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INVESTIGATION of STRUCTURAL EFFECTS on the AC MAGNETIC PROPERTIES of IRON OXIDE NANOPARTICLES by ERIC C. ABENOJAR Submitted in P

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INVESTIGATION of STRUCTURAL EFFECTS on the AC MAGNETIC PROPERTIES of IRON OXIDE NANOPARTICLES by ERIC C. ABENOJAR Submitted in P INVESTIGATION OF STRUCTURAL EFFECTS ON THE AC MAGNETIC PROPERTIES OF IRON OXIDE NANOPARTICLES by ERIC C. ABENOJAR Submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy Dissertation Adviser: Prof. Anna Cristina S. Samia Department of Chemistry CASE WESTERN RESERVE UNIVERSITY May, 2018 i CASE WESTERN RESERVE UNIVERSITY SCHOOL OF GRADUATE STUDIES We hereby approve the thesis/dissertation of ERIC C. ABENOJAR Candidate for the degree of Doctor of Philosophy*. Committee Chair Prof. Geneviève Sauvé (Department of Chemistry, CWRU) Committee Member Prof. Clemens Burda (Department of Chemistry, CWRU) Committee Member Prof. Carlos E. Crespo-Hernández (Department of Chemistry, CWRU) Committee Member Prof. Anna Cristina S. Samia (Department of Chemistry, CWRU) Committee Member Prof. João Maia (Department of Macromolecular Science and Engineering, CWRU) Date of Defense December 18, 2017 *We also certify that written approval has been obtained for any proprietary material contained therein. ii Table of Contents List of Tables ................................................................................................................... viii List of Figures .................................................................................................................... ix List of Symbols and Abbreviations................................................................................. xxii Acknowledgements ........................................................................................................ xxvi Abstract ........................................................................................................................ xxviii Chapter 1. Introduction to Nanomaterials ............................................................................1 1.1 General Introduction ..................................................................................................1 1.2 Fundamentals of Nanomagnetism..............................................................................2 1.2.1 Magnetic materials ..............................................................................................2 1.2.2 Superparamagnetism ...........................................................................................2 1.2.3 Iron Oxide Spinel Ferrites ...................................................................................5 1.3 Synthetic Methods .....................................................................................................6 1.4 Magnetic Hyperthermia .............................................................................................7 1.4.1 Heating of Magnetic Nanoparticles in an AC field ............................................8 1.4.2 Magnetic Hyperthermia Measurement .............................................................11 1.4.2.1 Calorimetric Method .............................................................................11 1.4.2.2 Magnetometric Method .........................................................................12 1.5 Magnetic Particle Imaging (MPI) ............................................................................13 1.5.1 Emerging Research Directions: Magnetic Imaging Guided–Hyperthermia .....15 1.6 Nanoparticle Characterization Methods ..................................................................17 1.6.1 Spectroscopic methods......................................................................................17 iii 1.6.1.1 Fourier-Transform Infrared Spectroscopy (FT-IR) ...............................17 1.6.1.2 Atomic Absorption Spectroscopy (AAS) ..............................................18 1.6.1.3 Energy Dispersive X-ray (EDS) ............................................................19 1.6.2 Electron Microscopy Methods ..........................................................................19 1.6.2.1 Transmission Electron Microscopy (TEM) ...........................................19 1.6.2.2 Scanning Electron Microscopy (SEM) ..................................................20 1.6.3 Thermogravimetric Analysis (TGA) .................................................................21 1.6.4 Powder X-ray Diffraction (PXRD) ...................................................................21 1.6.5 Dynamic Light Scattering (DLS) ......................................................................22 1.7 References ................................................................................................................23 Chapter 2. Size and Matrix Effect on the Magnetic Hyperthermia Properties of Iron Oxide Magnetite Nanoparticles ....................................................................................................29 2.1 Introduction ..............................................................................................................29 2.2 Experimental Methods .............................................................................................32 2.2.1 Materials and Reagents .....................................................................................32 2.2.2 Nanoparticle Synthesis and Nanocomposite Fabrication .................................32 2.2.2.1 Synthesis of Magnetite Nanoparticles ...................................................32 2.2.2.2 Fabrication of Fe3O4-PE Nanocomposite Films ...................................34 2.2.3 Fe3O4 NP Characterization ...............................................................................34 2.2.4 Fe3O4-PE Nanocomposite Characterization .....................................................35 2.2.5 Fe3O4 NP and Fe3O4-PE Nanocomposite Magnetic Characterization ............35 2.2.6 Magnetic Hyperthermia Measurements ............................................................36 2.3 Results and Discussion ............................................................................................37 iv 2.3.1 Structural and Magnetic Properties of the Synthesized Fe3O4 NPs .................37 2.3.2 Structural and Magnetic Properties of the Fe3O4-PE Nanocomposites ...........39 2.3.3 Magnetic Hyperthermia Properties ...................................................................41 2.3.3.1 Effect of NP Size and Immobilization ..................................................41 2.3.3.2 Effect of Varying the Alternating Current (AC) Magnetic Field Amplitude ..........................................................................................................45 2.4 Conclusions ..............................................................................................................46 2.5 References ................................................................................................................47 Chapter 3. Thermoresponsive Magnetic Hydrogel Nanocomposite for Combined Thermal and D-Amino Acid Assisted Biofilm Disruption...............................................................51 3.1 Introduction ..............................................................................................................51 3.2 Materials and Methods .............................................................................................56 3.2.1 Materials and Reagents .....................................................................................56 3.2.2 Synthesis of Iron Oxide (Fe3O4) nanoparticles ................................................56 3.2.2.1 Synthesis of Spherical Iron Oxide Nanoparticles ..................................56 3.2.2.2 Synthesis of Cubic Iron Oxide Nanoparticles .......................................57 3.2.3 Synthesis of Glycol Chitin Hydrogel ................................................................58 3.2.4 Preparation of Magnetic Hydrogels Using Water Soluble Fe3O4 Nanoparticles .....................................................................................................58 3.2.5 Biofilm Formation and Dispersal Assays .........................................................59 3.2.6 Magnetic Hyperthermia Aided Biofilm Dispersal Assays ................................59 3.2.7 Cell Viability Assays ........................................................................................60 3.2.8 Statistical analyses ............................................................................................60 v 3.3 Results and Discussion ............................................................................................61 3.3.1 Dose Dependent Effect of Antibiotics on S. Aureus Biofilm Disruption .........61 3.3.2 Concentration Dependent Effect of Amino Acids on S. Aureus Biofilm Disruption ..........................................................................................................63 3.4 Magnetic Hyperthermia Performance Evaluation of Fe3O4 Spheres and Cube for Biofilm Disruption .........................................................................................................69 3.5 Preparation of Magnetic Thermoresponsive Glycol Chitin Hydrogel ........................................................................................................................73 3.6 Biofilm Disruption Using D-AA Loaded Magnetic Thermoresponsive Glycol Chitin Hydrogel ........................................................................................................................77 3.7 Conclusions ..............................................................................................................79 3.8 References ................................................................................................................79
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