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Investigation of Nano-Scale, Self-Assembled, Polymeric Systems by Atomic Force Microscopy

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Investigation of Nano-Scale, Self-Assembled, Polymeric Systems by Atomic Force Microscopy Investigation of Nano-Scale, Self-Assembled, Polymeric Systems by Atomic Force Microscopy by James K. Li A thesis submitted in conformity with the requirements for the degree of Doctor of Philosophy Department of Chemistry University of Toronto © Copyright by James K. Li 2010 ii Atomic Force Microscopy of Nano-Scale, Self-Assembled, Polymeric Systems James K. Li Doctor of Philosophy Department of Chemistry University of Toronto 2010 Abstract The atomic force microscope (AFM) was used to study a series of self-assembled systems: alkanethiol self-assembled monolayer (SAM), diblock copolymer thin film, solid supported lipid bilayer membrane, and microgel with double interpenetrating polymer network. In the first system, packing and restructuring of self-assembled monolayers as exhibited by several alkanethiol systems (1-hexanethiol, 1-decanethiol, 11-ferrocenyl-1-undecanethiol) is demonstrated using conducting probe AFM (CP-AFM). Pressure is induced by an AFM tip, and simultaneously, electrical behavior is measured via detection of tunneling currents between metallic tip and substrate. The behavior is fit using a mechanical model that attempts to predict the observed junction resistance as a function of applied force with consideration for mechanical restructuring of the monolayer at higher loads. CP-AFM is also used to study self-assembled thin film of the diblock copolymer polystyrene- block-polyferrocenylsilane (PS-b-PFS) on gold substrate. Simultaneous height and electrical iii current imaging verify the phase separation of the two blocks of the polymer and additionally, distinguish each block due to differential conductivity. The phase separation of multi-component phospholipid bilayers (phosphatidylcholine/ sphingomyelin/ cholesterol) on supporting substrate into liquid-ordered and liquid-disordered phases is demonstrated using both topographical imaging, and the use of force map analysis through tip indentation and rupture measurements. The segregation and differential mechanical stiffness of the phases help to understand the important role of mechanical stability and rigidity membranes. An automated batch analysis process was implemented to facilitate the procedure. The mechanical properties of microfluidically produced microgels (cross-linked sodium alginate and poly(N-isopropylacrylamide)) are measured using indentation experiments, to evaluate the suitability of these gels as cell-mimics. Nanoscale heterogeneities were avoided by using a tipless cantilever. This body of work shows that the alginate content of these microgels can be varied to tune their mechanical properties and that a platform for mechanical measurement of cell and cell-mimics is possible. iv Acknowledgements Foremost, I would like to thank my supervisor committee for guidance in the course of my graduate studies and doctoral research: my Ph.D. advisor Professor Gilbert Walker, and Professor Al-Amin Dhirani and Professor Zhenghong Lu. Moreover from Gilbert, I have learned many lessons equally applicable to other areas outside of scientific research: how to be a good leader, how to bring out potential in others, how to be a good mentor, how to learn. My heartfelt gratitude goes to members of the Walker group, both past and present, for their suggestions and advice during group meetings and in discussion, their help in the lab, and for their support and camaraderie. To Dr. Weiqing Shi, Melissa Paulite, Adrienne Tanur, Isaac Li, Shell Ip, Dr. Nikhil Gunari, Christina MacLaughlin, Toan and Thang Nguyen, Claudia Grozea, Dr. Zahra Fakhraai, Ilia Auerbach-Ziogas, Mandy Koroniak, and Dr. Joyce Guest: graduate student life would not be the same without you! I would especially like to Dr. Shan Zou for inspiring greatness, easing the bumpy transition to research life, and assuaging the concerns of the new graduate student. I am also indebted to Ruby Sullan, who was a constant support throughout graduate school and with whom I've tried to crack the riddle of the Ph.D. 'career'. I am not sure if we were successful, because it was over before we got to the answer. I would like to thank the esteemed scientists I have had the privilege and pleasure to work with in a number of collaborations: Professor Alexei Tivanski, Dr. David Rider, Dr. Jean-Charles Eloi, Dr. Oksana Protsiv, Neta Raz, Professor Ian Manners and Professor Eugenia Kumacheva. I would also like to thank several colleagues from within and outside the Chemistry Department, for their hard work and efforts in informal collaborations and departmental duties, from which I learned something from and was glad that a working relationship and friendship was established: Ethan Tumarkin, Anna Lee, Dr. Mingfeng Wang, Tingbin Lim, Dr. Joyce Dinglasan-Panlillio, Zhibin Wang, and Michelle Xu. I would like acknowledge my friends for lending me an ear when needed, and offering their opinions and advice during the past five years. Although there are too many names to mention, I would like to especially thank Sara Khor, Dr. Bernard Fleet, Ivan Lin, and Bhavin Bijlani. v Lastly I would like to thank my family: for knowing how important this was to me, and for caring. James Li September 13th, 2010 vi Table of Contents Acknowledgements ........................................................................................................................ iv Table of Contents ........................................................................................................................... vi List of Symbols and Abbreviations................................................................................................ xi List of Tables ............................................................................................................................... xiii List of Schematics ........................................................................................................................ xiv List of Figures .............................................................................................................................. xvi 1 Introduction .................................................................................................................................1 1.1 Understanding and Creating at the Nanoscale .....................................................................1 1.2 The Self-Assembly Approach ..............................................................................................2 1.3 Surface Probe Microscopy ...................................................................................................3 1.4 Summary of Thesis ..............................................................................................................4 1.4.1 Use of the Atomic Force Microscope ......................................................................4 1.4.2 Scientific Scope .......................................................................................................4 1.4.3 Self-Assembled Systems ..........................................................................................5 1.4.4 Outline of Experimental Sections ............................................................................5 1.5 References ............................................................................................................................6 2 Tools of the Trade: Concepts in Contact Mechanics and the Atomic Force Microscope ...........8 2.1 Preliminary Mechanics Concepts ........................................................................................8 2.1.1 Hooke’s Law for 1-D Linearly Elastic Materials ....................................................8 2.1.2 Extension to Higher Dimensions: Shear and Poisson’s Ratio .................................9 2.2 Contact Mechanics .............................................................................................................12 2.2.1 The Hertz Model for Non-Adhesive Contact .........................................................12 2.2.2 Shortcomings of the Hertzian Model .....................................................................16 2.3 The Atomic Force Microscope ..........................................................................................18 vii 2.3.1 Contact Mode Imaging ..........................................................................................19 2.3.2 Tapping (Intermittent Contact) Mode Imaging ......................................................20 2.3.3 Force Curve Collection ..........................................................................................21 2.3.4 Force Mapping .......................................................................................................21 2.3.5 Conducting Probe AFM .........................................................................................22 2.4 References ..........................................................................................................................24 3 The Self-Assembled Systems ....................................................................................................29 3.1 Alkanethiol Self-Assembled Monolayers ..........................................................................29 3.2 Diblock Copolymer Thin Films .........................................................................................31 3.2.1 Diblock Copolymers ..............................................................................................31 3.2.2 Microphase Separation of Diblock Copolymers in Bulk .......................................32 3.2.3
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