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2015 Barua Bipul Dissertation.Pdf (5.577Mb) UNIVERSITY OF OKLAHOMA GRADUATE COLLEGE INVESTIGATION OF ELECTROSPINNING PROCESS PARAMETERS AND STUDIES OF STABILIZATION KINETICS OF POLYACRYLONITRILE-BASED ELECTROSPUN CARBON NANOFIBERS A DISSERTATION SUBMITTED TO THE GRADUATE FACULTY in partial fulfillment of the requirements for the Degree of DOCTOR OF PHILOSOPHY By BIPUL BARUA Norman, Oklahoma 2015 INVESTIGATION OF ELECTROSPINNING PROCESS PARAMETERS AND STUDIES OF STABILIZATION KINETICS OF POLYACRYLONITRILE-BASED ELECTROSPUN CARBON NANOFIBERS A DISSERTATION APPROVED FOR THE SCHOOL OF AEROSPACE AND MECHANICAL ENGINEERING BY Dr. Mrinal C. Saha, Chair Dr. M. Cengiz Altan Dr. Zahed Siddique Dr. Yingtao Liu Dr. Daniel E. Resasco © Copyright by BIPUL BARUA 2015 All Rights Reserved. ACKNOWLEDGEMENTS The work presented in this dissertation would not have been possible without my close association with many people. It is a great pleasure to express my sincere gratitude and appreciation to all those who made this dissertation possible. I would first like to thank Dr. Mrinal C. Saha, my dissertation committee chair and advisor, for his dedicated help, advice, inspiration, encouragement and continuous support, throughout my graduate study. I would also like to thank him for keeping his trust in my ability, and giving me the opportunity to work on various interesting research projects. My special words of thanks go to Dr. M. Cengiz Altan for his continuous encouragement and motivation to keep up the good work. I also thank him for providing me with the high voltage power system. I owe my deepest gratitude to Dr. Brian P. Grady for his tireless help with X- ray scattering measurements. I would like to recognize the efforts of the other committee members, Dr. Daniel E. Resasco, Dr. Zahed Siddique, and Dr. Yingtao Liu, for their comments and suggestions which positively guided this work. My heartfelt thanks go to Mr. Billy Mays and Mr. Gregory Williams. The experimental work presented in this study would not have been possible without their help. I also thank Mr. Carl B. Van Buskirk and Mr. Chad E. Cunningham for assisting with high voltage power cable. I would like to extend my gratitude to the all of the faculty and staff members and my colleagues in the AME department at OU. Finally, special recognition goes out to my parents, brother, and Neelima for their continued moral support without which none of this would have been possible. iv TABLE OF CONTENTS ACKNOWLEDGEMENTS ............................................................................................ iv TABLE OF CONTENTS ................................................................................................. v LIST OF TABLES .......................................................................................................... ix LIST OF FIGURES .......................................................................................................... x ABSTRACT .................................................................................................................. xvi Chapter 1: INTRODUCTION .......................................................................................... 1 1.1 Carbon Fibers .......................................................................................................... 1 1.2 Challenges with Conventional Spinning Methods for Further Improving the Mechanical Strength of Carbon Fibers ......................................................................... 6 1.3 Vapor Grown Carbon Fibers and Nanofibers ......................................................... 9 1.4 Carbon Nanotubes ................................................................................................. 11 1.5 Current Challenges with VGCNFs and CNTs ...................................................... 12 1.6 Electrospinning: An Innovative Technique to Produce Continuous Carbon Nanofiber with a High Degree of Morphological and Structural Perfection .............. 13 1.7 Fabrication of ECNFs from PAN Nanofibers ....................................................... 16 1.7.1 PAN ................................................................................................................ 17 1.7.2 Heat Treatment of electrospun PAN Nanofiber ............................................. 20 1.8 Scope of the Work ................................................................................................ 21 PART I: INVESTIGATION OF THE GOVERNING PARAMETERS IN THE ELECTROSPINNING OF POLYACRYLONITRILE NANOFIBERS ........................ 23 Chapter 2: ELECTROSPINNING .................................................................................. 23 2.1 History .................................................................................................................. 23 2.2 Fundamental Theory ............................................................................................. 25 2.3 Applications of Electrospun Nanofibers ............................................................... 27 2.4 Electrospinning Processing Parameters ................................................................ 28 2.4.1 Solution Parameters ....................................................................................... 28 2.4.2 Operational Parameters .................................................................................. 30 2.4.3Environmental Parameters .............................................................................. 31 2.5 Key Research Questions – Part I .......................................................................... 33 Chapter 3: ALIGNMENT OF ELECTROSPUN NANOFIBERS ................................. 36 3.1 Introduction ........................................................................................................... 36 v 3.2 Review on Electrospinning Designs and Nanofiber Assemblies .......................... 36 3.3 Design of Electrospinning Setup .......................................................................... 40 3.4 Effect of Collector Surface Velocity on Fiber Alignment .................................... 42 3.5 Chapter Conclusions ............................................................................................. 43 Chapter 4: INVESTIGATION OF ELECTRIC FIELD AND FLOW RATE ............... 44 4.1 Introduction ........................................................................................................... 44 4.2 Experimental ......................................................................................................... 45 4.2.1 Polyacrylonitrile (PAN)/DMF Solution Preparation ..................................... 45 4.2.2 Electrospinning Process ................................................................................. 45 4.2.3 Yarn Preparation ............................................................................................ 46 4.2.4 Taylor Cone Analysis ..................................................................................... 47 4.2.5 Fiber Current Measurement ........................................................................... 47 4.2.6 Diameter Distribution Characterization ......................................................... 51 4.2.7 Mechanical Testing ........................................................................................ 51 4.3 Results and Discussion ......................................................................................... 52 4.3.1 Investigation on Taylor cone Morphology ..................................................... 52 4.3.2 Upper and Lower Bounds of Flow Rate for Continuous Jet .......................... 55 4.3.3 Investigation on Fiber Current ....................................................................... 56 4.3.4 Diameter Distribution of Electrospun Nanofibers ......................................... 59 4.3.5 Effect of Electric Field and Flow Rate on Nanofiber Diameter ..................... 61 4.3.6 Mechanical Properties of Electrospun Nanofiber Yarns ................................ 62 4.3.6.1 Effect of Filament Diameter .................................................................... 62 4.3.6.2 Continuous Jet vs Discontinuous Jet ....................................................... 64 4.3.6.3 Effect of Flow Rate ................................................................................. 65 4.3.7 Modeling of the Nanofiber Diameter ............................................................. 67 4.4 Chapter Conclusions ............................................................................................. 69 Chapter 5: INVESTIGATOIN OF RELATIVE HUMIDITY (RH) AND TEMPERATURE ........................................................................................................... 70 5.1 Introduction ........................................................................................................... 70 5.2 Ternary Phase Diagram ........................................................................................ 72 5.3 Experimental ......................................................................................................... 76 5.3.1 Electrospinning Process ................................................................................. 76 5.3.2 Characterization Techniques .......................................................................... 77 vi 5.4 Results and Discussion ......................................................................................... 79 5.4.1 Construction of Ternary Phase Diagram for Water/DMF/PAN System ........ 80 5.4.2
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