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Molecular Thermodynamics of Superheated Lipid-Coated Fluorocarbon Nanoemulsions

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Molecular Thermodynamics of Superheated Lipid-Coated Fluorocarbon Nanoemulsions Molecular Thermodynamics of Superheated Lipid-Coated Fluorocarbon Nanoemulsions by PAUL A. C. MOUNTFORD B.S., University of Colorado Boulder, 2010 M.S., University of Colorado Boulder, 2011 A thesis submitted to the Faculty of the Graduate School of the University of Colorado in partial fulfillment Of the requirement for the degree of Doctor of Philosophy Department of Mechanical Engineering 2015 This thesis entitled: Molecular Thermodynamics of Superheated Lipid-Coated Fluorocarbon Nanoemulsions written by Paul Mountford has been approved for the Department of Mechanical Engineering Professor Mark Borden Mechanical Engineering, University of Colorado Boulder Professor Todd Murray Mechanical Engineering, University of Colorado Boulder Professor Yifu Ding Mechanical Engineering, University of Colorado Boulder Date: July 17, 2015 The final copy of this thesis has been examined by the signor, and finds that both the content and the form meet acceptable presentation standards of scholarly work in the above mentioned discipline. Abstract Mountford, Paul (Ph.D., Mechanical Engineering) Molecular Thermodynamics of Superheated Lipid-Coated Fluorocarbon Nanoemulsions Thesis directed by Associate Professor Mark Borden Diagnostic ultrasound is a safe, inexpensive and highly portable real-time imaging modality for viewing the human body. For over two decades, lipid-coated fluorocarbon microbubble contrast agents have been developed to help improve the diagnostic and therapeutic capabilities of ultrasound, but they have certain limitations. Recently, it was found that the microbubbles can be condensed into superheated liquid nanodrops capable of being vaporized by external optical or acoustic triggers. The compact form and vaporization effects of these phase-shift nanodrops may offer advantages over microbubbles for a number of current and future therapeutic and diagnostic applications. The goal of this dissertation work was to study the molecular thermodynamics and interfacial phenomena of these superheated phase-shift nanodrops. In the first part of this work, a custom microscopy pressure chamber with control over temperature and pressure was used to observe microbubbles during condensation. Compression behaviors of fluorocarbon microbubbles constructed with lipid shells of varying acyl chain lengths were quantified over a broad temperature range. Microbubbles containing lipids of longer acyl chains were found to resist ideal compression and condensation. Dissolution was found to dominate as temperature approached the lipid main phase transition temperature, resulting in incomplete condensation. However, successful condensation of gas-filled microbubbles to liquid- filled nanodrops could be achieved at lower temperatures, and fluorescence microscopy showed that the lipid monolayer shell buckles and folds into surface-attached bilayer strands. The iii nanodrops were found to be remarkably stable when brought back to standard temperature and pressure. The temperature-pressure data were used to construct condensation phase diagrams to determine the thresholds for successful nanodrop formation. In the second part of this study, the superheated nanodrops were vaporized back into microbubbles by changes in temperature and pressure. A custom optical chamber with control over temperature and pressure was used to track the kinetics of condensation, vaporization and dissolution of microbubble suspensions with varying fluorocarbon core and lipid shell compositions. A simple model was used to extract kinetic rates from the optical data, and Arrhenius plots were used to determine activation energies. The activation energy for thermal vaporization was found to vary with lipid acyl chain length, and a simple model of lipid intermolecular forces was used to explain this effect. Additionally, thermal vaporization was found to occur near 90% of the critical temperature of the fluorocarbon core, indicating that metastability of the superheated droplets was due to the low probability of homogenous nucleation rather than a Laplace overpressure. The superheated droplets could be reversibly vaporized and condensed to at least ten cycles, showing remarkable stability. In the final part of this study, the tunability of vaporization was examined through the mixing of fluorocarbon gases in droplet core. A clinical ultrasound imaging system was used to track vaporization as a function of temperature and mechanical index. Discrepancies were found in the vaporization thresholds owing to mass transfer; the high solubility of the lower fluorocarbon caused it to rapidly deplete. However, a successful acoustic temperature probe was demonstrated. The experimental data from all three parts of this study were examined and explained by conventional molecular thermodynamics theory, providing new insights into the behavior and properties of these novel theranostic agents. iv To my comrade, my brother Samuel C. B. Mountford v Upon being cut from the high school freshman basketball team, my father, Dr. Mark C. Mountford, provided me with this quote: It is not the critic who counts; not the man who points out how the strong man stumbles, or where the doer of deeds could have done them better. The credit belongs to the man who is actually in the arena, whose face is marred by dust and sweat and blood; who strives valiantly; who errs, who comes short again and again, because there is no effort without error and shortcoming; but who does actually strive to do the deeds; who knows great enthusiasms, the great devotions; who spends himself in a worthy cause; who at the best knows in the end the triumph of high achievement, and who at the worst, if he fails, at least fails while daring greatly, so that his place shall never be with those cold and timid souls who neither know victory nor defeat. - Theodore Roosevelt, 1910 It has resonated with me ever since and is embedded in this work. vi Acknowledgements First I would like to thank my advisor and mentor Dr. Mark Borden. He welcomed me into his lab with an unparalleled desire to teach and motivate. He was consistently critical and excited about this work and provided remarkable guidance throughout the past four years. He allowed me to “skin the cat” how I saw fit and utilize my skill sets while suggesting improvements as needed. He has been an exceptional mentor and friend. For this I am truly grateful. I would like to thank the entire Borden lab. I would like to thank Dr. Jake Dove for continuously sharing exciting results and knowledge which unveiled the fundamental mechanisms of this work. I would like to personally give thanks to Dr. Shashank Sirsi for having introduced me to the Borden lab. He took me under his wing and showed me how to become a graduate researcher. Additionally, he contributed to this work without hesitation and allowed me to collaborate on his studies as his peer. From the first day I joined the group he supported my research and treated me like a fellow scientist. He remains a great friend and collaborator. I would like to thank Julie Bielinski for being the constant light at the end of the tunnel during the final enduring year of this graduate work. Finally I would like to thank my family. My mother, Prof. Gillian Collie, who taught me to be critical of the world I live in since I could remember. My father, Dr. Mark Mountford, who taught me to appreciate the struggles and failures associated with success. My stepfather, John Moser, who motivated me to use my mind over my body and taught me that expedited respect is obtained through kindness. My brother, Samuel Mountford, who taught me how to be a mentor and take criticism with a light heart. vii Contents Abstract…………………………………………………………………………………………...iii Dedication…………………………………………………………………………………………v Acknowledgements………………………………………………………………………………vii Contents…………………………………………………………………………………………viii Tables……………………………………………………………………………………………xiii Figures…………………………………………………………………………………………..xiii Chapter 1 Introduction……………………………………………………………………………..1 1.1 Specific Aims………………………………………………………………………….1 1.2 Microbubbles…………………………………………………………………………..3 1.2.1 Microbubble Design and Behavior…………………………………………..3 1.2.2 Microbubbles for Diagnostic Imaging……………………………………….9 1.2.3 Microbubbles for Therapy………………………………………………….13 1.3 Phase Change Agents………………………………………………………………...17 1.3.1 Fluorocarbon Phase-Shift Droplets for Imaging and Therapy……………...17 1.3.2 Phase-Shift Droplet Fabrication and Actuation…………………………….21 1.3.3 Dual-Component PFC Droplets……………………………………………23 1.4 Microbubble Condensed Droplets……………………………………………………23 1.4.1 Condensation……………………………………………………………….23 1.4.2 Vaporization………………………………………………………………..25 1.5 Dissertation Objectives………………………………………………………………26 Chapter 2 Condensation and Vaporization Pure Fluorocarbon Drops……………………………37 2.1 Introduction…………………………………………………………………………..37 viii 2.2 Classical Phase-Shift Thermodynamics……………………………………………...38 2.2.1 Intermolecular Forces………………………………………………………38 2.2.2 Macroscopic Phase Change Behavior………………………………………40 2.2.3 The Effect of the Laplace Pressure on Condensation and Vaporization……44 2.3 Condensation of a Supersaturated Pure Fluorocarbon……………………………….47 2.3.1 Homogeneous Nucleation in a Supersaturated Fluorocarbon Gas…………47 2.3.2 Supersaturation Limit………………………………………………………52 2.4 Vaporization of a Superheated Pure Fluorocarbon…………………………………...57 2.4.1 Homogeneous Nucleation in a Superheated Fluorocarbon Liquid…………57 2.4.2 Limit of Superheat………………………………………………………….60 2.5 Conclusions…………………………………………………………………………..61 Chapter 3 Condensation
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