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{Replace with the Title of Your Dissertation} Gas-Phase Synthesis of Gold- and Silica-Coated Nanoparticles A DISSERTATION SUBMITTED TO THE FACULTY OF THE GRADUATE SCHOOL OF THE UNIVERSITY OF MINNESOTA BY Adam Meyer Boies IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY Steven L. Girshick January, 2011 © Adam Meyer Boies 2011 ACKNOWLEDGEMENTS I would like to thank my advisor Professor Steven Girshick, who guided me in both the methods of research and the craft of organizing and presenting ideas. I am grateful for his patience and insightful discussions. The funding for my research came from the National Science Foundation under Award Number CBET-0730184, by the MRSEC Program of the NSF under Award Number DMR-0819885, Nitto Denko Technical Corporation and by the 3M Science and Technology Fellowship. I would also like to thank several research collaborators who were instrumental in my academic development. In particular, I would like to acknowledge Professor Jeffrey Roberts (Purdue University) who actively provided feedback on my research throughout my tenure at the University of Minnesota even after his departure. Professor Joachim Heberlein provided helpful insights into plasma operation. Dr. Ozan Ugurlu (Characterization Facility, UMN) greatly assisted in characterization of samples within the TEM. I would like to thank the following graduate students for their assistance throughout the years: Pingyan Lei and Steven Calder, who collaborated to make many of these studies possible; Dr. Aaron Beaber and Dr. Lejun Qi, who gave me a great introduction to experimental methods within the laboratory; David Rowe and Rebecca Anthony for their thoughtful conversations; and Dr. Anil Bika, Dr. Luke Franklin and Dr. Jacob Swanson, who provided a welcome reprieve academic endeavors. I am also particularly thankful for the collaborations with Professor David Kittelson and Professor Julian Marshal, whose work helped to give me a larger sense of how technology can be applied to meet world challenges. As a part of those studies I also appreciated the contributions of Dr. Winthrop Watts, Professor Elizabeth Wilson, Professor Steven Taff and Professor Tim Smith. My thanks go out to the various departmental staff without whom the construction of my experiments would not be possible. Those staff include Bob Nelson, Robin Russell, Pat Nelson, Peter Zimmermann, Dale Lindbeck and Dave Hultman. I would also like to thank John Gardner for recruiting me to the University of Minnesota and helping with all of the academic paperwork once there. I would thank my wife Abigail Boies who was loving and patient with all of the late nights and early mornings. Last, but not least, I would like to thank all my friends and family for their support and encouragement. i To my wife whose perseverance through adversity serves as constant inspiration ii ABSTRACT Composite nanoparticles consisting of separate core-shell materials are of interest for a variety of biomedical and industrial applications. By combining different materials at the nanoscale, particles can exhibit enhanced or multi- functional behavior such as plasmon resonance combined with superparamagnetism. Gas-phase nanoparticle synthesis processes are promising because they can continuously produce particles with high mass-yield rates. In this dissertation, new methods are investigated for producing gas-phase coatings of nanoparticles in an “assembly-line” fashion. Separate processes are developed to create coatings from silica and gold that can be used with a variety of core-particle chemistries. A photoinduced chemical vapor deposition (photo-CVD) method is used to produce silica coatings from tetraethyl orthosilicate (TEOS) on the surface of nanoparticles (diameter ~5-70 nm). Tandem differential mobility analysis (TDMA) of the process demonstrates that particle coatings can be produced with controllable thicknesses (~1-10 nm) by varying system parameters such as precursor flow rate. Electron microscopy and infrared spectroscopy confirm that the photo-CVD films uniformly coat the particles and that the coatings are silica. In order to describe the coating process a chemical mechanism is proposed that includes gas-phase, surface and photochemical reactions. A chemical kinetics model of the mechanism indicates that photo-CVD coating proceeds primarily through the photodecomposition of TEOS which removes ethyl groups, thus creating activated TEOS species. The activated TEOS then adsorbs onto the surface of the particle where a series of subsequent reactions remove the remaining ethyl groups to produce a silica film with an open site for further attachment. The model results show good agreement with the experimentally measured coating trends, where increased TEOS flow increases coating thickness and increased nitrogen flow decreases coating thickness. iii Gold decoration of nanoparticles is accomplished by evaporation of solid gold in the presence of an aerosol flow. A hot-wire generation method is developed where gold particles are produced from a composite gold-platinum wire. Investigations of the hot-wire generator show that it can produce particles with a range of sizes and that more uniform, non-agglomerated particles are produced when using smaller diameter tubes where gas velocities across the wire are higher and recirculation zones are diminished. When gold is evaporated in the presence of silica nanoparticles, the silica aerosol is decorated by gold through either homogeneous gold nucleation and subsequent scavenging by the silica nanoparticles, or by heterogeneous nucleation on the silica surface in which the gold “balls up” due to the high surface tension of gold on silica. In both cases the resulting particles exhibit a plasmon absorbance resonance typical of gold nanoparticles (λ~550 nm). Finally, the silica coating and gold decoration processes are combined with a thermal plasma technique for synthesizing iron-oxide to produce tri-layer nanoparticles. iv TABLE OF CONTENTS ACKNOWLEDGMENTS .............................................................................................................................. i ABSTRACT .............................................................................................................................................. iii TABLE OF CONTENTS ............................................................................................................................. v LIST OF TABLES .................................................................................................................................. viii LIST OF FIGURES .................................................................................................................................... ix NOMENCLATURE .................................................................................................................................. xix CHAPTER 1 - INTRODUCTION AND MOTIVATION ......................................................... 1 1.1 INTRODUCTION ................................................................................................................................. 1 1.2 MOTIVATION ..................................................................................................................................... 3 1.3 CHARACTERIZATION TECHNIQUES ................................................................................................. 5 1.3.1 Tandem Differential Mobility Analyzer ............................................................................ 5 1.3.2 Chemical Characterization .................................................................................................... 9 1.3.3 Physical Characterization ................................................................................................... 10 CHAPTER 2 - PHOTOINDUCED CHEMICAL VAPOR DEPOSITION PARTICLE COATING .................................................................................................................................... 12 2.1 OVERVIEW ...................................................................................................................................... 12 2.1.1 Photochemical Vapor Deposition Experimental Setup ........................................... 14 2.1.2 Particle Synthesis .................................................................................................................... 17 2.2 TEOS CHARACTERIZATION .......................................................................................................... 19 2.3 SILICA COATING OF SODIUM CHLORIDE AND POLYSTYRENE LATEX PARTICLES .................... 23 2.4 SILICA COATING OF YTTRIUM ALUMINUM OXIDE PARTICLES .................................................. 29 2.5 SILICA COATING OF SILVER PARTICLES ...................................................................................... 33 2.6 SILICA COATING OF IRON OXIDE PARTICLES .............................................................................. 58 2.7 SUMMARY ....................................................................................................................................... 65 CHAPTER 3 - CHEMICAL KINETICS MODEL OF PHOTO-CVD SYSTEM ................... 67 3.1 OVERVIEW ...................................................................................................................................... 67 v 3.2 MODELING ...................................................................................................................................... 69 3.2.1 Model Theory ...........................................................................................................................
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