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Synthesis and Characterizations of Novel Magnetic and Plasmonic Nanoparticles

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Synthesis and Characterizations of Novel Magnetic and Plasmonic Nanoparticles SYNTHESIS AND CHARACTERIZATIONS OF NOVEL MAGNETIC AND PLASMONIC NANOPARTICLES by NAWEEN DAHAL B.S., TRIBHUVAN UNIVERSITY, 1995 M.S., TRIBHUVAN UNIVERSITY, 1997 AN ABSTRACT OF A DISSERTATION Submitted in partial fulfillment of the requirements for the degree DOCTOR OF PHILOSOPHY DEPARTMENT OF CHEMISTRY COLLEGE OF ARTS AND SCIENCES KANSAS STATE UNIVERSITY Manhattan, Kansas 2010 Abstract This dissertation reports the colloidal synthesis of iron silicide, hafnium oxide core-gold shell and water soluble iron-gold alloy for the first time. As the first part of the experimentation, plasmonic and superparamagnetic nanoparticles of gold and iron are synthesized in the form of core-shell and alloy. The purpose of making these nanoparticles is that the core-shell and alloy nanoparticles exhibit enhanced properties and new functionality due to close proximity of two functionally different components. The synthesis of core-shell and alloy nanoparticles is of special interest for possible application towards magnetic hyperthermia, catalysis and drug delivery. The iron-gold core-shell nanoparticles prepared in the reverse micelles reflux in high boiling point solvent (diphenyl ether) in presence of oleic acid and oleyl amine results in the formation of monodisperse core-shell nanoparticles. The second part of the experimentation includes the preparation of water soluble iron- gold alloy nanoparticles. The alloy nanoparticles are prepared for the first time at relatively low temperature (110 oC). The use of hydrophilic ligand 3-mercapto-1-propane sulphonic acid ensures the aqueous solubility of the alloy nanoparticles. Next, hafnium oxide core-gold shell nanoparticles are prepared for the first time using high temperature reduction method. These nanoparticles are potentially important as a high κ material in semiconductor industry. Fourth, a new type of material called iron silicide is prepared in solution phase. The material has been prepared before but not in a colloidal solution. The Fe3Si obtained is superparamagnetic. Another phase β-FeSi2 is a low band gap (0.85 eV) semiconductor and is sustainable and environmentally friendly. At last, the iron monosilicide (FeSi) and β-FeSi2 are also prepared by heating iron-gold core-shell and alloy nanoparticles on silicon (111) substrate. The nucleation of gaseous silicon precursor on the melted nanoparticles results the formation of nanodomains of FeSi and β-FeSi2. A practical application of these nanoparticles is an important next step of this research. Further improvement in the synthesis of β-FeSi2 nanoparticles by colloidal synthetic approach and its application in solar cell is a future goal. SYNTHESIS AND CHARACTERIZATIONS OF NOVEL MAGNETIC AND PLASMONIC NANOPARTICLES by NAWEEN DAHAL B.S., TRIBHUVAN UNIVERSITY, 1995 M.S., TRIBHUVAN UNIVERSITY, 1997 A DISSERTATION Submitted in partial fulfillment of the requirements for the degree DOCTOR OF PHILOSOPHY DEPARTMENT OF CHEMISTRY COLLEGE OF ARTS AND SCIENCES KANSAS STATE UNIVERSITY Manhattan, Kansas 2010 Approved by: Major Professor VIKTOR CHIKAN Copyright NAWEEN DAHAL 2010 Abstract This dissertation reports the colloidal synthesis of iron silicide, hafnium oxide core-gold shell and water soluble iron-gold alloy for the first time. As the first part of the experimentation, plasmonic and superparamagnetic nanoparticles of gold and iron are synthesized in the form of core-shell and alloy. The purpose of making these nanoparticles is that the core-shell and alloy nanoparticles exhibit enhanced properties and new functionality due to close proximity of two functionally different components. The synthesis of core-shell and alloy nanoparticles is of special interest for possible application towards magnetic hyperthermia, catalysis and drug delivery. The iron-gold core-shell nanoparticles prepared in the reverse micelles reflux in high boiling point solvent (diphenyl ether) in presence of oleic acid and oleyl amine results in the formation of monodisperse core-shell nanoparticles. The second part of the experimentation includes the preparation of water soluble iron- gold alloy nanoparticles. The alloy nanoparticles are prepared for the first time at relatively low temperature (110 oC). The use of hydrophilic ligand 3-mercapto-1-propane sulphonic acid ensures the aqueous solubility of the alloy nanoparticles. Next, hafnium oxide core-gold shell nanoparticles are prepared for the first time using high temperature reduction method. These nanoparticles are potentially important as a high κ material in semiconductor industry. Fourth, a new type of material called iron silicide is prepared in solution phase. The material has been prepared before but not in a colloidal solution. The Fe3Si obtained is superparamagnetic. Another phase β-FeSi2 is a low band gap (0.85 eV) semiconductor and is sustainable and environmentally friendly. At last, the iron monosilicide (FeSi) and β-FeSi2 are also prepared by heating iron-gold core-shell and alloy nanoparticles on silicon (111) substrate. The nucleation of gaseous silicon precursor on the melted nanoparticles results the formation of nanodomains of FeSi and β-FeSi2. A practical application of these nanoparticles is an important next step of this research. Further improvement in the synthesis of β-FeSi2 nanoparticles by colloidal synthetic approach and its application in solar cell is a future goal. Table of Contents List of Figures ................................................................................................................................. x List of Tables ............................................................................................................................... xvi Acknowledgements ..................................................................................................................... xvii Dedication .................................................................................................................................... xix Preface........................................................................................................................................... xx CHAPTER 1 - Introduction ............................................................................................................ 1 Importance of nanoparticles and nanochemistry ........................................................................ 1 Plasmonic nanomaterials ............................................................................................................ 2 Magnetic nanomaterials .............................................................................................................. 6 Semiconducting nanoparticles /quantum dots .......................................................................... 12 Nucleation and growth in colloidal synthesis ......................................................................... 17 CHAPTER 2 - Synthesis and characterizations of Fe-Au core-shell Nanoparticles .................. 26 Introduction ............................................................................................................................... 26 Experimental ............................................................................................................................. 27 Results and discussion .............................................................................................................. 30 Conclusions: .............................................................................................................................. 44 References: ................................................................................................................................ 45 CHAPTER 3 - Synthesis and characterizations of Water-Soluble Iron-Gold Alloy Nanoparticles ............................................................................................................................................... 49 Introduction ............................................................................................................................... 49 Experimental Section ................................................................................................................ 50 Preparation of Fe-Au Alloy Nanoparticles from Iron Sulphate Heptahydrate: ........................ 51 Preparation of Fe-Au Alloy Nanoparticles from Iron Pentacarbonyl: ...................................... 52 Results and Discussion ............................................................................................................. 52 Conclusions: .............................................................................................................................. 73 References ................................................................................................................................. 73 CHAPTER 4 - Synthesis of HfO2 @ Au Core-Shell Nanoparticles ............................................. 76 Introduction ............................................................................................................................... 76 Experimental section ................................................................................................................. 77 viii Results and discussion .............................................................................................................. 78 Conclusions ............................................................................................................................... 88 References ................................................................................................................................
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