 80 9
4 4 PS-A-P4VP INVERSE MICELLES AS NANOCONTAINER TEMPLATE Introduction Gold loaded PSm-b-P4VPn micelles as hydrophobic nanocontainer template Preparation of mp-itotr loaded with one AuNP per pore Electrochemical applications of mp-aunp-itotr electrodes Immobilization of small molecules Electrocatalytic CO oxidation Conclusion Experimental section Synthesis of mesoporous ITOTR thin films with one Au NP per pore Synthesis of AuNP 2D-arrays on ITO (AuNP-ITO) via micelle nanolithography Electrochemical Measurements 95 5 PS-B-P4VP INVERSE MICELLES AS NANOREACTOR TEMPLATE Increase of the gold loading From open pore to yolk-shell structure Preliminary results Formation mechanism of hybrid HAuCI4@lnxSnv02 core-shell micelles in solution Characterization of AuNPs@ITOTR yolk-shell based tin films Formation of the AuNPs Thermal stability of the NPs Influence of the synthetic parameters Conclusion Experimental section Materials PSm-fa-P4VPn characteristics Synthesis of AuNPs@ITOTRyolk-shell based thin films with spherical structure Synthesis of AuNPs@ITOTRyolk-shell based thin films with wormlike structure
5 6 HYDROPHOBIC NANOREACTOR TEMPLATING: A VERSATILE SYNTHETIC TOOLBOX FOR A VARIETY OF YOLK-SHELL MATERIALS Preparation of PtNPs@ITOTRyolk-shell materials Introduction Platinum loaded PSm-b-P4VPn micelles Synthesis of PtNPs@ITOTRyolk-shell based thin films Conclusion Preparation of bimetallic NPs@ITOTR yolk-shell materials Preparation of AgAuNPs@ITOTR yolk-shell materials Preparation of AuPtNPs@ITOTR yolk-shell materials Experimental section Materials PSm-b-P4VPn characteristics Synthesis of PtNPs@ITOTR yolk-shell materials with spherical or wormlike structure Synthesis of AgAuNPs@ITOTR yolk-shell materials with spherical Synthesis of AuPtNPs@ITOTRyolk-shell materials with spherical structure 182 structure CONCLUSION AND OUTLOOK APPENDIX PUBLICATION LIST ACKNOWLEDGMENT REFERENCES
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