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Polyelectrolyte Complexes Based on Poly(Acrylic Acid): Mechanics and Applications

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Polyelectrolyte Complexes Based on Poly(Acrylic Acid): Mechanics and Applications University of Central Florida STARS Electronic Theses and Dissertations, 2004-2019 2018 Polyelectrolyte Complexes Based on Poly(acrylic acid): Mechanics and Applications Xiaoyan Lu University of Central Florida Part of the Chemistry Commons Find similar works at: https://stars.library.ucf.edu/etd University of Central Florida Libraries http://library.ucf.edu This Doctoral Dissertation (Open Access) is brought to you for free and open access by STARS. It has been accepted for inclusion in Electronic Theses and Dissertations, 2004-2019 by an authorized administrator of STARS. For more information, please contact [email protected]. STARS Citation Lu, Xiaoyan, "Polyelectrolyte Complexes Based on Poly(acrylic acid): Mechanics and Applications" (2018). Electronic Theses and Dissertations, 2004-2019. 5769. https://stars.library.ucf.edu/etd/5769 POLYELECTROLYTE COMPLEX BASED ON POLY(ACRYLIC ACID): MECHANICS AND APPLICATIONS by XIAOYAN LU M.S. Beijing Institute of Technology, 2012 B.S. Taishan University, 2009 A dissertation submitted in partial fulfilment of the requirements for the degree of Doctor of Philosophy in the Department of Chemistry in the College of Science at the University of Central Florida Orlando, Florida Spring Term 2018 Major Professor: Lei Zhai c 2018Xiaoyan Lu ii ABSTRACT Poly(acrylic acid) (PAA) is a weak polyelectrolyte presenting negative charge at basic condition when the carboxylic group loses a proton. These carboxylate group can interact with polycations and metal ions to form stable polyelectrolyte complexes (PECs), leading to tunable properties and multifunctional nanoscale structures through chemical reactions. This research focuses on nanofiber and nanoparticle fabricated by PAA-based PECs. We demonstrated the effect of ferric ion concentration on the mechanical properties of PAA-based single naonofiber by using dark field microscopy imaging and persistence length analysis. The application of PAA-based nanofiber mats loaded with MnO2 for supercapacitors was also explored. As a free-standing and flexible supercapacitor electrode, the nanofiber mat exhibited outstanding properties including high specific capacitance, excellent reversible redox reactions, and fast charge/discharge ability. Since PAA is a biocompatible polymer, PAA-based PEC was applied as a drug-carrier in a drug delivery system. In this project, core-shell nanoparticles were fabricated with chitosan as the core and PAA as the shell to incorporate with the drug gemcitabine. Several parameters were investigated to obtain the optimal nanoparticle size. The as-prepared drug delivery system shows prolonged releasing profile. iii ACKNOWLEDGMENTS I am extremely thankful to Dr. Lei Zhai for being my dissertation advisor. I do not have enough words to describe my respect and gratitude for him. His constant support towards my research and academics in general made me more professional. I feel extremely thankful to to have him as my mentor and supervisor. He is not only an advisor, but also a good friend. I am also very grateful to Dr. Shengli Zou, Dr. Demitry Kolpashchikov, Dr. Karin Chumbimuni- Torres, and Dr. Yajie Dong for being part of my dissertation committee and for their encouraging and valuable comments and remarks. Each one of them is my role model for study and research. I gratefully acknowledge the support provided by the department of Chemistry, Nanoscience and Technology Center (NSTC), and Advanced Materials Processing and Analysis Center (AMPAC).I am also thankful to Ernie, Ted, Kirk, Matt, Mikhail and Karen for their help in the usages of instrumentations. I would also like to thank all my lab-mates Astha Malhotra, Jean Calderon, Matthew McInnis, Chen Shen, Nilab Azim, Zeyang Zhang, Elizabeth Barrios; my undergraduate researchers Ruginn Catarata and Olivia McClellan and the colleagues, like Angie Diaz from collaborating labs. It was a pleasure working with them. I am also immensely thankful to my friends who helped my stay here more enjoyable and my friends in China and around whose encouragement has really been a great support to me here in a foreign land. Words or expressions are not enough to thank my husband and parents, back home for their pa- tience, support, understanding and sacrifices. I have to thank my sisters for being there for me and encouraging me. My baby Daniel highly motivates me to acheive the study accomplishement. iv I would also like to express my thanks and sincere regards to everyone else whose help, encour- agement and prayers must have strengthened me and helped me achieve things in life. Finally but most importantly, I have to thank GOD for his continuous love and amazing grace. Without him, I couldn’t do anything. v TABLE OF CONTENTS LIST OF FIGURES . xi LIST OF TABLES . xx CHAPTER 1: INTRODUCTION . 1 Polyelectrolyte . 1 Polyelectrolyte complex . 4 Nanostructure of polyelectrolyte and PEC . 8 PEC nanoparticle . 8 PEC nanofiber . 10 PEC membrane . 14 PEC hydrogel . 16 Application of polyelectrolyte complex . 19 Biotechnology . 19 Tissue engineering . 19 Drug delivery . 21 Gene delivery . 23 vi Wound self-healing . 25 Actuator . 27 Energy storage . 28 Theme of the research . 29 CHAPTER 2: TUNABLE EFFECT OF METAL IONS ON POLYELECTROLYTE NANOFIBER MECHANICAL PERFORMANCE . 31 Abstract . 31 Introduction . 31 Materials and Methods . 35 Nanofiber synthesis by elecrospinning . 35 Scanning electron microscopy and transmission electron microscopy . 35 Fourier Transform Infrared Spectroscopy (FTIR) . 36 Confocal microscopy imaging and bending mechanics data analysis . 36 Results and Discussion . 37 Ferric ions modulate the mechanical properties and average length of polyacrylic acid nanofibers. 37 Chitosan helps ferric ions modulate the mechanical properties of PAA nanofibers. 43 Electrospun PAA:CS nanofibers could exist in hydrated states. 45 vii Characterization sheds light on how ferric metal ions affect individual PAA:CS nanofiber structure. 47 Conclusion . 51 CHAPTER 3: FLEXIBLE CORE-SHELL COMPOSITE FIBERS FOR HIGH PERFOR- MANCE SUPERCAPACITOR ELECTRODES . 52 Abstract . 52 Introduction . 53 Experimental Procedure . 55 Materials . 55 Materials synthesis . 56 Fabrication of Nanofibers . 56 Creating MnO2 Nanoparticles on PAA Nanofibers . 56 Depositing the Polypyrrole Shell on the Surface of MnO2@PAA Nanofibers ................................... 57 Characterization . 57 Results and Discussion . 59 Preparation of supercapacitor electrodes . 59 Electrochemical Characterization . 77 viii Conclusion . 83 CHAPTER 4: GEMCITABINE LOADED POLY(ACRYLIC ACID)-CHITOSAN NANOPAR- TICLES FOR TARGETED THERAPY OF PANCREATIC CANCER . 84 Abstract . 84 Introduction . 84 Experimental Procedure . 87 Materials . 87 Fabrication of Nanofibers . 88 Characterization of the nanoparticles . 89 Incubation and encapsulation . 90 In vitro drug releasing . 90 Results and Discussion . 91 Effect of CS:TPP ratio on CS/TPP nanoparticle properties . 91 Effect of PAA:CS ratio on CS/TPP nanoparticle properties . 93 Effect of CS:EDC ratio on CS/TPP-PAA nanoparticle properties . 95 Effect of pH value on CS/TPP-PAA nanoparticle properties . 97 In vitro drug releasing study . 99 ix Conclusion . 100 CHAPTER 5: SUMMARY . 101 APPENDIX A: LIST OF PUBLICATIONS . 103 APPENDIX B: PERMISSIONS FOR COPYRIGHTED MATERIALS . 105 Permission Request Policies from ACS Publications . 106 LIST OF REFERENCES . 107 x LIST OF FIGURES Figure 1.1: Molecular structures of common polyelectrolytes: (a) PSS, (b) PAA, (c) CS, (d) PDADMAC, (e) PAH, and (f) PPy. 3 Figure 1.2: Schematic illustration of three ways in which the addition of a polyelec- trolyte may affect the colloidal stability of negatively charged particles in an aqueous suspension [1]. 4 Figure 1.3: PEC formation by direct method (a) and indirect method (b). 5 Figure 1.4: Mechanism of PEC formation [2]. 6 Figure 1.5: Different dimentions of PEC materials . 8 Figure 1.6: Schematic illustration of PEC nanoparticles of polyanion and polycation at different charge ratios [3]. 10 Figure 1.7: Setup of electrospinning [4]. 11 Figure 1.8: Different poly(L-lactide) (PLA) nanofiber forms at different condition: (A) porous fibers with beads; (B)uniform fibers with high porousity; (C) belt- shaped solid fibers; and (D) aligned uniform solid fibers with a circular cross section. [5]. 13 Figure 1.9: Schematic illustrations of the nanoparticles formation on nanofibers from metal ions with different diffusion profile. [6] . 14 Figure 1.10: Illustration of layer-by-layer assembly. 16 xi Figure 1.11: Deswell and swelling of PEC hydrogels. 18 Figure 1.12: Basic principles of tissue engineering [7]. 20 Figure 1.13: The various uptake pathways of macromolecules and nanoparticles into cells according to size [8]. 22 Figure 1.14: The intracellular journey of gene delivery vectors [9]. 24 Figure 1.15: Schematic mechanism of PEC multilayers for self-healing. 27 Figure 1.16: Schematic mechanism of PEC hydrogel actuator. 28 Figure 2.1: (A) Schematic diagrams of polyacrylic acid (PAA) nanofiber fabrication process by electrospinning. Functional groups with negative charges on PAA and ferric ions associate through ionic interactions. Chitosan (CS) and ferric metal ions (Fe3+).
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