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Understanding Fundamentals of Plasmonic Nanoparticle Self-Assembly at Liquid-Air

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Understanding Fundamentals of Plasmonic Nanoparticle Self-Assembly at Liquid-Air A Dissertation entitled Understanding Fundamentals of Plasmonic Nanoparticle Self-assembly at Liquid-air Interface by Chakra P. Joshi Submitted to the Graduate Faculty as partial fulfillment of the requirements for the Doctor of Philosophy Degree in Chemistry _________________________________________ Dr. Terry P. Bigioni, Committee Chair _________________________________________ Dr. Dragan Isailovic, Committee Member _________________________________________ Dr. Mark Mason, Committee Member _________________________________________ Dr. Jacques G. Amar, Committee Member _________________________________________ Dr. Patricia R. Komuniecki, Dean College of Graduate Studies The University of Toledo December 2013 Copyright 2013, Chakra P. Joshi This document is copyrighted material. Under copyright law, no parts of this document may be reproduced without the expressed permission of the author. An Abstract of Understanding Fundamentals of Plasmonic Nanoparticle Self-assembly at Liquid-air Interface by Chakra P. Joshi Submitted to the Graduate Faculty as partial fulfillment of the requirements for the Doctor of Philosophy Degree in Chemistry The University of Toledo December 2013 Two-dimensional self-assemblies of plasmonic nanoparticles (NPs) could one day become a useful technology for mankind as it has a potential to produce desirable structures with various patterning and ordering that is difficult to achieve by the top- down approach. Furthermore, these patterned and ordered structures of NPs have been known to display interesting optoelectronic properties. While applications using self- assemblies of plasmonic NPs seem promising, the fundamental forces that govern the evolution of these structures are not fully understood yet. Interesting similarities between the interfacial NP self-assembly and epitaxial growth exist despite a number of differences such as diffusion, desorption, coalescence, and ordering. The goal of this dissertation is to determine to what extent established submonolayer epitaxy theories can be applied to modeling interfacial NP self-assembly, and thereby develop new tools for understanding NP-NP interactions and self-assembly. Different sizes of 1-dodecanethiol (DDT) capped Au NPs were used to study the submonolayer growth behavior of NP islands. However, for the study, synthesizing DDT iii Au NPs > 8 nm by a conventional method was a challenge. To solve this synthesis problem, large NPs were synthesized in water and a phase transfer-based method was developed and used. While solving this synthesis problem, we developed general guidelines for NP phase transfer and determined that successful phase transfer only depended on three key surfactant parameters: bulkiness, length, and ability to get onto the interface. Furthermore, we also shed light on the mechanistic details of NP phase transfer into the organic medium. The experimental results for the submonolayer growth study such as NP island size distribution (ISD), capture zone distribution (CZD), percolation threshold, diffusion, and flux were compared and contrasted with the known epitaxy theories. It was found that islands were compact and circular at low coverages, while at high coverages they were blobby and irregular due to coalescence. In addition, the critical nucleus size (i) was found to depend on NP size. Surprisingly, it was also found that for smaller NPs, ISDs and CZDs were described better by a Gamma function rather than the proposed scaling forms for the ISDs and CZDs. In stark contrast with epitaxy, interesting yet puzzling behavior of island ordering (due to a long-range repulsive interaction among islands) was also observed. We proposed that this repulsive interaction was due to a dipole-dipole interaction that could originate from an anisotropic distribution of thiol molecules around the NPs at the liquid- air interface. This idea was supported by Monte Carlo simulations that take into account dipole-dipole interactions. iv Dedicated to my family and friends Acknowledgements I am deeply indebted to a number of people for their outstanding support during my graduate career at The University of Toledo. First, I would like to thank my advisor Dr. Terry Bigioni for welcoming me in his laboratory. It was a great learning experience under him on chemistry and philosophy. It made me more independent, knowledgeable, and confident in my life. I would like to convey my special thanks to Dr. Jacques G. Amar for his collaboration in this project. Besides being a committee member, he also helped me to better understand the project. I would also like to thank my committee members Dr. Dragan Isailovic, Dr. Mark Mason, and Dr. Cora Lind for their outstanding support and guidance during my graduate career. I would also like to thank Mr. Brian Ashenfelter for correcting and improving my English grammar. I am also very grateful to our group and Dr. Amar group members for sharing their expertise. It is my pleasure to acknowledge all faculty and staff at the Department of Chemistry for their support. The author would like to acknowledge support from the National Science Foundation (NSF grant CHE-1012896) for the work carried out in this dissertation. Last but not the least, many thanks go to my family back in Nepal making me feel strong and relentless, throughout my graduate program. vi Table of Contents Abstract ............................................................................................................................. iii Acknowledgements .......................................................................................................... vi Table of Contents ............................................................................................................ vii List of Tables ................................................................................................................... xii List of Figures ................................................................................................................. xiii List of Abbreviations ..................................................................................................... xix 1 Introduction ............................................................................................................... 1 1.1 Molecular and nano-scale forces .......................................................................... 1 1.2 Goals of the dissertation research......................................................................... 9 1.3 The scope of the dissertation .............................................................................. 10 2 Synthesis and characterization of nanoparticles .................................................. 11 2.1 Introduction ........................................................................................................ 11 2.2 Salt reduction method......................................................................................... 12 2.3 Dodecanethiolated Au nanoparticles .................................................................. 12 2.4 Experimental section .......................................................................................... 14 2.4.1 Materials ..................................................................................................... 14 2.4.2 Synthesis of 6 nm DDT Au nanoparticles .................................................. 14 vii 2.4.3 Synthesis of 4.9 and 8 nm DDT Au nanoparticles...................................... 15 2.4.4 Synthesis of aqueous citrate Au nanoparticles............................................ 16 2.5 Characterization ................................................................................................. 16 2.5.1 Citrate Au nanoparticle sample preparation for electron microscopy ........ 16 2.5.2 Dodecanethiol Au NP sample preparation for electron microscopy .......... 17 2.5.3 Nanoparticle size distribution analysis using ImageJ ................................. 17 2.6 Results and discussion ........................................................................................ 22 2.7 Conclusion .......................................................................................................... 24 3 General guidelines for aqueous metal nanoparticle phase transfer.................... 25 3.1 Introduction ........................................................................................................ 26 3.2 Experimental section .......................................................................................... 28 3.2.1 Chemicals .................................................................................................... 28 3.2.2 Synthesis of citrate Au nanoparticles .......................................................... 29 3.2.3 Synthesis of citrate Ag nanoparticles .......................................................... 29 3.2.4 Synthesis of p-MBA stabilized Ag nano-clusters ....................................... 30 3.2.5 Synthesis of plasmonic p-MBA Ag nanoparticles ...................................... 30 3.2.6 Synthesis of citrate stabilized CdSe quantum dots (QDs) .......................... 30 3.2.7 Phase transfer of citrate Au nanoparticles using TOAB and CTAB .......... 31 3.2.8 DDT Au nanoparticles (~ 13 nm) procured via phase transfer ................... 31 3.3 Characterization ................................................................................................. 32 3.3.1 Citrate Au nanoparticles ............................................................................
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